materials science outlook 2005 - nims · part 1 prospects of materials science-history of materials...

Materials Science Outlook 2005

National Institute for Materials Science

Contents

Introduction • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • iii

PART 11 Prospects of Materials Science-History of Materials Science and Future Trends in Research • • • 3

PART 22 Policies of Materials Research in Japan, USA and EU • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 11

Chapter 1 Materials Research Policies of Japan, USA and EU • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 13

Chapter 2 Nanotechnology Research Policies of Japan, USA and EU • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 20

1. Research Policies of Japan, USA and EU • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 20

2. Societal Implications of Nanotechnology • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 28

PART 33 Public Research Institutes for Materials Research in Respective Countries • • • • • • • • • • • • • • • • • • • • • • • • • 33

Chapter 1 Public Research Institutes for Materials Research in Japan, USA and EU • • • • • • • • • • • • • • • • • • • 35

1. Japan • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 35

2. USA• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 40

3. Germany • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 47

4. France• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 51

5. Spain • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 53

Chapter 2 New Nanotechnology Research Institutes in Japan, USA and Europe • • • • • • • • • • • • • • • • • • • • • • • • 56

Chapter 3 Public Research Institutes in Russia Federation and Poland • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 64

1. Russian Federation • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 64

2. Poland• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 68

PART 44 Outlook of Materials Research • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 71

Chapter 1 Nanomaterials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 73

1. Nanotubes • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 73

2. Nanoparticles • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 77

3. Quantum Dots • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 79

4. Nanodevices • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 83

Chapter 2 Superconducting Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 87

1. Oxide Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 87

2. Metallic Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 91

Chapter 3 Magnetic Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 95

Chapter 4 Semiconductor Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 102

Chapter 5 Biomaterials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 106

1. Materials for Artificial Organ and Tissue Engineering• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 106

2. Bioelectronics • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 111

Chapter 6 Ecomaterials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 115

1. Environmental Function Materials (Photocatalytic and Environment Purification Materials) 115

2. System Element Type Ecomaterials - Supporting New Energies and Energy Conservation:

Materials for Hydrogen Energy and Fuel Cells • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 119

i

3. Ecomaterials of Lifecycle Design • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 123

Chapter 7 High Temperature Materials for Jet Engines and Gas Turbines • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 127

Chapter 8 Metals • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 131

1. Steel - Steel Technology for Strong, Safe Structures • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 131

Steel - Steel Technology for High-Efficiency Energy • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 133

Steel - Steel Technology for Hydrogen Utilization • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 135

Steel - Reliability of Steel Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 139

2. Nonferrous Alloys • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 142

3. Protective Coating for Severe Environments • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 148

Chapter 9 Ceramic Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 150

1. Non-oxides - Carbon • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 150

Non-oxides - Carbides, Nitrides, and Borides• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 153

2. Oxides - Alumina, Zirconia, and Magnesia• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 156

Oxides - 3d Transition Metal Oxides • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 160

Oxides - Niobate, Tantalate, and Rare Earth Oxide • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 163

3. Glass • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 166

Chapter 10 Composite Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 169

Chapter 11 Polymer Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 173

Chapter 12 Analysis and Assessment Technology • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 177

1. Nanoscale Measurement • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 177

2. Extreme Field Measurement• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 179

3. Electron Transport Modeling in Surface Analysis • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 181

4. Advancee Transmission Electron Microscope • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 183

5. Standardization of Assessment Methods • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 185

Chapter 13 High Magnetic-Field Generation Technology and Its Applications • • • • • • • • • • • • • • • • • • • • • • • • • • • 187

1. The Aim of Developing a High Magnetic Field NMR Facility• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 187

2. Development of High-Field Whole-Body MRI• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 189

3. Mass Spectrometry • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 191

Chapter 14 Nanosimulation Science • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 192

Chapter 15 Technologies New Materials Creation• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 197

1. Particle-Beam Technologies • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 197

2. Applied Technology of Vacuum Process • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 200

Chapter 16 Acquisition and Transmission of Materials Information Data and Information • • • • • • • • • • 202

1. Structural Materials Data Sheets • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 202

2. Materials Databases • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 204

Chapter 17 International Standard • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 206

1. Standard Materials • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 206

2. International Standardization Research, VAMAS• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 208

3. Standardization of Nanotechnology and Risk Management• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 210

Acknowledgements

ii

iii

Introduction

Teruo Kishi, President

Four years have passed since NIMS was established as an independent administrative institute. Dur-

ing the first five-year Mid-Term Program from fiscal 2001, we focused on efficient management and

creating a stimulating environment. Consequently, the number of papers, patent applications, and other

research achievements grew dramatically. Going forward, we intend not only to build on those achieve-

ments but also to improve the quality of materials science research at NIMS.

NIMS is Japan’s sole independent administrative institute specialized in materials science. From the

second Mid-Term Program from fiscal 2006, we will serve as the hub of all research related to materials

science in Japan, while also forging links with other countries and continuing our own research.

NIMS will centrally compile the latest data on domestic and international research on materials sci-

ence and make that data available globally. As part of such activities, we published a new book entitled

“Materials Science Outlook”, which identifies and analyzes trends in policies, measures, and research

related to materials science both within and outside Japan.

Materials Science Outlook is intended for policy makers, research institute managers, and materials

science researchers both domestic and overseas. The publication will provide readers with detailed

information to plan policies for their activities.

The 2005 edition is the first edition of Materials Science Outlook. It offers projections from Year

2004 based on past trends in the main fields of materials science research. NIMS also surveyed research

work, policies and organizations engaged in materials science of Japan, the United States, and European

countries.

As a public research organ, NIMS has long been involved in fundamental research and development.

Through Materials Science Outlook, NIMS looks forward to disseminating information about materials

science and promoting research in this fast-moving field both in Japan and abroad.

We look forward to your continued support for NIMS and Materials Science Outlook.

PART1

Prospects of Materials Science

History of Materials Science

and

Future Trends in Research

1. Classification and transition of materials

Materials can be classified by component: process,structure, property, and performance. They can also beclassified by dynamic, electronic, photonic, magnetic, andbiotic functions and by applications as is shown in Figure1. The most common method is first to classify materialsbroadly into organic and inorganic materials as shown inFigure 2, and then into metals, ceramics, semiconductors,polymers, and composites. Figure 3 shows another methodproposed by Allen et al., where materials are classified bynoncrystal phase, crystal phase, and liquid crystal phase.1)

This structure-based method attaches importance to struc-tural defects such as dislocations.

Figure 4 shows a forecast of the transition of materialspublished by Ashby in 1980.2) According to this forecast,metals will decline in relative importance after peaking at70 to 80% of all materials in about 1960, and the percent-ages of polymers, composites, ceramics, and glasses willincrease. It is interesting to note that the figure is horizon-tally symmetric. In other words, ceramics, composites, and

other materials will return to their original percentageseven as natural materials are replaced with artificial ones. Itis also interesting that nonmetallic materials reached aplateau around 2000, perhaps because ceramics and othercomposite materials, whose brittleness makes them unreli-able, failed to replace metals as structural materials. If theproblem of brittleness could be solved, the application ofnonmetallic materials may grow.

Figure 5 gives a history of materials, showing the devel-opment of metals, nanotechnology, semiconductors, poly-mers, and composites; the timings of emergence; the sup-porting techniques of measurement, analysis, and experi-mentation; the related theories and backgrounds; and actualproducts that have resulted. From the figure, we see that thesupporting techniques correspond well to the materials thatemerged, and that theories then appeared accordingly. Thehistory of each material reveals that measuring and analyti-cal techniques of metal started developing very early, fol-lowed in quick succession by their supporting techniques.Fine ceramics, which appeared after metals, show similartendencies to metals, having been supported by unique

3


Applications

Functions DynamicElectronicPhotonicMagneticBio

Public facilitiesAerospaceAutomobilesElectronics

Components ProcessStructurePropertyPerformance

MetalsCeramicsPolymers

(Semiconductors)(Composites)

Materials

Fig. 1 Components, functions, and application systems of materials.

Noncrystal phase: Statistical short-

distance regularity

Crystal phase: Parallel short-

distance regularity

Liquid crystal phase: Orientationregularity

Non-equilibrium process: Quick heating, quick cooling, large deformation, and mixing

Manufacture

Structure

Structural defect

Characteristics

Fig. 3 Materials classification by structure.1)

Inorganic materials

Metallic

Nonmetallic

Organic materials

MetalsIron, steel, aluminum, aluminum alloy, copper, copper alloy, titanium, and titanium alloy

CeramicsAlumina (Al2O3), silicon carbide (SiC), graphite (C), diamond (C), and silicon nitride (Si3N4)

SemiconductorsSilicon (Si), germanium (Ge), and gallium arsenide (GaAs)

PolymersPolyamide (PA), polycarbonate (PC), polyvinyl chloride (PVC), and polyethylene (PE)

CompositesGlass fiber reinforced plastics (GFRP) and carbon fiber reinforced plastics (CFRP)

Fig. 2 Classification of materials.

Reliability issues

Fig. 4 Transition of materials.2)

01 Prospects of Materials Science

– History of Materials Science and Future Trends in Research –

Teruo KishiPresident, NIMS

measuring techniques and theories, such as sintering andthermodynamics. More recently, many important polymershave appeared, as have semiconductor materials whichhave progressed rapidly through the linkage of importanttheories and analytical techniques. Regarding nanotechnol-ogy, it has been the newly developed scanning tunnelingmicroscope nanotechnology rather than the existing trans-mission electron microscope that has greatly benefitedmaterials development. For composites, nondestructiveinspection has been an important technique.

2. History of materials science

Table 1 shows the history of materials science, whichcan roughly be divided into three eras. In the era of Curios-ity Driven (until 1965), materials science was born fromcuriosity about metals, ceramics, polymers, and other mate-rials. In the era of Function Driven (until 1985), function-based structural materials and various other functionalmaterials entered practical use. And in the era of SystemDriven (until 2000), materials science increasingly foundits way into actual systems. The current era – Nanotechnol-ogy and Nanomaterials – merged from Curiosity Drivenand System Driven as shown in Fig. 6. New materials sci-ence is expected to emerge thanks to the nanoscale effect ofincreasing the surface area, and the quantum effect.

Figure 7 shows the relationship between materials inno-vation and business cycle.3) The business cycle is about 50to 60 years. Technical innovations brought by new materi-als have driven economic development as well as theIndustrial Revolution that produced the steam locomotiveand automobile. In future, materials innovations by nano-

materials are expected not only to solve problems related tothe environment and life science, but also to drive econom-ic development.

4


XPS, AES

MetalsNanotechnologySemiconductorsPolymersComposites

Emergedmaterials

Hemp Cotton Silk

Earthen ware Bronze Iron SteelCopper

Fiber reinforced plastics

Carbon nanotube

Si, GaAs HfO2

Vinyl chloride, nylon, conductive polymer

Aluminum Titanium Supersteel

Measurement, analysis,and experimentation

Reductive reaction

Refining Alloying

Discovery of tin

Natural rubber

Microscope

Refining Electrolysis

X-ray diffraction

Related theoriesand backgrounds

Quantum mechanicsSintering and thermodynamics Dispersion strengthening mechanism

Polymer chemistry

Alchemy Electrochemistry Reductive reaction Grain size refinement

Practical products

Hemp and cotton fabricsEarthenware Sun-dried bricks

Decorations Weapons

Chemical fibersFerroconcrete Transistors, IC, LSIVoltaic cells Duralumin Aircraft materials

10,000 B.C.

RBS

NMRTEMSEM

STM

LED

FRP

Fig. 5 Techniques and theories supporting the transition of materials.

Table 1 History of materials science.

Fig. 6 Future materials science.

Figure 8 shows two possible routes toward new materi-als science. On the one route, nanoscale not only reducesthe scale of handling but also yields new characteristics andfunctions. On the other route, organic and inorganic materi-als are handled uniformly in consideration of noncrystalphase, crystal phase, and liquid crystal phase. Nanomi-crostructures are created from non-equilibrium processesand new characteristics are discovered.

3. Future trends in materials research

In Materials Science Outlook, materials are broadlyclassified into the four types shown in Figure 9. First, thecharacteristic-seeds materials are: (1) Nanomaterials, (2)Superconducting materials, (3) Magnetic materials, and (4)Semiconductor materials. Second, the needs-oriented mate-rials are: (5) Biomaterials, (6) Ecomaterials, and (7) Hightemperature materials for jet engines and gas turbines.Third, the performance-seeking materials are: (8) Metals,(9) Ceramics, (10) Composite materials, and (11) Polymermaterials. And fourth, the fundamental research areas ofmaterials are: (12) Analysis and evaluation techniques, (13)High magnet field generation techniques and applications,(14) Nano-simulation science, (15) Technologies for creat-ing new materials, (16) Acquisition and transmission ofmaterials data, and (17) International standards. Researchtrends for these items were investigated and analyzed. Thischapter outlines future research trends and Chapter 4describes the research trends for each item.

3.1 NanomaterialsNanomaterials are now attracting great attention and are

widely used. Nanotubes, one of the most attractive groupsof nanomaterials, have to be synthesized with well-con-trolled methods to obtain semiconducting or metallic nan-otubes selectively. For the evaluation of the applicability ofnanotubes to future nanoelectronic devices, further funda-mental research is required to understand the functionalityof nanotubes. To create nanoparticles having a controlledsize with a precision of several to tens of nanometers andalso having controlled morphology which is usually relatedto the surface structure, we have to develop methods tocontrol or modify the surface structure of nanoparticles.Methods to arrange and integrate nanoparticles on a givensubstrate are also essential. It is important for the controlledsynthesis of nanoparticles to observe the process of synthe-sis in situ. Advanced colloid aerosol science and simulation

technology are also important. Since the quantum dot laserhas almost reached the stage of practical use, studies shouldbe made regarding its application to nanoelectronicdevices, quantum information processors, spin electronicdevices, and bio-molecular recognition devices. Since fur-ther development of semiconductor devices is limited,much emphasis should be placed on the development ofnovel nanoelectronic devices including single-electrondevices and atomic and molecular devices. Researchershave already been studying the practical application of acertain atomic device using nanoionic processes. Suchdevices will realize high-performance mobile terminals thatare indispensable to the ubiquitous information-orientedsociety in the future. These devices may also enable novelneural networks to be built.

3.2 Superconducting materialsSuperconducting materials can be classified into the

oxide type and the metallic type. Compared with metallicsuperconducting materials, oxide superconducting materi-als feature high critical temperature Tc and high upper crit-ical magnetic field Bc2. Unlike oxide superconductingmaterials, however, metallic ones offer excellent resistanceto stress and strain as well as ease of handling. As practicaloxide superconducting materials, bismuth oxides and yttri-um oxides are now being studied. Although the bismuth-type Bi2Sr2CaCu2Ox (Bi-2212) and Bi2Sr2Ca2Cu3Oy (Bi-2223) wires do not provide adequate characteristics forpractical use yet, they are thought to have good potentialand so ways of improving the characteristics are now beingstudied. Meanwhile, for the practical use of yttrium-oxidesuperconducting materials, it is necessary to develop a longwire production technology and to reduce manufacturingcosts.

5

Materials Science Outlook 2005B

usin

ess

IndustrialRevolution Mass Transit Start of Mass

Consumption SocietyHigh Economic Growth

and IT RevolutionSustained,

Safe Society

World War I World War II Life Science

Environment

Iron andsteel Polymers

Light alloysCeramics

SemiconductorsBonding materials Nanomaterials

Materials innovation as the prime mover of economic development

Fig. 7 Relationship between technical innovation and business cycle.3)

Noncrystal phase Crystal phase Liquid crystal phase

Atomic/Molecular Operations

Nanoscale Materials

Nanoscale Effects

Non-equilibrium Process

Nano/microstructures

New Characteristics

Fig. 8 Future materials development (Nanomaterials).

Characteristic-seeds materials

Performance-seeking materials R&D materials

Needs-oriented materials

(1) Nanomaterials(2) Superconducting materials(3) Magnetic materials(4) Semiconductor materials

(8) Metals(9) Ceramics(10) Composites(11) Polymers

(5) Biomaterials(6) Ecomaterials(7) High temperature materials for

jet engines and gas turbins

(12) Analytical and evaluation techniques(13) High field generation

techniques and applications(14) Nano-simulation science(15) New material creation techniques(16) Acquisition and launching of materials data(17) International standards

Fig. 9 Classification of materials in this publication.

For metallic superconducting materials, the characteris-tics of Nb3Sn and Nb3Al wires in a high magnetic fieldmust be improved. R&D is expected to lead to long andstable wires with low AC losses. MgB2 requires technicaldevelopment for improved characteristics, long wires, mul-tifilamentary wires, and stable composite wires. For bothmetallic and oxide superconducting materials, wires havinglow stimulated radioactivity must also be developed whenconsidering application to a fusion reactor.

For the development of high-performance superconduct-ing wires, the structure needs to be controlled at the nano-level. The important research themes for oxide supercon-ducting materials will be the preparation of nano-levelstarting materials and the modification of lamellar crystaland grain structures. Both for oxide and metallic supercon-ducting materials, the introduction of a nano-size artificialpinning centers dramatically increases the critical currentdensity Jc, so this should be further studied in future. Also,in the search for new superconducting materials, synthesesunder ultrahigh pressure, ultrahigh gas pressure and underother special environments, and application of soft chem-istry are interesting fields where progress is expected.

3.3 Magnetic materialsMagnetic materials are key industrial materials that are

widely used in the electric communication, electric powerand automobile industries. Since one automobile uses about25 to 30 motors, improvement of the performance of thepermanent magnets would lead to a substantial weightreduction. Hybrid cars or electric vehicles require perma-nent magnets that can be used at around 200˚C for theirmotors. To maintain coercivity at this temperature, currentmagnets use dysprosium; however, the natural resources ofdysprosium are limited and the stable supply of dysprosiummay face difficulty in the future. Therefore, a technologicalbreakthrough to achieve high coercivity without using dys-prosium is needed. In addition, the development of thin-film high-performance permanent magnets is required forfuture applications in MEMS and other small portable com-ponents.

Although no breakthrough has been made since theinvention of the nanocrystalline soft magnetic materials in1988, continuous efforts to optimize soft magnetic proper-ties for various specific applications are being made. Dueto the rapid increase of the size of data communication, thefrequency used in portable electro-communication devicesis reaching the GHz range. To solve the electromagneticinterference (EMI), soft magnetic materials that can beused for GHz-band communications will be particularlyimportant. Write heads for high-density magnetic recordingrequire materials of higher magnetic flux density than canbe achieved with Fe70Co30. To explore the superior proper-ties that cannot be achieved with the conventional material,searches for new intermetallic compounds with the help ofcomputational materials science will be necessary. In thefield of permanent magnetic materials, no compound offer-ing better intrinsic properties than those of Nd2Fe14B hasbeen found in the past 20 years. It will be impossible tofind new materials without the help of computational sci-ence. Magnetic recording technology is now shifting from

the longitudinal recording method to the perpendicularrecording method. In principle, perpendicular magneticrecording can attain a much higher recording density thanlongitudinal recording. To increase the areal density ofmagnetic recording to the range of 1 Tbit/in2, a materialwith high magnetocrystalline anisotropy must be adoptedas recording media to overcome thermal instability. How-ever, the coercivity of the media will then become too highto write using existing write heads. Therefore, soft/hardnanocomposite media and oblique recording media are nowbeing investigated as a possible alternative media for thefuture high-density recording. When the areal density ofthe current perpendicular magnetic recording methodreaches its highest limit, FePt and other high magnetocrys-talline materials must be employed as new media. To writeto particulate media composed of high anisotropy materialssuch as L10 FePt, the thermal assist recording method isproposed. A media structure that is appropriate for thismethod must be developed by that time, i.e., the two-dimensional array of nanoparticles, the suppression of coa-lescence of the particles during thermal treatment for L10ordering, and the c-axis orientation of particles.

As the areal density of recording media increases, thesensitivity of the read head must be increased. Current highdensity magnetic recording uses a giant magnetoresistance(GMR) head for reading, but higher sensitivity is requiredfor future higher density recording. The structure of theGMR heads such as spin-valves are becoming complicatedthree-dimensional nanostructures, thus detailed structuralcharacterization of GMR devices is required to understandthe structure–property relationships. Since elaborate 3Dnanostructure analysis is difficult to be executed in indus-trial laboratories, research collaboration among industryand academic institutions is becoming essential to obtain abetter understanding of the structure–property relationshipsthat is required for device designs in industry. For potentialapplications to magnetic random memory (MRAM) andtunneling magnetoresistance (TMR) heads, intensiveresearches are being performed in various industrial, gov-ernmental and academic laboratories. To achieve TMRdevices, fundamental research on spintoronics devices suchas half-metals is essential.

3.4 Semiconductor materialsTo date, Si-based electronic devices have been made

faster and more functional by integration using lithography.By modifying the materials and structures, this trend willcontinue until the gate node width reaches hp 22 nm nodegeneration (actual gate width: 10 nm). Therefore, high-dielectric gate insulating films, metal gates, and low inter-layer insulating films will be developed, probably aroundthe year 2015. In the next 10 years until then, Si devices aresure to account for more than 90% of semiconductordevices by using these techniques. For even faster process-ing, MOSFET using Ge or CNT channels, high-frequencytransistors using GaN, and Si-MOSFET may be packagedon a single chip to deliver multiple functions. Organicdevices now employed only for some display units couldbe applied to flexible and other unique devices. Meanwhile,compound semiconductors will separate into GaAs-based

6


materials for quantum dot and various other quantum effectdevices and GaN and related materials for light-emittingdevice, lighting apparatuses, THz high-frequency transis-tors, and other applications.

3.5 BiomaterialsRegarding artificial organ materials and genetic materi-

als for treatment, research should clarify the optimum con-ditions of spatial nanostructures with the manifestation lev-els of genes and proteins as indexes, for super-biocompati-ble materials to avoid foreign-body and immune reactions,materials to create an environment similar to the extracellu-lar matrix, and materials to induce cell differentiation andproliferation. To maximize cell functions, cell populationcontrol techniques are needed. Basic material design guide-lines and so forth to ensure safe and reliable nanobioticmaterials will also need to be created.

In the field of bioelectronics for diagnosis, high-sensitiv-ity biomolecular measurement using nanofabrication tech-niques and devices is attracting attention as a future trend.To meet the growing medical needs of the aging society,remote medical treatment will become increasingly impor-tant. Furthermore, to provide large amounts of useful infor-mation quickly, technical development is necessary for amicro chemical analysis system (µTAS) by semiconductornanofabrication, for a lab-on-a-chip, and for a remote med-ical examination system combined with IT.

3.6 EcomaterialsThe history of ecomaterials started in 1991 when the

term “environmentally conscious materials” was coined,meaning that the environment and resources should be con-sidered when developing every material. This has nowbecome a global issue. Ecomaterials are classified intofunctional ecomaterials that offer a purification functionand the chemical function of a catalyst or other substance;system-element ecomaterials necessary for creating an effi-cient clean energy system; and life-cycle ecomaterialswhich are friendly to the environment and can be recycled.

Regarding functional ecomaterials, the applications ofphotocatalysts are developing widely. It requires basicresearches indispensable to clarify the photocatalyst reac-tion mechanism and to improve activity, visibility, and sta-bility. The current task is to develop and implement a newvisible-light responsive photocatalyst. For the selective andefficient separation, decomposition, and elimination of haz-ardous chemicals, environmental purification materialswith sophisticated sensing functions need to be developedby using nanotechnology, self-organization, and templatereaction. However, various issues for these nanomaterialsremain, such as chemical stability in water, soil, and otherterrestrial environments and the desorption of adsorbedharmful chemical substances. Once these issues have beensolved, the benefits of environmental purification will helpcreate a safe and comfortable environment.

System-element ecomaterials are indispensable for anew energy system that adapts to the environment. Toenable the much-vaunted solid polymer fuel cells and tobring the hydrogen energy system into practical use at anearly stage, and for systematizing the uses of low-tempera-

ture heat sources, we must return to the basics of materialsand proceed with research on enhancing characteristics byprecise analysis and micro-structure control.

Life-cycle ecomaterials reduce environmental loadsthroughout the life cycle from mining of resources to dis-posal and recycling. One good example is lead-free solder,which is now becoming popular. To make an electronicpackage totally free of lead, solder alloys for any adequatetemperatures and their soldering techniques are needed.Bonding without using a solder alloy, such as conductivebonding, will become more widespread. In the near future,industry, government, and academia will need to standard-ize lead-free related techniques as a national strategy. Forrecycling, we should not only proceed with research forenhancing separation and refinement techniques but alsodevelop processing techniques that permit the existence ofartificial impurities or that utilize such impurities. To facili-tate recycling after use, a recyclable material design mayneed to be incorporated in advance.

3.7 High-temperature materials for jet engines and gas tur-bines

To solve global warming and other such problems byconserving fossil fuels and reducing CO2 emissions, higher-performance jet engines, natural gas combined-cycle gas turbines, and other advanced power systems arerequired and so high temperature materials will need to beimproved.

Among Ni-base superalloys which are typical high tem-perature materials, single-crystal alloys can withstand thehighest temperatures up to 1100˚C. Modern single-crystalalloys have evolved from the first generation to the secondgeneration containing about 3 wt% of rhenium (Re), and tothe third generation containing about 5 to 6 wt% of Re.Fourth-generation alloys with platinum-group metals addedand even fifth-generation Ni-base single-crystal superalloysare approaching reality for jet engines. Further work will becarried out to develop next generation single-crystal super-alloys.

Much work has been done on alloys based on Nb, Mo,W, and Ta as potential successors to Ni-base superalloys.However, they still do not have sufficient oxidation resis-tance, toughness, and high-temperature strength. Therefore,these alloys are now used only in vacuum, inert gas, orother protective atmosphere. Meanwhile, there are growingexpectations for superalloys that have high melting pointsand strong oxidation resistance, use high-melting pointplatinum-group metals for their bases, and have the sameγ/γ’ structure as Ni-base superalloys. In terms of price, spe-cific weight, and ductility, many issues remain to besolved. Base metals of γ solid solution mixed from Ni, Co,Ir, Rh, Pt, and other FCC metals will produce a series ofsuperalloys having a wide range of characteristics from Nibase to platinum group, and also offering high cost perfor-mance.

3.8 MetalsSince metal research is such a broad area, it is classified

into the fields of steel, nonferrous alloys, and thermalshield coating and thermal spraying.

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In the field of iron and steel, techniques for actual useneed to be developed. In East Asia, where temperature andhumidity are high and where earthquakes occur frequently,for example, steel materials must be resistant to corrosionand earthquakes. To ensure long-term safety, heat-resistantsteel requires research on the transition of nano-precipitateduring high-temperature use; on the high-temperature,long-term generation of nano-thick surface protection scaleand its peeling resistance, and also on the brittle fracturebehavior of a welded joint based on fracture mechanics.Regarding the development of hydrogen fuel cell vehicles,ways of increasing the storage pressure are now being stud-ied to achieve cruising distances equivalent to those ofgasoline-powered vehicles. Research on materials that arereliable in hydrogen environments will continue. To ensurethe reliability of materials, it is important to examine thereliability of structural materials by creating data sheets formaterials development.

In the field of nonferrous alloys, aluminum alloysrequire not only technical innovation of material propertiesand manufacturing processes but also technical develop-ment to maximize the performance of recycled aluminumalloys. Magnesium alloys will be widely applied to large-scale components of automobiles and other parts to reduceweight. R&D on nanostructural analysis and control for theoptimum dispersion of precipitates will also be sought todevelop new alloys that enable wrought products, liketwin-roll casting, to be produced at low cost. Titaniumalloys will be in high demand for engines of next-genera-tion aircraft and hard bio-tissue substitutes and other bioticapplications, and new alloys will need to be developed.Regarding porous alloys, we should study high-strengthlightweight materials having excellent shock absorbanceand damping capacity to enhance the collision safety ofvehicles, materials with new functions from in-cell sub-stances different from cell walls, and also hybrid materialsby making good use of cell structures. To extend uses andto increase the types of useful intermetallic compounds, weneed manufacturing techniques that reduce the cost yet canimprove ductility and toughness and can reduce manufac-turing cost. Meanwhile, there are estimated to be thousandsof types of intermetallic compounds whose properties andfunctions remain unknown or unused. Extensive fundamen-tal research based on new ideas is needed to use these com-pounds. For high melting point alloys, the advanced materi-al developments are required to make clear the strengthen-ing mechanism, oxidation resistance, corrosion resistance,manufacturability, and other conditions at low cost. Exten-sive researches are under way on shape memory alloys forgrowing applications, and a demand for such alloys isexpected to grow for sensors and actuators as multifunc-tional intelligent materials having high damping capacityand super-elasticity.

For thermal barrier coating, high heat resistance andlong service life are important. To withstand high heat flux,researchers have conventionally focused on designing topcoating materials and developing coating processes. Forlong service life, however, the first priority is on develop-ing a bond coating material where the under-coating oxidelayer (TGO) grows slowly, is stable, and suppresses struc-

tural changes of the base metal. Thermal spraying is a coat-ing process that can deposit a wide range of materials frommetals to plastics to large areas at high speed. Regardingthis process, the trend for coating by high-velocity andcolder particles will continue in order to refine the sprayedcoating. From materials having nanostructures, films fea-turing high abrasion resistance and adhesion could beobtained, and thermal spraying offers tremendous potentialin this field. This is an important technique with manyways of giving environmental resistance to material sur-faces. However, some basic phenomena behind coating for-mation still remain unclear and await further study.

3.9 Ceramic materialsAs a non-oxide ceramic material, carbon is widely used

for structural and electronic applications, and recently itsusage in bio- and environmental fields is also under study.Superconductivity in diamond and ferromagnetism inpyrolytic graphite and fullerene have been reported recent-ly as new phenomena. Thus, carbon is still attracting greatattention in many fields. Other representative non-oxidematerials in carbide, nitride, and boride are silicon carbide,silicon nitride, Sialon, boron nitride, boron carbide, andmetallic boride. These are widely used as engineeringceramics. Caused by recent discoveries of a new Sialonphosphor, MgB2 superconductor and boron nitride havingan electron emission characteristic, their optical and elec-tronic functions are also getting researchers’ attention.

Typical examples of oxide fine ceramics are alumina,zirconia, magnesia, and their composite oxides. Thesematerials have long been known but the main focus now isto design and control shapes and arrays or compositions ofintergranular and intragranular structures, grains, pores,etc., at sizes of 100 nm or smaller. This approach is becom-ing the mainstream of research. To optimize the combina-tions of functions, it is becoming crucial to research nanos-tructure-controlling techniques, experimental and theoreti-cal analyses of nanostructures, and the relationship betweenstructures and properties.

3d-transition-metal compounds show a great variety ofphysical and chemical properties, such as catalytic proper-ty, photocatalytic property, ferroelectricity, magnetism, andsuperconductivity, etc., and thus they are being widelystudied for applications in environmental, energy-related,information and communication, and electronic and opticalfields. These compounds will continue to be important andto be studied intensively. 4d and 5d compounds of niobiumand tantalum oxides are also being studied intensively dueto their ferroelectric functions. In particular, lithium nio-bate and lithium tantalate single crystals with stoichiomet-ric compositions are attracting great attention for their use-ful characteristics. Rare earth compounds are used as lightemitting materials for solid-state laser. In this field, translu-cent ceramics are being studied for application to laser hostsystems.

Glass materials are used for various purposes andrecently, higher performances are demanded to meet withusage in environmental, energy-related, and informationtechnology fields. One area where research is particularlyintensive is functional glasses called nanoglasses with

8


highly controlled structures and with new functions. Byusing various manufacturing processes, researchers areseeking highly sophisticated and functionalized glasses.

3.10 Composite materialsIn the field of composite materials, we may need tech-

niques for controlling overall performance, ranging fromthe conventional handling of materials by parameters suchas reinforcement, matrix, and interface, to the structuraldesign and control of each material itself and their inter-faces. For polymer and ceramic based composite materialsin particular, therefore, we need to study composite materi-als that offer much greater performance than the conven-tional characteristics by controlling the matrix and interfacenanostructures and using nano-order differences in themodulus of elasticity and the coefficient of thermal expan-sion. In future, new composite effects will be sought byusing nanomaterial techniques, and testing and measuringtechniques will be developed on the basis of recentprogress in general technologies. Meanwhile, the conven-tional techniques can no longer cope with the expansionand sophistication of applications of fiber reinforced poly-mers. In these fields, intensive research is expected to solveold and new issues such as processing, evaluation of char-acteristics, and reliability assurance. It is also necessary todevelop not only stand-alone applications of compositematerials but also hybrid applications in conjunction withother existing materials in order to maximize the character-istics and compensate for the disadvantages of compositematerials.

3.11 Polymer materialsPolymers are basic materials in industry, being widely

used for plastics, rubbers, adhesives, photoresists, separa-tion membranes, gels, and biomaterials. If fibers, styro-foam, and paper are included, polymers can be likened tothe varied complexity of industrial structures found today.

Like metals and ceramics, polymers are produced onlarge scales and have a major impact on oil and environ-mental problems. To reduce environmental loads, halogen-free fire retardants and water-soluble polymer coating com-pounds containing no volatile organic compounds (VOC)are being developed. Various research is now in progresson water treatment using polymer membranes, energy con-servation using lightweight polymer composite materials,fuel cell and other energy-related polymer films, and recy-clable carpets. The research has yielded noteworthy newtechniques, such as a non-phosgene polycarbonate processby using CO2, an auto-extinction epoxy resin, and a recy-clable coating system.

Polymers, which are also recognized as important ele-ments of nanotechnology, are indispensable materials inmedicine and biotechnology. Polymers are also importantfor solving environmental, safety, energy, and other relatedproblems in Japan today, and for supporting sustainablegrowth.

3.12 Analysis and evaluation techniquesMuch of the nano-scale-measurement techniques have

been developed as the target-oriented evaluation methods.

Therefore, they lack generality and cannot be applied to themeasurement of a wide variety of the materials. It is there-fore necessary to develop general and universal nano-scale-measurement instruments and techniques, particularly anano-measurement technique that can evaluate large-scaleintegrated circuits assembled with atomic-level precision.A super-parallel large-scale method for the multi-probemeasurement technique can go beyond the framework ofnano-scale-measurement, and provide a nanostructure fab-rication and measurement technique of large area withhigher accuracy and spatial resolution. In frontier fieldSTM measurement, new properties and functions are morelikely to appear at stronger magnetic field, so the competi-tion to develop strong magnetic fields may continue. Forthe development of sophisticated measurement techniques,methods for precision measurement and the creation offrontier field environments are essential. Since these fron-tier environments will be powerful tools to know the mech-anisms of functions and properties of nanostructures, thesetechniques may lead to the discovery of completely newphenomena of nanofunctions and quantum effects. In sur-face analysis, it will be important to develop two- andthree-dimensional analysis techniques with short measure-ment and calculation times to know the precise elementaldistributions and chemical state from the analysis of mea-sured spectra with metrological uncertainty and high spatialresolution. This analysis requires an accurate physicalquantity database describing interactions between electronsand materials in solids and also their modeling based on aprecise understanding of electron transportation phenome-na in solids. For transmission electron microscopes,research will be continued to improve the performance ofthe stability of the microscope, the coherent electron beamsand correction lens aberration. In-situ property measure-ment within the transmission electron microscope, includ-ing electric and magnetic characteristics as well as morpho-logical, structural, and compositions changes will assist theresearch for nanoproperties that depend on the structuresand compositions in nano-scale. For the standardization ofevaluation methods of nanomaterials, guidelines for accu-rate analysis should be developed, and the purpose of themeasurement should be clarified to ensure the reproducibil-ity and traceability of the analysis results. Standardizationof nano-scale measurements and their publication willbecome increasingly important.

3.13 High magnetic fields and their applicationsHigh-field magnets being developed for high-field NMR

include a driven-mode superconducting magnet (1.2 GHzclass) and hybrid magnet (1.5 GHz class). Although com-pared with a persistent-mode superconducting magnet, thefields of these magnets are much higher, the field stabilityis one order of magnitude lower. Therefore, equipment andtechniques should be developed to enable high-resolutionNMR even under these circumstances.

Another measurement technique using NMR is magneticresonance imaging (MRI). The technique has been used formedical purposes, such as detecting abnormal regions inorgans, but in future it is expected to be used for functionalmeasurement. Theoretically, the sensitivity of NMR

9


increases in proportion to the 3/2 power of the magneticfield. For functional measurement, therefore, high-fieldMRI is expected to be developed. Compared with the NMRspectrometer, whole-body MRI requires a space of about10 times larger in diameter. Research and development isnecessary to use not only NbTi wires but also brittle Nb3Snand Nb3Al wires which have higher critical fields underhigh electromagnetic force conditions.

Mass analysis has rapidly become important in biologi-cal science and nanotechnology. In mass analysis, the per-formance of the FT-ICR method will be improved remark-ably by using a high field of over 10 Tesla. Since the high-field TOF-MS method allows mass analysis and spec-troscopy simultaneously, the effects of a high field onstructures and reactivity of mass-selected protein moleculesand nanoclusters can be observed by spectroscopy. Thismethod will surely advance in the future.

3.14 Nano-simulation scienceA number of computational techniques have been devel-

oped depending on the size of the target material or thetime scale of phenomena, including first-principles calcula-tions at the electron level, the molecular mechanics methodwhich handles the collective motions of atoms and mole-cules, the finite element method and the statistical thermo-dynamics method for bulk materials, and the phase-fieldmethod for mezzo-scales. In particular, computational sci-ence is expected to play essential roles in the research ofnanobiomaterials, in which their innovative functions areintensively explored by atomic-scale design and control.This is because computational science will be able to pre-dict a function in a completely controlled environment byhigh-accuracy, high-resolution numerical analysis that isdifficult to achieve in experiments, so that the results canbe fed back to experiments. An advanced quantum simula-tion technique is required to clarify the correlationsbetween electron states, properties, and functions ofnanobiomaterials. There is an urgent need to develop andenhance super-large-scale calculations, multifunctionalanalysis (multiphysics), strong-correlation modeling, andmultiscale techniques.

3.15 Technologies for creating new materialsParticle beams and the vacuum process offer techniques

for creating new materials. In the particle beam technology,the fabrication of nanoparticles and nanostructures usingnon-equilibrium- and spatially controllable characteristicsof ion implantation will continue, to produce nanoparticlesand nanorods of metals, metal-oxides and other types. Toimprove the functionality of these nanomaterials, one- ortwo dimensional array structures of nanoparticles, insteadof randomly distributed ones, need to be developed.Hybridization of beam technology with micro-scale pro-cessing or laser irradiation will become more important.For nanostructure fabrication using electron beam-induceddeposition, it is necessary not only to develop technologyto precisely identify nanostructures created but also toimprove crystallinity and other characteristics of the nanos-tructures. In the vacuum-process technology, materials fornext-generation devices will expand from semiconductors

into nano-sized metals, which are difficult to handlebecause of gas adsorption, etc. Ultra-high vacuum process-es, which enable us to manipulate nanomaterials at atomicor molecular levels in an ultra-clean environment, will con-tinue to improve in performance.

3.16 Acquisition and transmission of materials data andinformation

To construct a structural materials database on creep, itis neccessary to acquire the long-term creep properties ofadvanced heat-resistant steels and alloys and also to studythe acquisition of creep data for Al alloys, Mg alloys, andother lightweight nonferrous materials which are in greatdemand for reducing automobile weight and thereforepower consumed. Fatigue studies are shifting toward theclarification of fractures in the ultrahigh-cycle fatigueregime of 107 cycles or more, especially internal fractures.In future, giga-cycle fatigue properties under average stressand the effects of plate thickness and notches on weldedjoints will be studied systematically. Future studies will tar-get the high-temperature fatigue properties of Ni-basedsuperalloys and other test conditions. Regarding corrosiondata, the corrosion properties of various materials includingpractical ones will be evaluated in an atmospheric corro-sion environment to compile basic data on the phenomenaof atmospheric corrosion. Space use materials strength datasheets will provide a collection of data on fatigue crackgrowth and fractured surfaces, as well as fatigue strength,for which there is strong demand. Such data sheets willalso consider the acquisition of fatigue data for otherengine materials such as copper alloys and for importantstructural materials. To provide universal and high-qualitybasic data about materials, data will be gathered underinternational cooperation and our knowledge of materialswill be extended through research on data mining.

3.17 International standardsFor the nano-area analysis of standard materials, sec-

ondary standards featuring field materials metrology andother practical standards will be established quickly.According to the Versailles Project on Advanced Materialsand Standards (VAMAS), many countries have incorporat-ed nanomaterials as national measures and have begun tocompete in international standardization. The VAMASinternational standardization activities will surely be ofgreat importance for countries and industries. The standard-ization of nanotechnology will progress dramatically in thenext few years. Japan should lead ISO and other interna-tional standardization activities to take the initiative in stan-dardizing nanotechnology.

References

1) S. M. Allen and E. L. Thomas, The Structure of Materials, JohnWiley & Sons Inc., (1999).

2) M. F. Ashby, Materials Selection in Mechanical Design, PergamonPress Ltd., (1992).

3) White Paper on Science and Technology 2002, Ministry ofEducation, Culture, Sports, Science and Technology, Japan [inJapanese].

10


PART2

Policies of Materials Research

in

Japan, USA and EU

• Materials Research Policies of Japan, USA and EU

• Nanotechnology Research Policies of Japan, USA and

EU

1. Materials research policies of Japan

Based on the comprehensive strategies planned by theCouncil for Science and Technology, the Second Scienceand Technology Basic Plan for five years from FY2001was agreed by the Cabinet in March 2001.1) To resolve theissues now confronting Japan and to develop goodprospects for the future, this Basic Plan defined Japan to be“a nation contributing to the world by creation and utiliza-tion of scientific knowledge” (creation of wisdom), “anation with international competitiveness and ability ofsustainable development” (vitality from wisdom), and “anation securing safety and quality of life” (sophisticatedsociety by wisdom).

The Science and Technology Basic Plan adopted the fol-lowing as important policies: Strategic Priority Setting inscience and technology (S&T), S&T System Reforms toCreate and Utilize Excellent Results, and Internationaliza-tion of S&T Activities.

The policies of Strategic Priority Setting in S&T were toevaluate S&T fields that contribute most to increasingintellectual assets, economic effects, and social effectsthrough creating knowledge; to put priority on the fields oflife sciences, information and telecommunications, envi-

ronmental sciences, and nanotechnology and materials; andto allocate research and development (R&D) resourceseffectively. In addition to the four fields, R&D is beingpromoted in the fields of energy, manufacturing technolo-gy, infrastructure, and frontier because the four fields arefundamentals for a nation and Japan should put priority onthem.

The policies of S&T System Reform to Create ExcellentAchievements were to innovate the R&D system first; tomaximize the capabilities of researchers by introducing theprinciple of competition widely, by doubling the funds forcompetition, by introducing indirect expenses, and by pro-moting the mobility of human resources; and to innovatethe evaluation system to ensure transparency, fairness, andappropriate sharing of resources.

The policies of Internationalization of S&T Activitieswere to expand voluntary international cooperation activi-ties; to strengthen the ability to distribute informationinternationally; and to internationalize the research envi-ronment in Japan.

Figure 1 shows the transition of Japan’s S&T budget (8fields) and Figure 2 shows the percentages by field.2) Thebudget in the field of nanotechnology and materialsaccounts for about 5% of the total S&T budget.

13


(100 million yen)

FY2001 FY2002 FY2003 FY2004 FY2005

Frontier Social infrastructure Manufacturing technology EnergyNaonotechnologies and nanomaterials Information and communications Life scienceEnvironment

Fig. 1 Transition of apportioned S&T budgets of 8 fields (except for university budgets).

FY20051,983 billion yen (18,031 million

dollars)

(billion yen)

451

188

242

18

633

97

149

206

Fig. 2 Percentages of FY2005 R&D budgets of 8fields in 2005 (except for university budgets).

Chapter 1. Materials Research Policies of Japan,USA and EU

Tomoaki Hyodo, Takahiro Fujita, Yoshio AbeInternational Affairs Office, NIMS

Regarding materials R&D, Japan decided to promote: 1)materials techniques to clarify and control material struc-tures and the shapes of atomic and molecular sizes as thebasis for information & communications and medicine andto control surfaces and interfaces, 2) energy/environment-related materials techniques with high added value to meetthe requirements for energy conservation, recycling, andresources saving, and 3) materials techniques for creatingsafe spaces to live securely.

In June 2002, the Ministry of Education, Culture, Sports,Science and Technology drew up policies to promote R&Don nanotechnology and materials. Concerning materialsS&T, the Ministry put priority on the exploitation of envi-ronmental conservation materials, energy-efficient materi-als, safe-space materials, and materials to produce evalua-tion, processing, and other basic functions, new functions,and high-level functions.

The Ministry of Agriculture, Forestry and Fisheries isperforming R&D to extend the uses of bio materials bydeveloping antithrombogenic materials from fibroin (a kindof silk protein) and materials for artificial bones and liga-ments by using bony ingredients from silk.

In order to innovate materials processes, the Ministry ofEconomy, Trade and Industry is promoting a project for thehigh-level evaluation of next-generation semiconductornanomaterials and R&D on synergetic ceramics and metal-lic glasses.

2. Materials research policies of the USA

Figure 3 shows the percentages of the FY2004 totalresearch expenses by U.S. department and Figure 4 showsthose of basic research expenses.3) The Department ofDefense (DOD) accounts for over 50% of the total expens-es, followed in order by the National Institute of Health(NIH), National Aeronautics and Space Administration(NASA), Department of Energy (DOE), and National Sci-ence Foundation (NSF). Regarding the basic researchexpenses, NSF, DOE, and NASA account for about 10%each if the 57% of NIH is excluded.

The DOE and NSF are mainly in charge of basicresearch related to materials. The R&D expenses of DOEfor science were about 3,200 million dollars in FY2004(Table 1) of which 559 million dollars was spent on materi-als research (Table 2 “Basic Energy Sciences: MaterialsSciences). Meanwhile, the NSF spent 251 million dollars ofthe basic research expenses on mathematical science (Table2 “Mathematical and Physical Sciences: MaterialsResearch”).

In the USA, the DOE and NSF wield great influenceover basic R&D related to materials. The DOE is a mainorgan of the Federal Government conducting basic researchin the field of physical science.4) On September 30, theDOE announced its strategic plan, which is revised everythree years. The DOE, which is in charge of domestic ener-gy supply and national safety, announced policies for thenext 20 to 25 years in the four fields of national defense,energy, science, and environment.

The overriding mission of the DOE is to assure the

national, economic, and energy safety for the United States.To achieve this mission, it promotes science and engineer-ing and ensures a clean environment for the nation’snuclear weapon facilities.

To achieve the mission, the DOE adopted a total ofseven long-term general goals in the four fields of nationaldefense, energy, science, and environment. The generalgoal in the field of science corresponds to the fifth goal ofthe entire project. The objectives are to supply a world-

14


Total R&Dexpenses

$126.3 billion(FY2004)

Basic R&Dexpenses

$26.5 billion(FY2004)

Fig. 3 Percentages of total R&Dexpenses by department.

Fig. 4 Percentages of basic R&Dexpenses by department.

DOD: Department of DefenseNIH: National Institute of HealthNASA: National Aeronautics and Space AdministrationDOE: Department of EnergyNSF: National Science FoundationUSDA: United States Department of Agriculture,Commerce:Department of CommerceEPA: Environmental Protection AgencyDOT: Department of TransportationDHS: Department of Homeland Security

Field

Total

Expenses($ million)

Energy supplyScienceFossil energyEnergy consevationAtomic energy defenseClean coal technologyRadioactive waste management

3823,229

547379

4,198– 98

758,712

Table 1 R&D expenses of DOE in FY2004.

Field of Science

Total

Expenses($ million)

Inc. Inc. Inc.

High energy physicsNuclear physicsFusion energy sciencesBasic energy sciences

materials scienceschemical sciences, geo sciences, energyconstruction

Advanced scientific computing res.Biological and environmental res.Small business, innovative res.

Table 2 FY2004 R&D expenses of DOE in science.

class scientific research capacity to enable the DOE toachieve its mission; to enhance knowledge in leading fieldsof physics, biology, medicine, environment, and computa-tional science; and provide global-class research facilitiesfor science projects by the nation.

To achieve these objectives, the DOE operates hugenational experimental facilities in order to make remark-able progress in the field of energy science, including highenergy physics, atomic physics, plasma science, materialsand chemical science, and biological and environmentalscience. In addition, the DOE gathers scientists, engineers,and technologists having unparalleled biological develop-ment skills to support the application of various energy-related sciences to medicine. The Department invests inlarge facilities necessary for basic research and the sciencecommunity itself for public benefit.

More specifically, the DOE has eight goals: 1) Advanc-ing high energy physics and nuclear physics, 2) Advancingthe theoretical and experimental understanding of plasmaand fusion science, 3) Advancing energy-related biologicaland environmental research, 4) Developing new diagnosticand therapeutic tools and technology for disease diagnosisand treatment, 5) Advancing nanoscale sciences builtaround foundations in materials, chemistry, engineering,geo science, and energy biosciences, 6) Significantlyadvancing scientific simulation and computation, 7) Pro-viding the Nation’s science community access to world-class research facilities that advance the physical sciencesand enable the study of complex, interdisciplinary sciencequestions, and 8) Providing or supporting the Nation’s sci-ence community access to world-class, scientific computa-tion and networking facilities.

The DOE strategic plan interim goals with specific lim-its of execution. Table 3 gives key intermediate objectivesin science. The key intermediate objectives related to thematerials research field are to complete the construction ofa spallation neutron source by the end of 2006, to put fivenanoscience research centers into operation by the end of2008, and to develop materials having a predictable charac-teristic for each atom by 2015.

As an independent agency of the U.S. Government, theNSF was established in 1950.5) The mission of the NSF isto promote basic research, education, and infrastructure atuniversities and research institutions. NSF has few researchorgans but mainly grants subsidies for research in all fieldsof science and engineering. NSF receives more than 35,000applications for grants every year and funds about 10,000of them.

The NSF’s vision is to strengthen the nation’s futurethrough discovery, learning, and innovation. By investingin People, Ideas, and Tools (PIT), the NSF strongly pro-motes science and engineering necessary for securing thesafety, property, and welfare of the nation.

The National Science Foundation Act established in1950 states in its preamble that the NSF’s missions are topromote the progress of science, to advance the health,prosperity, and welfare of the nation, and to secure thenational defense. The NSF Act states the following as itsduties:• Basic research for fundamental research and engineering

processes• Programs to strengthen the scientific and engineering

potential of research• Science and engineering education for all classes in all

fields of science and engineering• Basic information in science and engineering suitable

for developing national and international policiesThe NSF strategic plan (2003 to 2008) announced in

September 2003 defines the long-term strategic goals inscience and engineering by people, ideas, tools, and organi-zational excellence as follows:6)

• People Goal:A diverse, competitive, and globally-engaged U.S.workforce of scientists, engineers, technologists andwell-prepared citizens

• Ideas Goal:Discovery across the frontier of science and engineer-ing, connected to learning, innovation and service tosociety

• Tools Goal:

15


Timing Key Interim GoalEnd of 2006

End of 2006

By 2007End of 2008

End of 2008

End of 2009

By 2010

By 2013By 2015

By 2020

Developing a suite of specialized software tools for scientific simulations to utilize terascale computers, while handling trillions of bytes of data or terabytes (trillion-byte) and high-speed networks

Establishing new basic characteristics for nuclear matter of extremely high temperature and density by using the Relativistic Heavy Ion Collider (RHIC) at Brookhaven National Laboratory

Completing studies on several next-generation computer architecture to enable the development of a high-end supercomputer (1,000 times the performance available in 2003)

Advancing plasma science and computer modeling to obtain a comprehensive and fully validated plasma configuration simulation capability

Completing the construction of a spallation neutron source

Commencing operation of a large hadron accelerator (LHC), ATLAS, and CMS detector Commencing operation of five nanoscience research centers

Utilizing research into viewing the makeup of genes in living cells, tissues, and organisms by cliniciansUnderstanding nanoscale assemblies of materials results in the capability to create materials, atom by atom, having predictable properties

Starting experiments to determine which of the many unified theories of the fundamental forces could actually describe nature at the smallest scale

Table 3 Key intermediate objectives in the science division of DOE.

Broadly accessible, state-of-the-art S&E facilities,tools and other infrastructure that enable discovery,learning and innovation

• Organizational Excellence Goal:An agile, innovative organization that fulfills its mis-sion through leadership in state-of-the-art businesspractices

Figure 5 shows the budget requested by the NSF forFY2004 by strategic goal.6) The NSF classifies all researchprojects into four categories and invests most in Ideas, fol-lowed by Tools, People, and Organizational Excellence.

Table 4 classifies the budget requested by the NSF forFY2004 by accounts and strategic goals. Most of the bud-get is apportioned to research projects.

In the NSF strategic plan, the NSF selected the follow-ing research fields for priority investment:• Biocomplexity in the Environment (BE)• Human and Social Dynamics (HSD)• Information Technology Research (ITR)• Mathematical Sciences• Nanoscale Science and Engineering• Workforce for the 21st Century

To the above priority research fields, the following sixresearch fields were added for research activities acrossfields by the Federal Government:• Networking and Information Technology

Research & Development (NITRD)

• National Nanotechnology Initiative (NNI)• Climate Change Science• Homeland Security and Antiterrorism R&D• Molecular-level Understanding of Life Processes• Education Research

3. Materials research policies of the EU

In 1984, the European Union inaugurated the Frame-work Programme (FP) to integrate and strengthen individ-ual R&D activities by European countries. The currentSixth Framework Programme (FP6) will continue until2006, starting from the preparatory period of 2002.7) Thetotal budget of FP6 for the four years from 2003 to 2006 is17.5 billion euros, much greater than the 13.2 billion eurosof FP4 (1994 to 1998) and 15 billion euros of FP5 (1998 to2002). The research budgets of FP6 are separate from thegovernment-level ones of each nation.

The overriding aim of FP6 is to create a EuropeanResearch Area (ERA) through this program. The conceptof ERA is to integrate national research programs that hadbeen independent up to FP5 into one EU program and tocreate a joint market for research and technological innova-tion. As the economic unification of European countriesprogresses, the EU aims to build a foundation for R&Dthrough ERA. The construction of ERA is the central sub-

16


To promote the progress of science ; to advance the nationalhealth. prosperity & welfare ; to secure the national defense ; andfor other purposes

PEOPLE

MIS

SIO

NV

ISIO

NS

TR

AT

EG

ICG

OA

LS

INV

ES

TM

EN

TC

AT

EG

OR

IES

Enabling the Nation's future through discovery. learning and innovation

($1,153M)IDEAS

($2,696M)TOOLS

($1,341M)ORGANIZATIONAL

EXCELLENCE($291M)

• individuals• institutions• Collaborations

• Fundamental S&E• Centers Programs• Capability

Enhancement

• Large Facilities• Infrastructure and

Instrumentation• Polar Tools & Logistics• FFRDCs

• Human Capital• BusinessProcesses• Technologies and

Tools

Fig. 5 FY2004 requested budgets by strategic goals.

S T R AT E G I C G O A L S

P E O P L EAccount

388

765

0

0

0

1,153

I D E A S

2,557

139

0

0

0

2,696

T O O L S

1,120

19

202

0

0

1,341

E X C E L L .

O R G A N .

($ million)

42

15

0

226

9

291

Research and Related Activities

Education and Human Resources

Major Research Equipment

and Facilities Construction

Salaries & Expenses

Office of the Inspector General

Totala

aNumbers may not add to rounding.

Table 4 Ratios of FY 2004 budgets by accounts and strategic goals.

ject of the Lisbon Strategy (March 2000) to make the EU“the most competitive and dynamic knowledge-driveneconomy within 10 years.”

FP6 focuses on the fields of information technology,biotechnology, nanotechnology, aeronautics and space,food, energy, and ecosystems. Table 5 lists the researchfields of FP6.

FP6 specified seven fields as priority research fields andintroduced Integrated Projects (IP) and Networks of Excel-lence (NE) to promote research in those fields.

By mobilizing and integrating research resources scat-

tered across the EU, IP supports purpose-oriented researchto produce new knowledge. Under several basic andapplied themes, three or more countries from the EU andrelated countries (Norway, Switzerland, Liechtenstein, andIsrael) are conducting joint research for three to five years.

NE is a concept of networking resources and knowledgeof research across countries in order to boost achievements.The Joint Programme of Activities (JPA) will realize NEthrough information sharing, human resources exchange,and facilities sharing. With the participation of six or moreresearch institutions from three or more countries, a largenetwork of several hundred researchers will be formed. Theresearch periods range from five to seven years. The stan-dard research funds are 2 million euros/year for 100 partici-pants, 5 million euros/year for 500 participants, and 6 mil-lion euros/year for over 1,000 participants.

In the field of materials, Nanotechnologies andNanosciences, Knowledge-based Multifunctional Materi-als, and New Production Processes and Devices were

selected as priority themes. Table 6 lists the research sub-jects selected for FY2003.

The priority subjects for Nanotechnologies andNanosciences are: 1) Long-term interdisciplinary researchinto understanding phenomena, mastering processes anddeveloping research tools, 2) Nano-biotechnologies, 3)Nanometer-scale engineering techniques to create materialsand components, 4) Development of handling and controldevices and instruments, and 5) Applications in areas suchas health and medical systems, chemistry, energy, optics,food and the environment.

The priority subjects for Knowledge-based Multifunc-tional Materials are: 1) Development of fundamentalknowledge, 2) Technologies associated with the produc-tion, transformation and processing of knowledge-basedmultifunctional materials, and biomaterials, and 3) Engi-neering support for materials development.

The priority subjects for New Production Processes andDevices are: 1) Development of new processes and flexi-ble, intelligent manufacturing systems, 2) Systems researchand hazard control, 3) Optimizing the life-cycle of industri-al systems, products and services, and 4) Integration ofnanotechnologies, new materials, and new production tech-nologies for improved security and quality of life.

In April 2005, the European Committee announced theadoption of the Seventh Framework Programme FP7 from2007 to 2013 (total amount of subsidies: 67 billion euros,total amount including office and labor expenses: 72.7 bil-lion euros).8) This proposal will be finally settled afterapproval by the EU Council and the European Parliament.

FP7, subtitled “Building the Europe of Knowledge”,consists of four programs: 1) Cooperation (subsidy: 39.3billion euros), 2) Ideas (10.5 billion euros), People (6.3 bil-lion euros), and 4) Capacities (6.6 billion euros) and non-nuclear actions of the Joint Research Centre (1.6 billioneuros), and European Atomic Energy Community(EURATOM) (28 billion euros in 2007 to 2011).

Through research cooperation projects and networks forcoordinating the research programs of countries, the coop-eration program supports research activities in nine fields:1) Health, 2) Food, agriculture, and biotechnology, 3)Information and communication technologies, 4)Nanosciences, nanotechnologies, materials, and new pro-duction technologies, 5) Energy, 6) Environment, 7) Trans-port, 8) Socio-economic sciences and the humanities, and9) Security and space.

The goals of the cooperation program for nanosciences,nanotechnologies, materials, and new production technolo-gies are to improve the competitiveness of European indus-tries and to ensure its transformation from a resource-inten-sive to a knowledge-based industry by generating break-through knowledge for new applications at the crossroadsbetween different technologies and disciplines. InNanosciences and Nanotechnologies, the themes of activi-ties are the creation of new knowledge about interfaces andsize-dependent phenomena, the nanoscale control of mater-ial properties for new applications, the integration of tech-nologies at the nanoscale, nano-motors/nano-machines/nano-systems, impact on human safety, andhealth and the environment. In Knowledge-based Multi-

17


Thematic priorities• Life sciences, genomics and biotechnology for health• Information society technologies (IT)• Nanotechnologies and nanosciences, knowledge-based

multifunctional materials and new production processes and devices

• Aeronautics and space• Food quality and safety• Sustainable development, global change and ecosystems• Citizens and governance in a knowledge-based society

Specific activities covering a wider field of research• Supporting policies and anticipating scientific and

technological needs• Horizontal research activities involving SMEs• Specific measures in support of international co-operation

Structuring the European Research Area• Research and innovation• Human resources and mobility• Research infrastructures• Science and society

Strengthening the foundation of the European Research Area• Support for the coordination of activities• Support for the coherent development of research and

innovation policies in EuropeSpecific program nuclear energy

• Priority thematic areas of research• Controlled thermonuclear fusion• Radiation protection• Other activities in the field of nuclear technologies and

safetyNuclear Activities of the Joint Research Center

Table 5 Organization of FP6. 7)

functional Materials, the themes of activities are the gener-ation of new knowledge on high-performance materials fornew products and processes, knowledge-based materialshaving tailored properties, more reliable design and simula-tion, the integration of nano-molecular-macro levels in thechemical technology and materials processing industries;new nano/biotic/hybrid materials, including the design andcontrol of their processing. In New Production Processesand Devices, the themes of activities are the creation ofconditions and assets for knowledge-intensive productionincluding construction, development and validation of newparadigms responding to emerging industrial needs anddevelopment of generic production assets for adaptive, net-worked and knowledge-based production; development ofnew engineering concepts exploiting the convergence oftechnologies (such as nano, bio, information, and cognitivetechnologies and their engineering requirements) for thenext generation of high value-added products and servicesand adaptation to the changing needs. In Integration ofTechnologies for Industrial Applications, the themes ofactivities are the integration of new knowledge and tech-nologies on nano, materials and production in sectoral andcross sectoral applications such as: health, construction,

transport, energy, chemistry, the environment, textiles andclothing, pulp and paper, and mechanical engineering.

The Ideas program will improve the competitivestrength in Europe and strengthen the scientific foundationof Europe. The Human Resources program will strengthenactivities concerning career development and changes ofEuropean researchers. The Ability program will strengthenR&D skills to maximize the performance of the Europeanscientific community and to assist research and innovationacross Europe.

4. Conclusion

Research policies about materials were compared amongJapan, the USA, and the EU.1) By the Second Science and Technology Basic Plan forfive years from FY2001, Japan is apportioning R&Dresources to put priority on the fields of life science, infor-mation and communications, and nanotechnologies andmaterials, thus helping to strengthen its intellectual assets,economic effects, and social effects.2) In the United States, the Department of Energy (DOE)

18


Nanotechnologies and nanosciences• Long-term interdisciplinary research into understanding phenomena, mastering processes and developing research tools

- Expanding knowledge in size-dependent phenomena- Self-organisation and self-assembling

- Molecular and bio-molecular mechanisms and engines• Nano-biotechnologies

- Interfaces between biological and non biological systems• Nano-metre-scale engineering techniques to create materials and components

- Engineering techniques for nanotubes and related systems• Development of handling and control devices and instruments

- Handling and control instrumentation at the level of single atoms or molecules and/or <10 nm• Application in areas such as health and medical systems, chemistry, energy, optics, food and the environment

- Roadmaps for nanotechnology

Knowledge-based Multifunctional Materials• Development of fundamental knowledge

- Understanding materials phenomena• Technologies associated with the production, transformation and processing of knowledge-based multifunctional

materials, and biomaterials- Mastering chemistry and creating new processing pathways for multifunctional materials- Surface and interface science and engineering

• Engineering support for materials development- New materials by design- New knowledge-based higher performance materials for macro-scale applications

New Production Processes and Devices• Development of new processes and flexible, intelligent manufacturing systems

- New production technologies, based on nanotechnology and new materials- New and user-friendly production equipment and technologies, and their incorporation into the factory of the future- Creation of “knowledge communities” in production technologies- Support to the development of new knowledge based added value products and services in traditional less RTD

intensive industries - IP dedicated to SMEs• Systems research and hazard control

- Radical changes in the “basic materials” industry (excluding steel) for cleaner, safer and more eco-efficient production- Sustainable waste management and hazard reduction in production, storage and manufacturing

• Optimising the life-cycle of industrial systems, products and services- Optimisation of “production-use-consumption” interactions- Increasing the “user awareness”

• Integration of nanotechnologies, new materials, and new production technologies for improved security and quality of life- Systems, instruments and equipment for better diagnosis and/or surgery, including for remote operations- Tissue engineering, new biomimetic and bio-hybrid systems- New generation of sensors, actuators and systems for health, safety and security of people and environment

Table 6 Materials-related PF6 research subjects in FY2003.7)

and the National Science Foundation (NSF) are makinggreat contributions to basic R&D on materials. The Depart-ment of Energy defined its long-term strategic goals in thefield of science and engineering in a three-year strategicplan revised in September 2003 and the National ScienceFoundation stated its goals in a strategic plan from 2003 to2008 announced in September 2003 to promote basic R&Drelated to materials.3) The EU is planning the Framework Programme (FP) tointegrate and strengthen R&D activities across Europeancountries. The priority themes of research selected for theSixth Framework Programme (FP6) are Nanotechnologiesand Nanosciences, Knowledge-based MultifunctionalMaterials, and New Production Processes and Devices. TheSeventh Framework Programme (FP7) from 2007 to 2013,adopted by the EU in April 2005, will be finally settledafter being discussed and approved by the EU Council andthe European Parliament.

References

1) Web page of the Council for Science and Technoogyhttp://www8.cao.go.jp/cstp/

2) Meeting report for the Council for Science and Technology

(February 2005)http://www8.cao.go.jp/cstp/siryo/haihu43/siryo2-1.pdf

3) Web page of AAAS:http://www.aaas.org/spp/rd/

4) Web page of U.S. Department of Energyhttp://www.energy.gov/engine/content.do

5) Web page of National Science Foundationhttp://www.nsf.gov/

6) National Science Foundation Strategic PlanFY2003 - 2008 (September, 2003)http://www.cra.org/Activities/workshops/broadening.participation/nsf/FY2003-2008plan.pdf

7) Web page of European Union FP6http://fp6.cordis.lu/fp6/home.cfm

8) Web Page of European Union FP7http://www.cordis.lu/fp7http://europa.eu.int/comm/research/press/2005/pr0704-2en.cfm

19


In the FY2001 Budget Message dated January 21, thethen President Clinton positioned nanotechnologies as astrategic R&D field of the nation and the U.S. NationalNanotechnology Initiative (NNI) was inaugurated. Sincethen, nanotechnology R&D has been promoted undernational initiatives in Japan, the USA, Asia, and Europe.This section outlines the national strategies, policies, andbudgets of Germany, France, and the UK where researchinvestment in nanotechnologies is especially large.

1. Japan

As mentioned in the previous section, the field of nan-otechnologies and nanomaterials was selected as one of thefour priority fields in the Second Science and TechnologyBasic Plan.1) In addition, the Council for Science and Tech-nology Policy created the Priority Promotion Strategies byFields2) and clarified the current field statuses, priorityareas, and R&D goals and promotion measures. In the fieldof nanotechnologies and materials, the following five targetareas were determined and the goals and technical objec-tives were exemplified in each field.• Nanodevices and nanomaterials for the next-generation

information and communications systems• Materials for environment and energy-saving• Nanobiology for novel medical care technology and bio-

materials• Underlying technologies such as fabrications, analyses,

simulations, etc.• Novel materials with innovative functionsAs the basis of the R&D promotion policies, the followingitems were also selected:• Stimulating competition in R&D and its related areas• Promoting interdisiplinary research Collaboration• Constructing mechanisms leading to industries, and

sharing and linking the responsibilities and roles ofindustry, academia, and government,

• Securing and training human resourcesTable 1 shows the transition of national budgets for

R&D in the field of nanotechnologies and materials. Theactual budgets include additional budgets for nanotechnolo-

gy-related research technology categorized as other fieldssuch as life science and information.

Figure 1 shows national programs in the field of nan-otechnologies. Of the programs, the Nanotechnology Sup-port Project, the Knowledge Cluster Initiative, the Cooper-ation of Innovative Technology and Advanced Research incity areas, the 21 Century COE Program, and Nanotechnol-ogy Virtual Laboratories (NVL) are geared to promotinginterdisciplinary research and the collaboration amongindustry, academia, and government, characteristic to thepolicies in this field. These programs are outlined in section4(2) because they are also related to the creation of newresearch institutes. The section below outlines the govern-mental organization link project and the economy revitaliz-ing research and development project which are related toearly commercialization and industrialization.

1.1 Coordination Programs of R&D ProjectsTo study specific measures of promoting commercial-

ization and industrialization, the Council for Science andTechnology Policy set up a project team for promoting theresearch and development of nanotechnologies and materi-als in the Specialist Investigation Board for the PriorityField Promotion Strategy in December 2002.3) The industri-al exploitation strategy planned by the team pointed out thenecessity of the Coordination Programs of R&D Projectswhere governmental organizations can promote measurestogether, extending from R&D to improvement (safetyscreening standards, demonstration by model businesses,

20


FY2001

FY2002

FY2003

FY2004

FY2005

849

911

946

935

971

Table 1 Transition of national budgets for R&D in the fields ofnanotechnologies and materials (Unit: 100 million yen).

Chapter 2. Nanotechnology Research Policies ofJapan, USA and EU

Section 1. Research Policies of Japan, USA and EU

Masahiro TakemuraNanotechnology Researchers Network Center of Japan

standardization, government procurement to incubate mar-kets, and so forth). More specifically, strategies weredecided on nano-DDS, medical nanodevices, structuralmaterials, and nano-fabrication/measurement ( structuralmaterials are innovative ones in the field of materials).

1.2 R&D Projects for Economic RevitalizationIn the FY2003 budget request for science and technolo-

gy, the Council for Science and Technology Policy pro-posed the R&D Projects for Economic Revitalization toconstruct the next-generation industrial foundations that areexpected to become a reality reasonably soon, or in the dis-tant future. As Figure 1 shows, this proposal was actualizedby programs of governmental organizations.

2. USA

The NNI framework from FY2001-2003 consists of thefollowing five items:4)

• Long-term fundamental nanoscience and engineeringresearch

• Grand challenges – potential breakthrough –• Centers and networks of excellence• Research infrastructure• Ethical, legal, and societal implications, and workforce

education and training

Figure 2 shows the NNI system. Table 2 shows the tran-sition of R&D funds of each governmental organization.4), 5)

After the initiation of the NNI, the amount of funds quicklyincreased and reached 991 million dollars in total inFY2004. In addition to this, state and regional governmentsinvested about 50% of the amount invested by the NNI,and enterprises invested about the same amount as that bythe NNI. Table 3 summarizes the comments of Roco of theNational Science Foundation (NSF) concerning the NNI’sachievements in the first three years.4)

In addition, the 21st Century Nanotechnology Researchand Development Act6) was enacted with the signature ofthe president on December 3, 2003. This law materializesnational policies by the National Nanotechnology Program.The national policies are outlined next.

21


Com

mer

cial

and

indu

stria

l R&

DPe

rson

nel

traini

ngS

ecto

rlin

kage

Infr

astr

uctu

rede

velo

pmen

t

Nanomaterials Project: METI (NEDO)Virtual Laboratory in Nanotechnology Areas: MEXT (JST)Coordination Programs of R&D Projects

(Nano-DDS, medical nanodevices, structuralmaterials, and machining and measurement)

Economy Revitalizing Research and Development Project　　・Ultrahigh Function Research and Development: MIC　　・Focus 21 Project: METI　　・Incubator Advanced Medical Technology Promotion Research:

MHLW　　・Leading Project: MEXT

Nanomodeling Simulation: MEXTAdvanced Measurement and Analysis Technology and　Equipment Development Project: MEXT

Knowledge Cluster Initiative: MEXTCooperation of Innovative Technology　and Advanced Research in City AreasIndustrial Cluster Project: METI

21st Century COE Program: MEXT (JSPS)

Nanotechnology Business Creation Initiative (NBCI)

MEXT: Ministry of Education, Culture, Sports, Science and TechnologyMETI: Ministry of Economy, Trade and IndustryMIC: Ministry of Public Management, Home Affairs, Posts and TelecommunicationsMHLW: Ministry of Health, Labour and WelfareJST: Japan Science and Technology AgencyJSPS: Japan Society for the Promotion of ScienceNEDO: New Energy and Industrial Technology Development OrganizationNBCI: Nanotechnology Business Creation Initiative

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Fig. 1 Representative public programs of Japan in the field of nanotechnologies.

Fig. 2 Organization of U.S. National Nanotechnology Initiative (NNI).4)

• Developing a fundamental understanding of matter thatenables control and manipulation at the nanoscale.

• Providing grants to individual investigators and interdis-ciplinary teams of investigators.

• Establishing a network of advanced technology user

facilities and centers.• Establishing, on a merit-reviewed and competitive basis,

interdisciplinary nanotechnology research centers.• Ensuring the United States global leadership in the

development and application of nanotechnology• Advancing the United States productivity and industrial

22


Table 2 Transition of R&D funds by NNI4) Unit: million dollars.

Research Support for about 2,500 projects (universities and public institutions: 300, private companies: 200). Faster development than anticipated (very short lead time until prototyping)

Education Education of 7,000 students and teachers in 2003. Nanotechnology-related courses adopted by all universities of science and engineering. Education for young people.

Industry Same level of investment in mid-term and long-term R&D as NNI. Participation by large companies. Started up more than 1,000 companies. The USA holds more than 5,300 patents (two-thirds of world total) in 2003.

Economic effects Anticipated to reach one trillion dollars in 2015. Annual growth rate: 25% or more.

Federal-state linkage

Investment by more than 20 states. More than 22 local networks. (E.g. California Nanosystems Institute (CNSI))

Academic associations

Nanotechnology specialist subcommittees as major academic associations. Start of workshops and education.

Public investment Activities from the initiation of NNI (workshop held in 2000). Start of the NSF programs in 2000. Extension of activities and participation by legislative and judicial organs.

Social influence Activities from the initiation of NNI (workshop held in 2000). Start of the NSF programs in 2000. Extension of activities and participation by legislative and judicial organs.

Law The Nanotechnology R&D Act of 2003, the 21st Century of Nanotechnology R&D Act, and the 5-year National Nanotechnology Program

Creation of huge coalition

Creation of a nanotechnology community

Common infrastructure

Available to 60 or more universities. Establishment of 5 major networks (MCN, NNIN, OKN, DOE, and NASA). About 40,000 staff.

Field Achievements

Table 3 Main achievements by NNI in the first three years.4)

competitiveness through stable, consistent, and coordi-nated investments in long-term scientific and engineer-ing research in nanotechnology

• Accelerating the deployment and application of nan-otechnology research and development in the privatesector, including startup companies

• Encouraging interdisciplinary research, and ensuringthat processes for solicitation and evaluation of propos-als under the program encourage interdisciplinary pro-jects and collaboration

• Providing effective education and training for researchersand professionals skilled in the interdisciplinary per-spectives necessary for nanotechnology so that a trueinterdisciplinary research culture for nanoscale science,engineering, and technology can emerge

• Ensuring that ethical, legal, environmental, and otherappropriate social concerns, including the potential useof nanotechnology in enhancing human intelligence andin developing artificial intelligence which exceedshuman capacity, are considered during the developmentof nanotechnology

Besides, triennial evaluation of the national nanotechnolo-gy program by the National Research Council (NRC) of theNational Academy of Sciences

As part of the first triennial review, the NRC shall con-duct a one-time study to assess the need for standards,guidelines, or strategies for ensuring the responsible devel-opment of nanotechnology, including, but not limited to:• Self-replicating nanoscale machines or devices• The release of such machines in natural environments• Encryption• The development of national defensive technologies• The use of nanotechnology to the enhancement of

human intelligence• The use of nanotechnology in developing artificial

intelligenceThe greatest impact of legislation was that it recon-

firmed the R&D budgets and policies more than ever. Itseems appropriate that the national research plans for nan-otechnologies are the same as those of the NNI. They areexecuted through related governmental agencies or com-mittees and the National Nanotechnology CoordinationOffice (NNCO). In a strategic plan announced in December2004, the NNI set four goals.7)

• Goal 1: Maintain a world-class research and develop-ment program aimed at realizing the full potential ofnanotechnology

• Goal 2: Facilitate transfer of new technologies into prod-ucts for economic growth, jobs, and other public benefit

• Goal 3: Develop educational resources, a skilled workforce, and the supporting infrastructure and tools toadvance nanotechnology

• Goal 4: Support responsible development of nanotech-nologyRoco showed the vision for nanotechnology in the next

10 to 20 years, or timeline for beginning of industrial pro-totyping and commercialization:• First Generation (Until 2001): Passive nanostructures in

coatings, nanoparticles, and bulk materials (nanostruc-tured metals, polymers, ceramics)

• Second Generation (Until 2005): Active nanostructuressuch as semiconductor elements, drug targeting, andactuators

• Third Generation (Until 2010): 3D nanosystems withheterogeneous nanocomponents, complex networking,and new architectures

• Fourth Generation (Until 2020 (?)): Molecular with het-erogeneous molecules based on biomimetics and newdesigns

Besides, he suggested potential goals that may appear by2015: Nanoscale visualization and simulation up to threedimensions, 10 nm or smaller integrated CMOS, new cata-lysts for the chemical industry, no deaths from cancer, con-trol of nanoparticles in air, soil, or water, and othersRoco also emphasized that the concept of the NBIC:enhancing human performance by convergence of the fourtechnological fields of nano, bio, info, and cogno.8)

3. Europe

In May 2004, the European Commission (EC) announced“Towards a European Strategy for Nanotechnology”9) stat-ing the importance of nanotechnologies, the position of theEU in the world, and the following subjects for responsibleefforts:• R&D: Building the momentum – European public

investment in nanotechnology should increase by a fac-tor of 3 by 2010

• Infrastructure: European “Poles of Excellence”• Investing in human resources• Industrial innovation: Knowledge to technology• Integrating the Societal Dimension• Public health, safety, and environmental and consumer

protection• A further step: International cooperation

Figure 3 shows the governmental research funds ofEuropean countries in FY2003. The total amount of R&Dfunds in Europe is 1,150 million euros (about 15 billionyen). Of this amount, 350 million euros are from the ECand the remaining 800 million euros are from the govern-ments of the respective countries. In addition to thisamount, research funds are provided by the local govern-ments and the private sectors. It is interesting to note thatthe EC calculates the amount of research funds per citizenand sets a target amount for the future. According to the ECdata of 2003, Japan ranked first in the amount of researchfunds with 6.2 euros/citizen, the USA third with 3.6euros/citizen, and the EU (25 countries, including newmember countries) 12th with 2.4 euros/citizen. The reasonfor tripling the investment by 2010 is said to come fromthis data.

Research supported by the EC is now in progress in theSixth Framework Program (FP6). FP6 is a five-year pro-gram from 2002 until 2006. Hearings for the 7th Frame-work Program (FP7) from 2007 were started in the fall of2004.

23


4. Germany

In Germany, the Federal Ministry of Education andResearch (BMBF: Bundesministerium fur Bildung und

Forschung) is the center of nanotechnology R&D policies.The booklet “Nanotechnology Conquers Markets: GermanInnovation Initiative for Nanotechnology” issued by theMinistry in 2004 describes their strategies.10) Table 4 shows

24


Table 4 Transition of nanotechnology R&D funds by the German Government10) Unit: million euros.

400

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Asstria

Accedin

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Denmark

Spain

Greece

Portga

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Fig. 3 Nanotechnology R&D funds by the EC and European countries (200)9) Unit: million euros.

the transition of nanotechnology R&D funds by the FederalGovernment of Germany. In the period from 2003 to 2004,the research funds increased quickly from 8.82 to 123.80euros. As Table (b) shows, the main fields of investmentare nanomaterials, nano-optics, and nanoelectronics, whichtogether account for 84% of the total amount. Investmentsin nanomaterials include those in nanochemistry and Com-petence Centers for Nanotechnology (CCN). CCN is intro-duced in section 4(2). The funds total 293.10 million euros,including 24.5 million euros from the Federal Ministry ofEconomy and Labor (Bundesministerium fur Wirtschaftund Arbeit, BMWA) and 144.80 million euros to the groupof national institutes. The funding agency of the BMBF isthe German Association of Engineers (VDI: VereinDeutscher Ingenieure). According to Bachmann of VDI,the funding ratio of applied research to basic research isabout 5:3 (as of 2003).

In Germany, the regional governments also invest muchin the research and development of nanotechnologies,amounting to 50% of the funds by the federal government.To make the automotive, semiconductor, optical, and otherspecific local industries more competitive, a network ofresearch institutes of nanotechnologies is being construct-ed in each area. From the viewpoint of researchers, theyneed to collect 50% of research project funds from regionalgovernments and the private sector because only 50% isprovided by the BMBF.

5. France

“Programme Nanosciences – Nanotechnologies” announcedby the Ministry of Research (Ministère délégué à laRecherche) on December 16, 2004 states new efforts beingmade by France for nanosciences and nanotechnologies.11)

France announced a three-year subsidy (70 million euros ayear) for the Research Network in Nanosciences and Nan-otechnologies (R3N: Reseau National en Nanosciences eten Nanotechnologies) to be newly established (a total of210 million euros in the three-year period; 30 million eurosa year until that time). The main purpose is to support thefollowing three fields:• Plates-formes scientifiques et nanotechnologiques

(grandes centrals): Platform of nanosciences and nan-otechnologies (infra-network)

• Joint research project of basic nanoscience• R&D project by industry, academia, and the governmentR3N is also in charge of the social influences and interna-

tional relations of nanotechnologies. R3N is positioned aspart of the activities of the National Research Agency(ANR: Agence Nationale de la Recherche). (The budget ofANR is 350.00 million euros.)

Regarding the platform of nanosciences and nanotech-nologies, a new base is added to the conventional facilitynetwork consisting of five public research bases. In France,the allocations of research fields have long been clearlyseparated. Research mainly on basic nanosciences has beenassigned to universities and the National Science ResearchCenter (CNRS: Central National de la Recherche Scien-tifique), while mainly applied research has been assigned tothe National Micro and Nano Technology Network(RMNT: Reseau National de Micro-Nano Technologies)participated in by 740 industrial, academic, and govern-ment organizations. The main purpose of R3N also reflectsthis characteristic. The main research bases are introducedindividually in section 4(2).

Some examples of the funding of nanosciences and nan-otechnologies are introduced here. Regarding nanosciencesin 2003, 10 million euros were invested in research projectsinvited from the public by the Ministry of Research and 2million euros in education and training, researcher exchange,information support (Internet), and international pro-grams.12) Table 5 shows the adoption status of submittedresearch projects. Of 166 submitted subjects, 54 wereadopted and carried out at 100 laboratories (163 groups).

Regarding nanotechnologies, the RMNT (established inFebruary 1999), consisting of 740 organizations in theperiod from 1999 to 2004, adopted 59 R&D projects from146 applications. Investment amounts were 50.00 millioneuros from public funds and 150.00 million euros from pri-vate funds, and manpower spent was 1,069 person-years.13)

The public funds came from the Ministry of Research, theMinistry of Industry, the Ministry of Defense, and theNational Corporation of Research and Development

25


Table 5 Adoption of nanoscience projects in France (2003).12)

Fig. 4 Percentages of France RMNT projects by field.11)

(ANVAR) to support small and medium-sized companies.Figure 4 shows the percentages of projects by field.11)

About 50% of the projects were related to electronics.

6. UK

The nanotechnology R&D policies of the UK are largelyinfluenced by a report “New Dimension for Manufacturing:A UK Strategy for Nanotechnology”14) announced in June2002, by the Department of Trade and Industry (DTI) andthe Office of Science and Technology (OST) of the DTI.This report was issued by the Advisory Committee Con-cerning Application of Nanotechnologies headed by JohnTaylor, the chairman of the Research Council (RC) andconsisting of 12 members. The report lists the following sixpriority fields and also presents specific successes to bereached in each priority field in five years as “Success in2006”.

ELECTRONICS AND COMMUNICATIONS• The UK’s share of products in information and commu-

nications technologies begins to increase• Industrial R&D in this sector increased 10 fold, along

with a similar increase in patent filing• Annual spending by the Research Councils reaches £80

million: each year 150 PhDs, accompanied by 300 tech-nicians, graduate from training programmes

DRUG DELIVERY• Double or treble the number of postgraduates work in

drug delivery• 10 start-up businesses every year• The first start-ups would approach profitabilityINSTRUMENTATION, TOOLING AND METROLOGY• A national nanotechnology centre will generate SME

start-ups and provide prototyping and small-run manu-facturing for 50 new customers a year

• More than five UK companies will use directed self-assembly based on ‘disruptive’ methods compared toone today

NOVEL MATERIALS• Seven new products commercialised• Three product demonstrators at proof-of-conceptSENSORS AND ACTUATORS• 10 per cent a year growth in the number of UK gradu-

ates in nanotechnology• 100 per cent increase in funding for technology demon-

strators• One field trial of an integrated network of healthcare

sensors in a hospital• R&D, measured by such numbers as publications, cita-

tions and patents, to increase by 50 per cent• The UK’s share of nanotechnology-based sensor sys-

tems grows 10 per cent faster than our main competitorsTISSUE ENGINEERING• Five to 10 start-up businesses every year• 10 additional multidisciplinary groups every year• 2 per cent of a $50 billion market, worth $1 billion to the

UK• 85 to 90 per cent of UK tissue engineering companies

run by UK managers• New employment of 1500 jobs• Eight new products commercialised

This report also recommended the following:• National nanotechnology application strategy and Nan-

otechnology Application Strategy Board (NASB)• National Nanotechnology Fabrication Centers (NNFCs)• Roadmaps – technology and applications• Awareness, access portals and networking• Training and education• International – promotion and inward transfer

Figure 5 shows the nanotechnology R&D system of theUK Government.15) The Department of Trade and Industry(DTI) is in charge of industrialization. In the field of basicsciences, the Engineering and Physical Sciences ResearchCouncil (EPSRC), the Biotechnology and Biological Sci-ences Research Council (BBSRC), and the MedicalResearch Council (MRC) from the seven research councilsof the UK are in charge. Regarding the infrastructures(buildings and large-scale facilities) of universities andother institutes of higher education, the Higher EducationFunding Council for England (HEFCE) of the Departmentis in charge.

In July 2003, the DTI made a public commitment toinvest a total of 90 million pounds on the Micro and Nan-otechnology Manufacturing Initiative for six years.16) Ofthe amount, 50 million pounds will be appropriated for col-laborative R&D. In other words, the government willshoulder 25 to 75% of the expenses to reduce risks of R&Din specific fields. In the first invitation which ended in July2004, the DDI adopted 25 projects and decided to invest atotal of 15 million pounds in them. In addition, 40 millionpounds will be appropriated for Capital Projects for the

26


Fig. 5 Nanotechnology R&D system of the UK Government.15)

Micro and Nanotechnology Network (MNT Network).Under the MNT Network, regional centers are cooperatingto make facility operations efficient. In the Capital Projects,the appropriation of over 25 million pounds for the follow-ing research areas was already determined by the first andsecond general invitations (11 projects selected):• Manufacture and integration of micro and nano devices• Nano particles and novel materials• Bionanotechnology• Characterization and metrologyOn February 25, 2005, the third round of invitations wasstarted. The target research areas are:• Bionanotechnology• Microfluidic application centers• Carbon based electronics

Among RC research, nanotechnologies by EPSRC arebeing heavily invested in. The annual amount rose from 10million to about 13 million pounds from 1996 to 2000 butstarted increasing quickly in 2001, reaching about 36 mil-lion pounds (more if related fields are included) in 2003.17)

Figure 6 shows the percentages of investment by fields.Among research supported by RCs, the most noteworthyones are Interdisciplinary Research Collaborations (IRCs)by researchers of different fields, such as physics, electrici-ty, and chemistry. IRCs are introduced in section 4(2).

The Science Research Investment Fund (SRIF) byHEFCE is now at the third stage. Including fields otherthan nanotechnologies, a total of one billion pounds will beinvested in the two years from 2006.

References

1) The Council for Science and Technology: The Second Science andTechnology Basic Plan (March 2001).

2) Specialist Investigation Board for Priority Field PromotionStrategy, the Council for Science and Technology: PriorityPromotion Strategies by Fields (Draft) (September 2001).

3) The Council for Science and Technology: Promotion of IndustrialExploitation in the Nanotechnology Field – Promotion by thegovernmental organization linkage project – (July 2003).

4) Roco M.C., The National Nanotechnology Initiative: Plans for theNext Five Years. National Nanotechnology Initiative: From Visionto Commercialization. April 2004.

5) Tetsuharu Sato (2004), Information on FY2005 Budget Request forNanotechnologies in the U.S. Japan Nanonet Bulletin 61.Nanotechnology Researchers Network Center of Japan.http://www.nanonet.go.jp/japanese/mailmag/2004/061c.html

6) Congress of the U.S.A. 189, 21st Century NanotechnologyResearch and Development Act.

7) Nanoscale Science, Engineering and Technology Committee(NSET), The National Nanotechnology Initiative Strategic Plan.December 2004.

8) Roco M.C., Converging Technologies and Their SocietalImplications. International Symposium on EnvironmentalNanotechnology 2004. EPA & MEA, ROC. December 2004: 1-10.

9) European Commission (EC), Towards a European Strategy forNanotechnology. Communication from the Commission COM(2004) 338. May 2004.

10) Bundesministerium fur Bildung und Forschung (BMBF),Nanotechnology Conquers Market: German Innovation Initiativefor Nanotechnology. 2004.

11) Ministère délégué à la Recherche, Programme Nanosciences –Nanotechnologies. December 2004.

12) Marzin J., Nanoscience-Nanotechnology Program. October 2004(slides).

13) Roussille R., The French Research Network in Micro and NanoTechnologies (RMNT). October 2004 (slides).

14) Department of Trade and Industry (DTI), New Dimensions forManufacturing: A UK Strategy for Nanotechnology. June 2004.

15) Ryan J., Panel Discussion: International comparison of strategies,7th International Conference on Nanostructured Materials. June2004 (slides).

16) Micro and Nanotechnology Manufacturing Initiative, http://mntnetwork.com/

17) Engineering and Physical Sciences Research Council (EPSRC),Nanotechnology, September 2004.

27


Fig. 6 Percentages of UK EPSRC invested R&D funds by field.17)

Innovative technologies exert various impacts on societythrough industries. However, they may not only bring ben-efits but also unpredicted effects or even risks. This is alsotrue for nanotechnologies. So far, no apparent risks havebeen pointed out but there have been a considerable num-ber of concerns and warnings. In 1986, for example,Drexler portrayed a continuously self-reproducing robot ina book titled “Engines of Creation”1) predicting the emer-gence of nanotechnologies and named the multiplingnanoparticles Grey Goo. In a book titled “The Big Down:Atomtech - Technologies Converging at the Nano-scale”,2)

a Canadian NGO “ETC Group” proposed that the Govern-ment should call an immediate halt (a moratorium) to theindustrial production of nanomaterials and create a trans-parent international evaluation system. In the world of nov-els, Michael Crichton’s near-future SF “Prey”3) depictingswarms of nanobots self-assembling and attacking humansbecame a best-seller in the United States. In Europe andAmerica, many people involved in nanotechnology policiesthink it essential to make best possible predictions withoutignoring these concerns and to continue assessment andmanagement for maximizing benefits and minimizing risks.

1. Activities of the USA

Regarding the impacts of nanotechnologies on health,safety, environment, ethics, and society, the United Statesselected societal, ethical, and legislative issues as importantsubjects at the start of the NNI in 2000 as mentionedbefore. More specifically, the most important subjectsregarding the impacts of nanomaterials on health, safety,and the environment. On the whole, however, these are rel-atively short-term issues. From a long-term point of view,problems such as self- replicating, national defensive tech-nologies and the enhancement of human performance areraised, and were discussed in the first triennial review ofthe national nanotechnology program.4)

As one of the reasons for U.S. activities on the societalimplications, the case of Genetically Modified Organisms(GMO) is often introduced by people involved in nan-otechnology in the United States.5), 6) Genetically ModifiedOrganisms have caused great distrust because supplierscould not present adequate experimental data refuting thepotential risks that had been pointed out. In the UnitedStates data was then accumulated, and risks unique to

Genetically Modified Organisms were finally judged to benonexistent. As many people know, however, there is stilllittle public acceptance of Genetically Modified Organismsin Japan and Europe, and they hope there is no similarbacklash against nanotechnologies.

The first important activity by the United States was aworkshop called “Societal Implications of Nanoscience andNanotechnology”.7) This workshop was held in September2000, almost at the same as the start of NNI. From indus-try, government, and academia, natural scientists, socialscientists, and policy-makers gathered and held discus-sions. and it was followed by various programs. Undergeneral coordination by the NNCO, each department oragency is conducting programs on the safety of the prod-ucts and technologies they are in charge of.8)-12)

• Working environment: Occupational Safety & HealthAdministration (OSHA) and National Institute of Occu-pational Safety & Health (NIOSH)

• Pharmaceuticals: Food & Drug Agency (FDA)• Foods: FDA and Department of Agriculture (USDA)• Consumer goods: Consumer Product Safety Commis-

sion (CPSC)• Environment: Environmental Protection Agency (EPA)• Standardization and measurement: National Institute of

Standard & Technology (NIST)The NSF, Department of Energy (DOE), and Depart-

ment of Defense (DOD) are supporting research centers.Examples of ministry and agency linkage programs are theNational Toxicology Program (NTP) and the InteragencyWorking Group on Nanotechnology Environmental &Health Implications (NEHI). NTP is mainly organized fromthe National Institute of Health (NIH), the National Insti-tute of Environmental Health Sciences (NIEHS), theNational Center for Toxicological Research (NCTR) ofFDA, and NIOSH. This program will evaluate carbon nan-otubes, quantum dots, titanium dioxide, and fullerene.NEHI is mainly organized from the EPA, FDA, CPSC,OSHA, NIOS and USDA, and the program will evaluatewhether it is appropriate to keep or extend existing regula-tions on the industrialization of nanotechnologies. In 2004,NNI invested a total of 130 million dollars: over 20 milliondollars each on the environment and on society and educa-tion, and over 80 million dollars on health. (Both applica-tions and implications are included for the environment andhealth.)

The last examples in the United States are the American

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02 Nanotechnology Research Policies of Japan, USA and EU

Section 2. Societal Implications of Nanotechnology


National Standard Institute (ANSI)-Nanotechnology Stan-dard Panel (NSP), inaugurated in September 2004,13) andthe International Council on Nanotechnology (ICON).14)

ICON was inaugurated in October 2004 at the initiative ofthe Center for Biological and Environmental Nanotechnol-ogy (CBEN) of Rice University supported by NSF, and itincludes NGOs as members as well as industry and acade-mia.

2. Activities of Europe

The following three programs of the EU are related toenvironmental, health and safety (EHS) issues of nanotech-nology:15)

• NANO-PATHOLOGY Project: Developing diagnosticsmethods and equipment, clarifying pathological mecha-nisms, and verifying pathological importance. For threeyears from December 1, 2001 with a fund of about onemillion euros. Headed by the Italian Institute for thePhysics of Matter.

• NANODERM Project: Studying the influences of nano-materials on the skin. For three years from January 1,2003 with a fund of about 1.10 million euros. Headed bythe University of Leipzig.

• NANOSAFE Project: Assessing risks of nanomaterialsfrom production processes to consumers. For 15 monthsfrom April 1, 2003 with a fund of about 0.3 millioneuros. Headed by NANOGATE Technologies GmbH.

The first stage of NANOSAFE was completed in June2004 and the second stage is now being prepared. The firststage is introduced here.16), 17) This project will perform thefollowing activities related to nanoparticles:

• Assemble available information on the possible hazards• Evaluate risks to workers, consumers and the environ-

ment• Assess mechanisms of risks to human health• Formulate codes of good practice to obviate danger as

far as possible• Recommend guidelines for regulatory measuresFor the activities, six working groups were formed: For theactivities, six working groups were formed: WG1 (particlesize and shape, manufacturing and handling procedures),WG2 (applications, industrial and consumer), WG3 (poten-tial particle release, circumstances and conditions), WG4(danger to health, reaction mechanism with human organ-ism), WG5 (recommended preventive measures), and WG6(standards and regulatory recommendations). Regardingnanoparticles, the working groups discussed the expectedperformance of measuring equipment, risk evaluationitems, safety measures for workers, risk evaluation flow-charts, influences on the human body, and regulatoryframeworks and methods. Regarding influences on thehuman body, they concluded that the materials may beabsorbed through lungs or intestines but hardly permeatethrough the skin, that regions of distribution in the bodydepend on the surface properties of nanoparticles, and thatthere are no universal nanoparticles or materials that mustbe evaluated individually. The achievements in this project

are also summarized in “Industrial Application of Nanoma-terials – Chances and Risks, Technology Analysis” (August2004)18) edited by the German Engineers Association (VDI:Verein Deutscher Ingenieure).

In addition to the above programs, other investigationand workshop activities by the EU are summarized in somereports, such as: “The 4th Nanoforum Report: Benefits,Risks, Ethical, Legal and Social Aspects of Nanotechnolo-gy” (June 2004)19) and “Nanotechnologies: A PreliminaryRisk Analysis on the Basis of a Workshop Organized inBrussels on 1–2 March 2004” (March 2004).20) The formeris a summary of European discussions at Nanoforum (Nan-otechnology network of the EU) as of June 2004. The latteris a report on a workshop sponsored by the EC and summa-rizes the discussions and proposals by 17 specialists.

As well as R&D activities, the European countries areexamining social influences. A British report “Nanoscienceand Nanotechnologies: Opportunities and Uncertainties”(July 2004)21) created a sensation both within and outsidethe country. Commissioned by the UK Government, TheRoyal Society & Royal Academy of Engineering compiledthis investigation report. Through several workshops, opin-ions were collected from a total of 221 specialists and 151institutions such as universities and companies, and aware-ness surveys were conducted on the general public. In con-clusion, the report suggested 21 recommendations22) 23)

regarding industrial uses of nanotechnologies, the possibili-ties of adverse effects on health, restriction problems,social and ethical problems, stakeholder and dialogue withcitizens, and responsible R&D.

According to the report, the current industrial uses ofnanotechnologies are still on the stage of improving exist-ing products and the influences on health and the environ-ment are inhalation by workers during the process of manu-facturing nanoparticles and nanotubes. Meanwhile, the rec-ommendations propose a risk assessment by a third party,funding by a research council, handling as harmful sub-stances when there is not enough risk information, riskassessment throughout the lifecycle, information disclo-sure, and handling as a restricted new chemical substance.

In the awareness surveys on the general public, 29%replied that they had heard of nanotechnologies and 19%replied that they had talked about the definition of nan-otechnologies in some way. Of these respondents, 68% feltthat nanotechnologies will enrich their lives in future and4% felt that their lives will be made worse. Meanwhile, therecommendations propose open forums about nanotech-nologies and comprehensive and quantitative social scienceresearch.

3. International cooperation and its points

International cooperation is indispensable for takingactions on the societal implications of nanotechnologiesand there is now much international discussion. The mainrecent international conferences and their contents are out-lined below.

i) International Dialogue on Responsible Research andDevelopment of Nanotechnology (Alexandria, Virginia

29


State, USA from June 16 to 18, 2004)Convened by Roco of the NSF, technical policy-makers

gathered from 25 countries, including the representativesof EC. The attendants presented the nanotechnology poli-cies of their countries and held workshops on four topics:a) Environment, b) Health and safety, c) Society, economy,and ethics, and d) Nanotechnologies in developing coun-tries. They also discussed an international framework.9)

ii) The 7th International Conference on NanostructuredMaterials (NANO 2004 in Wiesbaden, Germany from June20 to 24, 2004)

Under the subject of “Chances and Risks of Nanotech-nology,” a panel discussion and lectures were held.24) Thepanel discussion was attended by Roco, Tomellini, andother representatives from the United States and Europeand also from Green Peace as panelists.25) A report meetingon the EU program NANOSAFE was held concurrently.iii) First International Symposium on Occupational Health

Implications of Nanomaterials (October 12 to 14, 2004 inBuxton, Derbyshire, UK)

This symposium was jointly sponsored by the U.K.Health & Safety Laboratory (HSL) and the U.S. NationalInstitute of Occupational Safety & Health (NIOSH), andmarked the world’s first international symposium of nan-otechnologies sponsored by a laboratory in charge of occu-pational safety and health.26) After lectures by technicalpolicy-makers, toxicologists, and safety & hygiene organi-zations, four workshops on measurement, management andrestrictions were held by four groups.

At international conferences including this, the riskassessment and management of nanomaterials attracts mostdiscussion. As of now, there are no obvious risks or stan-dardized specimens or test methods. Therefore, there is stillnot enough systematic data and the risks cannot be judgedyet. Some reports of individual research gave experimentalresults indicating toxicity.27) However, it is inappropriate tojudge risks immediately from these results. Systematic andstrategic research will be necessary in future.28)-30)

Judging from the conferences and reports introduced so far,those concerned generally agree to the following:• Most discussions start with the definition of nanomateri-

als. The typical dimension of nanomaterials (diameter ofparticle, cross-sectional diameter of fiber, or thickness offilm) is 100 nanometers or less.

• The knowledge held by safety and hygiene specialistsabout ultra fine particles should be made full use of.

• It is also important to evaluate whether nanomaterialsare fixed completely in a matrix like bulk materials, peellike coating, or are free to move.

• Regarding influences on the human body and environ-ment, nanomaterials can roughly be classified into onesthat are taken into the body intentionally for a medicalpurpose, such as a drug delivery system (DDS), andones taken into the body unintentionally.

• Even when chemical formulas are the same, bulk materi-als and nanomaterials should be handled differently.

• It is also necessary to distinguish nanoparticles generat-ed and discharged unintentionally, like diesel exhaustparticles, and industrial nanoparticles.

• As Figure 1 shows, priority subjects concerning expo-

sure are: 1) Safety and health of workers who have thehighest possibility of being exposed to nanomaterials, 2)Safety and of consumers who use products and tech-nologies, and 3) Protection of ecosystems and the envi-ronment. During the flow from upstream to downstream,nanomaterials tend to grow in size by cohesion and alsoto accumulate and degenerate.

• The framework of risk assessment, management, andcommunication about nanomaterials should be based onthe existing one applicable to chemical substances andfoods.

• Figure 2 shows an example of a flowchart far the riskassessment of nanomaterials. This is to judge “the neces-sity of assessment and management as nanomaterials”and not to evaluate the absolute size of a hazard. For amaterial soluble in water, the necessity of a new evalua-tion or management method is small because the con-ventional evaluation method can be applied. As theaspect ratio increases, the possibility of penetrating thelungs like asbestos grows. If a hazard is found, it is nec-essary to check the toxicity, the influence of size, andthe reaction by dosage.

• Figure 3 shows a general view of risk management. Therisk is a multiplication of hazard by exposure. Even ifthere is a hazard, the risk is small if the possibility ofexposure is low. Communication with the public is nec-essary at the stages of risk evaluation and management.

30


3. Maintenance of ecosystem and environment

1. Safety and healthof workers

Ecosystem, atmosphere, soil, and waters

Laboratoryin factory

Worker - Storage- Transportation

Consumer

2. Safety and healthof consumers

Disposal and recycling

Fig. 1 Priority subjects in the risk assessment and management ofnanomaterials.21)

- Aerosol generationand discharge

- Human body andenvironmental exposure

Aspect ratio Length

Toxicity screening- Influences on brain- Influences on lung- Influences on unborn child- Systemic influences- Oxidation factors- Environmental hormones- Sensitization and painkilling

Immediatelysoluble in water

Diameter Environmental toxicityscreening- Sustainability

(atmosphere and waters)- Long-distance move- Biological condensation- Influences on soil

Yes or Unknown

Necessity: SmallConventional evaluation

and managementmethod applicable

Necessity: Medium Necessity: Large

Fig. 2 Example of flowchart for judging the necessity of new methodsof evaluation of biological and environmental impacts of nanomateri-als.16), 20)

• Regarding the precautionary principle, there are gaps inthe recognition among the EU (excluding the UK), theUK and the United States. Besides, in terms of the eval-uation method, the former generally aims at the estab-lishment of method applicable to all nanomaterials whilethe latter aims at the selection of the best method foreach combination of material and application in thebelief that there is no universal evaluation method.31)

References

1) Drexler K.E., Engines of Creation. 1986.2) ETC Group, The Big Down: Atomtech - Technologies Converging

at the Nano-scale. 2003.3) Crichton M., Prey. 2002.4) Roco M.C., Converging Technologies and Their Societal

Implications. International Symposium on EnvironmentalNanotechnology 2004. EPA & MEA, ROC. (Dec. 1 to 10, 2004).

5) Yukihide Hirakawa, Biosafety and International Relationship –Issues and Subjects about Technical Governance. Revision of thepaper read at the 2003 Convention of the Japanese Political ScienceAssociation (Oct. 2003).

6) Masaki Misawa, Risk Analysis of Nanoparticles – Background andPresent Status –, AIST Forum “Nanotechnologies and Society”(Sep. 2004) (Slides).

7) Roco M.C. & Bainbridge W.S., Societal Implications ofNanoscience and Nanotechnology (Eds.).

8) Roco M.C., Broader societal issues of nanotechnology. Journal ofNanoparticle Research 5: 181–189 2003.

9) Meridian Institute, Proceedings of International Dialogue onResponsible Research and Development of Nanotechnology. (Jun.2004).

10) Roco M.C., Nanotechnology in U.S. – Research and education andrisk governance. First International Symposium on OccupationalHealth Implications of Nanomaterials. Health & Safety Laboratory.(Oct. 2004) (Slides).

11) Karn B., Nanotechnology and the Environment: What We HaveLearned Since Last Year. International Symposium onEnvironmental Nanotechnology 2004. EPA & MEA, ROC. (Dec.2004) (Slides).

12) Bond P.J., Responsible Development of Nanotechnology.Conference on nanotechnology “Small size-large impact”. SwissRe. (Dec. 2004) (Slides).

13) American National Standards Institute (ANSI), ANSINanotechnology Standards Panel Holds First Meeting.http://www.ansi.org/news_publications/news_story.aspx?menuid=7&articleid=783 2004

14) Lafranconi M., Addressing nanotechnology risk in an innovativeand proactive manner. Conference on nanotechnology “Small size-large impact”. Swiss Re. (Dec. 2004) (Slides).

15) Dürrenberger F., Höck J. & Höhener K., Overview of completedand ongoing activities in the field: Safety and Risks ofNanotechnology, TEMAS AG. 2004.

16) Naß R., Risk Assessment, Toxicological and Health Issues –Results of the EU Funded Project NANOSAFE. NANO2004Satellite Workshop The European Project “NANOSAFE”. (Jun.2004) (Slides).

17) Hoet P., Present knowledge of health effects of nanoparticles andfuture implications for workers and consumers. NANO2004Satellite Workshop - The European Project “NANOSAFE”. (Jun.2004) (Slides).

18) Verein Deutscher Ingenieure (VDI), Industrial application ofnanomaterials – chances and risks, Technology analysis. 2004.

19) Nanoforum, 4th Nanoforum Report: Benefits, Risks, Ethical, Legaland Social Aspects of NANOTECHNOLOGY 2004.

20) European Commission (EC), Nanotechnologies: A PreliminaryRisk Analysis on the Basis of a Workshop. (Mar. 2004).

21) Royal Society & Royal Academy of Engineering, Nanoscience andnanotechnologies: opportunities and uncertainties. (Jul. 2004).

22) Eiichi Ozawa, An investigation report by Royal Society & RoyalAcademy of Engineering: Nanoscience and nanotechnologies:opportunities and uncertainties. Japan Nanonet Bulletin 73.Nanotechnology Researchers Network Center of Japan.http://www.nanonet.go.jp/japanese/mailmag/2004/073c.html 2004

23) Welland M., Nanotechnology – Origins and Issues. Conference onnanotechnology “Small size-large impact”. Swiss Re. (Dec. 2004)(Slides).

24) DECHEMA, Proceedings of 7th International Conference onNanostructured Materials. (Jun. 2004).

25) Masahiro T., 7th International Conference on NanostructuredMaterials (NANO 2004) Part 2: Panel Discussion “NanotechnologyPolicies of Germany and Europe” Japan Nanonet Bulletin 71.Nanotechnology Researchers Network Center of Japan.

26) Health & Safety Laboratory (HSL), Proceedings of FirstInternational Symposium on Occupational Health Implications ofNanomaterials. (Oct. 2004).

27) Oberdörster E., Manufactured Nanomaterials (fullerenes, C60)Induce Oxidative Stress in the Brain of Juvenile Largemouth Bass.Environmental Health Perspectives 112(10): 1058–1062.

28) Colvin V.L., Environmental Impacts of Engineered Nanomaterials:A new kind of pollution? Conference on nanotechnology “Smallsize-large impact”. Swiss Re. (Dec. 2004) (Slides).

29) Kreyling W.G., Health Implication of Nanoparticles, InternationalSymposium on Environmental Nanotechnology 2004. EPA &MEA, ROC. (Dec. 2004): 93–110.

30) Oberdörster G., Nanotoxicology: an Emerging Discipline.International Symposium on Environmental Nanotechnology 2004.EPA & MEA, ROC. (Dec. 2004): 71–91.

31) Marburger J., Statement in International Dialogue on ResponsibleResearch and Development of Nanotechnology. (Jun. 2004).

31


Risk management

Risk communication

Risk analysisRisk evaluation

- Hazard verification

- Hazard characterization

- Exposure evaluation

- Risk characterization

Fig. 3 General view of risk assessment and management.20)

PART3

Public Research Institutes for

Materials Research

in Respective Countries

• Public Research Institutes for Materials Reseach in

Japan, USA and EU

• New Nanotechnology Research Institutes in Japan,

USA and Europe

• Public Research Institutes in Russia Federation and

Poland

1. Introduction

In the last decade, 7 public research institutes andresearch laboratories of about 40 universities have pub-lished papers on materials, excluding laboratories belong-ing to private companies.

Due to limited space, this report cannot cover allresearch institutes engaged in materials research. There-fore, this paper introduces some public research institutesand university laboratories to compare Japanese researchinstitutes that are engaged in materials research.

2. Comparison of public research institutions formaterials research

Regarding materials research in Japan, the NationalInstitute for Materials Science (NIMS), an independentadministrative institution under the jurisdiction of the Min-

istry of Education, Culture, Sports, Science and Technolo-gy, is conducting a wide range of basic R&D. Two otherindependent administrative institutions, RIKEN (under thejurisdiction of the same ministry) and the National Instituteof Advanced Industrial Science and Technology (AIST,under the jurisdiction of the Ministry of Economy, Tradeand Industry), are conducting applied research in someresearch divisions.

Table 1 compares NIMS and AIST. NIMS conductsmainly basic research on materials sciences, RIKEN con-ducts tests and research on technologies, and AIST con-ducts technical R&D and related activities for the miningindustry.

Figure 1 compares the budgets of the three researchinstitutes.1)-3) AIST ranks top with about 121 billion yen(approximately 1,100 million dollars), followd by RIKENwith 84 billion yen (approximately 764 million dollars) andthen by the NIMS with 23 bilion yen (approximately 209million dollars).

35


Expenditure120,975

million yen

Total83,956

million yen

Expenditure23,100

million yen

Directresearch42,163

Unit: million yen

Indirectdivisions14,117

Labor expenses34,945

Facilitymaintenance subsidy

3,340

Fusion related research3,078

Brainscience9,728Genome

science8,006

Plant science1,595

Generation andregeneration

5,214

Entrustedresearch

8,399

Dissemination andapplications

3,032

Laborexpenses

11,261Labor59

Business107

Entrustedresearch

32

Facilitymaintenance

3

Redemption30

Strategicresearchpromotion

8,424

Atomicpower5,859

Leading infrastructureresearch

4,018

Life science2,547

Polygene2,119

Immunityand

science3,864

Harima Laboratory - Synchrotron radiation6,813

Subsidy forredemption of facilitymaintenanceloan26,410

(a) National Institute for Materials Science (b) RIKEN (c) National Institute of Advanced Industrial Science and Technology

Fig. 1 Comparison of expenditures and budgets between National Institute for Materials Science, RIKEN and National Institute of Advanced IndustrialScience and Technology (FY2004).

Chapter 1. Public Research Institutes forMaterials Research in Japan, USAand EU

Section 1. Japan

Tomoaki Hyodo, Yoshio AbeInternational Affairs Office, NIMS

To promote research and development in the field ofnanotechnologies and nanomaterials, which is one of fourpriority fields selected in the Second Science and Technol-ogy Basic Plan, NIMS set the following fields as priorityR&D fields in the medium-term program from FY 2001 toFY2005:• Nanomaterials• Environment and energy materials• Safe materials• Improvement of research and intellectual infrastructure

Meanwhile, RIKEN is attempting to discover new mate-rials by studying electron states, magnetic statuses, andnanoproperties at a large synchrotron radiation researchfacility (SPring-8: mentioned later). To produce new func-tional materials, RIKEN is developing ultrahigh precisiontechniques to control the properties, structures, and func-

tions of materials on the atomic and molecular levels.RIKEN is also constructing a novel nanosystem using pho-tons and developing infrastructure techniques to observe,operate, control, and process carbon tubes, fullerene, andother materials in units of single atoms and molecules.

With nanometer control, nanosystem device creation,and micro-nanoprocessing technologies, AIST is research-ing and developing raw composite functional materials andnew carbon materials as the basis of ultrahigh-speed andlarge-capacity information processing technologies, as wellas precision-control polymer materials as the foundationfor sustainable development of economic society.

3. University research institutions for materials research

36


National Institute forMaterials Science (NIMS)

Rikagaku Kenkyujo (RIKEN)National Institute of Advanced Industrial

Science and Technology (AIST)

Established April 1, 2001Established by the merging of National Research Institute for Metals (established July 1956) and National Institute for Research in Inorganic Materials (established April 1966) as an independent administrative institution.

October 2003Established as RIKEN Foundation in 1917. Reorganized into the Scientific Research Institute Ltd. after the world War2 and inaugurated as the Institute of Physical and Chemical Research in October 1958. Established as an independent administrative institution in October 2003.

April 1, 2001Established in January 2001 by the merging of 8 research institutes previously under the former Agency of Industrial Science and Technology at Tsukuba Center and in 7 other areas. Established as an independent administrative institution in April 2001.

Purpose To raise the level of materials science and technology by conducting research and development on associated technologies, as well as research and intellectual infrastructure(Article of the Individual Law)

To raise the level of science and technology by comprehensive research in science and technology (excluding only humanities and social sciences)(Article 3 of the Individual Law)

To enhance industrial technologies and disseminate their achievements, and to contribute to economic and industrial development and the stable and efficient supply of mineral resources and energy by comprehensive research and development on technologies in the mining industry(Article 3 of the Individual Law)

Scope of Work 1. Basic research related to material science and technology, and R&D of related research and intellectual infrastructure2. Encouragement of dissemination and practical application of the above R&D results3. Shared use of institute facilities and equipment with those engaged in R&D on science and technology4. Training and development of researchers and technicians in materials science and technology5. Work related to 1 to 4 above(Article 14 of the Individual Law)

1. 1) Testing and research related to science and technology2) Encouragement of dissemination and practical application of the results of R&D3) Shared use of institute facilities and equipment with those engaged in testing and R&D on science and technology4) Training and development of researchers and technicians in science and technology5) Work related to the above2. As well as 1) to 5) above, work prescribed in Article 8 of the Law for Promoting the Shared Use of Specific Synchrotron Radiation Facilities(Article 16 of the Individual Law)

1. 1) R&D on mining science and technology and related work2) Geological survey3) Setting of measuring standards, inspection, examination, and R&D on measuring instruments, and related work and also training on measurement4) Technical guidance and dissemination of achievements related to the work in 3) 5) Work related to the above2. As well as 1) to 5) above, witnessed inspection prescribed in Clauses 1 and 2, Article 148 of the Measurement Law(Article 11 of the Individual Law)

Supervised By Ministry of Education, Culture, Sports, Science and Technology

Ministry of Education, Culture, Sports, Science and Technology

Ministry of Economy, Trade and Industry

Personnel ™Full-time staff• Laboratory staff (non-Japanese)

395 (16)[Tenured] [373][Fixed-term] [22]

• Engineering 41• Office 103Staff as of April, 2004 539 (16)

™Acceptance of researchers through various systems (in FY2003)• Special researchers (postdoctoral)

305• Special researchers (non-postdoctoral)

13• NIMS junior researchers 20• Guest researchers 197• Visiting researchers 393

™Full-time staff• Full-time staff (excluding temporary

staff)685 (as of Apr. 1, 2004)• Full-time staff (Fixed-term) 1,953 (as of March 31, 2003)

™Acceptance of researchers and technicians from universities and companies (in FY2003)• Linked graduate school system

193/year• Junior associate system (Students of the second-term doctorate

course) 141/year• Special fellow system for basic

science 205/year• Independent chief researcher 5/year

™Full-time staff• Laboratory staff (non-Japanese)

2,395 (55) [Tenured] [2,015] [Fixed-term] [380]• Office staff 719

Staff as of Apri1, 2004 3,114 (55)

™Acceptance of researchers through the industry-academia-government linkage system• Postdoctoral researchers 800• From private companies 800• From universities 1,700• From overseas 900 (Total number accepted in FY2003)

Table 1 Comparison of National Institute for Materials Science, RIKEN, and National Institute of Advanced Industrial Science and Technology.1) ~3)

As research institutes belonging to universities, Table 2gives the Institute for Materials Research, Tohoku Univer-sity, and a joint-use academic corporation, the Institute forMolecular Science.4), 5)

Aiming to examine the principles of materials science andways of applying them, the Institute for Materials Research,Tohoku University is conducting R&D to study materialsproperties, to design materials, to create structural and func-tional materials, and to process and evaluate materials.4)

To clarify the structures, functions, and reactions ofmolecules and molecular aggregates on the atom and elec-tron levels and to predict and attain new phenomena and

functions, the Institute for Molecular Science is conductingexperimental and theoretical research on the structures andfunctions of molecules and molecular aggregates.5)

The budget is about 6.3 billion yen (approximately 57million dollars in FY2001) for the Institute for MaterialsResearch, Tohoku University and about 8.1 billion yen(approximately 74 million dollars in FY2003) for the Insti-tute for Molecular Science.

4. Major research facilities for materials research

37


National University CorporationInstitute for Materials Research, Tohoku University (IMR)

University-shared Academic CorporationInstitute for Molecular Science (IMS)

History Established in April 1916Inaugurated as the Second Division of the provisional RIKEN attached to the Science School of Tohoku Imperial University. Reinaugurated as Laboratory of Metallic Materials attached to Tohoku Imperial University in August 1922 and re-inaugurated as a collaborative research institute attached to Tohoku University in May 1987.

Established in April 1975.Integrated with the General Research Organization of Biological Science in April 1981 and operated together as Okazaki National Research Institute. Integrated and reorganized with the National Astronomical Observatory, National Institute for Fusion Science, Laboratory of Basic Biology, and Laboratory of Physiology. Reinaugurated as a university-shared academic corporation “Institute for Molecular Science.”

Purpose To research principles in materials science and their applications(Article 2 in the rules of the Institute for Materials Research, Tohoku University)

[Goals of research]To find general rules and predict or attain new phenomena and functions by clarifying the structures, functions, and reactions of molecules and molecular aggregates on the atom and electron levels (Extract from mid-term goal)

Activities The research organization consists of four research divisions and four attached research institutions. The research divisions conduct the following:1. Materials Property Division

Theoretical and experimental research on macroscopic mechanisms related to the basic properties of materials

2. Materials Design Division Research on the development and design of new materials by controlling the basic properties of structural and functional materials

3. Materials Development Division Research on the creation of new structural and functional materials by physical and chemical methods

4. Materials Processing and Characterization Division Research on processing technologies for new materials and on the evaluation and analysis of their materials characteristics

(Article 6 of the rules of the Institute for Materials Research, Tohoku University)

The attached research institutions are: International Research Center for Nuclear Materials Science, Advanced Research Center for Metallic Glasses, High Field Laboratory for Superconducting Materials, and International Frontier Center for Advanced Materials.

[Actions to achieve goal]In the field of molecular science, experimental and theoretical research on the structures, functions, and reactions of molecules and molecular aggregates are conducted by advanced physiochemical methods using external fields such as optical X-rays, electron-rays, and magnetic fields and very low temperature; techniques of designing and synthesizing molecular materials; theoretical simulation design; and also synthesis simulation by ultrahigh-speed computation.1. Theoretically clarifying universal factors dominating chemical

reactions and molecular properties to create molecular theories for predicting reactions and designing new properties

2. Expanding fine and high-grade molecular spectroscopy to establish a technique of evaluating the statuses of molecules and molecular aggregates. Also proposing practical property evaluation devices and measuring devices.

3. Developing a new laser as a light source for spectroscopy or photochemical reactions, and also an extreme ultraviolet source by synchrotron radiation, and promoting research on the application of chemical reaction dynamics and creation of new materials

4. Researching properties to develop molecules, nanoscale molecular elements, and molecular solids and to establish guidelines for materials development

5. Proceeding with research by theory and computer simulation to deepen the fundamental understanding of chemical and physical phenomena that cannot be clarified by experimentation(Extract from the mid-term plan)

Personnel

Budget

™Staff (as of Apr. 1, 2002)• Professors 133 General staff 89

Part-time staff 80 Total: 302™Graduates (as of Apr. 1, 2002)

• First-tem course 100 Second-term course 49Total: 149

™Researchers (as of Apr. 1, 2002)• Special fellows 33

™Staff (as of Jan. 1, 2005)• Chief 1• Teaching staff 77• Technical staff 35 Total: 113

FY2001¥6,345 mil.

FY2003(Settled amount)

¥8,097 mil.

Property

Labor

Scholarship grants

Industry-academia research

Scientific research

Science and technologypromotion and coordination

Labor

Property

Facility maintenance

Table 2 Profiles of Institute for Materials Research, Tohoku University (IMR) and Institute for Molecular Science (IMS).4), 5)

Table 3 outlines the High Energy Research AcceleratorResearch Organization (KEK).6) KEK set up and is nowoperating the Institute of Particle and Nuclear Studies, theInstitute of Material Structure Science, Accelerator Labora-tory, and the Applied Research Laboratory as institutionsshared by universities.

The Japan Synchrotron Radiation Research Institute

possesses a large-scale synchrotron radiation facility calledSPring-8 (Figure 2).7) SPring-8 was jointly constructed bythe Japan Atomic Energy Research Institute and RIKENand put into service in October 1997 for shared use of syn-chrotron radiation. SPring-8 is now operated by the JapanSynchrotron Radiation Research Institute (JASRI). JASRIinvites and selects projects wishing to use the facilities andprovides domestic and overseas researchers with synchro-tron radiation. The organization also operates and main-tains tests and R&D facilities to support usage, the analysisof atomic arrangements and structures, the analysis of sta-tuses and components, and observation by the imagingmethod.

The budget is about 40.3 billion yen (approximately 366million dollars in FY2004) for the High Energy ResearchAccelerator Research Organization and about 10.5 billionyen (approximately 95 million dollars in FY2004) forSPring-8 at the Japan Synchrotron Radiation ResearchInstitute.

5. Conclusion

1) The National Institute for Materials Science handles awide range of materials research such as nanomaterials.

38


University Research Institute Corporation – High Energy Research Accelerator Research Organization (KEK)

History • July 1955 The Institute of Nuclear Study established• April 1971 National Laboratory for High Energy Physics established• April 1978 Meson Science Facility established as an institution attached to Department of Science, Tokyo University (Reorganized into

Meson Science Laboratory later)• April 1997 High Energy Accelerator Research Organization established (from National Laboratory for High Energy Physics, and Institute

for Nuclear Research and Meson Science Laboratory, University of Tokyo)• April 2004 Re-inaugurated as the Inter-University Research Institute Corporation High Accelerator Research Organization

Purpose To promote research as the basis of comprehensive development for Japan's accelerator science (experimental and theoretical research on elementary particles and atomic nuclei and on the structures and functions of materials including living organisms, research on enhancing the performance of the accelerator and on related infrastructure technologies using a high energy accelerator) and to provide domestic and overseas researchers in related fields with a place for conducting research

Work The Institute of Particle and Nuclear Studies, Institute of Material Structure Science, Accelerator Laboratory, and Applied Research Laboratory were established and are now jointly used by universities.™Institute of Particle and Nuclear Studies

Experimental research on elementary particles and atomic nuclei and their related theoretical research using a high energy accelerator™Institute of Material Structure Science

Experimental research on the structures and functions of materials and their related theoretical research using a high energy accelerator™Accelerator Laboratory

Study of high energy accelerators as key facilities for research on elementary particles and atomic nuclei in materials science, and operation and management of proton accelerators and electron and positron accelerators

™Applied Research LaboratoryOrganized from the Radiation Science Center, Computing Research Center, Cryogenics Science Center, and Mechanical Engineering Center for necessary research and research support with the large accelerator in related fields

Personnel

Budget

™Staff (as of April 1, 2004) 692 in totalChief/manager: 1 Teaching staff: 372 Technical staff: 161 Office staff: 158

™Joint researchers accepted (FY2003) 89,142 person-days in total™Overseas joint researchers accepted (FY2003) 30,611 person-days in total

FY2004¥40,216 mil.

Business (Education and research, general administration)

Facility maintenance

Industry-academia research and donations

Redemption of long-term loan

Table 3 Outline of High Energy Research Accelerator Research Organization.6)

Fig. 2 SPring-8. (Courtesy of SPring 8)

RIKEN is characterized by searching for new materials byusing the synchrotron radiation facility. AIST is engaged insuch as nanotechnology R&D utilizing nanometer controland nanodevice system creation technologies and alsomicro-nanoprocessing technologies.2) The Institute for Materials Research, Tohoku Universityis conducting R&D to study materials properties, to designmaterials, to create structural and functional materials, andto process and evaluate materials. The Institute for Molecu-lar Science is conducting experimental and theoreticalresearch on the structures and functions of molecules andmolecular aggregates.3) The High Energy Research Accelerator Research Orga-nization set up and is now operating the Institute of Particleand Nuclear Studies, Institute of Material Structure Sci-ence, Accelerator Laboratory, and others as shared institu-tions for materials science. SPring-8 is a shared facility forthe analysis of atomic arrangements and structures.

References

1) Web page of the National Institute for Materials Sciencehttp://www.nims.go.jp/eng/index.html

2) Web page of RIKENhttp://www.riken.jp/engn/index.html

3) Web page of AISThttp://www.aist.go.jp/index_en.html

4) Web page of the Institute for Materials Research, TohokuUniversityhttp://www.imr.tohoku.ac.jp/Eng/index.html

5) Web page of the Institute for Molecular Sciencehttp://www.ims.ac.jp/index.html

6) Web page of the High Energy Research Accelerator ResearchOrganizationhttp://www.kek.jp/intra-e/index.html

7) Web page of SPring-8http://www.spring8.or.jp/e/

39


1. R&D budgets in the United States

In the United States, basic research on materials is main-ly funded by the Department of Energy (DOE) – BasicEnergy Sciences, Materials Science (DOE-BES) and theNational Science Foundation (NSF) – Mathematical andPhysical Sciences, Materials Research (NSF-MPS).1)-3) InFY2004, the DOE-BES invested 559 million dollars, whilethe NSF-MPS invested 251 million dollars on materialsresearch. The DOE has 14 research institutes. The NSF,however, is specialized in research funding and has noresearch institutes, excluding part of the South Pole Station.

The National Institute of Standards and Technology(NIST) belongs to the Department of Commerce and con-ducts research on ceramics, polymers, and other materialsin the Materials Science and Engineering Division and oth-ers.4) The research budget is 63 million dollars (requestedin FY2005).

In this report, the NSF is excluded because it operates noresearch institutes for materials research.

2. Materials research in DOE-BES

The DOE research and development activities originatedfrom the Manhattan Project for the atomic bomb. To con-tinue the work of the Manhattan Project after World WarII, the Atomic Energy Commission was established by theenactment of the Atomic Energy Act in 1946. According tothe Energy Reorganization Act enacted in 1974, the Atom-ic Energy Commission was abolished and the Nuclear Reg-ulatory Commission and the Energy Research and Devel-opment Administration were established. The present DOEis an administrative organ that was set up in October 1977as the 12th department of the United States according to theDepartment of Energy Organization Act.

The DOE is primarily a national security organization; itplaces emphasis on energy development and regulation inthe latter half of the 1970s and on nuclear weapons R&D inthe 1980s. After the Cold War, the DOE focused on theenvironmental purification of nuclear weapons compoundfacilities, nuclear non-proliferation, property managementof nuclear weapons, energy supply and transportation, andefficiency enhancement and conservation of energies.

The strategic goals of the DOE announced in September2003 announce a mission of advancing the national, eco-nomic, and energy security of the United States to driveforward the supporting science and engineering. The gener-al goals in the field of science are to provide a world-classscientific research capability and to ensure that the DOEachieves its mission of national energy security, overseesan improvement in knowledge in advanced physics, biolo-gy, medicine, environment, and computational science, andprovides world-class research facilities for national scien-tific projects. The interim goals of materials research,announced at the same time, are to complete the construc-tion of a spallation neutron source by the end of 2006, toput nanoscience research centers into operation by the endof 2008, and to develop materials having characteristicsthat can be predicted from each atom based on an under-standing of materials nanoscale assembly by 2015.

Table 1 shows the DOE-BES expenses in FY2004.5) Ofthe 991 million dollars in total, 559 million dollars are allo-cated for materials research. Figure 1 shows the breakdownof the DOE-BES requested budget. Of the requested budgetin FY2006 ($1,105 million), 40% are for the facility opera-tions, 17% for infrastructure, and 14% and 26% respective-ly for research at universities and public research institutes.

Table 2 shows the DOE-BES expenses in the materialssciences and engineering fields in 2004. Of the totalexpenses, 261 million dollars (47%) are spent on researchand 298 million dollars (53%) on facility operations. Table3 shows the breakdown of research expenses totaling 261million dollars. The material research expenses, excludingthose for operating DOE-BES supervised facilities, weresubsidized in many research fields, particularly Neutronand X-ray Scattering (17.2%), Experimental CondensedMatter Physics (16.4%), and Materials Chemistry (15.5%).

The priority themes of the DOE-BES are nanoscale sci-ence research and hydrogen initiative research. Table 4shows the transition of budgets on nanoscale scienceresearch and Table 5 shows the budget for hydrogenresearch.

Of the total of 200 million dollars for nanoscale scientif-ic research in FY2004, 74 million dollars were spent onmaterials science and engineering research and 84 milliondollars on the construction of nanoscale scientific researchcenters. The expenses on materials research related to the

40


01 Public Research Institutes for Materials Science in Japan, USA and EU

Section 2. USA

Tomoaki Hyodo, Oliya V. OwenInternational Affairs Office, NIMS

41


Field of Science FY2004• Materials Sciences and Engineering• Chemical Sciences, Geosciences, and

Energy Biosciences• Construction

Total

558,831213,778

218,653991,262

Table 1 DOE-BES expenses in FY2004 ($1,000). 5)

Field of Science FY2004• Materials Sciences and Engineering

Research• Facilities Operations Total in the materials sciences and engineering field

260,693

298,138558,831

Table 2 Expenses in the materials sciences and engineering field of DOE-BES in FY2004 ($1,000). 5)

Fig. 1 Breakdown of research expenses in DOE - BES, Materials Science (FY2006 requested budget). 5)

Material Research FY 2004 %Neutron and X-ray ScatteringExperimental Condensed Matter PhysicsMaterials ChemistryStructure and Composition of MaterialsPhysical Behavior of MaterialsCondensed Matter TheoryMechanical Behavior and Radiation EffectsSynthesis and Processing ScienceEngineering ResearchThe Center for Nanoscale MaterialsExperimental Program to Stimulate Competitive Research (EPSCoR)Instrumentation for the Spallation Neutron SourceTransmission Electron Aberration Corrected Microscope (TEAM)Neutron Scattering Instrumentation at the High Flux Isotope ReactorLinac Coherent Light Source (LCLS)Nanoscale Science Research Centers

Total of Research Budgets in Materials Science and Engineering Field

44,92842,63140,33822,83322,14818,12613,44412,71010,97510,0007,6737,3873,1002,0002,000

400

260,693

17.2 16.4 15.5 8.8 8.5 7.0 5.2 4.9 4.2 3.8 2.9 2.8 1.2 0.8 0.8 0.2

100

Table 3 Breakdown of DOE-BES materials research expenses ($1,000). 5)

Expenditure Item in Nanoscale Science 2004 Estimated 2005 Budget 2006 RequestedResearch

Materials Sciences and EngineeringChemical Sciences, Geosciences, and Energy Biosciences

Capital EquipmentArgonne, Center for Nanoscale Materials

Nanoscale Science Research CentersBasic Expenses (All Centers)Construction Expenses

BNL, Center for Functional NanomaterialsLBNL, Molecular FoundryORNL, Center for Nanophase Materials SciencesSNL/A and LANL, Center for Integrated Nanotechnologies

Total Budget in BES Nanoscale Science

73,50127,833

10,000

2,982

034,79419,88229,674

198,666

66,99528,360

12,000

1,996

18,31731,82817,66930,650

207,815

112,63226,914

14,000

0

36,5539,606

04,626

204,331

Table 4 Transition of budgets on nanoscale science research ($1,000). 5)

Field of Science 2004Estimated

2005Budget

2006Requested

ResearchMaterials Sciences and EngineeringChemical Sciences, Geosciences, and Energy Biosciences

Total

3,0554,6557,710

14,76114,42229,183

16,60015,90032,500

Table 5 Transition of budgets by President in hydrogen initiative research ($1,000). 5)

hydrogen initiative were 3 million dollars in FY2004 andthe DOE is now requesting a large increase in budget forthe future.

3. Research institutions for materials research in DOE

As Figure 2 shows, the DOE has 14 public researchinstitutes throughout the United States,6) which are classi-fied by role as shown in Table 6. Table 7 lists the year ofestablishment, administration, budget, and number ofresearchers in these DOE research institutes.

The three institutes in Lawrence Livermore, Sandia, andLos Alamos are large, with budgets exceeding one billiondollars, and are mainly engaged in weapons research. MostDOE research institutes conduct materials research. How-ever, the most active institutes are the Ames Institute,

42


Fig. 2 Locations of DOE research institutes. 6)

Classification Research Institute

Multi-program

Materials

High Energy Physics

Nuclear Physics

Weapons

FusionEnergy EfficiencyNuclear Energy

ArgonneBrookhavenOak RidgeLawrence BerkeleyPacific NorthwestAmesFermi,Stanford: At the Stanford Linear Accelerator Center, X-ray facilities were recently added to High Energy Physics.Thomas Jefferson,(Also at Brookhaven)Lawrence LivermoreSandia (Albuquerque and California)Los AlamosPrincetonNational Renewable Energy LaboratoryIdaho

Table 6 Classification of DOE laboratories by role.

Research Institute Established Administration Budget (FY2004) Researchers/Total

Ames Laboratory 1947 Iowa State Univ. $30 million 240/420

Argonne National Laboratory (ANL)

1940s University of Chicago $500 million 1200/4,000

Brookhaven National Laboratory (BNL) 1946

Stony Brook Univ. – Battelle

$436 million (2003) Approx. 5,000 /7,000

Idaho National Engineering and Environmental Laboratory (INEL)

1949Bechtel – BWX Tech. – INRA

$800 million 8,000 total

Lawrence Berkeley National Laboratory (LBNL)

1931 Univ. of California $500 million 3,800/6843

Lawrence Livermore National Laboratory (LLNL)

1952 Univ. of California $1.6 billion 8,000 total

Los Alamos National Laboratory (LANL)

1943 Univ. of California $2.2 billion 7,500/10,700

National Energy Technology Laboratory

1910 DOE direct control $926 million 880/1100

National Renewable Energy Laboratory

1974Midwest Research Institute – Battelle – Bechtel

$230.1 million (2003)

?

Oak Ridge National Laboratory (ORNL)

1942Univ. of Tennessee – Battelle

$1.0 billion1,500/3,800 + over 3,000 visiting researchers

Pacific Northwest National Laboratory (PNNL)

1965 Battelle $650 million 3,900

Princeton Plasma Physics Laboratory (PPPL)

1951 Princeton Univ. $75.5 million 168/427

Sandia National Laboratories (SNL) 1945Sandia Corp. (Lockheed Martin)

$2.2 billion8,600 total(all locations)

Stanford Linear Accelerator Center (SLAC)

1960 Stanford Univ.$184 million (2000)

1,314 total (FY 2000)

Table 7 FY2004 budgets of DOE research institutes and the numbers of researchers.

which is mainly engaged in materials research and theArgonne, Brookhaven, Oak Ridge, and Lawrence Berkeleyinstitutes which are multi-program institutes with activeR&D initiatives in many fields. Pacific Northwest, one ofthe multi-program research institutes, specializes in chem-istry and is involved in relatively little materials research.The Oak Ridge Institute has a large budget ($1 billion) anda large personnel (1,500 researchers) whereas the AmesInstitute is comparatively small compared to other DOE

research institutes, with a budget of 300 million dollars anda staff of 240 researchers.

Apart from the National Energy Technology Laboratory,all DOE research institutes are operated either by universi-ties or private companies.

According to the mid-term goals set in 2003, the DOE isconstructing five nanotechnology and nanomaterialsresearch centers. Table 8 lists the fields and the purpose ofresearch and Figure 3 shows the locations of the research

43


Center (Operator) Field and Purpose

Center for Functional Nanomaterials(Brookhaven Nat’l Lab)

Six Scientific Themes:1) Strongly Correlated Oxides, 2) Magnetic Nanoassemblies, 3) Nanoscale Catalyst Materials, 4) Charge Injection and Transport in Nanoscale Materials5) Nanostructured Organic Films; Structure and Self-assembly6) Applications of Functional Nanomaterials

Center for Nanophase Materials Sciences(Oak Ridge Nat’l Lab)

Seven Scientific Thrusts: (80,000 ft2)1) Macromolecular Complex Systems, 2) Functional Nanomaterials3) Nanoscale Magnetism and Transport, 4) Catalysis and Nano Building Blocks,5) Nanofabrication, 6) Theory, Modeling, and Simulation7) Nanoscale Imaging, Characterization, and Manipulation

Molecular Foundry(La2)rence Berkeley Nat’l Lab)

*Six facilities: (94,500 ft2) *Affiliated Foundry Laboratories1) Inorganic Nanostructures Facility, 2) Organic, Polymer, and BiopolymerNanostructures Facility, 3) Nanofabrication Facility, 4) Biological NanostructuresFacility, 5) Imaging and Manipulation Facility, 6) Theory of Nanostructures Facility

Center for Nanoscale Materials(Argonne Nat’l Lab)

Eight Primary Research Themes: (24,000 ft2)1) Bio-Inorganic Interfaces, 2) Complex Oxides, 3) Nanocarbon, 4) Nanomagnetism,5) Nanophotonics, 6) Theory and Simulation, 7) Nanopatterning, 8) X-ray Nanoprobe

Center for Integrated Nanotechnologies(Sandia Nat’l Lab and Los Alamos Nat’l Lab)

Five Scientific Thrusts: (95,000 ft2)1) Nano-Bio-Micro Interfaces, 2) Nanophotonics and Nanoelectronics3) Complex Functional Nanomaterials, 4) Nanomechanics5) Theory and Simulation

Table 8 Nanomaterials and nanotechnology research centers of DOE.

Molecular foundry(Advanced Light Source: Second-generation synchrotron institute)

Comprehensive nanotechnology center (Composite Semiconductor Laboratory, Los Alamos Neutron Science Center, and High Magnetic Field Laboratory)

Nanoscale materials center(Advanced photon source: Third-generation synchrotron institute. High-strength pulse neutron source)

Nanotissue materials science center(Spallation neutron generation institute)

Nanofunctional materials center(Synchrotron orbital radiation institute. Laser beam acceleration institute.)

Lawrence Berkeley National Laboratory

Argonne National Laboratory

Oak Ridge National Laboratory

Brookhaven National Laboratory

Sandia National LaboratoryLos Alamos National Laboratory

Fig. 3 Locations of DOE nanomaterials and nanotechnology centers.

centers. At these five research centers, huge research facili-ties using synchrotron radiation or neutron beams will com-mence service by the end of 2008.

Table 9 lists the fields of materials research of the DOEresearch institutes. Many institutes, including Ames andOak Ridge, conduct materials research.

4. Main materials research organizations other thanDOE

The National Institute of Standards and Technology(NIST) is a federal governmental organization, establishedunder the Department of Commerce in 1901. The missionof NIST is to develop technologies, measuring methods,and standards necessary in industry to improve productivi-ty, smoothen trade, and improve the quality of life.4)

NIST achieves its mission through NIST research insti-tutes, Baldrige National Quality Program, ManufacturingExtension Partnership, and Advanced Technology Pro-gram. The NIST research institutes are developing techni-cal infrastructure and conducting standardization R&D inU. S. heavy industry. The Baldrige National Quality Pro-gram gives awards every year to encourage progress byU.S. manufacturing companies, service companies, educa-tional institutes, and medical institutes. The ManufacturingExtension Partnership is a nationwide network of local cen-ters that provide small and medium-sized companies withtechnologies and business support. The Advanced Technol-

ogy Program promotes innovative technological progressthrough joint investments in research by private companies.

Figure 4 shows the FY2005 budgets of NIST. The totalbudget is 858 million dollars, of which the NIST researchinstitute expenses account for the greatest amount with 373million dollars, followed by the technical service budget inindustry with 244 million dollars. The breakdown is 137million dollars for the Advanced Technology Program and

44


Research InstituteMaterials Research

DivisionMain Materials Research

Ames LaboratoryMaterials and Engineering Physics and others(3 of 10 divisions)

Experimental and theoretical research on rare earth elements in novel mechanical, magnetic, and superconducting materials

Argonne Nat'l LabMaterials Science and others(3 of 22 divisions)

Research on high-temperature superconductivity, polymeric superconductors, thin-film magnetism, and surface science

Brookhaven Nat'l Lab

Materials Science and others(4 of 13 divisions)

Research problems such as high-temperature superconductivity, magnetism, structural and phase transformations in solids, and polymeric conductors

Lawrence Berkeley Nat'l Lab

Materials Science and others(2 of 18 divisions)

Research on laser spectroscopy, superconductivity, thin films, femtosecond processes, biopolymers, polymers and composites, surface science, and theory

Lawrence Livermore Nat'l Lab

Chemistry and Materials Science and others(2 of 11 divisions)

Research on metals and alloys, ceramics, materials for lasers, superplasticity in alloys, and intermetallic metals

Los Alamos Nat'l Lab

Materials Science and Technology and others(2 of 21 divisions)

Research on electronic materials, the theory of evolving microstructures, and plasma immersion processes for ion-beam processing of surfaces for improved hardness, corrosion resistance, and wear resistance

Oak Ridge Nat'l LabMaterials Sciences and others(3 of 11 divisions)

Basic research which underpins the energy efficiency program in superconductivity, magnetic materials, pulsed laser ablation, thin films, lithium battery materials, thermoelectric materials, surfaces, polymers, structural ceramics, and alloys

Pacific Northwest Nat'l Lab

Energy and others(2 of 7 divisions)

Research on stress-corrosion cracking of metals and alloys, high-temperature corrosion fatigue of ceramic materials, and irradiation effects in ceramic materials

Sandia Nat'l LabMaterials and Process Science and others(2 of 13 divisions)

Processing and properties for sol-gel chemistry of ceramic coatings, the development of nanocrystalline materials, adhesion and wetting of surfaces of metals, glass, and ceramic materials

Table 9 Materials research at DOE research institutes.

Fig. 4 FY2005 budgets of NIST. 4)

108 million dollars for the Manufacturing Extension Part-nership. The total number of staff at NIST is about 3,000.

Table 10 provides materials research information at theNIST research institutes. NIST is researching ceramics,metals, and polymers mainly at their Materials Science &Engineering Laboratory.

Other research institutes, apart from those at the DOEand NIST are those of the military forces (Navy, Army, andAir Force) and NASA, as outlined in Table 11.7)-11) Theseinstitutes are involved in the metals and ceramics, andpolymers research for practical uses.

5. Conclusion

1) In the United States, basic research on materials is main-ly funded by the Department of Energy – Basic Energy Sci-ences, Materials Science and the National Science Founda-tion – Mathematical and Physical Sciences, MaterialsResearch.2) The Department of Energy has 14 research institutes.However, much of the basic research is also being done atthe Ames Institute which is mainly engaged in materialsresearch and at the Argonne, Brookhaven, Oak Ridge, andLawrence Berkeley institutes which are multi-programinstitutes.3) The Department of Energy is constructing five nan-otechnology and nanomaterials research centers using syn-chrotron radiation or neutron beams. These will enter ser-vice by the end of 2008.4) The National Institute of Standards and Technologyunder the Department of Commerce has a mission of devel-oping technologies, measuring methods, and standards. TheMaterials Science & Engineering Laboratory is leadingresearch on ceramics, metals, and polymers.

45


Research Institute/Supervising Government Office

EstablishedNo. of Researchers

Budget

Materials ResearchRelated Division

Outline

US Naval Research Lab. Department of the Navy7)

1923Civilian 2,700

$842 million(FY2004)

Materials Science and Component Technology, Nanoscience Institute, etc.(Total number of research divisions: Unknown)

R&D across fields to apply new materials, new technologies, and marine, space, and aeronautic technologies to marine purposes

Army Research Laboratory U.S. Army Research Office8)

1917Civilian 7,500

Unknown

Materials Science(1 of 12 divisions)

Development of materials having higher or special performance

Air Force Research Laboratory9)19979,500

$3.8 billion

Materials and Manufacturing(1 of 10 divisions)

Development of low-cost military technologies in space and aeronautics

NASAAmes Research Center10)

1939≥420

$30 million

Thermal Protection Materials,Nanotechnology Branch(Total number of research divisions: Unknown)

Development of new technologies

NASAGlenn Research Center(Former Lewis Research Center)11)

19413,300

Unknown

Metals Technologies Branch(Total number of research divisions: Unknown)

Space and aeronautic research

Tables 11 Public research institutes engaged in materials research, other than DOE and NIST. 7) - 11)

Materials Science & Engineering Laboratory–Ceramics Div.

Electronic & Optoelectronic Materials

Characterization Methods

Nanotribology

Data and Standards Technology

Nanomechanical Properties

–Materials Reliability Div.

Microstructure Sensing Group, etc.

–Metallurgy Div.

Electrochemical Processing

Magnetic Materials

Materials Performance

Structure and Characterization

Metallurgical Processing

–Polymers Div.

–NIST Center for Neutron Research (NCNR)

–Center for Theoretical and Computational Materials

Science

Chemical Science & Technology Laboratory (CSTL)–Biotechnology Div.

DNA Technologies Group

Bioprocess Measurements Group

Structural Biology Group

Cell & Tissue Measurements Group

–Process Measurements Div., etc.

Advanced Technology Program (ATP)–Chemistry & Life Sciences Office (CLSO)

Chemistry & Materials Group

Life Sciences Group

–Economic Assessment Office

–Information Technology & Electronics Office, etc.

Table 10 Materials research at NIST research institutes. 4)

References

1) Web page of DOEhttp://www.energy.gov/engine/content.do

2) Web page of the DOE Basic Energy Science Officehttp://www.er.doe.gov/production/bes/BES.html

3) Web page of NSFhttp://www.nsf.gov/

4) Web page of NISThttp://www.nist.gov/

5) FY 2006 BES Budget Request (February, 2005)http://www.er.doe.gov/production/bes/archives/budget/BES_FY2006budget.pdf

6) Web page of DOE (Map of National Labs)http://www.er.doe.gov/sub/organization/map/static-map.JPG

7) Web page of the US Naval Research Laboratoryhttp://www.nrl.navy.mil/

8) Web page of the Army Research Officehttp://www.aro.ncren.net/

9) Web page of the Air Force Research Laboratoryhttp://www.ml.afrl.af.mil/

10) Web page of NASA Ames Research Laboratoryhttp://www.external.ameslab.gov/

11) Web page of NASA Glenn Research Laboratoryhttp://www.nasa.gov/centers/glenn/about/index.html

46


1. Structure of technical institutions in Germany

Figure 1 shows the structure of technical institutes inGermany. Max-Planck-Gesellschaft zur Förderung der

Wissenschaften e.V. (hereafter, the Max Planck Society),the Fraunhofer-Gesellschaft zur Forderung der ange-wandten Forchung e.V. (hereafter, the Fraunhofer-Gesellschaft), and the Hermann von Helmholtz-Gemein-schaft Deutscher Forschungszentren (hereafter, theHelmholtz Association) belong to the Federal Ministry ofEducation and Research. Materials research by publicresearch institutes is mainly done at the laboratories of theMax-Planck Society, the laboratories of the Fraunhofer-Gesellschaft, and at the Forschungszentrum Karlsruhe, allof which belong to the Helmholtz Association. The FederalInstitute for Materials Research and Testing (BAM) con-ducts materials testing and research and belongs to the Fed-eral Ministry of Economy and Technology.

2. Public research institutes of Germany

Table 1 lists representative public institutes of materialsresearch in Germany.1) - 4) Established in 1948, the Max-Planck Society has a total of 78 research institutes, includ-ing the Institute of Metals (Max-Planck-Institut für Metall-forschung) and the Institute of Iron and Steel (Max-Planck-Institut für Eisenforschung GmbH). The Max-Planck Soci-ety is a comprehensive academic organization covering not

47


BundeskanzlerFederal Prime Minister

Bundeskanzleramt (BK) Federal Prime Minister’s Office

Bundesministerium fur Bildung und Forschung (BMBF) Federal Ministry of Education and Research

Bundesministerium fur Wirtschaft und Technologie (BMWi) Federal Ministry of Economy and Technology

Deutche Forchungs-gemeinschaft e.V. (DFG) German Research Association

Max-Planck-Gesellschaft zur Forderung der Wissenschaften e. V. (MPG) Max-Planck Academic Promotion Association

Fraunhofer-Gesellschaft zur Forderung der angewandten Forchung e.V. (FhG) Fraunhofer Applied Research Promotion Association

Hermann von Heimholtz-Gemeinschaft Deutscher Forschungszentren (HGF) Helmholtz German Research Center

Wissenschftsgemeinschaft Gottfried Wilhelm Leibniz (WGL) Union of Gottfried Wilhelm Leibniz Academy

¨

¨

¨

Fig. 1 Structure of technical institutes in Germany.

Name of InstituteEstablished

Staff (No. of Researchers)

Budget Main ResearchRatio of

National andFederal Grants

Outline

Max Planck 1948

12,300(4,200) 1,330 mil.

Fundamental research

About 95%Subdivided into 78 laboratories by field (polymers, metals, iron and steel, physics, and history). Five of them specialize in materials research.

Fraunhofer 1949

12,500 1,000 mil.Applied research

About 40%

More than 80 research units, including the 57 Fraunhofer laboratories. Materials research at six research units, including Manufacturing Engineering and Applied Materials Research

Karlsruhe 1956

3,800(1,420) 294 mil.

Fundamental/Applied research

About 70%

Invested by the Federal government (9/10) and by the Baden-Württemberg State (1/10). Materials research at two laboratories: Nanotechnology and Materials Research (22 laboratories in total)

BAM 1956

1,640(About 700)

113 mil.(FY2003 budget)

Fundamental testing

About 80%Serves as a basic research institute and as a test institute. Mainly engaged in the fabrication of standard samples and the survey of fractured materials.

Table 1 Number of researchers and research budgets of German public research institutes.

01 Public Research Institutes for Materials Research in Japan, USA and EU

Section 3. Germany


only science, but also biology (426 divisions), physics (379divisions), astronomy and astrophysics (105 divisions), his-tory and social science (98 divisions), as well as chemistry(96 divisions). This Society receives the largest grant ofabout 95% from the Federal government of all publicresearch institutes in Germany and conducts mainly funda-mental research. The percentage break down of expendi-tures from the FY2004 budget of the Association are 40%for labor, 21% for maintenance, and 13% for projects asshown in Figure 2.

Figure 3 compares the funds and research themes in theMax-Planck Society. Since the Fraunhofer-Gesellschaftmainly conducts applied research, the share of publicinvestment by the Federal government is no more thanabout 40%. Figure 4 shows the transition of income sources

of the Fraunhofer-Gesellschaft over time. Income fromindustry has almost doubled in the last decade. Figure 5shows the number of personnel at the Fraunhofer-Gesellschaft by research field: the Materials and Compo-nents field ranks third with about 1,300 staff, after theInformation and Communication Technology field and theMicroelectronics field. Figure 6 shows the breakdown of

48


Personnel costs

Allocations

Construction expenditure

Other investments

Project funding

Other operating coasts

40%

21%

13%11%

8%7%

Fig. 2 Expenditure by the Max-Planck Society in FY2004. 1)

Fig. 3 Comparison of research funds and themes between Max-PlanckSociety and Fraunhofer-Gesellschaft. 2)

Fig. 4 Income sources of Fraunhofer-Gesellschaft. 2)

Fig. 5 Number of personnel at Fraunhofer-Gesellschaft by research field(2003). 2)

Fig. 6 Breakdown of income sources of Fraunhofer-Gesellschaft. 2)

Research Field PercentageStructure of matter

Structure of matterEarth and Environment

Sustainability and TechnologyAtmosphere and Climate

HealthBiomedical ResearchMedical Engineering

EnergyNuclear FusionNuclear Safety ResearchEfficient Energy Conversion

Key TechnologiesMicrosystem TechnologiesNanotechnologyScientific Computing

10%

25%

15%

25%

25%

Table 2 Percentages of research fields of Forschungszentrum Karlsruhe. 3)

income sources of the Fraunhofer-Gesellschaft. Theresearch expenses are equally split between basic funding,through contracts with industry, and the federal and localgovernments.

The Forschungszentrum Karlsruhe was established in1956. Grants account for about 40%, of which 90% comefrom the federal government and 10% from the Baden-Württemberg State. The Forschungszentrum Karlsruhe isworking hard not only on basic research but also on appliedresearch, and has about 650 joint projects with industry.Table 2 shows the percentage break down of research fieldsof the Forschungszentrum Karlsruhe. Earth and Environ-ment, Energy, and Key Technologies (including Nanotech-nology) account for 25% each.

BAM was reorganized into the present laboratory orga-nization in 1954. Serving as both a basic research instituteand as a testing institute, BAM has produced approximate-ly 450 papers, 900 lectures (including short courses), and6,000 test reports. The fabrication of standard samples andsurvey of accidents such as fractures are important compo-nents of their work. In the field of nanotechnologies, BAMevaluates nanomaterials. The total number of personnel is1,670, including 1,174 permanent staff (60%).

About 200 research projects are currently in progress atBAM. As Table 3 shows, they can be classified into fivefields: Technical and public safety, Materials technologies,Analytical chemistry, Technical and scientific service func-tion, and Environmental compatibility. Technical and pub-lic safety accounts for as much as 40% of the total numberof researchers, followed by materials technologies with20%. Table 4 gives the percentages of researchers by activ-ities: 59% are in research and development, 20% in adviceand information, and 14% in testing, analysis, andapproval.

3. Materials research by German public research institutes

Tables 5 to 8 show the materials research divisions ofthe Max-Planck Society, the Fraunhofer-Gesellschaft, theForschungszentrum Karlsruhe, and BAM.

The Max-Planck Society conducts research on metals,iron and steel, colloids, biomaterials, nanomaterials, and

polymers at five laboratories. The Fraunhofer-Gesellschaftconducts materials research at the Materials and Compo-nents Institutes and the Nanotechnology Institutes. TheForschungszentrum Karlsruhe, organized from 11 researchcenter programs and 22 laboratories, conducts R&D onnanotechnologies and materials structures. BAM special-

49


Research Field ResearchersTechnical and public safetyMaterials technologiesAnalytical chemistryTechnical and scientific servicesEnvironmental compatibility

41%20%17%12%10%

Table 3 Percentages of BAM researchers by field. 4)

Activities ResearchersResearch and developmentAdvice and informationTesting, analysis, approvalInfrastructure

59%20%14%7%

Table 4 Percentages of researchers at BAM by work. 4)

Max-Planck-Institut für Metallforschung – Materials synthesis and microstructure design – Structural materials and thin film systems – Theory of inhomogeneous condensed matter – Metastable and low-dimensional materials – Mechanics and mechanical properties of thin films,

dynamic characteristics of smart materials, materials failure mechanisms

– Phase transformations; thermodynamics and kinetics

– Microstructures and interfaces – Modern magnetic materials: analysis and synthesis

of modern magnetic materials – Physical understanding of the regulation of adhesive

cell contacts and cell mechanics; consequences fordiseases

Max-Planck-Institut für Eisenforschung GmbH – Computational materials design – Interface chemistry and surface engineering – Materials technology – Microstructure physics and metal forming – Metallurgy and process technology

Max-Planck-Institut für Kolloid und Grenzflächenforschung – Colloid Dept.

Polymer dispersionsBioorganic-synthetic hybrid polymers, others

– Theory Dept.Molecular motors and active systemsMembrane adhesion, polyelectrolytes, others

– Interfaces(Quasi) Planar interfaces-fluid interfacesNon-planar interfaces, solid interfaces, others

– BiomaterialsMicroscopic fracture and deformation mecha-nisms of mineralized tissuesComputer modeling of mechanics, growth andadaptation of biomaterialsBiotemplatingMicroscopic fracture and deformation mecha-nisms of mineralized tissues, others

Max-Planck-Institut für Mikrostrukturphysik – Experimental Department 1

Correlations of magnetic film properties withstructure and morphology, others

– Experimental Department 2Quantum structures, ordered porous materialsnanowires, nanoengineering of functional oxides0D and 1D nanomaterials, others

– Theory DepartmentMagnetic properties and spin-dependentscattering in ferromagnets, others

Max Planck Institute for Polymer Research – Polymer physics – Material science – Polymer theory – Synthetic chemistry, others

Table 5 Materials research by Max-Planck Society. 1)

izes in materials research, testing, and accident surveys.

4. Conclusion

In Germany, materials research is conducted mainly atthe Max-Planck Society, Forschungszentrum Karlsruhe,and the Fraunhofer-Gesellschaft. The former two organiza-tions specialize in fundamental research, while Fraunhofer-Gesellschaft mainly conducts applied research. Anotherinfluencial organization, BAM, specializes in testing andsafety. Applied research activities tend to be financed bythe private sector.

References

1) Web page of the Max-Planck Societyhttp://www.mpg.de/

2) Web page of the Fraunhofer-Gesellschafthttp://www.fraunhofer.de/fhg/EN/index.jsp

3) Web page of the Forschungszentrum Karlsruhehttp://www.fzk.de/

4) Web page of the Federal Institute for Materials Research andTesting (BAM)http://www.bam.de/

50


Materials and Components Institutes (11 units) – Applied polymer research – Ceramic technologies and sintered materials – Manufacturing engineering and applied materials

research – Mechanics of materials – Silicate research, others

Nanotechnology Institutes (17 units) – Ceramic technologies and sintered materials – Interfacial engineering and biotechnology – Environmental, safety and energy technology, others

Polymer Surfaces Institutes (7 units) – Electron and plasma technology, others

Surface technology and photonics (6 units) – Applied optics and precision engineering – Electron beam and plasma technology – Laser technology – Material and beam technology – Physical measurement techniques – Thin films and surface engineering

Table 6 Materials research by Fraunhofer-Gesellschaft. 2)

Research Center Programs (11 programs) – Nanotechnology

Electron transport in nanoscale systemsNanostructured materials and low dimensionalsystems with new functionalities

– Microsystem technologiesManufacturing / system integrationmaterials development, others

– Structure of matter – Sustainability and technology – Scientific computing, others

Scientific Institutes (22 laboratories) – The Institute of Nanotechnology

Molecular electronicsNanostructured materialsStructure / property correlations in nanoscalesystems

– The Institute for Materials ResearchApplied materials physicsMaterials and structural mechanicsMaterials processing technology

– The Institute for Solid-State PhysicsUnconventional superconductivity close to thetransition to magnetic order, others

– The Institute for Synchrotron Radiation – The Institute for Instrumental Analysis, others

Table 7 Materials research by Forschungszentrum Karlsruhe. 3)

Analytical chemistry, reference materialsChemical safety engineeringContainment systems for dangerous materialsEnvironmental compatibility of materialsMaterials engineering, safety of structuresPerformance of polymeric materialsMaterials protection, non-destructive testingInterdisciplinary scientific and technological operations

Table 8 Materials research by BAM. 4)

1. Public materials research institutes of France

The budget of the French Space Development Organiza-tion (CNRS: Centre National de la Recherche Scientifique)accounts for about 25% of the total civil R&D budget,which amounts to 90,400 million dollars, followed by inde-pendent research institutes, the French Space Agency(CNES) with about 1% and the Atomic Energy Agency(CEA) with about 10%.1), The research systems of CNRSand CEA, regularly publish papers on the subject of materi-als. These institutions` research personnel and budget arecompared in Table 1, not inclusive of CNES. CNRS andCEA conduct fundamental and applied research respective-ly.

2. Materials research by CNRSCNRS was established in 1939 and has been part of the

Ministry of Research (MRT: Ministére de la Rechererche etde la Technology) since 2000. Figure 1 shows the incomesources of CNRS. The subsidies from the Ministry of Tech-nology and Research account for about 77% and the VATcompensatory subsidies account for 11%.The CNRSreceives funding from other institutions through researchcontracts and royalties of patent rights, which account forabout 12%.

Figure 2 shows the percentage breakdown of expensesby CNRS. Salaries for research units (62%) account for thelargest share of the organization’s expenses. About 24% ofthe expenses are spent on laboratories and research pro-grams, and 14% for support work.

Figure 3 shows the CNRS organization. CNRS is orga-nized into eight research divisions (Engineering Sciences

51


Research InstituteNo. of

ResearchersBudget

(¥100 mil.)Main Research Remarks

CNRS (Centre National de la Recherche Scientifique)

26,000 3,149 Fundamental 8 research divisions subdivided into 1,260 small units and 18 regional offices. Materials research at about 90 units.

CEA (Commissariat à l'Energie Atomique)

15,024 3,645 Applied Three fields: Energy, IT and health technologies, and military

Table 1 Numbers of researchers and budgets of CNRS and CEA in France. 1), 2)

1. Government subsidies: 1,938.753 million euros2. VAT compensatory subsidies: 278.637 million euros3. Own funds: 315.389 million euros

Fig. 1 CNRS income sources (2002). 1)

1. Activity conducted by the research units: 284.258 million euros

2. Common actions and backup functions, support for research: 64.244 million euros

3. Collective investment: 108.677 million euros

Fig. 2 Breakdown of CNRS expenses (2002). 1)


Section 4. France

Tomoaki HyodoInternational Affairs Office, NIMS

and other divisions). These research divisions are subdivid-ed into 1,256 smaller units. Table 2 lists the number ofunits classified by field. About 90 research units havematériaux (material), métallurgie (metallurgy), nano,polymères (polymer), céramiques (ceramics), or molécule(molecule) in their names. From this, about 7% of theresearch units are estimated to be involved in the researchof materials.

3. Materials research by CEA

CEA conducts applied R&D in their civil and militaryresearch units.2) Table 3 shows the CEA income data in2003. The share of subsidies is approximately 60% for civilresearch and 98% for military research. Of about 40research divisions, seven divisions relate to materialsresearch.

References

1) Web page of CNRS: http://www.cnrs.fr/2) Web page of CEA: http://www.cea.fr/

52


Scientific Departments

Board of Trustees Chairman

Research Units

Directorate-GeneralMission to improve the role of women at the CNRS

Studies andProgrammingDepartment

InternationalRelationsDivision

IndustrialAffairs

Delegation

Detense andSafety Official

Hygiene andSecurityService

Scientificand Technical

InfomationDelegation

Departmentin charge of

Relations with Higher Education

Organizations

MediatorCommittee for the History of the CNRSNational

Committee on scientific research

Nuclearand Particle

PhysicsIN2P3

Communicationand Information

Science andTechnology

ChemicalSciences

LifeSciences

Sciences ofthe Universe

and INSU

EnginearingSciences

RegionalOffices

SecondaryAccoutants

PrincipalAccounting

Agency

Officeof the

Secretary-General

Humanitiesand SocilSciences

Physical Sciences andMathematics

EthicsCommittee

Fig.3. CNRS organization chart. 1)

Division UnitsNuclear and Particle Physics – IN2P3Physical Sciences and MathematicsCommunication and Information Science and TechnologyEngineering SciencesChemical SciencesSciences of the UniverseLife SciencesHumanities and Social SciencesOutside departments and institutes

Total

2115083

9720210524334411

1,256

Table 2 Numbers of research units by field. 1)

ItemAmount

1 mil.Percentage

%

Civil (Financement Civil)

Subsidies (Subvention)

For research (Recherche)

For industry (Industrie)

External funds (Recettes

externes)

Other

Total of civil

Military (Financement Défense)

Subsidies (Subvention)

Other

Total of military

Total

486

414

485

138

1,523

1,265

25

1,290

2,813

31.9

27.2

31.9

9.1

100.0

98.0

2.0

100.0

100.0

Table 3 CEA income in FY2003. 2)

1. Profile of CSIC

CSIC is Spain’s largest public institute for basicresearch, supervised by the Ministry of Education and Sci-ence (Ministerio de Educación y Ciencia).1) This instituteconsists of 120 centers as listed in Table 1. Among the pub-lic research institutes of Spain, CSIC specializes in basicresearch whereas Centro de Investigaciones Energéticas,Medioambientales y Tecnológicas (CIEMAT) specializesin applied research.

CSIC operates according to the basic plan, called“National Plan for Scientific Research and TechnologicalDevelopment”, which is enacted every few years. Sincenanotechnology research began quite recently, its activitiesare not based on the National Act, but will be included in

the next national plan. The National Plan is determined by12 members of a commission, of whom 6 or 7 are scientists(university professors or researchers at private enterprises).

The number of personnel at CSIC is 11,115 in total, ofwhom 2,063 are permanent staff. The general budget ofCSIC is 110.9 million euros, of which about 11.6 millioneuros are spent on materials research.

2. Materials research at CSIC

At CSIC, the nine laboratories listed in Table 2 conductmaterials research. The total number of personnel includingpostdoctoral researchers is 1,282. The map of Spain in Fig-ure 1 shows the locations of the laboratories: five for mate-rials research in Madrid and one in each of Barcelona,Zaragoza, Seville, and San Sebastian.

Table 3 gives the characteristics of the nine laboratories.Of the five laboratories in Madrid, four (CENIM, ICV,ICTP, and IETCC) are involved in research of metals,ceramics, polymers, and structural materials. These labora-tories support the economy of Spain through close linkswith industry. The laboratories in Barcelona (ICMAB),Madrid (ICMM), and Seville (ICMS) are more orientedtoward basic research, and those in Barcelona and Sevilleare closely linked with universities. Both the laboratories inZaragoza (ICMA) and San Sebastian (UFM) also haveclose links with universities.

Table 4 lists the numbers of personnel at the nine labora-tories. Among the seven laboratories which give the num-ber of personnel on their Web page, ICMS (Seville) has the

53


Research Division Centers

Humanities and Social Sciences

Biology and Biomedicine

Natural Resources and Environment

Agricultural Sciences

Physics

Material Science and Technology

Food Science and Technology

Chemistry

Other

Total

18

18

17

12

19

9

5

11

11

120

Table 1 Number of research centers in each division of CSIC. 1)

i) Centro Nacional de Investigaciones Metalúrgicas (CENIM) Madrid

ii) Instituto de Cerámica y Vidrio (ICV) Madrid

iii) Instituto de Ciencia de Materiales de Aragón (ICMA) Zaragoza

iv) Instituto de Ciencia de Materiales de Barcelona (ICMAB) Barcelona

v) Instituto de Ciencia de Materiales de Madrid (ICMM) Madrid

vi) Instituto de Ciencia de Materiales de Sevilla (ICMS) Sevilla

vii) Instituto de Ciencia y Tecnología de Polímeros (ICTP) Madrid

viii) Instituto de Ciencias de la Construcción “Eduardo Torroja” (IETCC) Madrid

ix) Instituto de Física de Materiales (UFM) San Sebastian

Table 2 CSIC laboratories engaged in materials.


Section 5. Spain

Tomoaki HyodoInternational Affairs Office, NIMS

fewest with 69 and ICMM (Madrid) has the most with 340.CENIM (Madrid: metal research) and IETCC (Madrid:steel structure research) have many research assistants thatare not considered technicians. The seven laboratories withpublished numbers of personnel feature a high percentageof students, ranging from 11% to 40% of total staff. Someresearchers that work for CSIC also teach at universities asprofessors. This strong linkage produces close ties betweenstudents and CSIC.

Some institutes in CSIC in part are supported by univer-sities, while other CSIC institutes are sponsored by CSICalone. Shared sponsorship with universities are more com-mon among CSIC institutes due to closer ties betweenCSIC and universities in recent history.

3. Research systems of representative CSIC materialslaboratories

This section details the organizations and budget alloca-tion of the Materials Science Institute of Barcelona(ICMAB: Instituto de Ciencia de Materiales de Barcelona),the Materials Science Institute of Madrid (ICMM: Institutode Ciencia de Materiales de Madrid), and the MadridNational Central Institute of Metals (CENIM: CentroNacional de Investigaciones Metalúrgicas).

3.1 Materials Science Institute of Barcelona (ICMAB)2)

The Materials Science Institute of Barcelona has 194personnel (including 40 full-time researchers). The totalbudget is 7.59 million euros. Of this budget, 58% comesfrom subsidies, 13% from the National Plan, 10% fromcompetitive grants, and 5% from companies.

The research activities of the Barcelona Institute areevaluated by the International Scientific Committee andFAME as external organizations. Through an interviewwith the director of each CSIC laboratory, the former takesone week every four years to scrutinize the contents ofresearch and issues an evaluation report. FAME, initiatedin 2004 and organized from 20 groups in European coun-tries, discusses Interconnection and Integration and spends5 million euros on Integration with representatives from thecountries at the same table.

The Barcelona Institute established a new organizationcalled MATGAS. CSIC’s mission is basic research butMATGAS will focus on applied research (Gases and Mate-rials) in a new building next to the Barcelona Institute.With 66% investment from a private company, CarburosMetalicos (60% investment from U.S. Air Products and

54


San Sebastian

Madrid

BarcelonaZaragoza

Fig. 1 Locations of CSIC laboratories for materials research. 1)

Classification Laboratory City Characteristics

Specialized in metal researchSpecialized in ceramics researchLinked with Universitat Autònoma de MadridSpecialized in polymer researchSpecialized in steel structure researchLinked with Universitat Autònoma de BarcelonaThe most specialized in basic research among the five laboratories in MadridLinked with Universidad de SevilleLinked with Universidad de ZaragozaLinked with Universidad del País Vasco and two other universities

Madrid

Madrid

Madrid

Madrid

Barcelona

Madrid

Seville

Zaragoza

San Sebastian

CENIM

ICV

ICTP

IETCC

ICMAB

ICMM

ICMS

ICMA

UFM

Close links with industry

More basic research

Other

Table 3 Characteristics of CSIC laboratories engaged in materials research. 1)

Laboratory CityBudget

1 mil. (¥100 mil.) Professors Researchers Other Total

Regular staff Contractstaff

Postdoctoral/students/visitors

Total

i) CENIM

ii) ICV

iii) ICMA

iv) ICMAB

v) ICMM

vi) ICMS

vii) ICTP

viii) IETCC

ix) UFM

Madrid

Madrid

Zaragoza

Barcelona

Madrid

Seville

Madrid

Madrid

San Sebastian

8.11 (10.9)

Unknown

3.81 (5.1)

7.59 (10.2)

13.43(*) (18.1)

Unknown

2.22(*) (3.0)

8.95(*) (12.1)

Unknown

7

11

10

20

6

6

44

30

40

74

9

29

83

12

17

35

8

?

95

134

53

67

129

23

?

130

Not on web page

Not on web page

52

33

43

50

21

9

63

86

93

84

161

25

39 ?

40

272

179

194

340

69

134

233

Budget: FY2002 data marked * and FY2003 data not, Visit: Includes laboratory-permitted stay.

43

Table 4 Enrollment at nine laboratories engaged in materials research. 1)

Chemicals), 22% from CSIC, and 12% from the MaterialsScience Institute of Barcelona, the new building was com-pleted within 2004 and research equipment have beenbrought in from the beginning of 2005 to prepare for open-ing in June 2005.

3.2 Materials Science Institute of Madrid (ICMM)3)

The Materials Science Institute of Madrid had the great-est enrollment of 340 among the CSIC laboratoriesengaged in materials research, of who about 37% were per-manent staff.

Of the FY2002 total budget of this laboratory amountedto 13.4 million euros, of which 61.2% came from CIS sub-sidies and 1.7% from companies.

Figure 2 shows the percentages of expense items in theFY2002 budget of this laboratory. Of the 13.4 millioneuros in total, 51.6% was spent on labor and 36.9% wasspent on research project.

3.3 Madrid National Central Institute of Metals (CENIM)4)

The Madrid National Central Institute of Metals has antotal staff of 272. The total number of professors andresearchers combined is 51. Seven professors and 27researchers of the 51 are tenured scientists.

The number of projects almost doubled from 68 (1994)to 130 (2003) in a decade. As Figure 3 shows, however,CENIM was funded one-third by national institutions(Spanish Government) and one-third by private companies.The European Union sponsors about one-sixth of the pro-jects.

The FY2003 budget of this laboratory was 8.1 millioneuros, of which about 60% were labor expenses.

4. Conclusion

(1) Of the 120 research centers of CSIC, nine are engagedin materials research. In particular, the three laboratories ofICMAB (Barcelona), ICMM (Madrid), and ICMS (Seville)are specialized in basic research. MATGAS was recentlyestablished with links to the industry entered service inJune 2005. ICMM (Madrid) has a total of 340 staff, whichis greater than those of eight other CSIC research centersengaged in materials research.(2) CENIM (metals), ICV (ceramics), ICTP (polymers),and IETCC (steel structures) in Madrid are research centersthat are involved in research through close links withindustry.

References

1) CSIC Annual Report 2002.2) Web page of Instituto de Ciencia de Materiales de Barcelona

(ICMAB)http://www.icmab.es/org/eng/index.html

3) Web page of Instituto de Ciencia de Materiales de Madrid (ICMM)http://www.icmm.csic.es/eng/

4) Web page of Centro Nacional de Investigaciones Metalúrgicas(CENIM)http://www.cenim.csic.es/

55


8×106

Euros

Salary51.6% Research

project38.9%

Total : 13,434,154 Euros

Ordinarybudget

5.0%

Salarios d

e Personaly S

.S.

Salaries Presu

puesto O

rdinario

Ordinary Budget

Ayudasy

Acciones E

specia

les

Extraordinary

Budget

Proyecto

s de In

vestig

acion

Reseach

Projects

Specialbudget

6.5%

6×106

4×106

2×106

8×106

6×106

4×106

2×106

Fig. 2 Breakdown of FY2002 budgets of Materials Science Institute ofMadrid. 3)

Fig. 3 Percentages of research projects at Materials Science Institute ofMadrid. 3)

In Chap.2, section 1, the nanotechnology research poli-cies of Japan, the USA, the EU, Germany, France, and theUK were outlined. This section introduces nanotechnologyresearch institutes established by new national programs ofthese countries. One of the greatest features of nanotech-nology R&D is the convergence of multidisciplinaryresearch fields in the nanoscale area. To promote such inte-gration, priority is given to building a network consisting ofcore infrastructure of research information and its sur-rounding networks (also called a cluster or consortium).Such a system is designed to accelerate commercializationand industrialization by linking industry, academia, and thegovernment.

1. New nanotechnology research institutes in Japan

In Japan, based on the Second Science and TechnologyBasic Plan, new policies were initiated in the field of nan-otechnology and materials, one of the four priority fields,and new technology research bases were established inJapan. The main ones are as follows.

1.1 Nanotechnology Support ProjectTo support all the researchers of industriay, academia,

and government in terms of both information and facility,this project was initiated by the Ministry of Education, Cul-ture, Sports, Science and Technology in FY2002.1) TheNanotechnology Researchers Network Center of Japan,established in the National Institute for Materials Science,is in charge of information support. This Center dissemi-nate information by website and e-mail newsletters, holdssymposia and seminars, and exchanges researchers withother countries. For facility support, the following 14research institutes provide external users with the opportu-nities to use four kinds of large-scale cutting-edge facilitiesfree of charge.

i) Ultrahigh-voltage transmission electron microscopes• National Institute for Materials Science• Institute for Materials Research, Tohoku University• Research Center for Ultra-High Voltage Electron

Microscopy, Osaka University• Research Laboratory for High Voltage Electron

Microscopy, Kyushu Universityii) Nano foundries

• National Institute of Advanced Industrial Science andTechnology

• Nanotechnology Research Laboratory, Waseda Univer-sity

• Quantum Nanoelectronics Research Center, Tokyo Insti-tute of Technology

• Research Center for Nanodevices and Systems, Hiroshi-ma University

• Nanoscience and Nanotechnology Center, Osaka Uni-versity

iii) Synchrotron radiation• SPring-8

Japan Synchrotron Radiation Research Institute (JASRI)Japan Atomic Energy Agency (JAEA)National Institute for Materials Science

• SR Center, Ritsumeikan Universityiv) Molecular synthesis and analysis• Institute for Molecular Science, National Institutes of

Natural Sciences• Institute for Chemical Research, Venture Business Lab-

oratory, and Advanced Research Institute of NanoscaleScience and Engineering, Kyoto University

• Graduate School of Engineering, Kyushu UniversityTable 1 lists data on facility-sharing support provided in

FY2003 (2.3 billion yen funded by the Ministry of Educa-tion, Culture, Sports, Science and Technology).

56


UniversityPublic

InstituteCompany Total

Ultrahigh-voltage

transmission

electron

microscope

group

Nano foundry

group

Synchrotron

radiation group

Molecular

synthesis and

analysis group

Total

97

106

93

157

453

(81)

(66)

(92)

(94)

(333)

23

49

16

39

127

(20)

(16)

(13)

(11)

(60)

35

102

30

57

224

(30)

(34)

(10)

(38)

(112)

155

257

139

253

804

(131)

(116)

(115)

(143)

(505)

Table 1 Nanotechnology Support Project.Support for facility-sharing in FY2003

( ): FY2002

Chapter 2. New Nanotechnology ResearchInstitutes in Japan, USA and Europe


1.2 Knowledge Cluster InitiativeTo strengthen global competitiveness while respecting

the independence of local governments, the Ministry ofEducation, Culture, Sports, Science and Technology initiat-ed the Knowledge Cluster Initiative in FY2002.2) With uni-versities and public research institutes as the core, this pro-ject is organized from related research institutes and R&D-type enterprises. In the three-year period until FY2004, 18clusters were selected and R&D has been conducted insome of the four priority fields. Of the cluster areas, nan-otechnology R&D has been conducted in the followingfour (core research institutes in parentheses):• Toyama and Takaoka Area: Toyama Medical-Bio Clus-

ter (Japan Advanced Institute of Science and Technolo-gy Hokuriku, Toyama Medical and Pharmaceutical Uni-versity, Toyama University, Toyama Prefectural Univer-sity, and Toyama Industrial Technology Center)

• Nagano and Ueda Area: Nagoya/Ueda Smart DeviceCluster (Shinshu University)

• Nagoya Area: Nagoya Nanotechnology ManufacturingCluster (Nagoya University and Nagoya University ofTechnology)

• Kyoto Area: Kyoto Nanotechnology Cluster (KyotoUniversity)

1.3 Cooperation for Innovative Technology and AdvancedResearch in City Evolutional Areas (CITY AREA)

To produce new technology seeds, create new business-es, and cultivate local industries based on R&D by usinglocal characteristics and the wisdom of universities andother organizations, the Ministry of Education, Culture,Sports, Science and Technology initiated this project inFY2002.3) Local voluntary business plans are solicited andareas for this project are selected. Here, “city areas” arecore cities of prefectures (including ordinance-designatedcities) and their surroundings having R&D potential. Theyare substantially areas where universities and other publicresearch institutes exist and core organs can be used as pro-ject entities. The areas can be classified into three types byproject development pattern:

i) Linkage infrastructure establishment type: Mainly sub-ject research and research exchange aiming at establishingindustry-academia-government infrastructure

ii) General type: Mainly joint research for creating newtechnical seeds in specific fields (includes some industry-academia-government projects)iii) Achievement cultivation type: Many industry-acade-

mia-government projects done mainly for joint researchand achievement cultivation.

In the three-year period until FY2004, 37 areas wereselected where R&D is being conducted in some of the fourpriority fields. Nanotechnology R&D is being done in thefollowing eight (core research institute in parentheses).

i) Linkage infrastructure establishment type: Noneii) General type

• Iwate Prefecture: Kitakami River Area – “High FunctionManifestation R&D for Triazinethiol Organic NanothinFilm” (Iwate University)

• Gunma Prefecture: Kiryu and Ota Area – “R&D forNext-generation Processing” (Gunma University)

• Fukui Prefecture: Fukui Central Area – “Developmentof Energy-related Functional Materials Creation Tech-nology by Nanoplating Technology” (Fukui University,Fukui University of Technology, Fukui National Collegeof Technology, Industrial Technology Center of FukuiPrefecture)

• Mie Prefecture: Mie and Ise Bay Area – “Creation ofNew Functional Materials for Next-generation Displayand Their Applied Equipment” (Mie University)

• Hyogo Prefecture: Harima Area “Development andIndustrialization of Extremely Thick DLC and High-speed Nitriding Technologies” (University of Hyogoand Toyota Technological Institute)

• Wakayama Prefecture: Wakayama City Area “Develop-ment of Organic Materials for Next-generation Electron-ic Devices” (Industrial Technical Center of WakayamaPrefecture)

iii) Achievement cultivation type• Osaka Prefecture: Osaka/Izumi Area “Nanostructure

Photonics and Its Applications” (Osaka Prefecture Uni-versity, Osaka University, and Technology ResearchInstitute of Osaka Prefecture)

• Kumamoto Prefecture: Kumamoto Area “Developmentof Biocompatible Microsensors (Smart Microchips)”(Kumamoto University)

1.4 21st Century COE ProgramTo form the world’s highest-level research and educa-

tion bases for improving research levels and creatinghuman resources leading the world according to “Universi-ty Policies of Structural Reform” (June 2001), the Ministryof Education, Culture, Sports, Science and Technology ini-tiated this program in FY2002.4) The Japan Society for the

57


Strategic Goal Research Area

Creation of ultrafast, ultralow power, super-performance nanodevices and systemsCreation of nanodevices/system based on new physical phenomena and functional principlesNano factory and process monitoring for advanced information processing and communicationCreation and application of nano-structural materials for advanced data processing and communicationCreation of bio-device and bio-systems with chemical and biological molecules for medical useCreation and application of “soft nano-machine”, the hyperfunctional molecular machineCreation of novel nano-material/system synthesized by selforganization for medical useCreation of nano-structured catalysts and materials for environmental conservationDevelopment of advanced nanostructured materials for energy conservation and storageCreation of innovative technology by integration of nanotechnology with information, biological, and environmental technologies

Creation of nanodevice and nanomaterials systems to overcome integration and function limits in information processing and communication Creation of Nanodevice / Material / System for Overcoming Integration / Function Limits in Data Processing and Communications Creation of Functional Materials/ System that Utilize Nano Biotechnology for Realizing a Noninvasive Medical Treatment System

Creation of Nano Materials/ System for Realizing Environmental Conservation and Advanced Energy Recycling to Minimize Stress on the Environment

(Convergence of three fields)

Table 2 Research areas of virtual laboratories by nanotechnology field.5)

Promotion of Science set up the 21st Century COE Pro-gram to examine and evaluate this program and makegrants to subsidize the formation of program bases.

COE categories under this program do not include thenanotechnology and materials field. However, about 40COEs related to this field were selected in the three-yearperiod until FY2004.

1.5 Nanotechnology Virtual LaboratoriesNanotechnology also serves as the foundation for the

three other priority fields of life science, information, andthe environment, so the Japan Science and TechnologyAgency initiated this program in FY2002. As the nameindicates, there are no physical laboratories; this is a newtype of research program to promote academic research. AsTable 2 shows, strategic goals were set respectively in thethree fields and 10 research areas were defined underthem.5) In each area, a research team is integrated from theresearch administrator responsible for its operations andalso research groups. Each research group conductsresearch as a member of the research institute. For interre-lations, these research areas are physically operated andconnected by information exchange, collaboration, jointsymposia, and area meetings spanning the boundaries ofresearch areas.

2. New nanotechnology research institutes in the USA

To promote discovery and technological innovation, theNNI has been apportioning budgets to a wide range of spe-cial fields (universities and other research organs: 2/3, gov-ernmental research organs: 1/4, small enterprises and pri-vate divisions: the rest). Research can be roughly classifiedinto individual research, team research, and center research.Team research is represented by the Nanoscale Interdisci-plinary Research Teams (NIRT) of the NSF. The NSF allo-cates at least 20% of the NNI investment to research com-bined from different fields. For center research, centerswith human resources and infrastructures are being set upin a wide range of fields to cultivate human resources,industry-academia-government linkage, and internationaljoint research. The annual amount invested by the NNI isabout 2 million dollars, highlighting the policies.

Table 3 lists the nanotechnology research centers of theNNI.6) The NSF supports the Nanoscale Science and Engi-neering Centers (NSECs), the National NanotechnologyInfrastructure Network (NNIN), and the Network for Com-putational Nanotechnology (NCN). Most research centersof the NSF are in universities, and the departments andresearch centers have a tightly-knit relationship: a professorbelongs to only one department but may belong to severalcenters. (The professor is paid by the department but fund-ed by the centers for research.) There are also centers ofNASA, DOE, and DOD. Regarding the DOE in particular,the Molecular Foundry of the Lawrence Berkeley NationalLaboratory and other infrastructures are actively beingextended.

The Materials Research Science & Engineering Center(MRSEC, 28 centers) and the Nanobio Technology Center

(NBTC, 6 centers) do not belong to the NNI but are sup-ported by the NSF, conducting similar activities to the nan-otechnology research centers (only NBTC of Cornell Uni-versity is positioned as an NNI center). With a mission ofconducting R&D for nanoscale metrology, databases, andstandardization, the U.S. National Institute of Standardsand Technology (NIST) established the Advanced Mea-surement Laboratory for advanced metrology. This labora-tory has the best environment for equipments (temperature,humidity, and vibration) in the world. In addition, the Cali-fornia Nanosystems Institute (CNSI) was established inUCLA and UCSB as nanotechnology research centers sup-ported by the state government.

The future trends of the nanotechnology research centersare described next.

2.1 National Nanotechnology Infrastructure Network(NNIN)

The NNIN was initiated in January 2004, inheriting theNational Nanofabrication Users Network (NNUN) orga-nized from common facilities of five universities, includingthe Nanoscale Science & Technology Facility (CNF) ofCornell University and the Stanford Nanofabrication Facili-ty (SNF) of Stanford University. The NNIN consists of 13universities, with fairness in race and area considered.7)-11)

Figure 1 shows the percentages of application fields in2003 when the institution was still the NNUN (5 universi-ties). The numbers of users are as follows:• Total number of users: about 2,000

(Including about 700 at CNF and about 600 at SNF)• Graduates: 1,050 or more• Postdoctoral or higher researchers: More than 250• Enterprises: About 350 (including 158 at ventures)• Other (undergraduates, public institutes, and foreign

countries): More than 250• Users from 33 states• External users: About 50%• Average payment by user: 4000 dollars/yearOther characteristics of users are as follows:• The average annual rate of increase was about 20% in

the past, and exceeds 50% among corporate users.• Users are increasing in all fields but the rate of increase

is especially remarkable in materials (especially fornanoelectronics) and its process and evaluation.

• Since 250 new users are trained at the CNF alone everyyear, the NNIN may be a training facility.

Since users at universities account for about 50%, theNNIN is certainly very advantageous for the member uni-versities.

At the time of the NNUN, NSF support for operationsincreased from 2.4 million dollars (1998) to 6 million dol-lars (2003). In the five years of the NNIN, the amount isexpected to exceed 70 million dollars or 14 million dol-lars/year on average. Note that grants from the NSF tothese research bases are not used to construct buildings; inmany cases, construction expenses are paid from grants bythe state governments or donations. For example, DuffieldHall of Cornell University cost 62.5 million dollars to buildand was paid entirely from donations by graduates. Thisalso applies to NSECs and NCN.

58


Not only the NNIN but U.S. universities generally tendto promote equipment-sharing and reduce maintenance andmanagement costs mainly because professors try to employas many researchers as possible. They prefer equipmentthat is very general but not used often to be provided, sothat they can share the equipment and pay only usagecharges. Technicians handling the shared equipment arepaid from the facility charges.

Regarding the service quality, if the NNIN is comparedwith the shared facilities of the aforementioned Nanotech-nology Support Project of Japan (2.3 billion yen support inFY2003, support for external users only, 804 cases, and nouser burden), the latter receives a higher amount of supportper case on average, and is provided equipment and equip-ment contents.

59


Table 3 Nanotechnology centers and facility networks of U.S. NNI.6)

2.2 Center for Biological and Environmental Nano-tech-nology (CBEN), Rice university

As an example of NSECs, the Center for Biological andEnvironmental Nanotechnology (CBEN) of Rice Universi-ty,12) which has recently become conspicuous both inresearch and policy, is introduced here. As Table 4 shows,the CBEN is taking the lead in the United States in researchmainly on the application of nanomaterials to bio and envi-ronmental fields but also their safety. The CBEN has astrong influence on the American National Standard Insti-tute (ANSI) – Nanotechnology Standard Panel (NSP)13)

(inaugurated in September 2004). The annual budget, how-ever, is over 3 million dollars.

2.3 New NSEC in 2005As the new support areas of the NSF, “Nanoscale Sci-

ence and Engineering: Program Solicitation for FY 2005”14)

listed the following eight high-risk high-return research andeducation areas:• Biosystems at the Nanoscale• Nanoscale Structures, Novel Phenomena, and Quantum

Control• Nanoscale Devices and System Architecture• Silicon Nanoelectronics and Beyond (SNB)• Nanoscale Processes in the Environment• Multi-scale, Multi-phenomena Theory, Modeling and

Simulation at the Nanoscale• Manufacturing Processes at the Nanoscale

• Societal and Educational Implications of Scientific andTechnological Advances on the NanoscaleFrom the above, applications for the following two

NSECs were solicited for FY2005:• Center on Hierarchical Manufacturing (CHM): Center of

nanoscale manufacturing processes• Center for Nanotechnology in Society (CNS): Center of

social influences of nanotechnologiesIn October 2005, Arizona State University and UCSB

were selected as the CNS. They have been also activelyconstructing networks with Europe and Japan holdinginternational conferences on nanotechnology involvingsociologists, political scientists and ethicists.

3. Nanotechnology research institutes in Germany

In Germany, the Competence Centers for Nanotechnolo-gy (CCN) are networks of nanotechnology research centersof industry, academia and government designated by theFederal Ministry of Education and Research (BMBF: Bun-desministerium fur Bildung und Forschung).15) Each net-work has its own special fields in nanotechnology researchto play the leading role in the country. Besides, there arealso networks supported by the local governments mainlyaiming at promoting local industries although not intro-duced here.

3.1 Competence Centers for Nanotechnology (CCN)Table 5 lists CCNs. There were six networks in the five-

year period until September 30, 2003, but this numberincreased to nine on October 1. Each CCN is a membershipnetwork but has several main institutes. The percentage offederal funding in the total funds for each CNN used to be100% under the old system but is now 50%, with theremaining 50% provided by the local government and oth-ers. The federal funds are all provided from VDI, exceptfor Nanomat. Nanomat is based on the Institute for Nan-otechnology (INT) of the Karlsruhe Research Center (FZK:Forschungzentrum Karlsruhe). Since Nanomat belongs to a

60


Fig. 1 Percentages of U.S. NNUN users by field (2003).11)

Theme of Research (Major) Theme of Research (Medium) Main ResearchConcatenation of proteins and nanoparticlesDetermination of physical nanoscale charge state by electron microscopePhysical fluorescent imaging using single-layer carbon nanotubeDetermination of SWCNT micelles dynamic characteristics by surface-active agentDetermination of electrical characteristics of single-layer carbon nanotubeNanostructure continuous manufacturing in the liquid phaseCancer treatment by nanoshell (nucleus: silica, shell: gold)Cell welding by nanoshellCancer diagnosis by nanoshellBone regeneration by polymer composite nanostructure

Development of ceramic film for water purificationDetermination of molecular nanopore transmission behaviorElimination of environmental contamination factors by nanocatalyst (titanium oxide)Elimination of impurities from water by iron oxide nanoparticlesToxicity evaluation of industrial nanoparticlesEvaluation of physical exposure to nanomaterials released into the environment

Theme 1: FundamentalBio-Chemistry(Nanoscience at the Interface)

Theme 2: Nanomaterials in Bioengineering(Nanoparticles that Detect Treat Disease)

Theme 3: Nanomaterials in Environment(Effetive, High-Performance Water Purification Systems)

Activity of BionanoconjugatesImaging Biological Charge DistributionsBiomedical Applications of SWNTSWNT Modeling in MicellesFullerene/SWNT TheoryNanomanufacturingNanoshell-based Cancer TherapyNanoshell Assisted Tissue WeldingNanomaterials for ImagingNanostuctured Bone ReplacementsAnti-fouling CoatingsCut SWNT for TherapyNanostructured Membances and theirPolymer Flow on the NanoscaleNanocatalysis for Remediation of Environmental PollutantsSorption of Contaminants onto Engineered NanomaterialsNano-cell InteractionsEnvironmental Exposure Routes

Table 4 Research themes of the Center for Biological and Environmental Nanotechnology (CBEN).12)

national laboratory, Helmholtz-Gemeinschaft (HGF), how-ever, its funding is provided not through VDI but directlyfrom the federal government.16), 17)

As an example CCN, this section describesNanoBioTech, which was established for the first timeunder the current system. The name “NanoBioTech” comesfrom “Nanotechnology: Functionality by means of chem-istry.” The main members are Nano+Bio Center, Kaiser-slautern University of Engineering (Technische UniversitatKaiserslautern – TU Kaiserslautern), NanoBioNet e.V., andtp21. NanoBioTech is funded by the federal government,the EU, the Rhinelang-Palatinate State, Saarland State, andthe university. The working funds, except forNanoBioTech research, total 950,000 euros in three years,including funds for workshops, meetings, and other eventsand network activities. The Nano+Bio Center is the foun-dation of this network and has a dedicated research build-ing with a clean room in the campus of TU Kaiserslautern.The laboratory of Ziegler, a director of NanoBioTech, isconducting pioneering work at TU Kaiserslautern.NanoBioNet e.V. is a organ of network operations in a nar-row sense. tp21 (Your technology partner for the 21st Cen-tury) is a group of small and medium-sized enterprises.

3.2 National research institutesAs mentioned in Chap 2, section 1, there are four large

national research institute groups in Germany: Wis-senschaftsgemeinschaft G.W. Leibniz (WGL), Helmholtz-Gemeinschaft deutscher Forschungszentren (HGF), Max-Planck-Gesellschaft (MPG), and Fraunhofer-Gesellschaft(FhG). As recognition of the importance of nanotechnologyR&D is growing, each group is constructing new frame-work for nanotechnology R&D. For example, WGL isconstructing the Institutes for New Materials (INM), HGFis constructing the aforementioned FZK INT, MPG is con-

structing the Institute for Solid State Research and MetalsResearch, and FhG is constructing the Institute for Bio-medical Technology. These efforts to build bases are notlimited to the conventional framework; emphasis is placedon shifting to priority fields, strengthening in-group net-works, reforming the organization by introducing and culti-vating human resources, and constructing infrastructure.Regarding FZK, for example, the main area of researchwas atomic power but this has been shifted to nanotechnol-ogy. In terms of not only R&D but also societal implica-tions, the Institute for Toxicology and Genetics (ITG) ofsafety and health, and the Institute for Technology Assess-ment and Analysis (ITAS) of sociology are moving fromatomic power to nanotechnology and strengthening theirlinks with INT.

4. France

In the nanotechnology field in France, the facility net-work “Reseau National en Nanosciences et en Nanotech-nologies (R3N)” consisting of CNRS and CEA researchbases and MINATEC led by an R3N member “CEA-LETI”, are the central bases of national strategies.18)

4.1 Reseau National en Nanosciences et en Nanotechnolo-gies (R3N)

R3N was first organized from five research centers: fourfrom national science research centers “Central National dela Recherche Scientifique (CNRS)” and one from atomicpower agency “Commissariat a l’energie atomique (CEA)”.• Laboratoire d’Analyses et d’Architectures des Systemes

(LAAS), Toulouse: Microsystems for bio and IT indus-tries

• Laboratoire de Photonique et de Nanostructures (LPN),Marcoussis: Photonics and nanostructures19)

• Institut d’Electronique Fondamentale (IEF), Orsay:Basic electronics

• Institut d’Electronique, de Microelectronique et de Nan-otechnologies (IEMN), Lille: Nanoelectronics andmicrowaves

• CEA-Leti, Grenoble: MicroelectronicsFurthermore, the following research center joined them lastyear:• Franche-Comte Electronique Mechanique Thermique et

Oprique – Sciences et Technologies (FEMTO-ST),Besancon: Mechanics and optoelectronics

With these five areas (LPN and IEF are both in the suburbsof Paris) as cores, R3N plans to keep growing by addingnew research centers.

4.2 Laboratoire d’electronique et de technologie de l’infor-mation (CEA-LETI) and Micro and Nano-technologyInnovation Center (MINATEC)

The nanotechnology institutes of France in the field ofelectronics are in Grenoble. Among them, CEA-LETI isplaying a key role in mediating between basic science andindustrialization, as outlined below:20)

• Staff: 900 regular staffs and 600 tie-up staffs (dispatchedfrom companies and postdoctoral staff) (CEA: 15,000,

61


Until Sept. 30, 2003 (5 years)

Oct. 1, 2003 – Sept. 30, 2006

*New establishment or participation (including derivation)

CeaseContinue

Continue

Continue

Split

Split

Table 5 CCN in Germany.15)

Grenoble district: 3,200)• Annual budget: 160 million euros (1/3 funded by the

government) (CEA: 3,000 million euros, Grenoble Dis-trict: 250 million euros)

• Achievements: 30 newly established companies and 180patents/year (about 55% of CEA)The percentages of R&D activities by CEA-LETI are

60% in the field of silicon electronics, 20% in optoelectron-ic parts, and 20% in bio, medical, and communications sys-tems. In particular, the field of silicon electronics is led bya project to develop 300-mm wafer technology called“Nanotec 300”.

A typical company newly established by CEA-LETI isSOITEC, a company which specializes in single-crystallinesilicon on insulators (SOI).21) SOITEC was established in1992, and sales in the first fiscal year amounted to 1.4 mil-lion euros. As production capacity was extended, salesincreased quickly from 16.3 million euros in FY1999 to43.3 million euros in FY2000 and reached 101.4 millioneuros in FY2002.

To further strengthen micro-nanotechnology R&D inGrenoble, MINATEC was established in 2001.21)

MINATEC consists of CEA-LETI, Institut National Poly-technique de Grenoble (INPG), and local autonomous bod-ies and private organizations. Currently, MINATEC is con-structing a new administration center for education,research, and industrialization beside CEA-LETI, for atotal cost of 170 million euros (to enter service in February2006). The new center will occupy a site of 60,000 m2,with clean rooms of Classes 10 to 1000 totaling 2,645 m2

and laboratory rooms totaling 3473 m2. After completion ofthe center, MINATEC will have a workforce of 4,000,including 1,000 at INPG mainly in charge of education,1,500 at CEA-LETI mainly in charge of research, and1,000 at private enterprises mainly in charge of industrial-ization.

5. UK

In the United Kingdom, universities are the core of pub-lic research bases.

(1) Nanotechnology research centers sup-ported by Research Councils (RCs)

Interdisciplinary Research Collaborations (IRCs) aregroups of research centers supported by the EPSRC. Theycan be divided into Nanotechnology IRC and Bionanotech-nology IRC. Nanotechnology IRC is led by the Universityof Cambridge, with the University College London andUniversity of Bristol22)-24) as partners. They have the fol-lowing four core projects:• Characterization of nanostructures by Scanning Probe

Microscopy (SPM)• Nanofabrication• Computational methods for molecular nanotechnology• Smart biomaterialsThe Bio-nanotechnology IRC is led by the University ofOxford, with the University of York, the University ofGlasgow, and the National Institute for Medical Research

as partners. They have the following three research areas:• Molecular motors• Functional membrane proteins• Nano-electronics & photonics

In addition, the ESPRC has funds for platform grants,networks, and nanotechnology training outlined below.

i) Platform GrantsFunds for long-term research by universities taking the

lead in five research areas and for global networking• Nanostructured surfaces: University of Birmingham• Thin film ferroelectronics for nanotechnology applica-

tions: Cranfield University• Nanocharacterization and nanofabrication of materials:

University of Oxford• Soft nanotechnology: University of Sheffield• Rapid prototyping of templated nanomaterials: Universi-

ty of Southamptonii) Networks

Funds to support networks to encourage communicationbetween researchers, inter-field fusion, and technical trans-fer (core research organs in parentheses)• Ferroelectric materials network (University of Leeds)• Biomedical applications of micro and nanotechnology

(University of Newcastle-upon-Tyne)• Molecular machines in nanotechnology (University of

Portsmouth)iii) Nanotechnology Training

Funds to support the training of graduates in doctoralcourses• Nanoscale science and technology: University of Leeds• Microsystems and nanotechnology: Cranfield University• Nanomaterials: Imperial College London• Microengineering: Heriot-Watt University• Life Science Doctorial Training Center in Bio-Nan-

otechnology (For doctoral course): Bio-NanotechnologyIRC

References

1) Nanotechnology Researchers Network Center of Japan, theMinistry of Education, Culture, Sports, Science and Technology.http://www.nanonet.go.jp/

2) The Ministry of Education, Culture, Sports, Science andTechnology, Knowledge Cluster Initiative of FY2004 (April 2004).

3) List of Industry-Academia-Government Linkage PromotionProjects by the Ministry of Education, Culture, Sports, Science andTechnology in City Areas, 2004.http://www.mext.go.jp/a_menu/kagaku/chiiki/city_area/index.htm

4) The 21st Century COE Program, the Nanotechnology ResearchersNetwork Center of Japan, the Ministry of Education, Culture,Sports, Science and Technology. http://www.nanonet.go.jp/japanese/info/nanoproject.html?org=2040

5) Nanotechnology Measures in Research Promotion Project forStrategic Creation by the Japan Science and Technology Agency.http://www.jst.go.jp/kisoken/nano.html

6) Nanoscale Science, Engineering and Technology Committee(NSET), the National Nanotechnology Initiative Strategic Plan.December 2004.

7) Bordogna J., National Nanotechnology Infrastructure Network(NNIN) Informational Meeting. January 2003.http://www.nsf.gov/news/speeches/bordogna/03/jb030130nninjsp

8) National Science Foundation (NSF), National NanotechnologyInfrastructure Network (NNIN), Program Solicitation, NSF 03-519.

62


2003.9) Cornell Nanoscale Facility (CNF), Nanometer, Vol. 14. No. 3.

September 2003.10) Cornell Nanoscale Facility (CNF), Cornell Nanoscale Facility

2003-2004 Research Accomplishments. 2004.11) Tiwari S., The National Nanotechnology Infrastructure Network

(NNIN). National Nanotechnology Initiative: From Vision toCommercialization. April 2004.

12) Center for Biological and Environmental Nanotechnology (CBEN).http://cohesion.rice.edu/centersandinst/cben/

13) American National Standards Institute (ANSI), ANSINanotechnology Standards Panel Holds First Meeting. 2004.http://www.ansi.org/news_publications/news_story.aspx?menuid=7&articleid=783

14) National Science Foundation (NSF), Nanoscale Science andEngineering (NSE), Program Solicitation, NSF 03-043. 2003.

15) Bundesministerium fur Bildung und Forschung (BMBF),Nanotechnology Conquers Market: German Innovation Initiativefor Nanotechnology. 2004.

16) Masahiro Takemura, Naontechnologies in German KarlsruheResearch Center (1) Institute of Nanotechnology). http://www.nanonet.go.jp/japanese/mailmag/2004/055c.html

17) Masahiro Takemura, Naontechnologies in German KarlsruheResearch Center (2) – NanoMat –. http://www.nanonet.go.jp/japanese/mailmag/2004/059c.html

18) Ministère délégué à la Recherche, Programme Nanosciences –Nanotechnologies. December 2004.

19) Marzin J., Laboratory of Photonics and Nanostructures. October2004 (slides).

20) Holden D., Technological research in micro and nanotechnologiesat CEA-Leti. October 2004 (slides).

21) Soitec, Pamphlet of Soitec. July 2004.22) Micro and Nanotechnology Innovation Center (MINATEC),

Pamphlet of MINATEC. 2004.23) Department of Trade and Industry (DTI), New Dimensions for

Manufacturing: A UK Strategy for Nanotechnology. June 2004.24) Engineering and Physical Sciences Research Council (EPSRC),

Nanotechnology. September 2004.25) Ryan J., Panel Discussion: International comparison of strategies,

7th International Conference on Nanostructured Materials. June2004 (slides).

63


1. Public research institutes of Russia

The Russian Academy of Science was established by theCzar Pyotr I of Russian Empire in 1724.1) This is an inde-pendent non-profit organization and the outmost authorityon science in Russia. This comprehensive academic organi-zation covers not only science but also Russia’s education,economy, and culture. The Academy is the center of Russ-ian basic research in natural science and social science. Byarea and research, the Academy can be divided into 9 sci-entific divisions, 3 regional divisions, and 13 regionalresearch centers, which have more than 30 physical labora-tories in total.

The main purpose of the Academy is to promote basicscience and scientific innovation to develop the technologyand economy of the nation. The Acadamy regularly pub-lishes a great variety of academic journals. Table 1 givesthe percentage breakdown of academic journals publishedin one year by field; the academic journals in the field ofchemistry and material science account for about 15% ofthe total journals published.

2. Scientific research budgets in Russia

In the Russian Federation, the total scientific budget was46.0 billion roubles (about 1.6 billion dollars) in FY2004but is anticipated to increase about 20% to 56.0 billion rou-bles (about 2.0 billion dollars) in FY2005. While increasing

the budget, the government announced a plan to reform andscale down the initiative of Russia.

In Russia, research funds from outside the countryaccount for about 20% of scientific expenses. The mainsources of international funds since 1990 have been theOpen Society Institute, the Russian Foundation for BasicResearch, CORDIS, the IEU Science and Technical Fund-ing Program, the International Science and TechnologyCenter, and the Eurasia Foundation.

3. Public research institutions of Russia engaged inmaterials research

Table 2 lists materials research institutes that are part ofthe Russian Academy of Science. Tables 3.1 and 3.2 listthe main physical research institutes involved in materialsresearch. The large number of institutes suggests that theresearch activity in Russian in the field of materials andphysics is very broad.

4. Actions for nanotechnologies in Russia

Since the time of the former USSR, research on nano-particles and nanomaterials has been active in the RussianFederation, particularly research on metals having nanos-tructures. In 1976 a paper about nanostructures was pub-lished in Russia, and in 1979 a research division for disper-sion systems (Ultra-dispersed Systems) was set up in theAcademy of Science.

The Russian Federation is funding nanotechnologyresearch through the Ministry of Science and Technology,the Russian Academy of Science, the Ministry of HigherEducation, the Federal National Technology of Russia Pro-gram, and the Ministry of Atomic Energy. In particular, theMinistry of Science and Technology is currently undertak-ing various nanomaterials research, such as electronic andoptical properties of nanostructures (the Ioffe Institute andothers), solid state physics program, modern problems ofsurface science, fullerene and nanotubes, biology, andadvanced materials.

64


*Number of annual issues

1. General and Interdisciplinary journals2. Specialized journals

2.1 Mathematics and physics2.2 Technical2.3 Chemistry and Material Science2.4 Life Sciences2.5 Earth Sciences2.6 Humanities

3. Mainstream Science journals

Table 1 Percentages of RAS-published academic journals by field.

Chapter 3. Public Research Institutes in RussiaFederation and Poland

Section 1. Russian Federation


References

1) Web page of each research institute of the Russian Academy ofSciencehttp://www.pran.ru/eng/, and others

65


Tackling the most basic subjects in the physics, chemistry, and engineering of iron and nonferrous metals

• Physicochemistry and technology of the production of ferrous, nonferrous and rare metals

• Physicochemical principles in the development of new metallic materials

• New production technologies and processes for the treatment of metals and alloys

• Computerized and automated metallurgical processes• Research methods for studying metals and alloys

Conducting basic research on microelectronics and micro-nanomaterials characteristics. Concluding science agreements with France, UK, and Germany

• Spectroscopy of magnetics materials• Physics of semiconductor microstructures• X-Ray Acousto-Optics Laboratory, X-ray optics• Local characterization of semiconductor materials• Quantum electron kinetics of metallic nanostructures• Computational Diagnostic Laboratory• Laboratory of Epitaxial Structures

Research on explosives and rocket propellants in the past and research for thermal explosions in the past

• Center for Macrokinetic ResearchCombustion of dispersed systems, Division of Nonlinear Dynamics, dynamics of microheterogeneous processes, heterogeneous chain processes, macrokinetics of catalytic processes, X-ray investigation

• Center for SHS Research(SHS: Self-propagating high-temperature synthesis)Chemical analysis of SHS materials, experimental equipment and standardization, fundamentals of SHS processes, macrokinetics of SHS processes, materialsPhysical properties investigations, physical stimulation of physico-chemical processes, physico-chemical analysis and research, rheodynamics and plastic deformation of SHS materials, shock-driven processes, SHS melts and cast materials, synthesis of functional oxide materials

Expanding mesomechanics fused from continuum dynamics and plastic physicsDept. of the Mechanics of Structured MediaDept. of the Physics of Strength and Wear-resistanceDept. of Physical and Technological Problems of Solid SurfacesDept. "Republican engineering and technical center for reconditioning and hardening of parts of machines and mechanisms at ISPMS SB RAS"

One of the oldest Siberian scientific facilities, established as a laboratory of chemistry and metals

• Ceramic materials and powders, material science, nanostructures, inorganic chemistry

• Environment, construction technologies, structural chemistry, solid state, physical chemistry, photochemistry

Institute Name,Location,

EstablishedMain Fields of Research Researchers

A.A. Baikov Institute of Metallurgy and Materials Science

Moscow1938

Institute of Microelectronics Technology Problems and High Purity Materials

Moscow Region1984

Institute of Structural Microkinetics and Material Science

Moscow Region1987

Institute of Strength Physics and Material Science

Tomsk1928

Institute of Solid State Chemistry and MechanochemistryNovosibirsk, 1944

Institute of Experimental Mineralogy

Moscow region1969

Institute of Non-Metallic Materials (Yakutsk, Year of establishment unknown) Details unknownInstitute of Physico-Chemical Ceramic Materials (Moscow, Year of establishment unknown) Details unknown

Part of researchers doubling as teaching staff at the Moscow State University

Laboratory of Fluid-Magmatic Interactions, Mineral Thermodynamics Laboratory, Laboratory of Ore Deposits Modeling, Laboratory of Metamorphism, Laboratory of Lithosphere, Laboratory of Hydrothermal Systems Thermodynamics, Laboratory of High-Temperature Electrochemistry, Laboratory of Mineral Synthesis

D.Sc(Included)

* **C.Sc

(Included)

Unknown

Unknown

* D. Sc: Doctor of Science - Professor-class senior doctorate researcher** C. Sc: Candidate of Science - Ph.D equivalent doctorate researcher

Table 2 Materials-related research institutes of the Russian Academy of Science.

66



Established

Ioffe Physico-Technical Institute

St. Petersburg1918

Institute for Physics of Microstructures

Nizhny Novgorod1993

P. L. Kapitza Institute for Physical Problems

Moscow1934

A. V. Shubnikov Institute of Crystallography

Moscow1925

Lebedev Physical Institute

Moscow1934(or 1724)

L. D. Landau Institute for Theoretical Physics

Moscow1965

One of Russia’s largest research institutes in physics and engineering• Centre of Nanoheterostructure Physics• Division of Solid State Electronics• Division of Solid State Physics• Division of Plasma Physics, Atomic Physics and Astrophysics• Division of Physics of Dielectric and Semiconductors• Educational Centre

Independent from the Institute of Applied Physics. Closely linked to the Nizhny Novgorod State University, with 20 or more researchers teaching at the university• Semiconductor physics• Superconductor physics• Surface physics, interface and multilayer structures• Heterostructure technology• Mathematical techniques and computer simulation• Thin films and technological equipment technology• Radio engineering• Microwave spectroscopy

Department of Theoretical Physics headed by Prof. Landau, winner of the Nobel prize for physics• Experimental physics• Theoretical physics• Applied physics

Specialized in crystallography, based on the three topics of growth, structure and properties• Crystal growth

Dept. of High-temperature Crystallization, Dept. of Crystallization from Smelting, Dept. of Crystallization from a Solution, Crystallization from High-temperature Solutions

• Crystal structureDept. of X-ray Methods in Modern Organic and Inorganic Materiology, Dept. of Electronic Microscopy, Dept. of X-ray Structure and Neutronographical Analysis

• Crystal propertiesDept. of Crystallophysics, Dept. of Track Membranes

• The Astrospace Center• Quantum radiophysics• Optics• Theoretical physics• Solid state physics• Nuclear physics and astrophysics• Neutron physical department• Dept. of Physics of Relativistic Multipartial Systems• Sector of the theory of the plasma phenomena• Group FIAN’s “Nonlinear optics and dispersion of light”

Established by five pupils of Prof. Landau. Not only a research institute but also a unique school of science and known as “Landau School”• Condensed matter theory• Quantum field theory• Nuclear and elementary particle physics• Computational physics• Nonlinear dynamics• Mathematical physics

Main Fields of Research Researchers D. Sc(Included)

C. Sc(Included)

206261266332208

About 100

About 60

Unknown

180UnknownUnknown

8514657580

UnknownUnknownUnknown

21

3219466

104

17 66

3043614636

12114114618297

57

39459226

Entire institute

Entire institute

Entire institute


* **

Table 3.1 Main physical research institutes of the Russian Academy of Science engaged in materials research.

67



EstablishedMain Fields of Research Researchers D. Sc

(Included)C. Sc

(Included)

Institute of Spectroscopy

Moscow region1968

Institute of Solid State Physics

Moscow region1963

Institute of Thermo-physics of Extreme Conditions

Moscow1987 or earlierDetails unknown

Bereskov Institute of Catalysis

Novosibirsk1958

NikolaevInstitute of Inorganic Chemistry

NovosibirskYear of establishment unknown

Researching a wide range of spectroscopy from X-ray to microwave• Atomic Spectroscopy Department• Molecular Spectroscopy Department• Department of Solid State Spectroscopy• Laser Spectroscopy Department• Department of Laser-Spectral Instrumentation• Theoretical Department• Laboratory of Spectroscopy of Nanostructures• Laboratory of Experimental Methods of Spectroscopy

Spectroscopy of defective structures, nonequilibrium electronic processes, electronic kinetics, quantum transport, quantum crystals, spectroscopy of surface of metals, superconductivity, theoretical department, structural research, real structure of crystals, spectroscopy of molecular structures, spectroscopy of surface of semiconductors, physics of high pressures, optical durability and diagnostics of crystals, materiology, reinforced systems, interfaces in metals, crystallization from high-temperature solutions, controlled growth of crystals, physical and chemical bases of crystallization, metallurgical chemistry, chemical bases of complex oxides

One of the five large research centers in Russia• Thermo-physics of extreme conditions• Physics of pulse influences• Materiology• Physics of low temperature plasmas• Pulse power and geophysics• Physical gas dynamics• Experimental thermo-physics• Department thermo-physical properties of substances• Chemical thermodynamics

(V.P. Glushko Thermo Center of the Russian Academy of Science)• Theoretical department (named after L.M. Biberm)

Established as the Siberian branch of RAS. Conducting catalyst and petrochemical research• Heterogeneous catalysis• Homogeneous and coordination catalysis• Mathematical modeling of catalytic processes• Nontraditional catalytic processes and technologies• Physicochemical methods for catalyst investigation• Catalytic process engineering• Catalytic methods for environmental protection• Applied catalysis problem

• Chemistry of inorganic connections, including coordinate, cluster and super-molecular connections

• Physical and chemical bases of processes of separation and purification of substances

• Physico-chemical and technology of functional materials• Crystal chemistry, electronic structure and thermodynamics of

inorganic substances, and others

High Energy Physics and Physics of Particles (Protvino, 1963)Proton accelerator U-70 (70 billion electron-volt) set up in 1967. Details unknown.

183227311811102

40 ≧100

203 48 146

200

≧270

Unknown

Unknown

40 100

Entire institute

* **


Table 3.2 Main physical research institutes of the Russian Academy of Science engaged in materials research.

1. Outline

Poland’s science and technology policies are planned bythe Science Council for the Ministry of Education and Sci-ence (formerly the State Committee for Scientific Research– KBN). The Council is a governmental body establishedin 2005. It advises the Ministry, among others, on the allo-cation of research funding responsible for basic researchand the other with projects relevant to industry. The factthat the Undersecretary of State of the Ministry of Educa-tion and Science is Professor Kurzydlowski, an eminentmaterial scientist, suggests that there is a strong emphasison materials research in Poland.

Materials research in Poland is funded by national pro-jects, financial support Networks and Centres of Excel-lence, and individual projects (Figure 1). In total about 50research institutions and 4,000 researchers are undertakingmaterials research with an emphasis on advanced materialsand nanotechnologies. According to ISI national citations,dated November 2005, Poland is ranked 22nd among 75countries in the field of materials science. However, if theaverage funding per publication is taken into account,Poland is in the group of countries which are the most effi-cient in maintaining an internationally respected position.

2. Materials research institutes

The organizations undertaking materials research inPoland are universities and institutes of the Polish Acade-my of Sciences (PAS). They are networked into consortiainvolved in national projects, materials networks, and cen-tres of competences (see further text). Most of them arecoordinated by professors from the major universities.

The top two universities of technology are Warsaw Uni-versity of Technology and the AGH University of Scienceand Technology in Krakow.

The Warsaw University of Technology has 32,000 stu-dents and consists of 17 faculties. The Faculty of MaterialsScience and Engineering (MSE) has 60 academic staff and415 students engaged in study and research. The MSE Fac-

ulty is the centre of materials research in Poland becausethe former Dean, Professor Kurzydlowski, has been servingon a number of national committees, including the impor-tant post of Deputy Vice-Chairman of the Reseach ScienceCouncil in the recent past and currently holds the post ofUndersecretary of State of the Ministry of Education andScience. He is also Chairman of the Council of Centre ofAdvanced Materials and Technologies, CAMAT.

The acronym “AGH” of the AGH University of Scienceand Technology translates from Polish as “Academy ofMining and Metallurgy”. The 15 faculties of the universitycover mining, casting, and other engineering disciplines.Material faculties include metallurgy, non-ferrous metals,foundry and ceramics for metals and other materials. AGHis perhaps the world’s largest materials education andresearch institute, with as many as 8,000 students majoringin materials.

The Polish Academy of Science (PAS) is organized intoseven divisions and has 79 research units. The Institute ofFundamental Technological Research (Warsaw) and theInstitute of Metallurgy and Materials Science (Krakow) areactively conducting materials research.

68


Fig. 1 Concept of the Polish materials policy.

03 Public Research Institutes in Russia Federation and Poland

Section 2. Poland

Krzysztof Jan KurzydlowskiUndersecretary of State, Ministry of Education and Science, Poland

Takahiro FujitaInternational Affairs Office, NIMS

3. National projects

KBN established the national related project “Metallic,Ceramic and Organic Nanomaterials” in 2000 with the par-ticipation of 25 research teams from universities, PASInstitutes, and industrial research units. Recently, this pro-ject has been followed by two new initiatives concerningnano-metallic components produced by plastic forming andpolymers modified by nano-particles.

Other national projects completed recently coveredintermetallics (ended in 2004) and materials for bio-med-ical applications (ended in 2005). Newly launched projectsare devoted to (a) functionally graded materials, and (b)plastic forming of ultra-hard materials.

4. Materials networks

In the past four years, two materials networks wereformed to help increase the Polish contribution to EuropeanResearch Area in the Materials Domain of FP6.

The Nanomaterials Network (Figure 2), in which 18 uni-versities, 4 PAS institutes, and 3 industries are participat-ing, covers five fields of nanomaterials, biomaterials, poly-mers, corrosion and degradation, and characterization ofmaterials. The network is intended to achieve the criticalmass necessary for further development of the researchgroups, to contribute to the wider use of knowledge basedmaterials in Polish industry and to participate in FP6.

The International Scientific Network for AdvancedMaterials and Structures (AMAS-ISN) consists of 36 Pol-ish research institutions and 24 research teams from variousEuropean countries. There are four subject groups in thenetwork: material microstructure, biomaterials, intelligentsystems, durability and safety.

5. Centres of Competence

Several Centres of Competences in materials sciencehave emerged in Poland in recent times, partly in responseto the encouragement by the European Commission. Oneof them is the Nanocenter set up at the Faculty of MSE of

the Warsaw University of Technology. Under the theme ofnano-crystalline materials, the Nanocenter is researchingmagnets, intermetallics, aluminum alloys, and compositeswith financial support from the EC and the Polish Govern-ment. There are similar centers in Krakow and Wroclaw.

6. Research funds

In the Financial Year 2004, the Polish Governmentinvested the equivalent of 37 million Zloty in total in thematerials research field: 23 million Zloty for research pro-jects and 14 million Zloty for industrial projects. Theinvestment ratios are 30% for research projects (engineer-ing area) and 34% for industrial projects. This indicatesthat the government is strongly committed to materialsresearch.

Materials research is also funded by the EU and otherorganizations. For example, “Knowledge-Based Multicom-ponent Materials” proposed by the Institute of FundamentalTechnological Research was adopted as an FP6 Network ofExcellence and received funding equivalent to about 8.1million Euro in two years.

7. Researchers

The materials research field of Poland is characterizedby a steady increase in the number of young researchers.Regarding the MSE Faculty of the Warsaw University ofTechnology, the number of students in the doctoral coursehas increased more than five-fold in the last 12 years (Fig-ure 3). This tendency can be seen throughout Poland.

These facts confirm that the Polish Materials ScienceCommunity has a great potential for collaboration in theinternational forum. In recognition of this, the EuropeanMaterials Research Society has awarded a series of FallMeetings to be held in Warsaw. It is expected that the meet-ings promote cooperation within the European ResearchArea and between researchers from Western, Central andEastern Europe.

69


Fig. 2 Nanomaterials Network in Poland.

Fig. 3 Number of doctoral course students in the Faculty of MaterialsScience and Engineering, the Warsaw University of Technology.

PART4

Outlook of Materials Research

• Nanomaterials

• Superconducting Materials

• Magnetic Materials

• Semiconductor Materials

• Biomaterials

• Ecomaterials

• High Temperature Materials for Jet Engines and Gas

Turbines

• Metals

• Ceramic Materials

• Composite Materials

• Polymer Materials

• Analysis and Assessment Technology

• High Magnetic-Field Generation Technology and Its

Applications

• Nanosimulation Science

• Technologies New Materials Creation

• Acquisition and Transmission of Materials Information

Data and Information

• International Standard

1. Introduction - Global Trend

As a material falls in size to nanoscale, it begins to dis-play a property completely different from that in a bulkstate. Therefore, new nanoscale materials are receiving spe-cial attention as nanomaterials that hold the key to nan-otechnology development. In particular, nanotubes,nanowires, and other one-dimensional nanoscale materialsare expected to be applied as new materials for electronics,environment and energy conservation, and biotics becausethey show peculiar forms and structures and excellent char-acteristics. The representative one-dimensional nanoscalematerial is carbon nanotube (CNT). Since its discovery byIijima in 1991, carbon nanotube has been actively studiedthroughout the world in many fields, such as synthesis,growth mechanism, structure analysis, properties analysis,theoretical analysis, and applied development and research.No other new materials are attracting as much attention ascarbon nanotube among many researchers and engineers inbasic to applied fields, nor causing such fierce developmentcompetition among colleges, public laboratories, and com-panies throughout the world. With new discoveries made

every day, carbon nanotube technology is progressing veryrapidly.

In addition to carbon, several compounds are known toform nanotubes. Table 1 lists the main compounds of nan-otubes found so far. Among them, molybdenum sulfide(MoS2), boron nitride (BN), and nickel chloride (NiCl2) aresimilar to carbon in that they have atomic arrangements ofnanotube-unique wall structures, such as the zigzag andarmchair types. In contrast, zinc sulfide (ZnS), galliumnitride (GaN), and silicon (Si) form nanotubes with the sp3

type structure as they do in the bulk state. These com-pounds form fine tube structures from hollow capillarycrystals. Strictly speaking, these nanotubes should be dis-tinguished from carbon and other nanotubes with nanotube-unique atomic arrangements. However, they are both callednanotubes.

Among non-carbon nanotubes, BN nanotube is nowbeing studied most actively, because it has excellent prop-erties not seen in carbon nanotube, such as heat resistanceand chemical stability. Because of these properties, BNnanotube is expected to be applied as electronics materials,super heat-resistant light weight materials, and hydrogenstorage materials. Since BN nanotube is difficult to synthe-size in a large volume, its properties and functions are stillnot clear. Unlike carbon nanotube, the study of BN nan-otube has begun. TiO2, V2O5, and other oxide nanotubeswere also recently discovered. Surface decoration and dop-ing with organic and inorganic substances without impair-ing the innate characteristics of oxides is expected to makeoxide nanotubes applicable to luminescent materials, cata-lysts, and high-performance magnets. Studies in this fieldhave also just begun.

2. Trends in and outside Japan

This section introduces recent trends in studies of carbonnanotube and various other nanotubes, includingnanowires.

2.1 Carbon nanotubeFigure 1 shows the numbers of papers and patents con-

cerning carbon nanotube by year. Since the discovery ofcarbon nanotube, both papers and patents have been

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Compound Synthesizing Method Documentation

C Arc discharge S. Iijima1)

(1991)

BN High-temperature heatingof MoOx (WOx) and H2S

N. G. Choprra et al.2)

(1995)

MoS2,WS2 Plasma discharge R. Tenne et al.3)

(1995)

NiCl2High-temperature heating

of precursorY. R. Hacohen et al.4)

(1998)

ZnS CVD with template J. Q. Hu et al.5)

(2004)

GaN CVD with template J. Goldberg et al.6)

(2003)

Si Two-stage heating,template

B.K. Teo et al. (2003) 7)

J.Q. Hu et al. (2004) 8)

V2O5 CVD with template P. M. Ajayan et al.9)

(1995)

TiO2 Sol-gel process P. Hoyer et al.10)

(1996)

Table 1 Main compounds of nanotubes.

Chapter 1. Nanomaterials

Section 1. Nanotubes

Yoshio BandoFellow, NIMS

increasing exponentially every year. So far, more than10,000 papers have been published. The statistical dataindicates active studies of carbon nanotube on a globalscale. Regarding the total number of patents, Japanaccounts for about 53%, the United States for about 13%,and Europe for about 7%. Japan ranks top in the world withdomestic patents but owns no more than about 10% ofinternational licenses, far less than the approximately 50%owned by the United States. The percentage in the field ofpatents is about 40% for synthesis and processing, 20% forelectron emission, 9% for composition, 6% for hydrogenstorage, and the rest for others. The trends in the studies oncarbon nanotube can be discussed in terms of 1) synthesisand processing, 2) structural analysis, functional investiga-tion, and theoretical calculation, and 3) device and otherapplied development. This paper describes synthesis andapplied development.

Noteworthy achievements in synthesis and processingare the volume synthesis of multi-wall nanotubes in 1992,filling into a carbon nanotube in 1993, the volume synthe-sis of single-wall nanotubes in 1995, the creation of a pea-pod (fullerene in a single-wall nanotube) in 1998, and theunidirectional growths of nanotubes on a Si wiring board in2000. In addition, large volumes of carbon nanofibers andnanotubes were synthesized successfully by thermaldecomposition in 1995 and a volume synthesis technologyusing a large continuous reactor was developed for multi-wall nanotubes in 1999. Now that the volume synthesizingtechnology for multi-wall nanotubes is almost established,researchers are directing their efforts mainly toward thevolume synthesis of single-wall carbon nanotubes and thedevelopment of a chirality control method. Single-wall car-bon nanotubes used to be synthesized by the laser ovenmethod and the arc discharge method. These methods,however, could synthesize only small volumes of impurenanotubes but not highly pure single-wall nanotubes.Because of this disadvantage, many groups are now devel-oping a synthesizing method for highly pure single-wallnanotubes from the CVD method that uses various metalparticles of several nanometers in diameter as catalysts.

Recently, it has been reported that a new synthesizingmethod using ethanol instead of hydrocarbons produceslarge volumes of single-wall nanotubes at low temperaturesand cost. Thus, the synthesis of single-wall nanotube is alsoprogressing rapidly.

Since the field emission phenomenon of carbon nan-otube was discovered in 1995, mainly Japanese and Koreancompanies have been promoting practical applications tosuper high-intensity light source tubes and full-color flatpanel displays by utilizing such excellent characteristics aslong service life and high intensity. Active studies are alsoin progress to find ways to use nanotubes as hyperfine linesreplacing silicon conductors. Prototype field effect transis-tors and diodes using nanotubes are being fabricated andthe effectiveness of nanotubes is becoming clear. However,it is extremely difficult to route wires freely in a complicat-ed electronic circuit. As elemental techniques, researchersare actively using an electric field to study the growth ofnanotubes in specific places on boards and the orientationof nanotubes.

2.2 BN nanotubeWhen carbon nanotube was discovered, researchers

began to search for non-carbon nanotubes and investigatetheir functions. BN nanotube was predicted in 1994 anddiscovered in 1995. A trace of multi-wall nanotube wasfound by plasma arc discharge or laser irradiation. Now thesubstitution reaction and CVD with precursor are beingestablished as synthesizing methods. Single-wall BN nan-otube, however, is synthesized in trace quantities because itis less stable than carbon nanotube. Regarding the proper-ties of BN nanotube, excellent oxidation and hydrogenstorage are now becoming apparent.

2.3 Other nanotubesV2O5 nanotube is the first oxide nanotube synthesized by

the CVD method with carbon nanotube as a template.Afterwards, TiO2, SiO2, MoO3, ZrO2, ZnO, WO3, and otheroxide nanotubes were synthesized by the sol-gel processand other soft chemical techniques or various synthesizingmethods, such as CVD and thermal decomposition. Nan-otubes are now synthesized not only from oxides but alsofrom sulfides, carbides, and nitrides, including WS2, MoS2,ZnS, PbS, CdS, GaN, AlN, and SiC. Bi, Au, Ni, and othermetallic nanotubes are also synthesized by a method usinga mesoporous alumina template. However, almost all theproperties and functions of these nanotubes are unclear.Investigations are in progress globally to discover new non-carbon nanotubes having excellent semiconductor and opti-cal characteristics.

2.4 One-dimensional nanoscale materials, such asnanowire

One-dimensional nanoscale materials other than nan-otube are classified by shape into nanowire, nanorod,nanobelt, and nanocone. Researchers are actively lookingfor such new materials and clarifying their functions. Allmaterials found as nanotubes are synthesized as nanowireand other capillary crystals of more than 100 types. In par-ticular, wide-gap semiconductor nanowires of ZnO and

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Num

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of p

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s (p

aten

ts ×

10)

/yea

r

Paper

Patent

Year

Fig. 1 Numbers of papers and patents on carbon nanotube.

SnO2 are also being studied to develop field emission, FETtransistor, and gas sensor applications. Figure 2 shows thechange in the number of papers on nanowire and other one-dimensional nanoscale materials. Their total is now almostequal to the number of papers on carbon nanotube. Recent-ly, especially active research and development in this fieldare underway.

3. Current status and study of NIMS

While effectively utilizing the world’s most advancedelectron microscope technology, the author’s group is tack-ling the search, creation, and structural analysis of newnanotubes and nanowires. In particular, the group is takingthe lead in the synthesis and structural analysis of BN nan-otube. The group developed a substitution reaction methodwith carbon nanotube as a template in 1998, a CVDmethod using a precursor in 2001, and laboratory-level vol-ume synthesis of high-purity BN nanotube using a carbon-free synthesizing method in 2002. Unlike carbon nanotube,BN nanotube was found to prioritize the zigzag type atomicstructure and the existence of cone-shaped BN nanotubewas clarified in 2002. In addition, the hydrogen storagecharacteristic of BN nanotube was discovered in 2002.

Meanwhile, new findings by Bando led to a new appli-cation field: using carbon nanotube as a temperature sensorin 2002, which is called a nanothermometer10). This nanoth-ermometer measures the temperature in fine space by usingthe volume expansion and contraction phenomena of liquidgallium enclosed in a carbon nanotube under varying tem-perature of the outside air. Because of its extremely smallsize, the nanothermometer was listed in the Guinness Bookof Records as the world’s smallest thermometer (2004). Asthermometers of non-carbon nanotube, nanothermometerswere also created successfully from MgO, In2O3, SiO2, andother oxide nanotubes featuring excellent heat resistanceand oxidation resistance.

Studies of carbon nanotube include the development of atechnology for fabricating a carbon nanotube by elec-trophoresis for use as a probe for an atomic force micro-scope and also a technology for arranging carbon nan-otubes in one direction. A new method was also developedfor low-cost production of carbon nanotubes. In thismethod, electrodes dipped in alcohol or another liquid areheated. Unlike the conventional arc discharge, a methodrequiring no external carbon supply successfully synthe-sized carbon nanotubes. In addition, fullerene nanotubescomposed of C60 or C70 fullerene molecules (hollow capil-lary crystals of hundreds of nanometers in diameter and

75

Materials Science Outlook 2005N

umbe

r of

pap

ers/

year

Year

Fig. 2 Number of papers on nanowire and other one-dimensionalnanoscale materials, excluding nanotube.

Fig. 3 Main achievements by recent NIMS studies.Discovery of carbon nanothermometer.

(a) Fullerene nanotube

(b) New nanotube found by NIMSFig. 4 Main achievements by recent NIMS studies.

76


hundreds of microns in length) were also synthesized.In studies for new nanotubes, other than carbon and BN

ones, researchers are looking for and creating various inor-ganic nanotubes and nanowires. The high-temperaturereaction of ZnS and SiO powders produced more than 10types of nanotubes and nanowires for the first time in theworld and their structures were clarified. They include sin-gle-crystal Si-nanotube (having a bulk structure of the sp3

type and about 100 nm in diameter), Si-microtube by SiOthermal decomposition (several microns in diameter), andones from ZnS and AlN.

4. Outlook

Since the discovery of carbon nanotube, many basicstudies have been done almost completely clarifying suchbasic characteristics as electrical conductivity, mechanicalstrength, thermal conductivity, and field emission. Howev-er, there is still no successful synthesizing technology thatcontrols chirality, the major issue related to carbon nan-otube. To achieve the applied development of various nan-otubes, it is essential to selectively synthesize and controlnanotubes showing only semiconductor or metal properties.In the future, the study phase needs to shift from the con-ventional basic studies toward the industrial sector: appliedand practical studies. It is particularly important to promoteresearch and development for practical uses in a wide rangeof industrial fields, including the fields of electronics andnanotechnology (flat display panels and nanotube molecu-lar elements), environment and energy (cathodes of lithiumion batteries and hydrogen gas storage), biotechnology(DNA biosensors), and composite materials (reinforcedplastics).

Concerning BN nanotube, however, a high-purity syn-thesizing method is being established by NIMS and an

environment is being set up to clarify its basic electromag-netic, optical, and thermal properties. Through the func-tional clarification of BN nanotube, basic and fundamentalresearch will play an even more important part in discus-sions of whether the hydrogen storage characteristic of BNnanotube can be improved to a practical level and whetherthe conventional insulators can be converted into semicon-ductors by element doping and used as nanotube elements.We are also anticipating the discovery of a new nanotubewith better semiconductor and optical characteristics thancarbon nanotube.

References

1) S. Iijima, Nature, 354, 56 (1991).2) N. G. Chopra, P. J. Luyken, K. Cherrey, V. H. Crespi, M. L. Cohen,

S. G. Louie and A. Zettl, Science, 269, 966 (1995).3) R. Tenne, L. Margulis, M. Genut and G. Hodes, Nature, 360, 444

(1992).4) Y. R. Hacohen, E. Grunbaum, R. Tenne, J. Sloan and J. L.

Hutchison, Nature, 395, 336 (1998).5) J. Q. Hu, Y. Bando, J. H. Zhan and D. Golberg, Angew. Chem. Int.

Ed., 43, 4606 (2004).6) J. Golberger, R. R. He, Y. F. Zhang, S. W. Lee, H. Q. Yan, H. J.

Choi and P. D. Yang, Nature, 422, 599 (2003).7) a) B. K. Teo, C. P. Li, X. H. Sun, N. B. Wong and S. T. Lee, Inorg.

Chem., 42, 6723 (2003).b) J. Q. Hu, Y. Bando, Z. W. Liu, J. H. Zhan and D. Golberg,Angew. Chem. Int. Ed., 43, 63-66 (2004).

8) P. M. Ajayan, O. Stephan, P. Redlich and C. Colliex, Nature, 375,564 (1995).

9) P. Hoyer, Langmuir, 12, 1411 (1996).10) Y. H. Gao and Y. Bando, Nature, 415, 599 (2002).

1. Introduction1)

A nanoparticle generally refers to a particle of 100 nmor smaller in diameter and of cluster size or greater. Sys-tematic research on nanoparticles was initiated by a studyon nanoparticle crystals by Uyeda (Nagoya University),and the theory of the electronic properties of nanoparticleswas predicted by Kubo (University of Tokyo) from about1960 to the mid 1970s. Uyeda fabricated nanoparticles byan inert gas evaporation method, and by observing themunder an electron microscope, discovered new crystallinestructures and morphologies not seen among bulk materi-als, thus proving the peculiarity of nanoparticles. Thistrigged intense research based on the contemporary theorythat Kubo’s effect causes great changes in the specific heatand magnetic rate of metallic nanoparticles. However,although many studies have been conducted, Kubo’s effectremains unverified. And although magnetic nanoparticlesattracted great attention for various applications, and inspite of excellent properties and characteristics, magneticnanoparticles failed to be used. This is for several reasons:magnetic nanoparticles have unstable properties, it is diffi-cult to obtain a large volume of uniform magnetic particlesat low cost, and it is difficult to handle magnetic particles,as they are active and easily coagulate.

Thereafter, Hayashi’s ultrafine particle project, ERATO,was established in 1981. In the project, the conditions ofnanoparticles could be checked successfully much moreprecisely with an electron microscope having high perfor-mance and resolution. In particular, the dynamic observa-tion of gold nanoparticles by Iijima is well known andhelped the later discovery of carbon nanotube. Regardinghandling, a nanoparticle gas transportation technologycalled the gas deposition method was developed and hassince been improved. In addition, advanced research wasconducted on two-dimensional arrays of nanoparticles, theconversion of an organic compound into nanoparticles, andmagnetotactic bacteria that contain magnetic nanoparticles.At the time, fine ceramics were attracting much attentionand many fine ceramic particles were prepared by variousmethods, greatly contributing to the development of theelectronic ceramics industry. However, when the newmaterials boom ended, research on nanoparticles faded.

2. Trends in research

Since President Clinton’s nanotechnology policy in2001, nanoparticle research has become active again. Fig-ure 1 shows the number of hits upon searching ScienceDirect, Japanese patents,2) and US patents3) using the key-words “nano” and “particle,” revealing a rapid increasesince 2001. Figure 2 shows the breakdown of internationaljournals on materials and US patents by country (areas) in2004. In Korea and China, the number of journals is largebut that of US patents is small, reflecting the United States’emphasis on patents. Japan used to hold the lead in nan-otechnology research but perhaps no longer.

According to a 2002 report,4) about 320 companies inthe world are manufacturing the primary products of nano-materials: nanoparticles (160), nanotubes (55), nano-multi-

77


Cou

nt

Japanese patents

US patents

International journals

Year

Fig. 1 Number of hits when searching international journals, Japanesepatents, and U.S. patents with the keywords “nano” and “particle”.

Rat

io (

%)

USA JapanEurope Korea China Taiwan Other

US patents

International journals

Fig. 2 Breakdown of international journals and US patents by country(areas) in 2004.

01 Nanomaterials

Section 2. NanoparticlesYoshio Sakka

Fine Particle Processing Group, Materials Engineering Laboratory, NIMS

pore materials (22), fullerene (21), quantum dots (19),nanomaterials (16), nanofibers (9), nanocapsules (8),nanowires (6), and dendrimers (5). The numerals in paren-theses are numbers of companies. As shown by the grow-ing number of US patents in Figure 2, many companies areUS venture firms which are ready to provide users withvarious nanoparticles.

According to a questionnaire conducted by NikkeiShimbun on 1700 companies (535 responses) from Octoberto November,5) the main focus of technology developmentin Japan is micromachining (72 companies), followed bynanoparticles (70 companies). The number of companiesinvolved in micromachining is over 100 if those companiesnow considering research are included. However, Japan isconsidered to be lagging behind the United States in termsof pricing and variety.

At present, the major markets for nanoparticles (includ-ing fine particles of up to 250 nm) are automotive catalysts(11,500 tons), abrasives (9,400 tons), magnetic recordingmaterials (3,100 tons), and sun-screen materials (1,500tons).4) The numerals in parentheses indicate the final prod-uct quantities. Table 1 lists the ratios of companies devel-oping products that use nanoparticles.4) The efforts in themedical and pharmaceutical industry, such as for drugdelivery, are particularly noteworthy.

3. Subjects

Nanoparticles are of zero dimension but can be used asfine lines in one dimension, as films in two dimensions,and as bulk materials in three dimensions. Issues concern-ing nanoparticle fabrication technologies are: 1) particlesize control, 2) morphological and interface control for sta-ble nanoparticles, and 3) low-cost mass production. Inorder to produce quantum effects in particular, sharp parti-cle size control (up to tens of nanometers) is necessary. Asnanoparticles easily coagulate, technologies to modify thesurfaces of nanoparticles and arrange and integrate thenanoparticles on a substrate are needed.1)-6) Depending onthe particle generation phase, nanoparticle synthesis can be

classified into solid, liquid, and gas phase methods. So far,the fabrication of nanoparticles has been done mainly byexperimentation. Technical problems are expected to besolved by in-situ observation of the generation process, bythe introduction of colloidal and aerosol science and engi-neering, and by better simulation. The known requirementsfor nanoparticle utilization are stabilization processing, dis-persion processing, microspace use, nano-order composite,formation of a film of generated particles, and advancedhandling for bulk formation. Theoretical work is necessaryto utilize conventional metals, ceramics, and polymersbeyond the framework of materials and for the fusion ofgenetic engineering and materials, such as the use of DNA.Regarding the process of converting ceramic nanoparticlesinto bulk materials, the previous new materials boomshowed the importance of pre-sintering process science forsolving problems of surface contamination with particlesand particle coagulation, including its resultant inhomoge-neous formation. Some researchers are therefore studying acolloidal process based on a colloidal science techniqueand bio-inspired processing.

4. Conclusion

Japan used to hold the lead in the nanoparticle field butis being outstripped by the United States with advancedtechnologies and by China and Korea with existing tech-nologies. However, Japan still maintains technical superior-ity in manufacturing equipment, and so collaboration withJapanese companies is indispensable for production. Toensure the current demand continues and is not a temporaryboom, further systematic academic studies are required.

The risks and social influences of nanoparticles areemerging mainly in Europe and America. In particular,there is concern about the influence of nanoparticles onhealth and the environment because they may be taken intothe human body during production, utilization, and dispos-al. Therefore, not only the advantages but also the disad-vantages of nanoparticle applications should beresearched.7)

References

1) M. Koizumi, K. Okuyama and Y. Sakka: Latest Technologies ofNanoparticle Manufacture, Application, and Equipment (CMCPublishing) (2002) (in Japanese).

2) http://www1.ipdl.ncipi.go.jp/FP1/cgi-bin/3) http://www.uspto.gov/4) M. J. Pitkethly, Nanotoday, December, 36 (2003).5) Nikkei Sangyo Shimbun (Dec. 1, 2003) (in Japanese).6) Z. Tang and N. A. Kotov, Adv. Mater., 17, 951 (2005).7) Asahi Shimbun (Mar. 30, 2005) (in Japanese).

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Medical and pharmaceutical

Chemical applied products

Information and communications

Energy

Automobile

Space and aeronautics

Textile

Agriculture

30 (%)

29

21

10

5

2

2

1

Table 1 Ratios of companies developing products using nanoparticles.

1. Introduction

Since a zero-dimensional artificial nanostructure madeof semiconductor (the so-called quantum dot) shows quan-tum size effects, new functions not available from bulk-state semiconductor may emerge. Various countries havebeen researching quantum dots in the expectation that usingsuch materials will produce devices having much higherperformance than the conventional silicon-based semicon-ductor devices whose performance seems to have reached aplateau.

Based on the results of searching a database of academicpapers (SCI Expanded), this chapter summarizes the trendsin research on quantum dots. From all papers publishedsince 1970, papers containing a term meaning quantum dotin their title, abstract, or keywords were searched and sort-ed, including those containing a term meaning bottom-upor top-down fabrication. The number of papers publishedby year and the transition by country was summarized.Also, the transition in research regarding bottom-up appli-cations is summarized by country.

2. Trends in research

Figure 1 shows the transition in the number of paperspublished about quantum dots, both worldwide and in

major countries. Figure 2 shows the transition in the num-ber of papers published about quantum dots, containing aterm meaning top-down or bottom-up fabrication.

In 1982, the concept of the quantum dot was proposedfor the first time by Arakawa and Sakaki of the Universityof Tokyo, with respect to application to an advanced semi-conductor laser.1) This triggered much nanotechnologyresearch.

Fewer than 20 papers were published annually in 1989and earlier years, but the number increased quickly from1990 and now more than 2,000 papers are published everyyear. To date, over 16,000 papers have been published, anumber that is almost the same as that of papers on carbonnanotubes on which research started at about the sametime. This indicates intensive research on quantum dotsthroughout the world. Among papers related to quantumdots, ones from Japan account for about 16%, rankingabout second with Germany after the United States andverifying the global importance of research in Japan. It isalso noteworthy that the number of papers from China isquickly increasing recently, and will exceed that of Japanor Germany in the near future.

The number of papers related to quantum dots, contain-ing a keyword meaning top-down or bottom-up fabrication,was not more than two a year until 1989 but increasedquickly from 1990, and now more than 900 such papers areissued every year (including more than 800 papers contain-

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Num

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Fig. 1 Numbers of papers on quantum dots.

Quantum dot Top-down/Bottom-up Bottom-up

Num

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Bottom-up

Top-down

Bottom-up

Fig. 2 Number of papers on quantum dots and papers containing akeyword meaning top-down or bottom-up fabrication.

01 Nanomaterials

Section 3. Quantum Dots

Nobuyuki KoguchiNanodevice Group, Nanomaterials Laboratory, NIMS

ing a keyword meaning bottom-up fabrication). The num-ber of published papers shows a similar tendency as thetotal number of papers on quantum dots.

In1985, the CNRS group reported the formation ofthree-dimensional nanostructures in the semiconductorthin-film fabrication process.2) However, the above dataclearly indicate that there was little research on quantumdots and few papers were published until 1989, becausethere were no effective methods of fabrication. The propos-al of top-down and bottom-up fabrication techniques forquantum dots in 1990 triggered today’s active research onquantum dots. Of these fabrication techniques, the dropletepitaxy method proposed by the National Research Insti-tute for Metals (presently the National Institute for Materi-als Science) in 19903) and the technique proposed by theUniversity of California and others in 19934) that usesnano-size islands structure based on the Stranski-Kras-tanow (S-K) growth mechanism manifested during thin-film formation were pioneering bottom-up fabrication tech-niques for quantum dots, while the selective growthmethod proposed by NTT in 19905) was a pioneering top-down fabrication technique for quantum dots. These tech-niques are frequently used to fabricate quantum dots forvarious semiconductor materials.

For quantum dots, the bottom-up fabrication techniqueswill be popular. Compared with the technique based on theS-K growth mechanism, the droplet epitaxy method couldnot be established soon after it was proposed, so a tech-nique based on the S-K growth mechanism is now usuallyused. Unlike this technique, however, the droplet epitaxymethod6) allows quantum dots to be fabricated from evencombinations of materials called lattice matching, which isnot possible by the technique based on the S-K growthmechanism, and also allows the shapes of quantum dots tobe controlled.7) Thanks to these features, the droplet epitaxymethod will develop further as a major bottom-up fabrica-tion technique for quantum dots.

3. Outlook

Quantum dot research started based on a few principlesbut without clear applications, but the directions and appli-cations of much research are now converging.

1. Application of quantum dots to light emitting devices(1,942 papers since 1982)

2. Application of quantum dots to infrared detectors andlight recieving devices (245 papers since 1991)

3. Application of quantum dots to single-electron effectdevices (1,772 papers since 1989)

4. Application of quantum dots to quantum informationprocessing (429 papers since 1995)

5. Application of quantum dots to spin electronics (35papers since 1999)

6. Application of quantum dots to artificial atoms and mol-ecules (386 papers since 1992)

7. Application of quantum dots to biological labeling (86papers since 1998)

Figures 3 to 9 show the transition in the number of pub-lished papers by major country. Only papers employing thebottom-up fabrication technique are counted here becauseit is considered the technique will become increasinglyimportant.

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Fig. 3 Application of quantum dots to laser and light emitting devices.

Num

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Fig. 4 Application of quantum dots to infrared detectors and lightreceiving devices.

Num

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Year

Fig. 5 Application of quantum dots to single-electron effect devices.

These figures show that Japan, the USA, and Europe(mainly Germany) are competing in research. Regarding“Application of quantum dots to light emitting devices”that triggered quantum dot research, the number of pub-lished papers leveled off or started to decline in all coun-tries since 2000. This is probably because the quantum dotlaser has now almost reached a practical level8) andresearch in this field has begun to shift to production. Inthis field, standardization will be particularly important.

Regarding “Application of quantum dots to infrareddetectors and light receiving devices”, Japan tends to pub-lish fewer papers than the United States and other coun-tries, perhaps because Japanese research focuses on appli-cation to civil equipment.

Regarding “Application of quantum dots to artificialatoms and molecules,” there is not much research aimed atspecific devices, yet this is very important from the basicviewpoint of clarifying and controlling the unique proper-ties of nanostructures.

Regarding research on application to single-electroneffect devices, quantum information processing, and spin-tronics, the number of published papers is growing steadilyand research will continue. Particularly concerning quan-tum information processing and spintronics, the total num-

ber of published papers is still small but is starting to riserapidly, and the trend needs to be monitored.

Although different from application to solid elements in1 to 6, research on the application of quantum dots of II-VIgroup compound semiconductors like CdSe to biologicallabeling is being stepped up, especially in the UnitedStates.

Research trends can also be investigated by searchingfor papers on quantum dots published in the 5-year periodfrom 2000 for papers that are cited often. From the paperspublished in each year, 10 papers are selected in descend-ing order of citation frequency. By checking the contents ofthe selected papers, we see that the percentages of paperson “Application to quantum information processing” and“Application to biological labeling” are very high. Of the50 papers (total number of citations: 6,111) here, 14 paperswere on “Application to quantum information processing”and were cited 2,424 times in total, 19 papers were on“Application to biological labeling” and were cited 2,142times in total.

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Fig. 6 Application of quantum dots to quantum information processing.

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Fig. 7 Application of quantum dots to spintronics.

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Fig. 8 Application of quantum dots to artificial atoms and molecules.

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Fig. 9 Application of quantum dots to biological labeling.

4. Conclusion

Research on quantum dots may lead to the developmentof devices far superior to the conventional semiconductordevices of mainly silicon, which have nearly reached theirperformance limit.

Regarding quantum dot applications related to soliddevices, the quantum dot laser that triggered quantum dotresearch and the single-electron memory for room-tempera-ture use9) that uses polysilicon have nearly reached a practi-cal level, although more than 20 years have passed sincethe first papers were published. Application to biologicallabeling has started to some extent, following years ofintensive research on fine particles. For the application ofquantum dots to various practical purposes, ongoingresearch is necessary in each field, especially for the fabri-cation and characterization of nanostructures.

This paper used the academic paper database “SCI Expand-ed” of ISI and the data is based on the search results as ofMarch 11, 2005. The keywords used for the quantum dotsearch were “quantum dot*, quantum-size* dot*, quantumwell box*, quantum box* and multidimensional quantumwell* ”. (* means that some characters may be added afterthe word.)

The author would like to thank Ms. W. Yamada for herassistance in searching and sorting the database.

References

1) Y. Arakawa and H. Sakaki, Appl. Phys. Lett., 40, 939 (1982).2) L. Goldstein, F. Glas, J. Y. Marzin, M. N. Charasse and G. Le

Roux, Appl. Phys. Lett., 47, 1099 (1985).3) N. Koguchi, S. Takahashi and T. Chikyow, Proc. of 6th Intern.

Conf. on MBE, San Diego, VIB-4 (1990), J. Crystal Growth, 111,688 (1991).T. Chikyow and N. Koguchi, Jpn. J. Appl. Phys., 29, L2093 (1990).

4) D. Leonard, M. Krishnamurthy, C. M. Reaves, S. P. Denbaas and P.M. Petroff, Appl. Phys. Lett., 68, 3203 (1993).

5) T. Fukui, S. Ando, Y. Tokura and T. Toriyama, Extended Abstractsof the 22nd Conf. on Solid-State Devices & Mater., 1990. (TheJapan Society of Applied Physics, Tokyo, 1990), p. 99, Appl. Phys.Lett., 58, 2018 (1991).

6) N. Koguchi, K. Watanabe, T. Mano, T. Kuroda and K. Sakoda,OYO BUTSURI, 74, 343(2005). Explaining the droplet epitaxymethod and summarizing related references.

7) T. Mano, T. Kuroda, S. Sanguinetti, T. Ochiai, T. Tateno, J. S. Kim,T. Noda, M. Kawabe, K. Sakoda, G. Kido and N. Koguchi, NanoLett., 5, 425 (2005).

8) Y. Arakawa and S. Tsukamoto, OYO BUTSURI, 74, 293 (2005).9) K. Yano, T. Ishii, T. Hashimoto, T. Kobayashi, F. Murai and K.

Seki, IEEE Trans. Electron Devices, 41, 1628 (1994).

82


1. Introduction

Semiconductor transistors, which underpin today’ssophisticated information-oriented society, have been inte-grated and enhanced by reducing the device size. Newmaterials are now being employed and structures are beingoptimized to improve the performance even further. How-ever, once the minimum feature size enters the nano-scale,the leakage current generated by the tunneling effectbecomes obvious and conventional semiconductor devicesno longer function properly,1) so a new technology is need-ed to enhance the performance of electronic devices. Aglobal strategy for semiconductor device development, theInternational Technology Roadmap for Semiconductors(ITRS), has therefore focused attention on nanodevices andis now studying the performance and size of devices, andalso manufacturing costs and materials to realize nanode-vices.2) Figure 1 compares semiconductor devices and nan-odevices by ITRS. Since nanodevices have various charac-teristics depending on their type, optimum ones should beselected according to the intended product. Fierce competi-tion is underway throughout the world to replace semicon-ductor devices with electronic devices of higher perfor-mance based on these nanodevices.

This chapter reports the current status of nanodevicedevelopment by introducing those of single-electrondevices in which single electrons are controlled using quan-

tum effects, and atomic or molecular devices in which sin-gle atoms or molecules are used as a device component.

In many cases, nanodevice R&D began with basic scien-tific research, then demonstration of the principle becamepossible due to the nanotechnology advances. Some of thenanodevices are now at the stage of being researched forpractical use, where integration techniques are being devel-oped. For example, basic research on quantum effects suchas the metallic particle charging effect (Kubo’s effect)announced in the 1960s led to the proposal of single-elec-tron devices in the 1980s.3) By using a micro fabricationtechnique and a scanning probe microscope, the basicstructure of the single-electron devices was constructed andtheir operations were confirmed.

Meanwhile, molecular devices use molecules as devicecomponents. It was theoretically shown that one organicmolecule could function as a diode in 1974,4) and variousresearch has been conducted.

Research on a new type of device that controls atomtransfer instead of electron transfer has started. With theinvention of the scanning tunneling microscope, individualatoms could be observed and manipulated, and hence adevice for controlling atom transfer was achieved at last.

Today, all the nanodevices mentioned above are beingresearched to clarify their individual performance and alsoto integrate them and form circuits for practical use.

As nanotechnology advances, various kinds of nanode-vices and their applications are being proposed andresearched. Due to limited space, this chapter introducesthe characteristics, development status, and potential ofnanodevices, and examines the significance of using newmaterials in developing new nanodevices.

2. Research trends

A single-electron device is a nanodevice that controlsthe transfer of single electrons by using quantum effects.As the quantum dot size becomes smaller, the electrostaticenergy changes by a greater amount when electrons go inand out. Therefore, if small quantum dots are used, singleelectrons can be controlled easily without operation errordue to the thermal effect. When developing a single-elec-tron device, it is important to fabricate quantum dots thatare small and of uniform size.

83


Fig. 1 Comparison of semiconductor devices and nanodevices.

01 Nanomaterials

Section 4. Nanodevices

Tsuyoshi HasegawaAtomic Electronics Group, Nanomaterials Laboratory, NIMS

Initially, metallic and semiconductor quantum dots weremade by using the conventional micro fabrication tech-nique, which is a top-down technique. However, this wasimpractical because only quantum dots with an operatingtemperature lower than that of liquid helium could be fabri-cated.5) Therefore, more practical bottom-up techniquessuch as using the self-organization of materials have beenemployed. These techniques are now being used to producesingle-electron transistors,6) single-electron memorydevices,7) and even logic circuits using the single-electroneffects.8) Indeed, integration technologies for some of theseare now being developed for practical applications. Forexample, prototyping of a 128M-bit memory device usingpolycrystalline silicon9) has already been fabricated.

Single-electron devices positively employing new nano-materials are also being researched. This is because usingnanomaterials that are uniform in size and characteristicsenables reducing the quantum dot size to make single-elec-tron devices of higher performance. Specifically, single-electron devices have been fabricated by using carbon nan-otube,10) fullerene, and single atoms11) as quantum dots. Thesingle-electron transistor using carbon nanotube hasalready been verified to function normally at room temper-ature,12) paving the way for early actualization of a single-electron device.

Figure 2 shows the transition in the number of papers onsingle-electron transistor by year. The figure reveals thatthe number has increased remarkably since the latter half ofthe 1990s, and the number from Japan is as great as thosefrom Europe and the United States, indicating that researchin Japan is active.

Molecular devices are one of the nanodevices wheremost intensive research is being done, boosted by the factthat the scanning probe microscope has enabled not onlycharacterization of individual molecules to be measured butalso manipulation of the molecules themselves, and that amonomolecular film can now be formed thanks toadvanced research on self-organizing films.

Molecular devices can be classified into one type thatuses single molecules as the functional parts (operationalelements) of a nanodevice and another type that controlsthe reactions between molecules and uses the resultantfunctions as operational elements and wires. Regarding theformer, a molecular switch using rotaxane molecules isbeing researched. A two-terminal device using conductivitythat changes by molecule oxidization was also formed anda logic circuit using the device was also reported.13)

Research on the latter includes the utilization of electronicstate changes by the polymerization of porphyrin mole-cules, diacetylene molecules,14) and fullerene.15)

For a molecular device, the reversibility or irreversibilityof phenomena used for operations, such as oxidation-reduc-tion reaction and polymerizing reaction, greatly influencesapplicability of the device. A recent experiment by a groupof the National Institute for Materials Science that provedthe reversibility of the polymerizing reaction for fullerenemolecules is thus of particular interest.

A device using atom transfer is also under development.Though the atom transfer speed is lower than the electrontransfer speed; for a nanodevice whose transfer distance is

of nano-scale, the transfer time or the time necessary fordevice operation is shorter than a nanosecond, which is thesame level as the operation time of an electronic device. Onthe contrary, using atoms not lost by the tunneling effectmay enable the fabrication of a device having higher per-formance than the conventional device that controls elec-trons.

A nanodevice controlling atom transfer was verified firstunder a scanning tunneling microscope.16) A rare gas atomwas transferred between the probe of the scanning tunnel-ing microscope and the surface of a sample to vary the con-ductivity between the probe and sample. Thereafter, adevice where a metal atomic bridge appears and disappearsbetween two electrodes was developed. To control theappearance and disappearance of an atomic bridge, a scan-ning tunneling microscope was used first but a techniqueusing an electrochemical reaction was developed later. Thelatter can be classified into a method using liquid electro-chemical reaction17) and another using solid electrochemi-cal reaction;18) the latter is considered to be practicalbecause it can be easily adapted to the existing semicon-ductor device fabrication process. In fact, research is notlimited to element verification but has already been extend-ed to logic circuit fabrication19) and integration20) by intro-ducing new materials called mixed electronic and ionicconductors to device fabrication.

3. Outlook

So far, research on nanodevices has been merely basicresearch. This is because improvement of device perfor-mance meant that of semiconductor devices regarding prac-tical devices. However, as the improvement of the perfor-mance of semiconductor devices has almost reached itslimit, work is progressing on developing practical nanode-vices. Researchers are attempting to develop an integratedcircuit using nanodevices and to construct an architectureutilizing the characteristics of nanodevices that operateaccording to a different principle from that of conventionalsemiconductor devices.

For single-electron devices, architectures utilizing the

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Fig. 2 Numbers of papers on single-electron transistor by years.

single-electron device characteristics are being researched,as well as the conventional logic architecture based onBoolean algebra. The new architectures include CellularAutomaton21) and Binary Decision Diagram,22) and devicesbased on these architectures are now being prototyped.

For molecular devices, logic circuits13) and memorydevices23) are being prototyped, as well as switches, transis-tors, and other basic element structures. In addition, newarchitectures24) are being studied using their characteristics.Molecular devices are expected to be applied to sensors byusing molecular characteristics and there is growingdemand for devices that cannot be created with convention-al semiconductor devices. Organic molecules are alreadybeing used for liquid crystal displays and seem to be easyto put to practical use as materials.

With this background, research on practical atomicdevices will accelerate because atomic devices may solvealmost all the problems inherent in semiconductor devices.For example, the ON resistance of conventional semicon-ductor devices increases as they become finer. Even if anano-scale semiconductor device is developed successfully,integration is thought to be impossible due to power con-sumption. On the contrary, atomic devices using metals arefree of such problems (see Figure 3). These characteristicsenable the development of electronic devices for new typesof products that cannot be realized with conventional semi-conductor devices. For example, research has started ondeveloping programmable devices indispensable for high-performance mobile terminals in the ubiquitous informa-tion-oriented society.25)

Device development using solid electrolytes is not limit-ed to nanodevices and is already reaching a practical level.In the United States, for example, device manufacturers arenow developing memory devices using metallic bridges,indicating that companies are trying to shake themselvesfree from device development that is dependent solely onsemiconductor devices.

Using nanodevices not only enhances the performanceof conventional electronic devices but enables new elec-tronic devices and products to be developed. As an exam-ple of using molecular switches, a defect-tolerant architec-ture of a crossbar structure26) has been proposed. Thisarchitecture is also applicable to other molecular switches.Single-electron devices and atomic devices can also beused to construct neural networks, which may lead toremarkable development in the field of electronics.

4. Conclusion

This chapter examined single-electron, molecular, andatomic nanodevices and described their development statusand future progress. As semiconductor devices reach adevelopment plateau, nanodevice development is shiftingfrom the basic level to the practical level.

Nanodevices not only enhance the performance of elec-tronics using semiconductor devices but also enable newelectronic products and computer architectures to be devel-oped that cannot be attained with conventional semicon-ductor devices. As the examples in this chapter show, thekey to nanodevice development is how the new functionsof materials can be used in device operations. Therefore,the development of materials for new functions will contin-ue to play a crucial role in nanodevice development, as willthe development of practical circuits and integration tech-niques.

References

1) P. Gelsigner, Tech. Dig. 2001 IEEE Int. Solid-State Circuits Conf.,San Francisco, p. 22.

2) ITRS web site: http://public.itrs.net/Nanodevices are handled asemerging technology.

3) D. V. Averin and K. K. Likharev, Mesoscopic Phenomena inSolids, Eds. B. Altshuler, P. A. Lee, R. A. Webb, Elsevier SciencePublishers, (1991) Chap. 6.

4) A. Aviram and M. A. Ratner, Chem. Phys. Lett., 29, 277 (1974).5) L. L. Sohn, L. P. Kouwenhoven and G. Schon, Proc. of the NATO

Advanced Study Institute on Mesoscopic Electron Transport, 1996,Dordrecht, Kluwer Academic Publishers (1997).

6) K. Ishibashi, Quantum Dot and Single-electron Device, ComputerToday, No. 109, 30. Science (2002).

7) K. Yano, T. Ishii, T. Sano, T. Mine, F. Murai and K. Seki, IEEEInt. Solid-State Circuits Conf., p. 266 (1996).

8) H. Hasegawa, S. Kasai and T. Sato, Oyo Butsuri 74, 320 (2005).9) K. Yano, T. Ishii, T. Sano, T. Mine, F. Murai, T. Kure and K. Seki,

IEEE Int. Solid-State Circuits Conf. p. 344 (1998).10) M. Bockrath, D. H. Cobden, P. L. McEuen, N. G. Chopra, A. Zettl,

A. Thess and R. E. Smalley, Science, 275, 1922 (1997).11) J. Park, A. N. Pasupathy, J. I. Goldsmith, C. Chang, Y. Yaish, J. R.

Petta, M. Rinkoski, J. P. Sethna, H. D. Abruna, P. L. McEuen andD. C. Ralph, Nature, 417, 722 (2002).

12) H. W. Ch. Postma, T. Teepen, Z. Yao, M. Grifoni and C. Dekker,Science, 293, 76 (2001).

13) C. Collier, E. W. Wong, M. Belohradsky, F. M. Raymo, J. F.Stoddart, P. J. Kuekes, R. S. Williams and J. R. Heath, Science,285, 391 (1999).

14) Y. Okawa and M. Aono, Nature, 409, 683 (2001).15) M. Nakaya, T. Nakayama and M. Aono, Thin Solid Films, 464-465,

327 (2004).16) D. M. Eigler, C. P. Lutz and W. E. Rudge, Nature, 352, 600 (1991).17) F. Q. Xie, L. Nittler, Ch. Obermair and Th. Schimmel, Phys. Rev.

Lett., 93, 128303 (2004).18) K. Terabe, T. Hasegawa, T. Nakayama and M. Aono, Riken

Review, 37, 7 (2001).19) K. Terabe, T. Hasegawa, T. Nakayama and M. Aono, Nature, 433,

47 (2005).20) S. Kaeriyama, T. Sakamoto, H. Sunamura, M. Mizuno, H.

Kawaura, T. Hasegawa, K. Terabe, T. Nakayama and M. Aono,IEEE J. Solid-State Circuits, 40, 168 (2005).

21) N. Koguchi and J. Takano, S&T Trends 20, 18 (2002).22) H. Hasegawa, S. Kasai and T. Sato, Oyo Butsuri 74, 320 (2005).23) W. Wu, G. Y. Jung, D. L. Olynick, J. Straznicky, Z. Li, X. Li, D. A.

A. Ohlberg, Y. Chen, S. Y. Wang, J. A. Liddle, W. M. Tong and R.

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Sw

itch

resi

stan

ce (Ω

)

Atomic switch

Switch size

Fig. 3 Switch size and ON resistance.

S. Williams, Appl. Phys., A 80, 1173 (2005).24) G. Snider, P. Kuekes, T. Hogg and R. S. Williams, Appl. Phys.,

A80, 1183 (2005).25) H. Kawaura, T. Sakamoto, J. Sunamura, S. Kaeriyama, M. Mizuno,

G. Hasegawa, T. Nakayama, K. Terabe and M. Aono, KogyoZairyo 52, 46 (2004).

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86


1. Introduction

There are many kinds of oxide superconducting materi-als, among which the high-temperature oxide supercon-ducting materials of bismuth-based oxides andYBa2Cu3Oz(Y-123) are now being studied in detail towardpractical use. Two bismuth-based oxides areBi2Sr2CaCu2Ox(Bi-2212) and Bi2Sr2Ca2Cu3Oy(Bi-2223).Figure 1 shows the transition in the number of papers pub-lished about these three superconducting materials in thepast decade; many are published every year on all of thesematerials, indicating the active state of research.

This section introduces research on wires and tapesmade of these high-temperature oxide superconductingmaterials. The powder-in-tube (PIT) method is the mostpopular for making wires of both bismuth-based oxidesBi2Sr2CaCu2Ox(Bi-2212) and Bi2Sr2Ca2Cu3Oy(Bi-2223).Oxide superconducting materials have a problem of weakcoupling between crystalline grains. To avoid this problem,it is necessary to orient the crystalline grains of oxidesuperconductor, which greatly improves the couplingbetween crystalline particles and allows a large supercon-ducting current. All oxide superconductors have layeredcrystalline structures. The crystalline grains of bismuthoxides are relatively easy to orientate because the materials

have strong anisotropy (two-dimensionality). However, thetechnique of orientation differs between Bi-2212 and Bi-2223: heat treatment by partial melting and gradual coolingis used for Bi-2212, with the Bi-2212 heated just beyondthe melting point and then cooled slowly.1) In contrast, Bi-2223 is oriented by a combination of machining and heattreatment.2)

Compared with the bismuth-based oxides, YBa2Cu3Oy

(Y-123) has much smaller two-dimensionality and its criti-cal current characteristic at the temperature of liquid nitro-gen (77 K) is far superior. To overcome the problem ofweak coupling, however, uniaxial orientation (c-axis orien-tation) alone is insufficient; biaxial orientation is also nec-essary.3) Therefore, the vapor method is mainly usedthroughout the world to deposit a thick film of Y-123 on ametallic substrate tape. The product is usually called coatedconductor.4) There are two main methods for achievingbiaxial orientation, one of which is called Ion Beam Assist-ed Deposition (IBAD). This method deposits a film on anon-oriented metallic substrate tape of hastelloy or othermaterial. The key technique is the deposition of biaxiallyoriented intermediate layer of yttria stabilized zirconia(YSZ). The biaxially oriented Y-123 film is epitaxiallygrown on the oriented intermediate layer by pulsed laserdeposition (PLD). The other method is called rolling assist-ed biaxially textured substrate (RABiTS); a metallic sub-strate of Ni or other metal is oriented by machining and aY-123 film is deposited on the substrate through an inter-mediate layer.

2. Global trends

This section examines the trends in R&D on wires andtapes in major countries. Research is most advanced in theUnited States where many companies, universities, andnational laboratories are engaged in research, with the goodlinks among them perhaps being a factor for success. TheUnited States has several national projects on the applica-tion of oxide superconducting materials. There is an estab-lished system whereby companies are in charge of wire andtape development and universities and national laboratoriesare in charge of related basic research.

Regarding Bi-2212, Oxford has been developing wires

87


Num

ber

of p

aper

s

Year

Fig. 1 Numbers of papers on Bi-2212, Bi-2223, and Y-123.

Chapter 2. Superconducting Materials

Section 1. Oxide Materials

Hiroaki KumakuraSuperconducting Materials Center, NIMS

and tapes and recently began to fabricate high-performancewires in lengths of several kilometers. Regarding the char-acterization of Bi-2212 tapes and wires, Florida State Uni-versity is conducting research with Oxford. The universityis also researching the application of Bi-2212 to high mag-netic fields. The National Renewable Energy Laboratory isproceeding with tape research by the coating method andWisconsin University is also researching Bi-2212 althoughon a small scale.

A Bi-2212 wire and tape show far superior characteris-tics to metallic wires at low temperature in a high magneticfield, and so a high-field magnet is one promising applica-tion of Bi-2212 wire. The National High Magnetic FieldLaboratory, Florida University plans to fabricate high-fieldmagnets from Bi-2212 wires. They have already fabricateda small coil from a 2 km long Bi-2212 tape and installedthe coil in a normal-conduction magnet of 19.85 Tesla togenerate 5.20 Tesla, achieving a magnetic field of 25.05Tesla in total.

Regarding Bi-2223, American Superconductor (AMSC)is the world-leader in the development of Bi-2223 tapes ofpractical lengths. As the world’s leading producer of Bi-2223 tape, the company has fabricated many tapes of sever-al kilometers length for national projects, and their Bi-2223tapes are also used in the test coils of Japan’s Maglev,which will be mentioned later. Meanwhile, Wisconsin Uni-versity is actively conducting basic research and supportingAMSC, which is further supported by the Los AlamosNational Laboratory (LANL) and the Argonne NationalLaboratory (ANL).

Since as-cold rolled tapes have large pore in the core ofa Bi-2223 tape, the Bi-2223 filling factor was not large andneeded to be improved. US Wisconsin University recentlydeveloped a high-pressure thermal treatment method thatimproves the filling factor of Bi-2223 core and increases Jc

greatly.5) This high-pressure heat treatment method alsoreduces the percentage of Bi-2212 and other impurities,thus increasing Jc. Geneva University of Switzerland andSumitomo Electric Industries are also conducting similarresearch.

Regarding coated conductors, such national laboratoriesas LANL, Oak Ridge National Laboratory (ORNL), andANL are powerfully promoting national projects. LANLadopted the IBAD method and ORNL adopted the RABiTSmethod to produce long tapes. ANL is proceeding withresearch by a method called Inclined Substrate Deposition(ISD). The relationship between microstructure and super-conductivity is under intensive research by Wisconsin Uni-versity, which is the center of basic wire research in theUnited States, including metallic wires. IGC-Superpowerand AMSC are also making progress, such as fabricatinghigh-performance coated conductors.

Many organs are conducting research also in Europe, butthe links among them seem to be weaker than in the UnitedStates. In Germany, Gottingen University has long beenresearching superconducting wires and tapes and is nowfocusing on coated conductors. In Switzerland, GenevaUniversity is conducting research to solve various materialsscience problems concerning Bi-2223 and Y-123 tapes. Inthe UK, IRC in Superconductivity of Cambridge University

is conducting basic research on Bi oxide wires and tapes. InFrance, Nexans is engaged in the research of Bi-2212 wiresand fabricating wires of several kilometers length. In Spain,the Institut de Ciencia de Materials de Barcelona isresearching coated conductors. In Austria, Vienna Univer-sity of Technology is making progress in research on theirradiation effects of superconducting wires and other sub-jects.

In Australia, the University of Wollongong has the Insti-tute for Superconducting and Electronic Materials whereBi-2223 wires and coated conductors are being researchedintensively in relation to microstructure and superconduc-tivity. The institute has close links with Australian Super-conductors in the country.

In Asia, Innova Superconductor Technology, which wasrecently established in China, successfully fabricated 1-kmBi-2223 tapes and is now setting up a supply system.Regarding the critical current characteristic, the companystill lags behind others, but is anticipated to improve thecharacteristic in the near future and will then become astrong competitor for Bi-2223 tape manufacturers in Japanand the United States. Note that this company has closelinks with the Applied Superconductivity Research Centerof Tsinghua University, where basic research is being doneon Bi-2223 tapes. The Institute of Electrical Engineering isalso conducting applied research on Bi-based oxides buttheir basic research on materials may not be enough.

In Korea, oxide superconducting materials are nowbeing developed intensively and the Korea Institute ofMachinery and Materials is conducting research to enhancethe performance of Bi-2223 wires and also on coated con-ductors. In addition, Seoul National University is research-ing coated conductors.

3. Domestic trends

In Japan, much research on oxide superconducting wiresand tapes is underway and the general research activitiesare similar to those in the United States. The main organsconducting research on Bi-2212 are the University ofTokyo, Hitachi Limited, Hitachi Cable, Showa ElectricWire & Cable, and NIMS. The University of Tokyo is con-ducting research on the Pb substitution of Bi-2212 andother basic studies, rather than on wire fabrication itself.Hitachi Limited and Showa Electric Wire & Cable havebeen developing Bi-2212 multicore round wires which areadvantageous for practical use. Hitachi Limited successful-ly achieved 100 m-long round wires and Showa ElectricWire & Cable attained 500 m-long round wires. Mean-while, Hitachi Cable succeeded in the experimental fabrica-tion of 2 km-long round wires with no thermal treatment.These companies are conducting basic research withNIMS. Regarding applications, Chubu Electric Power andShowa Electric Wire & Cable are developing coils forSuperconductive Magnetic Energy Storage (SMES) byusing Showa’s Bi-2212 round wires. In addition, ShowaElectric Wire & Cable is manufacturing assembled conduc-tors, called Rutherford cables, from Bi-2212 round wiresand delivering them to the US Lawrence Berkeley National

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Laboratory.Regarding Bi-2223 wires, Sumitomo Electric Industries

is the central manufacturer. The company has alreadydeveloped tapes of several kilometers length and has start-ed supplying tapes by participating in the US superconduct-ing cable project. In addition, Furukawa Electric andShowa Electric Wire & Cable are proceeding with R&Dfor Bi-2223 tapes. Regarding basic research, Kyoto Univer-sity is conducting research on the relationship betweenmicrostructure and characteristics and also conductingmodel analysis and research on stress effects. Meanwhile,Kyushu University and Kyushu Institute of Technology areactively researching electromagnetic characteristics. How-ever, for Bi-2223 tapes, in general the links among manu-facturers, universities, and national laboratories are notstrong. The most popular application of Bi-2223 is powertransmission cables. The Central Research Institute of Elec-tric Power Industry is performing various characteristictests on 500-m power transmission cables experimentallyproduced by Furukawa Electric. By using Bi-2223 tapes,coils for magnetically levitated trains (Toshiba and JRTokai) and superconducting transformers (Kyushu Univer-sity) are also being prototyped and tested.

Regarding coated conductors, the SuperconductivityResearch Laboratory is performing research through anational project with domestic companies and universi-ties,6) with the participation of Fujikura, Sumitomo ElectricIndustries, Showa Electric Wire & Cable, Furukawa Elec-tric and other firms, and is promoting R&D mainly on theIBAD method and Metal Organic Deposition (MOD)method. In addition, Fujikura is proceeding with uniqueR&D. In this field, Japan is in fierce competition with theUnited States. In basic research, Kyoto University is study-ing the fabrication process, while Kyushu University andYokohama National University are conducting precisionanalyses of the critical current characteristic and evalua-tions of the AC loss. Regarding length, the recent success-ful fabrication of 100-m tape having good characteristicsput Japan one step ahead of the United States.

Coated conductors used to have a problem that it takes along time to form an intermediate layer by the IBADmethod, but the Superconductivity Research Laboratory ofJapan recently found that a CeO2 layer having a higherdegree of grain orientation than the intermediate layercould be quickly obtained if the CeO2 film is further evapo-rated on the intermediate layer as the cap layer by the PLDmethod (self orientation). If a Y-123 layer is deposited onthis CeO2 layer, a Y-123 film having high orientation canbe obtained for very high Jc.

Compared with the above PLD method, an easier appli-cation method (MOD method) is being researched and ahigh Jc characteristic can now be obtained. Since no vacu-um chamber is necessary, this method can be easily scaledup and industrialized to enable tapes to be fabricated at lowcost.

4. Current status of NIMS and research by NIMS

NIMS is proceeding with Bi-2212 wire and tape fabrica-

tion mainly by the PIT method and the dip coating method.NIMS has already developed the partial melting and slowcooling method for the c-axis orientation of crystallinegrains and the Pre-Annealing & Intermediate Rolling(PAIR) method, thus successfully achieving the world’shighest critical current density Jc. The partial melting andslow cooling method is now used worldwide as the stan-dard heat treatment for Bi-2212 wires and tapes. Comparedwith the conventional metallic superconductors, Bi-2212wires produce much higher Jc especially in a high magneticfield, which is extremely promising for application to highmagnetic field generation. Nano-level structural control isalso useful. For example, the oxygen partial pressure uponheat treatment changes the grain boundary structure and Jc.Research is also underway on the microstructure and char-acteristics, such as biaxial orientation by temperature gradi-ent heat treatment and the resultant enhancement of Jccharacteristic. NIMS is also conducting joint research withShowa Electric Wire & Cable to increase Jc of Bi-2212multicore round wires. NIMS recently found that slowcooling from a narrow temperature range just above thepartial melting temperature of Bi-2212 greatly improves Jc,probably because Bi-2212 filaments do not become irregu-lar or coarse, and they have attained the world’s highest Jcfor round wires.

Regarding applications, NIMS is proceeding withresearch to enhance the magnetic field generated by asuperconducting magnet using Bi-2212 wires and tapes. Byusing Bi-2212 tapes small test coils were fabricated jointlywith Hitachi Limited and Hitachi Cable, and were theninstalled at the center of existing superconducting magnetssystem to increase the magnetic fields by the Bi-2212coils.7) NIMS attained a total magnetic field of 21.8 Teslawith coils by the dip coating method and 23.4 Tesla withcoils by the PIT method, the latter being the world’s high-est magnetic field generated by a superconducting magnetsystem. When small magnets fabricated from Bi-2212wires were cooled by a cryocooler not requiring liquid heli-um, the magnetic field was high enough and the magnetswere thermally stable at temperatures around 20 K. Sothere are high expectations for superconducting magnetsmade of Bi-2212 wires which can be cooled very efficient-ly by a cryocooler.

In addition to the above application research, NIMS hasbeen searching for new superconducting materials and alsodeveloped high-pressure equipment. With these devices,NIMS immediately started searching for new high-temper-ature superconductors under high pressure and successfullyfound more than half of the existing oxide superconductorsthat had a transition temperature exceeding 100 K. Througha chemical oxidation process, NIMS obtained a hydratedcobalt oxide superconductor (NaxCoO2/yH2O).8) Its Tc isnot higher than about 5 K, however, this is the first cobaltoxide that showed superconductivity. This discovery pro-vides a new direction for superconducting materialsresearch and may help clarify the mechanism of supercon-ductivity of high-temperature oxides.

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5. Outlook

Bi-2223 and Bi-2212 wires and tapes having high Jc

were recently produced in various studies both within andoutside Japan but have not yet reached a practical level. Invarious experiments, both Bi-2223 and Bi-2212 wires andtapes locally showed sufficiently high Jc for practical use,so both materials offer good potential. Actual bismuth-based wires and tapes, however, have many defects thathinder a superconducting current, such as voids, impurities,and misorientation, and so a sufficient superconductingtransport current cannot be obtained. There are alsounknown mechanism in terms of materials, such as thetransfer mechanism of a superconducting current at thecrystalline grain boundary.

To solve these problems, R&D on a new techniqueseems indispensable. The basic parameters that character-ize superconducting materials include coherence length.Since this parameter is on the nanometer level, structuralcontrol of the nanometer level may be effective for improv-ing the characteristics. For example, it will be important touse nanoparticle starting materials, to modify layered crys-talline and grain boundary structures, and to introducenanometer particles. Through such techniques, Jc of Bi-2212 should be improved at 4.2 K and 20 K and that of Bi-2223 should be improved also at 77 K.

Meanwhile, coated conductors showing excellent Jccharacteristics on short tapes have been developed. Forpractical use in future, technologies for creating tapes ofseveral kilometers length and reducing the manufacturingcost are needed. In both cases, close links among compa-nies, universities, and national laboratories will be crucialfor efficient R&D.

To enhance characteristics by nanostructure control, it isimportant to establish a technology for evaluating themicrostructure of wires and tapes and the distribution ofsuperconducting current densities on the nanometer level

and to feed back such information to the wire and tape fab-rication process. For this nanometer-level analysis, we willestablish a technique of analyzing the microstructure andproperties of a micro-area with a scanning SQUID magnet-ic microscope for the two-dimensional analysis of currentdistribution and a microwave STM, as well as a transmis-sion electron microscope.

Meanwhile, research on new superconductors havingbetter characteristics than the existing oxide superconduc-tors will be important not only academically but also forapplications. For new materials synthesis, synthesis in aspecial environment (ultrahigh pressure, ultrahigh gas pres-sure, and soft chemistry) may be promising. We shouldpromote R&D on these techniques to obtain new supercon-ductors as the seeds for next-generation superconductingmaterials.

References

1) H. Kumakura, Bismuth-based High-Temperature Superconductors,Eds. H. Maeda, K. Togano, Marcel Dekker, Inc., New York (1996)451.

2) Y. Yamada, Bismuth-based High-Temperature Superconductors,Eds. H. Maeda, K. Togano, Marcel Dekker, Inc., New York (1996)289.

3) D. Dimos, P. Chaudhari, J. Mannhart and F.K. LeGoues, Phys. Rev.Lett., 61, 219 (1988).

4) Y. Shiohara and N. Hobara, Adv. Superconductivity XII (2000) p.567.

5) Y. Yuan, R. K. Williams, J. Jiang, D. C. Larbalestier, X. Y. Cai, M.O. Rikel, K. L. DeMoranville, Y. Huang, Q. Li, E. Thompson, G.N. Riley and Jr., E. E. Hellstrom, Physica C 372-376, 883 (2002).

6) Y. Shiohara: Cryogenic Engineering, 39, 511 (2004).7) M. Okada, K. Tanaka, T. Wakuda, K. Ohata, J. Sato, T. Kiyoshi, H.

Kitaguchi, H. Kumakura, K. Togano and H. Wada, Advances inSuperconductivity, XI (1999) 851.

8) Y. Sakurai, K. Takada, and E. Muromachi: Appl. Phys., 74, 22(2005).

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1. Introduction

Among thousands of kinds of superconducting materialsdiscovered, only the four kinds of metallic superconductingmaterials (Nb-Ti alloy and Nb3Sn, Nb3Al, and MgB2 com-pounds) listed in Table 1 are already in service or expectedto be used, along with one kind of Y-type oxide supercon-ductor and two kinds of Bi-type oxide superconductors.Compared with oxide superconductors, metallic supercon-ducting materials are low both in critical temperature Tc

and critical field Bc2, and so metallic superconductingmaterials may be replaced with practical oxide supercon-ducting materials in future. Regarding superconductingapplications (Table 1), oxide superconductors cannot beused yet because of poor mechanical characteristics and thedifficult superconducting joint, so the performance ofmetallic superconductors still needs to be improved.

To review the trends in R&D of metallic superconduc-tors, an academic database was searched for papers thatcontain materials names in their titles. Figure 1 shows thenumber of published papers by year. The number of paperson MgB2 just discovered in 2001 is far larger than those onother metallic superconducting materials. This reflects thehigh expectations for the new MgB2 material which fea-tures the highest Tc and low-cost metallic materials.Regarding comparisons of Nb-Ti, Nb3Sn, and Nb3Al,research on their bulk state properties was completed in the1960s and 1970s, and the research was shifted to the practi-cal form of wires and thin films in the 1990s. A search ofthe academic paper database revealed that papers contain-ing wires or thin films in their titles (gray) accounted forabout 20 to 30% of the total number of papers on MgB2,

which was about 1.5 to 2 times the number of papers onNb3Sn. Figure 1 shows that research on MgB2 has beenparticularly active in the past few years but the number ofpapers on other metallic superconductors has notdecreased. This may be because many MgB2 researchershave returned from the field of oxide superconductors.

According to OST’s unique survey,1) Nb-Ti and Nb3Snaccounted for most of the world’s output of superconduct-ing materials by weight in FY2004 (Figure 2(a)). Of 1,100tons in total, Nb-Ti accounted for 97.8%, followed byNb3Sn with 1.5%. The rest, just 0.7%, is Bi-type oxidesuperconductor. According to statistics on wire sales byequipment type in FY2004 (Figure 2(b)), magnetic reso-

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Num

ber

of p

aper

s

Year

Fig. 1 Numbers of papers on metallic superconductors (Source: Web ofScience).

Nb-Ti alloy9.6 K11.5 TDuctility (Handling: Easy)Low cost10 T or lessMedical MRINMRAcceleratorMagnetic levitated train

Nb3Sn18 K26-28 TStrain sensitivity: High

High-field NMR•MRICoil for properties researchAcceleratorFusion reactor

Nb3Al17.5-18.5 K26-30 TStrain sensitivity: Low

Fusion reactorHigh-field NMR•MRIAcceleratorCoil for properties research

MgB2

35-39 K10-50 T20 K runLightweight

Liquid hydrogen coolantMagnetic levitated trainSpace environment

Critical temperature Tc

Critical field Bc2 (4.2 K)Feature

Superconduction application

Table 1 Comparison of main metallic superconductors.

02 Superconducting Materials

Section 2. Metallic Materials

Takao TakeuchiMetallic Wire Group, Superconducting Materials Center, NIMS

nance imaging (MRI) apparatuses and nuclear magneticresonance (NMR) spectrometers account for about 60% ofwire sales, for which Nb-Ti and Nb3Sn are employed. Thetotal number of MRI and NMR units sold annually isincreasing at the rate of 8 to 10% and much research isbeing done to enhance the performance of Nb-Ti andNb3Sn and to reduce their cost.

2. Global trends

Advanced medical institutes in and outside Japan areexperimentally using MRI apparatuses of which the mag-netic field is as high as almost 10 Tesla. To enable suchhigh-field MRI to be widely used in medical hospitals infuture, we need to develop a low-cost Nb3Sn (or Nb3Al)wire available for the R&W method that winds a coil afterforming the Nb3Sn phase. With a view to achieving high-performance analysis of protein structures, Japan, the US,and Europe are strategically developing 1 GHz (23.5 Tesla)NMR, for which the high-field superconducting materialsNb3Sn and Nb3Al are key to success. For large-scale appli-cations, the performances of Nb-Ti, Nb3Sn, and Nb3Al needto be improved continuously. Metallic superconductorresearch was led by the CERN accelerator (LHC) andfusion reactor (ITER) in the mid 1990s, and by the next-generation accelerator and other large projects since 2000.The total demand for superconducting materials for ITERmagnets is as large as 550 tons for Nb3Sn or 250 tons forNb-Ti. Production facilities need to be built to produce anddeliver the materials within a few years after the start ofconstruction.

The keys to raising the performance of Nb3Sn are toincrease the amount of Sn which contributes to the diffu-sion reaction and to control microstructures on the nano-level. Consequently, the critical current density per crosssection excluding stabilizing copper (non-Cu Jc) at 12 Teslaand 4.2 K was doubled to 3000 A/mm2 in the past decade.In other words, the bronze method increased the Sn con-centration in Cu to the solubility limit (16%) to make thegrain finer and thus increase Jc. However, it is difficult toraise the Sn concentration of bronze further. Meanwhile,the internal Sn diffusion method uses a Cu matrix contain-ing not only Nb filaments but also Sn as cross-sectional

components. This method has been actively studied inJapan, the US, and Europe (Mitsubishi Electric, Out-okumpu, Bochvar, and Alstom) because it allows the Sncontent to be increased, thus raising Jc, although themethod is inferior to the bronze method in terms of ACloss. Recently, OST in the US made further improvementsto satisfy the high Jc specification for the next-generationaccelerator. By minimizing the Cu ratio, they successfullyachieved a high non-Cu Jc of 3000 A/mm2 at 4.2 K and 12Tesla. To overcome the problem of low mass-production, adummy salt placeholder was adopted instead of Sn so as toallow the hot extrusion of large 200 kg multi-billets. Imme-diately after extrusion, the salt is substituted with Sn andprocessed by cold wire drawing to attain adequate unitlengths and low cost. In future, it will be important toimprove the stability (Cu contamination with Sn), AC losscharacteristic, and mechanical characteristics that havebeen sacrificed in order to achieve high Jc. The NorthwestInstitute for Non-ferrous Metal Research of China recentlystarted large-scale production not only of Nb-Ti but alsoNb3Sn by the internal Sn diffusion method. Although theInstitute’s products are inferior in the Jc characteristic, theprices are low for the global market and so the situationshould be monitored. SMI of Europe improved the powder-in-tube (PIT) method; NbSn2 powder filled diffusion-reactswith an Nb tube to form Nb3Sn, which is advantageous forattaining high Jc. With cooperation from EAS, SMI suc-cessfully extended the unit-length by large billets (50 kg).This has an advantage of less Sn contamination of the Custabilizer placed outside Nb.

As mentioned later, Nb3Al is mainly being developed inJapan.2) In the United States, Ohio State University, OST,IGC, and Supercon have been developing rapid-quenchedNb3Al for the next-generation accelerator. Recently,EURATOM-ENEA of Italy also started research on rapid-quenched Nb3Al.

Although other metallic superconductors require liquidhelium as a coolant, MgB2 has a high critical temperatureand so the cooling costs can be greatly reduced if environ-ment-friendly liquid hydrogen – a possible future energysource – is used as the coolant for superconductor. Becauseof its lightweight characteristic, MgB2 is expected to beused for magnetically levitated trains and space applica-tions. When discovered, MgB2 had a problem of low Bc2

for high Tc. However, the trace oxygen soluble thin filmdeveloped by Wisconsin University and the SiC nanoparti-cles added by the University of Wollongong, Australia,greatly improved Bc2 by substituting C with B, thus provingthe immense potential of the material as wires for highmagnetic fields. Intensive research is now in progress inJapan, the US, Europe, and Australia to produce MgB2

wires by the PIT method. Compared with other metallicsuperconductors, however, MgB2 is still at an early stage ofresearch. Wires of 1000-m class have already been fabri-cated, suggesting that the length can be increased easily, asexpected. As shown by a collection of data3) comparing thenon-Cu Jc characteristic between various superconductingwires, the Jc values of MgB2 long wires are still low.

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Other

Big Physics

Total annual output: 1,100 tons Wire sales (2004): 185 million dollars

Fig. 2 (a) Wire output by materials, (b) Wire sales by application type1)in 2004.

3. Trends in Japan

Regarding Nb-Ti, Furukawa Electric produced anddelivered 92 tons in total to CERN in Europe as a conduc-tor for the LHC accelerator from 2000 to 2003. CERNbestowed an award on Furukawa Electric for higher qualityof the products than other overseas manufacturers, demon-strating the high technical power and competitiveness ofNb-Ti wires.

Regarding Nb3Sn,4) note that Kobe Steel produced high-Sn-content bronze-route Nb3Sn wires for the first time inthe world. Now Kobe Steel, Furukawa Electric, and HitachiCable are developing high-Sn-content bronze-route Nb3Snwires for high-field NMR. The high-Sn-content bronze-route Nb3Sn is about to be used not only for NMR but alsoITER. The wires of the ITER fusion reactor require bothlow hysteresis and high Jc. Like the internal Sn Nb3Snwires of which inter-filament coupling is suppressed, thehigh-Sn-content bronze Nb3Sn wires with high Jc are verypromising materials for fusion uses. The Ta-Sn PIT Nb3Snwires jointly developed by Tokai University and KobeSteel are attracting attention as new candidate wires forhigh-field NMR. Regarding the development of Nb3Snwires of high Jc for the next-generation accelerator, Japanlags behind the United States because wire developmentprograms used to be led by the US. Recently, however,Mitsubishi Electric started developing wires featuringimproved the internal Sn Nb3Sn wire, and this work isworth monitoring.

Regarding Nb3Al, the Japan Atomic Energy Agency hasbeen developing Nb3Al wires by the low-temperature diffu-sion method jointly with Sumitomo Electric Industries bynoting lower strain sensitivity and hence better strain toler-ance. By using a trial manufactured Nb3Al coil with theR&W technique, a high current as large as 46 kA was suc-cessfully achieved at 13 Tesla in 2003. However, the val-ues of Bc2 and Jc of the low-diffusion processed Nb3Al arelower than those of rapidly quenched Nb3Al. Since themagnetic field required by the next-generation fusion reac-tor will increase from 13 Tesla to 16–20 Tesla, low-temper-ature diffusion processed Nb3Al will not be able to satisfythe requirement and thus the rapid-heating, quenching andtransformation (RHQT) processed Nb3Al will be developedjointly with NIMS. The High Energy Accelerator ResearchOrganization started developing RHQT Nb3Al for the next-generation accelerator jointly with Hitachi Cable andNIMS.

Regarding MgB2,5) JR Tokai and Hitachi Limited started

developing MgB2 wires by considering application to coilsfor magnetically levitated trains and to MRI. By the ex-situmethod that fills MgB2 powder directly into a Cu/Fe com-posite pipe, they fabricated a small coil experimentallyfrom a single-core wire of about 50 m and succeeded ingenerating a magnetic field. Future issues are to make longlengths of wire, to increase the number of filaments to sup-press instability in a low magnetic field, and to develop asuperconducting joint technique. By mixing indium metal-lic powder of a low melting point into raw MgB2 powder,Tokai University successfully improved the connectivitybetween MgB2 particles and greatly increased Jc.


Regarding the RHQT Nb3Al initiated in 1996, NIMS hasbeen collaborating with Hitachi Cable to develop it as acandidate wire for the insert coil of high-field NMR nowunder development at the Tsukuba Magnet Laboratory.Nb/Al precursor wires are rapidly heated and quenched toprepare a supersaturated bcc solid solution once and thentransformed into Nb3Al by additional heat treatment.Unlike the low-temperature diffusion method, this methodproduces stoichiometric and fine microstructures and fea-tures high non-Cu Jc over the whole range of magnetic fieldup to 20 Tesla or more. Excellent strain tolerance is notlost. NIMS is also developing wires jointly with the HighEnergy Accelerator Research Organization, Japan AtomicEnergy Agency, and National Institute for Fusion Sciencefor the next-generation accelerator and fusion reactor aswell as for high-field NMR. Regarding making long-lengthwire, a Nb/Al precursor wires of 2.5 km long were success-fully manufactured. Techniques for rapidly heating andquenching such long wires, and also for stabilizing thewire, need to be developed urgently. NIMS is now devel-oping a method of mechanical cladding after RHQ opera-tion for NMR uses, an internal stabilization technique ofdispersing Nb-jacketed Ag-rods for accelerators and fusionuses, and also a copper ion plating/electroplating method. Itwill also be necessary to take measures against a flux jump,to pin the flux line by nano-scale microstructure, and tooptimize the transformation processing conditions toenhance non-Cu Jc.

Regarding Nb3Sn, NIMS started research in 2003 toraise Jc by a new method using a Cu-Sn compound (εphase, η phase) having a higher Sn concentration thanbronze as the starting material. The future tasks are toenhance and stabilize the Jc characteristic and to extend thelength. Regarding the bronze-route Nb3Sn, a basic studywas also started to convert the residual bronze into copperby selective oxidization of Sn, after the Nb3Sn-formationheat treatment.

Regarding MgB2, NIMS started fabricating wires by thePIT method immediately after Aoyama Gakuin Universitydiscovered its superconductivity in 2001. NIMS used theex-situ method that fills MgB2 compound power into ametallic tube and the in-situ method that fills Mg and Bblended powder into a metallic tube and generates MgB2 byheat treatment. In the latter method, we used MgH2 powderinstead of Mg powder because the surface of commerciallyavailable Mg powder was found to be partially oxidizedand this suppressed reaction between Mg and B. SinceMgH2 was decomposed at around 450˚C and became Mgpowder having an active surface, and thereby the denseMgB2 cores were achieved and Jc was successfullyincreased. It became clear that adding SiC nanoparticles tothe mixed powder of MgH2 and B improves the high mag-netic field characteristic and raises Bc2 at 4.2 K to 23 Tesla,about equal to that of Nb3Sn. The compound Jc at 20 K is600 A/mm2 at 3 Tesla, which is far too low for practicalpurposes. From thin film and other data, a grain boundarywas proved to be an effective flux-pinning center. In future,one research approach to improve Jc dramatically will be to

93


reduce the grain size to the scale of single- or double-digitnanometers. NIMS also began to develop a method thatuses Mg2Cu instead of MgH2 as the starting material. WhenMg2Cu is used as the starting material, MgB2 formation ispromoted and high Tc can be obtained by short-time heattreatment at low temperature.

Regarding alloy-type superconducting materials, NIMSbegan to study a constitute-element diffusion method thatdoes not require the melting and casting process.

5. Future outlook

Compared with compound-type superconducting materi-als, alloy-type superconducting materials are very easy tohandle and allow easy coil rewinding, for example. There-fore, many magnet designers wish to build equipment thatpartially uses Nb3Sn all with alloy-type superconductingmaterials if a high magnetic field becomes available forsuch alloy-type wires. It is therefore important to raise theavailable magnetic fields with Nb-Ti and other alloy-typesuperconducting wires. One effective way to increase Jc ofalloy-type superconducting materials remarkably is tointroduce nano-size artificial pins, which are being investi-gated by Tokyo Metropolitan University and other insti-tutes, but costs will need to be reduced for practical use.

Regarding Nb3Sn, Tokai University has been developinga new method that superimposes a Sn sheet made of Ta-Sncompound powder on an Nb sheet and inserts them into anNb tube, and will now start research on lengthening andstabilizing.

Regarding MgB2, currently Cu, Fe, SUS, and steel areused as sheath materials but magnetic sheathing materialsare not favorable for precision magnetic field or AC appli-cations. For wire drawing, hard materials are preferable for

high filling density. In relation to making a multifilamen-tary structure, incorporating stabilizers, and developing thesuperconducting joint technique, the selection of sheathingmaterials will be important. Since it is essential to improveJc, the introduction of effective pinning centers is a matterof some urgency.

In addition, it will probably be important to developsuperconducting materials supporting low induced radioac-tivity with a view to a post-ITER fusion demonstrationreactor. The lightweight superconductor MgB2 has lowinduced radioactivity even against neutron irradiation. Thedevelopment of a lightweight V-base conductor is alsoworth noting.

In 2005, a paper from the user’s perspective rather thanthe manufacturer’s appeared in an academic journal onsuperconductors and attracted much attention. This paper6)

discussed how superconducting material costs for the next-generation accelerator should be determined and what mul-tiple of the raw material cost would be an appropriate pricefor such materials. Research on metallic superconductors,aimed at achieving a balance between high performanceand low cost, will surely become more active.

References

1) K. Marken, 2004 Appl. Supercond. Conf., Jacksonville, 2MW05.2) The Japan Institute of Metals 68, No. 9 (2004) “Superconducting

Materials - Materials Science to Practical Use”.3) http://www.asc.wisc.edu/plot/plot.htm4) Cryogenic Engineering 39, No. 9 (2004) “Current Status and Future

Outlook of Nb3Sn Wires - Commemorating 50 Years afterRecovery”.

5) Cryogenic Engineering 38, No. 11 (2003) “Development of MgB2

Materials”.6) L. D. Cooley et al., Supercond. Sci. Technol. 18, R51, (2005).

94


1. Introduction

Magnetic materials are key industrial materials that areused in various applications such as magnets, inductorcores, sensors, data storage media, and recording heads.Components made of magnetic materials are used in vari-ous industrial areas including electrical communication,power electronics, and transportation. The scale of industri-al applications of magnetic materials is much larger thanthat of superconducting materials, but their importanceappears to be underestimated in the materials science com-munity probably because the research field is regarded asfully matured. As mobile electrical communication equip-ment becomes more and more compact, the magnetic mate-rials for data storage and electronic circuits are required toexhibit even better properties for downsizing. The improve-ment of the performance of the permanent magnets formotors and generators, and that of soft magnetic materialsfor power electronics transformers would result in signifi-cant energy savings.

Japan was once a leader in the fields of permanent mag-nets, soft magnetic materials, and magnetic recordingindustries. Around 1985, researchers of magnetic materialswere observing research trends in Japan. After the 1990s,however, Japan quickly lost its competitive edge and theUnited States gained strength in the magnetic recordingindustry. The research and manufacture of permanent mag-nets is now shifting to China. Since magnetic materialshave a great industrial impact as mentioned above, indus-try, universities, and governmental labs need to make astrategic research plan on magnetic materials research,which will in turn increase Japan’s industrial competitive-ness.

2. Permanent magnet materials

2.1 Research trendsFigure 1 shows the annual trend in the maximum energy

product of permanent magnet material. Approximatelyevery 20 years, there were breakthroughs in the maximumenergy product corresponding to the developement of newcompounds for permanent magnets. The most recent break-through was the invention of the Nd2Fe14B sintered magnetby Sagawa of Sumitomo Special Metals in 1982. Sincethen, optimization of the microstructure constantlyimproved the maximum energy product. However, during

the past 20 years, no new magnetic materials superior tothe Nd2Fe14B compound have been found and the increasein energy product is becoming saturated.

There are two approaches for achieving another break-through in the future. The first one is to discover a com-pletely new ferromagnetic compound that surpassesNd2Fe14B, but there are no guidelines for this approach.Compositional search without guiding principles has anextremely small chance of success; there is no way to findnew materials other than predicting compounds havinghigh magnetocrystalline anisotropy and saturation magneticflux density using a computational materials scienceapproach. The second one is nanostructure control. Thecoercive force of the current Nd2Fe14B sintered magnet isno more than about 15% of the ideal coercive force, theanisotropic magnetic field HA, which can be estimated fromthe coherent rotation of fully isolated single-domain parti-cles. Increasing the coercivity to 50% of HA, for example,would greatly improve the performance of the magnets. Todo so, we must understand why the current magnet materi-als cause magnetization reversal at only 15% of HA. Themagnetization reversal of a sintered magnet is consideredto occur when a reverse magnetic domain is nucleated froma locally low anisotropy area at grain boundaries. Thenanostructure control of the grain boundary structure withan understanding of this mechanism may significantlyimprove the performance of permanent magnet materials.According to recent theoretical predictions, the maximumenergy product that is higher than that of single-phase mag-net can be obtained by the nanocomposite of a hard mag-netic phase with a high magnetocrystalline anisotropy and asoft magnetic phase with a high saturation magnetic fluxdensity. Based on this theoretical calculation, nanocompos-ite magnets are now actively investigated. Thus, controlling

95


Fig. 1 Annual changes of the energy products of permanent magnets. 1)

Chapter 3. Magnetic Materials

Kazuhiro HohnoFellow, NIMS

the nanostructure of magnet materials may give break-through in the performance of permanent magnets.

2.2 Future outlookPermanent magnet materials are mainly used for indus-

trial motors. In Japan, the power consumption of motors isestimated to be about 53% of the total power consumption.Therefore, development of a high-performance magnet thatcan improve motor power efficiency by 1% was estimatedto save electric power equivalent to one small-scale nuclearpower plant.2) This is just one example of the potentialimpact of development of a higher performance permanentmagnet. Since the Kyoto Protocol was enacted, automotivemanufacturers have been working to achieve fuel savingsand to suppress carbon dioxide emissions by reducing vehi-cle body weights. About 25 to 30 motors are used on eachautomobile, so enhancing the permanent magnet perfor-mance would significantly reduce the vehicle weight. Forenvironmental friendliness, automobiles will change tohybrid cars and then eventually to electric cars. For thistransition, permanent magnets usable at 200°C are essen-tial. Figure 2 shows the energy product, coercive force, andbasic alloy composition of commercial Nd2Fe14B perma-nent magnets. The motor of an electric automobile requirescoercive force as high as 30 kOe at room temperaturebecause the coercivity decreases as temperature reaches theoperating temperature of the motors of hybrid cars. Thecurrent Nd-Fe-B sintered magnets on the market containthe heavy rare earth element Dy to increase the coerciveforce. However, this addition has the serious disadvantageof reducing magnetization, thereby decreasing the maxi-mum energy product. A large amount of Dy is added to themagnet for an electric car, which secures coercive force butreduces the energy product. The natural resource of Dy isquite limited and China alone accounts for almost the entireworld production. If Nd magnets with Dy contents beyondthe natural abundance are supplied in large quantities forelectric car manufacturing in Japan, the Dy market pricewill soar and electric car manufacturing in Japan will beaffected by the supply of Dy raw materials. To avoid thissituation, development of a permanent magnet that can pro-duce coercive force without Dy addition is strongly

desired.Theoretically, the nanocomposite magnets that are com-

posed of exchange coupled hard and soft phases are expect-ed to achieve maximum energy products that are higherthan those of conventional sintered magnets. However, theNd-Fe-B nanocomposite magnets that were recently com-mercialized do not exhibit higher performance than the sin-tered magnets because they are isotropic magnets. Sincethe rare earth content is lower than that for sintered mag-nets, the Nd-Fe-B nanocomposite magnets are only used asmedium-performance permanent magnets with low costand good corrosion resistance.3) However, if the crystal ori-entation of the hard magnetic phase can be aligned to a cer-tain direction, an anisotropic magnet with higher maximumenergy product may be achieve. In fact, it has been demon-strated that an energy product that is higher than the theo-retical limit of a single-phase magnet can be achieved byfabricating the ideal anisotropic nanocomposite microstruc-ture in a multilayer thin film.4)

There is a strong demand for developing thin film mag-nets of approximately 100 µm thick for various applica-tions in portable information devices and MEMS. Sincethe nucleation of a reverse magnetic domain occurs fromthe surface processed layer, the coercivity of magnets islost when bulk magnets are processed to less than 100 µmthick,. Therefore, there is a growing interest in developingan industrial production method of high performance thinfilm magnets .

These days, the number of university laboratories thatstudy permanent magnet materials are decreasing in Japan.If this trend continues, universities will no longer be able toconduct fundamental research to support the industrialresearch and development of permanent magnets, whichwill seriously affect permanent magnet research in Japan.Since the development of high-performance permanentmagnets is expected to give large industrial and environ-mental impact, it is necessary to promote national projectswhereby scientists from universities, public research sec-tors and industries can participate in research and develop-ment of high performance permanent magnets.

3. Soft magnetic materials

3.1 Research trendsSoft magnetic materials can be roughly classified into

those used for transformers and those used as inductorcores of electronic circuits. For the former, electric steelhad been used for a long time in large quantities. Althoughthere were attempts to use amorphous alloys as transformercores in the 1980s, Japan quickly gave then up because ofinternational patent disputes. Since environmental prob-lems have become a major issue today, transformers withmagnetic cores made of amorphous alloys have begun toappear on the market. In 1988, Yoshizawa from HitachiMetals invented the Fe-Si-B-Nb-Cu nanocrystalline softmagnetic material. Since the Fe contents of the nanocrys-talline soft magnetic materials are higher than those ofamorphous soft magnetic alloys, higher saturation magneticflux density is achieved. With their high magnetic flux den-

96


Ene

rgy

prod

uct (

MG

Oe) MRI, speaker HD, CD, DVD, MD, VCR, digital camera, headphones

ABS sensor

OA/FA motor

ServomotorAir-conditioner motor

Robot motorGenerator

Electric car motor

Coercive force (kOe)

Fig. 2 Characteristics, uses, and compositions of Nd-Fe-B sinteredmagnets (by Sagawa).

sity and extremely high permeability, the new material isbeing used for magnetic cores for choke coils and smalltransformers.5) The nanocrystalline soft magnetic materialis inferior to silicon steel in magnetic flux density but hasextremely high permeability. Both the permeability andmagnetic flux density are superior to those of amorphousalloys. Recently, Co is added for high induced magneticanisotropy to improve the material as a magnetic materialthat can be used in the high frequency range. Unlike amor-phous soft magnetic materials, the magnetic properties ofnanocrystalline soft magnetic materials are sensitive totheir microstructures. Thus, the mechanism of nanocrys-talline microstructure formation by amorphous crystalliza-tion has also been actively investigated.6) More recent stud-ies are clarifying the origin of induced magneticanisotropy.7)

With the recent increase in the size of data communica-tion in mobile phones, the frequencies of electronic infor-mation devices have reached the GHz band. In addition, theminiaturization of mobile equipment is causing electromag-netic interference in electronic circuits of high mountingdensity. This is hampering further miniaturization andtransfer to higher frequencies. Thus, the development ofsoft magnetic materials that can be used in the GHz band isrequired. Under these circumstances, nanogranular softmagnetic materials are being developed by dispersingnanoscale ferromagnetic particles in oxide matrixes.8)

Soft magnetic materials are also being investigated forthe applications to magnetic recording heads or as softmagnetic underlayer for perpendicular recording media.For a recording head to generate a large magnetic field, amaterial of high magnetic flux density is necessary.Numerous research activities have been performed on ironnitrides, with the expectation that they might have huge sat-uration magnetic flux densities. However, due to poorreproducibility of experimental results, recent studies castdoubt on the possibility of achieving a large magneticmoment. Therefore the research is shifted to more practicallevel such as how to enable Fe65Co35 alloy that has thelargest saturation magnetic flux density to be processed assoft magnetic thin film. Since coercivity of lower than 10Oe is sufficient for the application to a recording head, softmagnetism is achieved by hybridization of the Fe65Co35

alloy with Permalloy and nanocrystallization by nonelec-trolytic plating.

3.2 Future outlookOne of the breakthroughs in soft magnetic materials is

the development of Fe-base nanocrystalline soft magneticmaterials by Yoshizawa in 1988. Although there have beenno further breakthroughs since then, development of higherperformance soft magnetic materials is still required tomeet various demands for the advanced electric communi-cation devices and for increasing the areal density of mag-netic recording. Since the frequency range of electrocom-munication is increasing to transfer large digital amounts ofinformation, the development of high resistance soft mag-netic materials that can be used in the GHz range isrequired. The enhancement of recording density is reducingthe recording bit size to the nanoscale dimension, which

requires the use of recording media having high magne-tocrystalline anisotropy to maintain the thermal stability ofthe magnetization of ferromagnetic nanoparticles. As aresult, the coercivity of future recording media will becomevery high, and new materials with saturation magnetic fluxdensities beyond 2.4 T, which is the upper limit of the cur-rent FeCo alloy, will be required for recording heads.Searching this kind of material without any guiding princi-ple will be extremely difficult. Exploring such materialswith higher magnetization will only be possible with theaid of the prediction based on computational materials sci-ence. Many investigations reported that FeCo thin filmsshow soft magnetic properties if they are grown on aPermalloy or as multilayer with soft magnetic materials,but the mechanism of this is not yet understood. Under-standing this mechanism will also provide a guideline fordeveloping even better soft magnetic materials.

4. Magnetic recording media

4.1 Research trendsThe magnetic recording system of a hard disk drive

(HDD) can be classified into longitudinal recording andperpendicular recording, and is now changing from the for-mer to the latter. The longitudinal recording method uses athin film of Co-Cr base alloy where easy axes are orientedin the plane. When a Cr underlayer is deposited on a glasssubstrate by the sputtering method, the (011) plane, thedensely packed plane of a bcc metal, is preferentially ori-ented. When a Co-Cr base alloy of an hcp structure is sput-tered on the textured Cr underlayer, the (10

–11) plane grows

epitaxially. In addition, the preferred orientation of the Cr(001) plane develops under an appropriate condition, whichmakes the c-axis of the hcp Co-Cr completely in the planeof the film. If the Co-Cr based alloy film is deposited onheated substrates of about 300°C, phase separation pro-gresses according to the miscibility gap of the hcp phase inthe Co-Cr system, and Cr is segregated at grain boundaries.Because of the formation of Cr-rich grain boundary phase,Co-rich grains are magnetically isolated from each other,making the microstructure that is suitable for recordingmedia. The current longitudinal recording media contain Ptto enhance anisotropy and Ta to promote Cr phase separa-tion. In the longitudinal magnetic recording method, ferro-magnetic grains are magnetized in the in-plane direction bya leakage field from a ring head. For longitudinal magneticrecording, reduction of film thickness is required becauseof the increasing demagnetizing field between the record-ing bits as the recording density increases. Since the headsignal become weak accordingly, the recording limit isexpected to be around 100 Gbit/in2.

On the other hand, the perpendicular magnetic recordingmethod uses the media structure having the easy axis per-pendicular to the plane. Magnetization opposite to the ver-tical direction becomes stable by magnetostatic interactioneven when the bit size becomes nanoscale. In 1979, Iwasa-ki at Tohoku University proposed the perpendicular mag-netic recording method that can enhance the recording den-sity much higher than the limit for the longitudinal record-

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ing method. After about 25 years, the perpendicular record-ing method is about to be used commercially.9) In the per-pendicular magnetic recording media, the c-axis of hcpmust be oriented perpendicular to the plane. Cr is segregat-ed at the grain boundaries using the same principle as thelongitudinal recording method, which decouple the ferro-magnetic particles magnetically. Current research interestin perpendicular magnetic recording media is directed togranular-type media, in which CoCrPt columnar grains areisolated by the SiO2 matrix.9) To achieve 1 Tbit/in2 magnet-ic recording in the future, the size of magnetically isolatedferromagnetic particles is estimated to be approximately 5nm in the granular media having the bit size of about 65 nmand the distance between the head and media is 5 nm.However, such a recording system would be extremely dif-ficult to achieve. Due to various technical restrictions, theupper limit of the perpendicular recording method is esti-mated to be 600 Gbit/in.10) Therefore, a completely newrecording method must be developed to achieve a recordingdensity of 1 Tbit/in2.

To ensure a bit size of about 65 nm and an adequate S/Nratio at a recording density of 1 Tbit/in2, the media must becomposed of 5 nm isolated ferromagnetic particles. For ahigher density of about 10 Tbit/in2 in future, magneticinformation must eventually be written to individual ferro-magnetic particles, then the thermal stability of the magne-tization of the nanoparticles will become a serious problem.If the magnetocrystalline anisotropy is Ku and the volumeof crystalline particles is V, the thermal barrier becomesKuV. If the thermal barrier is 60 times the thermal energykBT, the recording information could be maintained for 10years. To achieve the recording density of Tbits, therefore,a ferromagnetic phase of sufficiently high Ku must beselected as the recording media material. Ku of L10-FePt isone order of magnitude higher than that of hcp Co. This iswhy FePt is regarded as the most promising recordingmedia. Nd2Fe14B, SmCo5, and other permanent magnetmaterials also have high magnetocrystalline anisotropy butare not suitable as media because they are inferior in corro-sion resistance. Therefore, the research interest in the mag-netic properties of FePt, SmCo5, and other high Ku materi-als thin films has increased recently.

However, most research activities are concerned withthe perpendicular magnetic anisotropy and high coerciveforce of continuous films of high Ku materials and are farfrom the stage of application to media. In the future, moreresearch efforts are needed to process the thin-film struc-

tures that are suitable for magnetic recording media usingthe high Ku materials. The films as recording media musthave the following features: (1) magnetically isolated parti-cles of approximately 5 nm with narrow size distribution,(2) c-axes must be oriented in the direction normal to thefilm plane, (3) FePt particles must be fully ordered to theL10 structure without high temperature annealing, and (4)the switching field must be reduced for writable mediawhile maintaining the energy barrier. All of these are chal-lenging problems and it may take more than 10 years tosolve then. Since the switching field of FePt particles ismuch higher than the magnetic filed that can be generatedfrom the current write head materials, a new recordingmethod such as heat assisted recording will have to beintroduced. Since FePt media are expected to be seriouslyconsidered when the areal density of the current perpendic-ular recording method reaches its highest limit, there is stillsufficient time for further research.

4.2 Future outlookTo increase the recording density by the perpendicular

magnetic recording method, a media material having a highcoercive force is becoming necessary, and recording by thecurrent heads is becoming extremely difficult. Therefore,an oblique recording system with high Ku materials orient-ed obliquely12) and nanocomposite media with exchangecoupled soft and hard phases13) is proposed. Materialsresearch to attain these media structures will becomeactive.

As a recording method to be employed after the perpen-dicular recording method has reached the limit, the thermalassist method using FePt self-assembled nanoparticles isproposed.11) However, there are still many issues to beresolved for adapting FePt to a media structure that is suit-able for the thermal assist method, such as the process toorder FePt nanoparticles to the L10 structure, the two-dimensional arrangement of nanoparticles, the suppressionof the coalescence of particles by thermal treatment forordering, and the alignment of the easy axis of FePtnanoparticles.

5. Materials for magnetoresistance devices

5.1 Research trendsThe conventional hard disk drives employed magneto-

resistive heads using the anisotropic magneto-resistanceeffect of Permalloy. Since MR head sensitivity is given bythe voltage output per unit track width, the output decreasesas the recording density becomes higher and the trackwidth becomes smaller. To overcome this problem, IBMemployed a GMR head for a hard disk drive for the firsttime in 1997. The GMR device uses the giant magneto-resistance phenomenon that was discovered by Fert for thefirst time with an Fe/Cr/Fe artificial lattice in 1988. If amultilayer film of Fe/Cr/Fe is fabricated by changing theCr film thickness, the antiferromagnetic coupling of two Felayers with an appropriate Cr layer thickness reverses thedirection of magnetization. Applying a unidirectional mag-netic field to this film makes Fe magnetization parallel. If a

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Fig. 3 3D nanostructure of CCP-CPP spindle valve. 15, 16)

current is applied to this kind of element, electrons causespin-dependent scattering with a relative magnetizationchange of Fe, and the electric resistance changes accordingto the magnetic field. However, if an antiferromagneticcoupling is used, a large magnetic field is necessary formagnetization reversal. To allow the magnetization rever-sal in a lower magnetic field, an element called a spin valvewas developed. If FeNi or similar soft magnetic layers areused for ferromagnetic film and a soft magnetic layer onone side with a nonmagnetic field in between is pinned byan antiferromagnetic phase, such as L10-FeMn, the magnet-ic field sensitivity of electric resistance change becomesextremely high because magnetization reversal occurs at alow magnetic field.

Thanks to the improved sensitivity of the GMR head,the recording density of HDDs has increased to 4 Gbit/in2.However, to achieve areal density exceeding 10 Gbit/in2, aGMR head of a simple configuration is not sufficient.Because of this limitation of the read heads, the rate ofincrease of recording density is slowing down. For an arealdensity over 40 Gbit/in2, a GMR head of higher sensitivityis required. The GMR head so far is of the current-in-planetype in which the current flows in parallel to the multilay-ers. A current-perpendicular-plane (CPP) spin valve isexpected to show a greater regenerative output because theelectron scattering occurs not only at the interface but alsowithin the ferromagnetic electrode layers. The CPP spinvalve with the current-confined path (CCP) structure isexpected to exhibit an even higher MR value. A metallicnanobridge is self-organized in an oxide layer of severalnanometers thick and the current is constricted in thenanobridge to increase the MR value. This kind of devicehas a complicated three-dimensional nanostructure asshown in Figure 3 and detailed nonstructural informationcannot be acquired only by cross-sectional TEM observa-tions. Now that the properties of magnetoresistive devicesare dominated by the three-dimensional nanostructures, ahighly sophisticated nanostructure analysis technique mustbe employed for device development.

The GMR structure has a metallic nonmagnetic layerbetween two ferromagnetic layers. If the two ferromagneticlayers are separated by an oxide layer, electron transportoccurs by tunneling. Since spin-dependent scatteringoccurs even in the case of electron tunneling, a MR effectappears. This type of MR is called tunneling magneto-resistance (TMR). TMR is electron conduction by tunnel-ing and was considered unsuitable for applications to a readhead because of large electric resistance. Recently, howev-er, a TMR junction of low electric resistance with a MRvalue of 230% was developed.17) The TMR value is consid-ered to follow Julliere’s formula, TMR = 2P1P2/ (1–P1P2),where P1 and P2 are spin polarization of ferromagneticmaterials. If a half metal with P=1 is used as the ferromag-netic electrode, an infinite value of TMR is predicted. Thisis the reason why tunnel junctions with half-metal elec-trodes receive so much research interest now. Althoughthere are various types of half-metals like oxides andalloys, Heusler alloys are considered to be most promisingmaterials as ferromagnetic electrode for TMR junctionsbecause some of the Heusler alloys have Curie tempera-

tures that are higher than room temperature. Nevertheless,only TMR values of less than 16% have been obtained sofar even from the TMR junctions with the Heusler alloyelectrodes whose spin polarization are theoretically predict-ed to be 1.18) To achieve high TMR values from the TMRjunctions using the Heusler alloy electrodes, the spin polar-ization of the ferromagnetic electrodes must be determinedexperimentally, as high spin polarization was predictedfrom fully ordered L21 phase. Since sputtering is a highlynonequilibrium process, it is very unlikely that equilibriumL21 phase is formed from the as-sputtered conditions. Inmany previous investigations, the structure of electrodefilms has not been characterized thoroughly and the spinpolarization was estimated from the TMR values experi-mentally measured from the TMR junctions. To achieve alarge TMR value in the near future, the characterization ofelectrode phase and the analysis of interface structure arenecessary in addition to TMR measurements.

While many groups have been trying to realize largeTMR values with half-metal tunnel junctions, Yuasa et al.at the Agency of Industrial Science and Technology suc-cessfully manufactured a Fe(001)/MgO(001)/Fe(001) tun-nel junction with rigorous interface control at the atomlevel and demonstrated a TMR value as great as 88% atroom temperature.19) This is because the MgO single crystalhas a spin filtering effect, so that the MR value can beenhanced. The electrodes were then changed to amorphousFeCoB to achieve TMR as great as 230%17) and are nowexpected to be applicable to MRAM in the future.Although TMR devices were considered unsuitable forread head applications because of their large electric resis-tance, the electric resistance was successfully reduced withthe TMR junction using an ultrathin MgO single crystallineinsulator layer.

5.2 Future outlookThe bottleneck in increasing the areal density of magnet-

ic recording is the development of an read head. A GMRelement of higher sensitivity is always necessary. The con-ventional simple multilayer film structure is not sufficientto achieve high magnetoresistance and GMR devices arebecoming complex 3D nanostructures in which electronpaths are constricted in narrow metal paths. Head manufac-turers are fiercely competing in development, and large-scale film deposition and microfabirication facilities arenecessary for the development of GMR devices. Devicedevelopment and application can no longer be competitivesubject among universities or national laboratories. In thefuture, collaborative research programs for industry, acade-mia, and governmental labs are necessary, and universitiesand national labs should share the research effort towardunderstanding basic principles and characterization of high-ly complicated nanostructures.

The largest TMR so far reported was acquired from theTMR junctions using coherent MgO insulators. Half-metalTMR should theoretically produce a large TMR value andfurther research is necessary. Since the research method ofmanufacturing a tunnel junction first and measuring its MRvalues has reached its limit, the research direction shouldbe changed to acquire better understandings of the process-

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ing conditions for half-metal electrodes. We also need atechnique for measuring the spin polarization of ferromag-netic films directly. Thereafter, we should try to fabricatejunctions from the electrodes that have been confirmed tohave high spin polarization. Before device development,we should understand the intrinsic properties of electrodematerials.

6. Current status and future activities of NIMS

As part of the 5-year project on “Development of newadvanced nanohetero metallic materials” supported by theSpecial Coordination Funds on Science and Technology,NIMS coordinated the collaborative research program forindustry, university, and governmental labs. In this pro-gram, NIMS carried out fundamental researches on thecharacterization of nanostructures of magnetic materials,such as nanocomposite magnets, nanocrystalline soft mag-netic materials, nanogranular soft magnetic materials, andFePt thin films. The nanostructure analysis results wereused to optimize the nanostructures of the materials toobtain improved properties.20)

As to nanocomposite magnets, NIMS systematicallystudies the effects of adding alloying elements onnanocomposite microstructure and magnetic propertieswith NEOMAX and has greatly contributed to their devel-opment of medium-performance permanent magnet materi-als. To verify the possibility of surpassing the properties ofthe current sintered magnet by nanostructure control, NIMSfabricated a [Sm(Co,Cu)5/Fe]6 anisotropic nanocompositethin film and proved that it could realize an energy productthat is higher than the theoretical limit of a single-phaseSmCo5 magnet. Regarding nanocrystalline soft magneticmaterials, NIMS proposed a nanostructure control methodfor the Co-added Fe-Si-B-Nb-Cu type nanocrystalline softmagnetic materials with Hitachi Metals, and contributed tothe development of soft magnetic materials with high fre-quency properties. By clarifying the mechanism of inducedmagnetic anisotropy of stress-annealing, NIMS establisheda guiding principle for achieving the nanocrystallinemicrostructure that is suitable for high frequency applica-tions. As to the nanogranular soft magnetic materials, softmagnetic properties and induced magnetic anisotropy wereexplained from the viewpoint of the nanostructures.Regarding the FePt thin films as a potential ultrahigh-den-sity magnetic recording media of the next generation, themechanism of ordering by low temperature annealing wasclarified and the size dependence of ordering was discov-ered. In addition, it was demonstrated that the switchingfield could be lowered remarkably by nanocompositemedia without impairing the thermal stability of thenanoparticles. Some of the nanostructures observed in themagnetic materials were modeled by the phase-fieldmethod in the computational materials science group, andthe conditions required to optimize the nanostructure forbetter magnetic properties were predicted.

In the next 5-year plan starting from FY2006, NIMSaims at establishing a guideline for developing nanostruc-tured magnetic materials for the ubiquitous society from

the viewpoint of materials science through the project“Development of high performance nanostructured mag-netic materials by nonstructural control.” To achieve thisgoal, experimentally fabricated magnetic materials andspintronics materials will be studied in view of nanostruc-ture and magnetic properties, and their relationships will beestablished. The nanostructures of the following materialswill be thoroughly characterized with atom scale resolu-tion: Application to magnetic recording techniques – (i)thin film for high-density magnetic recording media, (ii)soft magnetic materials of high magnetic flux density forrecording heads, (iii) CPP-GMR spin valve for HDD heads,and (iv) half-metal thin film for TMR devices; applicationto an electromagnetic noise absorber for small mobileequipment – (v) nanogranular soft magnetic thin film forhigh frequency; application to magnetoelectric microsys-tems (MEMS) – (vi) thin-film permanent magnet materials.Based on the acquired knowledge, data storage techniquesand nanomagnetic materials for GHz band electronics willbe developed to establish a guideline for materials sciencefor the corporate development of magnetic device systems.

7. Conclusions

Since it is not possible to cover all of various magneticmaterials, this article reviewed the current status and futuretrends in the fields related to NIMS research activities. Sofar, NIMS has not made serious effort in the research anddevelopment of magnetic materials. However, NIMS willset clear goals for the research of magentic materials in thenext 5-year plan. Among various magnetic materials,NIMS will put its emphasis on the materials whose proper-ties are expected to improve through nanostructure control.NIMS is devoted to research on magnetic materials that arenecessary for developing devices and systems because it isnot practical to compete with industry research in thedevelopment of magnetic devices and their applications.While strengthening the linkage between industry, univer-sities, and governmental labs as far as possible, NIMS willproceed with basic research in its strongest field. NIMS hasthe potential to conduct complementary research withindustries in the fields of nanostructure characterization,understanding mechanisms, predicting microstructure evo-lution, and measuring magnetic properties using high mag-netic field facilities.

References

1) M. Sagawa, Proc. 18th Inter. Workshop on High PerformanceMagnets and Their Applications, Annecy, France (2004) pp. 7

2) Subsidized general research in FY2000 Interim report of “Researchfor the fabrication of new metallic materials by clarifying thefunction manifestation mechanism of nano-hetero metals”subsidized by the Science and Technology Fund in 1999

3) S. Hirosawa, Trans. Magn. Soc. Jpn, 4, 101 (2004)4) J. Zhang, Y.K. Takahashi, R. Gopalan, and K. Hono, Appl. Phys.

Lett., 86, 122509 (2005)5) http://www.hitachi-metals.co.jp/prod/prod02/p02_21.html6) K. Hono, M. Ohnuma, D.H. Ping and H. Onodera, Acta. Mater, 47,

997 (1999)

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7) M. Ohnuma, K. Hono, T. Yanai, H. Fukunaga and Y. Yoshizawa,Appl. Phys. Lett., 83, 2859 (2003)

8) H. Shimada, The Magnetic Society of Japan, 26, 135 (2002)9) http://www.toshiba.co.jp/about/press/2004_12/pr_j1401.htm

10) T. Shimatsu, H. Sato, T. Oikawa, Y. Inaba, O. Kitakami, S.Okamoto, H. Aoi, H. Muraoka and Y. Nakamura, IEEE Trans.Mag., 40, 2483 (2004)

11) D. Weller, IEEE Distinguished Lecturer (2004)12) K. Gao and H. Bertram, IEEE Trans. Magn., 38, 3675 (2002)13) R.H. Victora and H. Shen, IEEE Trans. Magn., 41, 537 (2005)14) O. Kitakami, Jpn. J. Appl. Phys., 42, L455 (2003)15) H. Fukuzawa, H. Yuasa, S. Hashimoto, K. Koi, H. Iwasaki, M.

Takagishi, Y. Tanaka and M. Sahashi, IEEE Trans Magn., 40, 9464(2004)

16) H. Fukuzawa, H. Yuasa, K. Koi, H. Iwasaki, Y. Tanaka, Y.K.Takahashi and K. Hono, J. Appl. Phys., 97, 10C509 (2005)

17) D.D. Djayaprawira, K. Tsunekawa, M. Nagai, H. Maehara, S.Yamagata, N. Watanabe, S. Yuasa and K. Ando, INTERMAG.,CA-01 (2005)

18) K. Inomata, S. Okamura, R. Goto, and N. Tezuka, Jpn. J. Appl.Phys., 42, L419 (2003)

19) S. Yuasa, A. Fukushima, T. Nagahama, K. Ando and Y. Suzuki,Jpn. J. Appl. Phys., 43, L588 (2004)

20) http://www.nims.go.jp/apfim/nanohetero_j.html

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1. Introduction

The history of semiconductor materials as electronicmaterials can be traced back to 1833 when Faraday foundthat the electrical resistance of AgS changes as the temper-ature changes.1) Later, the rectification theory was proposedby using such materials and sulfide and copper dioxide todeepen understanding of the semiconductor band structurebased on quantum theory. During such research, it wasfound that semiconductors could be classified by type ofimpurity into n type and p type and that electrical conduc-tivity can be controlled by the impurity density. RussellOhl of Bell Labs developed a Ge semiconductor in 1939and then a high-frequency diode using Ge. These achieve-ments led to the development of a point-contact diode byBardeen and Brettin of Bell Labs in 1946 and a junctiontransistor by Shockley in 1948.1)

After the War, Teal of Texas Instruments announced aSi transistor in 1954, triggering the modern development ofsemiconductor devices. In particular, Kilby created an inte-grated circuit (IC) in 1958, Homy announced the first pla-nar transistor using photolithography in 1959, then Hof-stein and Heyman of RCA developed the MOS field-effecttransistor (MOSFET) in 1961. Through this series ofachievements, the basic technology for the current Si-typeintegrated circuits was completed. Since then, circuits havebeen further integrated with related materials, mainly Si(substrate and gate), SiO2 (gate oxide film and interlayerdielectric), and Al (electrode and interconnection).

With the advance of integration, however, Moore’s Lawconcerning the pace of integrated circuit development,began to show its limit. Attempts are now being made toextend this limit with new materials.2)

This chapter outlines the changes and future trends inSiMOSFET related materials which account for 90% ormore of all semiconductor devices, as well as the trends inorganic materials and compound semiconductor materials.

2. Research trends

2.1 Current status of SiMOSFET and future materialsFor gates, the current Si devices use hp 65 nm nodes

(hp: half pitch; the actual gate width is 30 nm, about half).The width will finally be reduced to about 10 nm and thepost-scaling generation will begin to emerge around 2015.2)

SiMOSFET related research includes many subjects

regarding materials, such as gate dielectric materials (high-k materials), metal gate materials, interlayer dielectricmaterials (low-k materials), channel materials, and inter-connecting materials.

i) Gate dielectric materials (high-k materials)Existing gate dielectric materials are made of SiON but

materials of greater permittivity will be needed for thenext-generation MOSFET. These are called high-k materi-als. Research on gate dielectrics began to accelerate around1996. For gate dielectrics, amorphous materials noncrystal-lized by adding SiO2 or Al2O3 to high-permittivity oxideHfO2 are regarded as promising. The next dielectrics willbe expected to have higher permittivity, to offer excellentelectrical matching (low interface states) with Si, to notform SiO2 with Si and to withstand high-frequency opera-tion. The probable gate oxides of the next generation arerare earth oxides based on La2O3 that has f electrons. Con-sidering MOSFET operations, the permittivity of gatedielectrics may be limited to about 30. Since this value isdifficult to achieve with amorphous materials, gatedielectrics made by epitaxial growth or similar structureswill emerge eventually.

ii) Gate materialsThe conventional gate materials are made of polycrys-

talline Si metallized by doping impurities to high densities.As integration advances, metals may be used as they are.The requirements are reduction of resistance and control ofwork function; research is underway on metallic nitrides(TiN and other) and metallic silicides (alloys with Si) aspossible candidates. In terms of electrical resistance, how-ever, materials of even lower resistance are expected.Regarding control of work function, there is a growingnumber of reports on intermetallic compounds, metallicnitrides of excess metals, and various metallic silicides. Forcontinuous control of work function, an entirely solid solu-tion is preferable. If the work function is fixed for self-matching, however, alloys having many intermetallic com-pounds may become advantageous. Research on metal gatebegan to take off around 2003 and is still on the increase.

iii) Interlayer dielectric materials (low-k materials)For high-speed signal operation, materials of low per-

mittivity (low-k) are expected for interlayer dielectrics ofmultilayer interconnection. The required permittivity ise=2.7 or less but it is difficult to find bulk materials satisfy-

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Chapter 4. Semiconductor Materials

Toyohiro ChikyowNanomaterials Configuration Group, Nanomaterials Laboratory, NIMS

ing this condition, so the interlayer dielectrics SiO2 is madehollow to create a multipore structure of low permittivity.As next-generation low-k materials, carbon-type andorganic materials of low permittivity are attracting atten-tion and research took off around 1995. However, employ-ing a multipore structure or organic materials results ininadequate structural strength. Integrated circuits also havea serious problem of inadequate strength because they arepolished during the chemical mechanical polishing (CMP)process to make the interlayer dielectrics uniform.2) Forfuture interlayer dielectrics, composite materials should bedeveloped from organic materials of low permittivity andreinforcing materials (structural materials) having mechani-cal strength. These trends are summarized in Figure 1.

iv) Channel materialsThe next-generation devices are expected to operate

faster at high frequency. Therefore, studies are now under-way on varying the effective mass of a carrier and changingthe carrier mobility by straining the channel area and intro-ducing Ge of large mobility into the channel layers of Sidevices.

v) Interconnection materialsAl used to be the main interconnection material for inte-

grated circuits. For high-speed signal operation, however,low-resistance materials were investigated and plated Cuinterconnection is now becoming popular. This materialwill also pose a problem of an increase in resistance due tofine patterning. For higher speed, interconnection materials

of even lower resistance will be necessary. In future, opti-cal interconnecting materials will also be incorporated.3)

For gate interconnection, metallic silicides are formedon polycrystalline Si gates by self-matching. Recently,research was started on the full silicide (FUSI) of this poly-crystalline Si area (see Figure 2).

vi) Other related materialsMagnetic random access memory (MRAM), combined

from magnetic metal films and insulation layers, is nowattracting attention as a material to replace today’s flashmemory. However, MRAM still has many unresolvedissued, such as magnetic intermetallic insulating materialsand large power consumption.

Perovskite oxide materials have a wide range of charac-teristics from conductor to insulator and also dielectric andmagnetic functionalities. Judging from these characteris-tics, perovskite oxide materials will certainly be used assemiconductor related materials in future. Resistance ran-dom access memory (RRAM) that writes and erases databy voltage is now also being developed on the basis of per-ovskite oxide materials, and such research will pick uppace. Figure 3 shows the trend.

vii) Organic materialsResearch and papers on organic devices have also been

increasing since around 1995. Organic devices may be usedfor display elements and other limited purposes becausethey are driven by current control and their electron mobili-ty is far less than that of Si. Since organic materials do not

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produce great environmental loads and can be bent, theymay be applied to devices having different functions (seeFigure 4).

2.2 Compound semiconductorsThe typical material for compound semiconductors is

GaAs, which has been used for light emitting devices andhigh-speed transistors (HEMT). Research in this field hasbeen active since the 1980s and many studies have beenperformed. In 1992 and 1993, research intensified probablybecause new structures, such as quantum wires and quan-tum dots, were proposed and III-V diluted magnetic semi-conductors emerged.

However, GaAs research began to diminish in 1998 andGaN research has been increasing instead. In 2000, the InNband gap was reported to be 0.7 eV, indicating the possibil-ity of achieving a wide range of light wavelength from redto blue by controlling GaInN composition. In addition,GaN-HEMT for the hundred-GHz band using the strongfield resistance of GaN was proposed. Thus, researchseems to be shifting from GaAs to GaN. Figure 5 shows thetrend.

Last year, an LED using ZnO was announced byTohoku University and attracted great attention. UltravioletLEDs made by ZnO are expected to become a new sourceof white light replacing the fluorescent lamp. In terms ofresources and costs, ZnO is superior to GaN.

3. Future development

It is predicted that ArF excimer laser and immersiontechnologies can integrate Si semiconductors up to the hpgate node of 22 nm (actual gate width: 10 nm) by around2015. Until that time, Si devices will surely be the maintype of semiconductor devices. However, many new mate-rials have begun to enter the process. Si-type electronicdevices have so far achieved high speed and functionalityby integration, and this trend will be maintained by chang-ing materials and structures. The tendency toward fasterprocessing speed while maintaining the current process willnot change for the time being. Although MOSFET relatedmaterials were mainly introduced in this report, it is neces-sary to develop other materials, including carbon nanotubeas a plug material for vertical interconnection from source

and drain and also lead-free solder for mounting.Si devices will then enter the post-scaling generation

and their device structures and materials will change.Three-dimensional devices having vertical structures innarrow areas may emerge to replace the conventional two-dimensional ones. FinFET and Tri-Gate transistors areexamples featuring structures.

Among them, MISFET using carbon nanotube (CNT) isattracting attention. CNT is superior to other materials inthat a large ON current can be acquired, the field strength isgreater than that of Si, and impurities can be incorporatedinto CNT without reducing the mobility due to scattering ofthe impurities. Stanford University created an experimentaltransistor using CNT and verified its operation, andresearch on CNT transistors is growing each year (see Fig-ure 6).

A future issue is how to integrate nanodevices. Toshibaproposed an attempt to integrate MOSFET having verticaland surrounded gates.4) Such research may lead to the post-scaling generation of Si devices.

Atomic switches and other devices of atomic-level oper-ations are also expected to emerge in future.5)

4. Conclusion

Si-based electronic devices have been further integratedby micromachining to achieve higher processing speedsand functions, a tendency that will not change even in thepost-scaling generation, and so Si will remain the dominantbasic material for the time being. MISFETs using Ge orCNT, high-frequency transistors using GaN, and opticalinterconnection will also be packaged on a single chip torealize a multifunctional single-chip device. Gatedielectrics, dielectrics between organic layers, and manynew related materials will be developed and will need to beintegrated by gathering knowledge from many fields.

Compound semiconductors can be classified into GaAsmaterials applicable to quantum devices of quantum dots;GaN materials applicable to light emitting devices, lightinginstruments, and high-frequency transistors; and oxidematerials (oxide electronics) to deliver characteristic func-tions.

In 2010, a ubiquitous society will emerge in which all

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equipment and systems are networked through high-speeddata communication networks. Semiconductor materialsare becoming increasingly important as an infrastructure tosupport society, and materials that make many functionspossible will need to be developed accordingly.

References

1) “Semiconductor Engineering” (By K. Takahashi).S. M. Sze, “Physics of Semiconductor Device”, “High-SpeedSemiconductor Device”, “Semiconductor Device”, and others.

2) About Semiconductor Technology Roadmap of Japan http://strj-jeita.elisasp.net/strj/

3) About Si Optics: http://developer.intel.com/technology/silicon/sp/index.htm and other.

4) T. Endoh, M. Suzuki, H. Sakuraba and F. Masuoka, IEEE Trans.Electron Devices, 48, 1599-1603 (2001).

5) K. Terabe, T. Hasegawa, T. Nakayam and M. Aono, Nature, 433,7021 (2005).

105


1. Introduction

For the next generation of medical treatment which issafe and kind for both people and the environment, it isessential to develop biomaterials having biological func-tions that can control the manifestation of functions fromcells and tissues (aggregates of cells and extracellularmatrix). The interaction between organism and materialsbegins with the adsorption of biomolecules to nanostructur-al surfaces and their structural changes, and then progressesto microic and macroic high-degree functions and spaceswith such additional factors as cell adhesion, proliferation,and differentiation and intercellular action. This series ofreactions starts with the mechanism of a nanostructuredreceptor on a cell membrane recognizing a material andtransducing a signal into the cell. This mechanism plays akey role in determining a biological reaction. The recentimplementation of nanotechnologies as tools has enableddetail research on the interaction between materials andcells. From the “nano-bio” area which is a fusion betweennanotechnology and biotechnology, new scientific knowl-edge is being acquired successively and a new knowledgeinfrastructure is starting to be built. Based on this knowl-edge, R&D has started on new functional materials ofmicrostructure and macrostructure control, devices, andcell-material composites.

This section first discusses research on biomaterials,artificial organ materials, and regenerative materials byexamining the transition in the number of papers, and thenlooks at the medical applications of biomaterials as theproduct of R&D in the same way. It also discusses the posi-tion of nanotechnologies in pharmaceuticals relatedresearch, including tissue engineering and drug deliverysystems which are recently attracting attention as applica-tions of biomaterials research. Then the research trends inthe nano-bio fusion area of each materials field is discussedby examining the number of papers, and the research statusfor each type of material is reviewed. In addition, the pastresearch trends are surveyed based on the number of bio-materials studies by each organ. Lastly, the section intro-duces some advanced research activities in related areas,discusses the future directions of these areas, and describes

subjects for future research.

2. Research trends

2.1 Transition in number of papersIn the current survey, we examined papers published in

science magazines from 1970 until 2004. By using key-words related to this section, we searched a database usingSCI Expander as a search engine for papers containing theabove keywords in their titles or abstracts.

First, a materials search with Bio* and a biomaterialssearch (Biomaterial*) were clearly distinguished from eachother. Then the following rough search was performed tocheck the research trends and the implications betweennanotechnologies and nanomaterials. Figure 1 shows theresults of searched papers for the combinations of Bio*,Nano*, and Biomaterial* each with Material*. Regardingpapers containing both the terms Bio and Material, the

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Fig. 1 Number of papers containing the combinations of Bio*, Nano*,and Biomaterial* each with Material*.

Chapter 5. Biomaterials

Section 1. Materials for Artificial Organ and Tissue

Engineering

Hisatoshi KobayashiArtificial Organ Materials Group, Biomaterials Center, NIMS

number of papers started increasing explosively in 1990and reached about 6,500 in the year 2004, totaling 60,300.The number of papers containing the term Biomaterial alsostarted increasing in 1990 and reached about 1,200 in theyear 2004, totaling 8,500. This indicates that the range ofmaterials research expanded to encompass the bio field,and that about 20% of materials research directly concernsmedical applications. Papers were also searched for Nano*and Material* to extract materials research for nanotech-nology applications and nano-sizes. The number of papersstarted increasing dramatically in 1990 and reached about5,500 in the year 2004. To check the fusion of nanore-search and bioresearch which are rapidly growing areas,papers were searched for the terms Nano*, Bio*, and Mate-rial*. The results showed that research in this field startedin 2000. This indicates that the fusion of the areas began topick up speed 10 years after the start of each area. About370 papers were published in 2004, totaling 1,250. To gath-er additional information, the annual number of papers waschecked as of March 2005; the number of published papershad already reached 165, so the number at the end of 2005is estimated to be about double that in 2004, indicating thatthis area has started quickly.

Figure 2 shows the transition in the number of papers ontechnologies, materials, and devices in the fusion area ofNano* and Bio*. In this area, the number of papers startedincreasing remarkably in 1990 and reached 2,700 in theyear 2004, totaling 11,100. Of the papers, the number con-taining the term Material* as a keyword reached about 370in 2004, totaling 1,250 as mentioned before. The number ofpapers containing the term “Technolog*” as a keywordreached an annual output of about 250, totaling about 810.The number of papers containing the term “Device*” as akeyword reached an annual output of about 270, totalingabout 790. This indicates that R&D on materials anddevices has just started in the fusion area of Nano* andBio*. When the annual output of papers by March 2005was surveyed, Material* was found in 165 papers (annual

estimate: 660 papers), Technolog* in 82 papers (annualestimate: 328 papers), and Device* in 83 papers (annualestimate: 332 papers), and so by the end of 2005 the num-ber of papers will reach about 1.3 or 2.0 times that in 2004.These results suggest that practical research on functionalmaterials and devices will accelerate.

Figure 3 shows the results of an AND search for Medic*(medical care) and Therap* (therapy), meaning the fields ofapplication of biomaterials, with Nano* for analysis fromthe aspect of application. Papers containing the termMedic* (for Medicine or Medical) with Nano* began toappear in 1988. The number of papers increased at anannual rate of over 10% until 2001, showed a three-digitincrease in 2002, and reached an annual output of about180 in 2004, totaling about 800. The number of papers con-taining Therap* (for Therapy or Therapeutic) with Nano*also showed the same tendency, reaching an annual outputof about 400 in 2004, totaling about 1,600. This indicatesthat research on the application of nanotechnology to med-ical treatment has taken off quickly. Among medicalresearch fields, the regenerative area is growing remarkablyand attracting much attention as a future medical treatment.Figure 4 shows the results of searching papers for the com-binations of Tissue*, Engineer*, and Regenerative medi-cine each with Nano* to check the situation of regenerativemedicine and related research. The number of papers relat-ed to regeneration started increasing around 1995 andreached an annual output of about 1,800, totaling about8,700. In this area, however, the number of papers relatedto Nano* reached double digits in 2002 and the aggregatenumber until 2004 was only about 220, indicating thatresearch has just started in this Nano area. Pharmaceuticalsresearch represented by DDS and scaffolding materials(Scaffold*) research related to tissue engineering are themain targets of biomaterials research. Figure 5 shows theresults of searching for the combinations of Drug* andScaffold* each with Nano* to check the research trends inthis area. Regarding research on Nano* and pharmaceuti-

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Fig. 2 Number of papers containing Material*, Technology, andDevice* in the fusion area of Nano* and Bio*.

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Fig. 3 Number of papers containing Medic* (medical treatment) andTherap* (therapy) with Nano*.

cals, papers began to appear in 1990. The number of papershas been increasing and reached an annual output of 700 in2004, totaling 3,470. Papers related to regenerative scaf-folding and Nano* began to appear in 2000. The number ofpapers reached an annual output of 150 in 2004, totalingabout 370. This indicates that regeneration related researchstarted even later than pharmaceuticals research. The annu-al number of papers as of March 2005 was 63, and so thenumber of papers is estimated to reach 250 by the end ofthe year, indicating quick fusion with Nano*.

Figure 6 shows the results of searching papers for thecombinations of Inorg* (inorganic), Metal*, and Polym*(polymer) each with Nano* and Bio* to examine researchtrends by materials. Research using polymer materialsbegan to be published actively in 1990. The number ofpapers reached three digits in 1999 and an annual output of600 in 2004, totaling 2,150. In 2005, the annual output isestimated to be about 900, indicating active research. Thisdata reveals that research in the fields of inorganic, metal-lic, and composite materials has started about 5 years laterthan in the field of polymer materials. However, the num-

ber of papers started to surge in 2000, and in 2004 the num-ber was about 300 (1,000 in total) in the field of metallicmaterials, about 130 (520 in total) in the field of inorganicmaterials, and about 180 (515 in total) in the field of com-posite materials. In 2005, the number of papers is estimatedto reach about 1.5 to 2.0 times that in 2004, indicating thatthe scope of research is extending in each field of materialsto cover bio and nano.

Figure 7 shows the results of searching papers for thecombinations of Fiber* or Fibr*, Particle* or Sphere*, andTube* or Tubular* each with Nano* and Bio* to check thetransition in the number of papers by materials. In thefusion field of nano and bio, research using particles is tak-ing the lead, quickly followed by research on fibrous mate-rials. Due to papers on the application of carbon nanotubeto the nanobio area, the number of papers on tubular fibersis increasing but more slowly than those about fibers andparticles.

Lastly, we checked the total number of papers byapplied organs of the body to examine artificial organresearch. Figure 8 shows the results of searching papers for

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Fig. 4 Number of papers containing terms about regenerative medicineand tissue engineering (Tissue, engineer*) with Nano* and about theirfusion research.

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Fig. 5 Number of papers containing Scaffold* (for regenerativemedicine) and Drug* with Nano*.

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Fig. 6 Number of papers containing Inorg* (inorganic), Metal*, Polym*(polymer), and Composite* in the fusion area of Nano* and Bio*.

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Fig. 7 Number of papers by material types (fiber, particle, and tube) inthe fusion area of Nano* and Bio*.

combinations of the major organs and related terms eachwith Bio* and Material*. There is clearly a positiveapproach toward various organs, with active research ontissues and organs of comparatively simple functions, suchas blood, vessel, bone, cartilage, joint, tendon, ligament,and others. Further research is necessary on organs havingmultiple advanced functions such as the liver and pancreas.

So far, we have discussed research trends based on thenumber of papers. Next, we look at the circumstances ofresearch.

In Japan, the framework of nanomedical research isexpanding in each ministry or agency with the rapidadvance of genome analysis and nanotechnology. In theNanomedicine Project, the Ministry of Health, Labour andWelfare is conducting research to enhance diagnostic tech-nology in the direction of preventive medicine. The Min-istry of Economy, Trade and Industry is developing organsby using technology for integrating cell functions forregenerative medicine and conducting R&D for industrial-ization, targeting medical treatment for elderly people. Inthe Core Research for Evolutional Science and Technolo-gy, the Japan Science and Technology Agency is mainlydeveloping polymer materials, DNA, protein nano-tissues,function-integrated chips, and diagnostic technologies tocreate nanostructures where self-organization and othermolecular-order arrangements are controlled on the nano-level.

Regarding global research, nano-tissue, micro-tissue,and macro-tissue structural materials are being researchedindividually, without a systematic approach to the interac-tion between materials and cells. Regenerative medicine isthe most advanced medical technology and there is fierceglobal competition on its supporting biomaterials and cellcomposition technology. For medical applications, howev-er, reproducibility, stability, and precision are key issues tobe solved. An urgent research topic throughout the world isthe safety of nano-materials: rapid progress in nano-materi-als research is producing a succession of high-functionmaterials, but research on the biocompatibility and environ-mental compatibility of these materials lags far behind. Asnational policies, the US and Europe are tackling the bio-

logical expansion of nanomaterials and evaluation of theirsafety by public institutes. In particular, the area of fusionwith bio may be greatly affected by safety issues. Alsofrom the viewpoint of safety evaluation, nanobio is a cru-cial area of research.

2.2 Examples of advanced research in related fieldsThe nanobio research area includes not only direct

research on artificial organs and regeneration which hasbeen considered in this section, but also research on animaging tool to monitor intercellular information transmis-sion and status, research on early high-precision diagnosisof various diseases by quantitatively capturing ultra-tracequantities of biomolecules, and research on nanomedicalequipment. Examples of leading research in these relatedresearch fields are introduced below.

i) Imaging technologyPaul Alivisatos of the University of California in Berkleydeveloped a technology for staining cells with CdSe-CdSshell particles by applying quantum dot technology andindustrialized the research results.1)

Quantum Dot Corporation (California)http://www.qdots.com/live/index.asp

ii) Nanomedical equipmentC.D. Montemagano of Cornell University created a newbiomotor-driven nanomechanical device that drives thepump and valve of a micro-fluid device by converting ATPsynthesis and hydrolytic reaction into mechanical kineticenergy. To apply this research, they are now developingnanomedical equipment.2)

iii) New concept of nanodiagnosisIBM and the University of Basel developed a nanomechan-ical cantilever array. Biomolecules are fixed on the surfaceof the cantilever of the probe microscope. This array sys-tem senses kinetic changes generated by molecule recogni-tion.3)

iv) Tissue engineeringDavid J. Mooney of Michigan University introducednanoparticles sealing arterialization factors as a vasculariz-ing technology indispensable for regenerative medicine anddeveloped cellular scaffolding materials.4)

v) Safety of bionanomaterialsAs an environmental project, DuPont is addressing the bio-logical safety of nanomaterials. By using the SWCNT pul-monary toxicity screening test, they showed that a largedosage (5 mg/kg) could cause 15% of patients to die.5)

3. Conclusion

In the fields of artificial organs and regenerative medi-cine, materials research will be diverse, making it difficultto assess global research trends. However, research willlikely vary from basic materials research in the followingrespects or by techniques given below to applied research,such as device creation for clinical application. The keyaspects and techniques for research are as follows:1. Research to create super-biocompatible materials that

allow active control of cell differentiation and functionmanifestation by controlling their nano-level structures

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Esophagus, stomach,intestines, bladder

Kidney

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Heart

Lung and trachea

Cornea, lens, retina, ear

Nerve

Vessel, blood

Skin

Muscle, tendon, ligament

Bone, joint, cartilage

Number of papers

Fig. 8 Total number of papers about biomaterials by organ.

to avoid foreign-body and immune reactions against thematerials.

2. Materials research to create an environment similar toextracellular matrix by using the inorganic-organic com-position technology and the phenomenon of self-organi-zation.

3. Research to clarify the optimum conditions of spatialnanostructures in terms of cell differentiation or prolifer-ation inducing materials, using the levels of gene andprotein manifestation as indexes, by immobilizing (coor-dinate bond, covalent bond, and hydrogen bond) celladhesion molecules.

4. Research on microstructure and macrostructure controltechnologies to promote the penetration and activationof cells and capillaries.

5. Development of various devices using the above materi-als.

6. Development of cell group formation control technologyto fully utilize the functions of cells (intercellularactions).

7. Development of medical technologies using cells andcell materials having composite functions for artificialorgans.

8. Research on technologies to evaluate the physiochemi-cal characteristics of biomaterials, the surface character-istics of materials, biological molecular adsorption andcell adhesion, and their functional changes under a bio-logical or similar environment.

9. Research to create systems and devices for materialsresearch to clinical applications, including materials andbiological information sensing systems to recognize andmeasure biological function molecules.To develop the next generation of medical materials

which are kind to both people and the environment, com-plementary and comprehensive efforts are needed in theseresearch fields. For practical applications, materials mustbehave safely in human bodies. The current survey ofresearch trends clarified that various materials are being

developed rapidly. However, nanobiomaterials are a dou-ble-edged sword, for if they are used without adequatesafety considerations, public trust will be lost. If skepticismabout the safety of nanobiomaterials is spread by incorrectinstructions or uses, non-scientific reasoning, or mererumor, then research on nanobiomaterials which have suchgreat potential will be severely affected. We must accumu-late the academic knowledge and technology necessary forcreating highly functional, biocompatible, and safe materi-als and draw up basic guidelines for materials design forsafe nanobiomaterials.

Notes:1) Keywords marked * in the text refer to all words con-

taining the keywords. The author set the keywords tominimize noise during the search, but note that noisecould not be entirely eliminated.

2) For biomaterials, various keywords are set dependingon their uses. Since the author attempted to grasp thegeneral trend in this survey, note that many searchesfailed.

3) One paper may be counted in multiple items becauseduplications were not eliminated.

References

1) M. Bruchez, Jr., M. Moronne, P. Gin, S. Weiss and A. P.Alivisatos, Science, 25, 2013 (1998).

2) J. Z. Xi, J. J. Schmidt, C. D. Montemagno, Nature Mater., 4, 180(2005).

3) Y. Arntz, J. D. Seelig, H. P. Lang, J. Zhang, P. Hunziker, J. P.Pamseyer, E. Meyor, M. Hegner and C. Gerber, Nanotechnology,14, 86 (2003).

4) T. P. Richardson, M. C. Peters, A. B. Ennett and D. J. Mooney,Nature Biotechnol., 19, 1029 (2001).

5) A. A. Shvedova, V. Castranova, E. R. Kisin, D. Schwegler-Berry,A. R. Murray, V. Z. Gandelsman, A. Maynard, P. Baron and J. ofToxicology and Environmental Health Part A, 66, 1909 (2003).

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1. Introduction

The micro electro mechanical system (MEMS) technol-ogy now being researched for application to analyticalchemistry, molecular biology, medicine, and the chemicalindustry has established a new field called micro totalanalysis system (µ-TAS) or “lab-on-a-chip”. This is achemical analysis system which combines fluid control ele-ments (channels, pumps, and valves) fabricated by semi-conductor micromachining technology and analysis ele-ments (detectors, sensors, and electronics). The basic con-cept is to integrate all functions necessary for sample pre-treatment, reagent mixing, chemical reaction, and detectiononto a single chip for thorough processing in the fields ofchemistry, biology, and medicine. Compared with the con-ventional biological and chemical analyzers, such a systemfeatures: (1) smaller size and lower price, (2) lower runningcosts and less environmental load because smaller quanti-ties of samples and reagents are used, and (3) shorter analy-sis time because of localized chemical reaction fields.Miniaturization and integration with microsensors and sig-nal processing circuits will enable new styles of use, suchas high throughput analysis by parallel processing, bedsideclinical testing, and on-site environment monitoring. In theµ-TAS field, technological development is progressingrapidly. Based on silicon, glass, polymer, and other materi-als as well as micrometer- to nanometer-scale machiningtechnologies, µ-TAS is being studied for application to awide range of biological and chemical analyses, includingelectrophoresis, DNA chips, chromatography, flow injec-tion, biochemical analysis, protein analysis, and cell analy-sis. Research on µ-TAS is focusing on application to fieldswhere the µ-TAS features of miniaturization, parallel pro-cessing, and function integration can be exhibited or to newfields.

The author surveyed research trends by searching anacademic paper database (Web of Science) for keywordsand counting the number of papers contributed to the MicroTotal Analysis System (µ-TAS), a major international con-ference in the field of bioelectronics. This report summa-rizes the results. From papers published since 1990, thosecontaining specific terms (µ-TAS, lab-on-a-chip, elec-trophoresis chip, DNA chip, and DNA microarray) in theirabstracts or keywords were extracted and sorted by years toidentify research trends. To predict the future of research inthis field, the number of recent papers on biodevices using

nanotechnologies was also checked.

2. Research trends

As the initial research on µ-TAS, Stanford Universityreported an example of a gas chromatograph in 1979. Thegas chromatograph consists of a sample injection valve, aseparation column, and a thermal conductivity detectorintegrated on a single silicon substrate. This technologywas systemized with a small gas cylinder and commercial-ized as a portable gas chromatograph. In 1990, Dr. Manzproposed the concept of µ-TAS and introduced a chip inte-grated with a liquid chromatograph separation column andan electric conductivity detector.1) At the time, microma-chining technology was maturing and fields of applicationwere being sought. When it was shown that the technologycould be applied to the chemical and biological fields,many researchers converged on µ-TAS and the researchtook off rapidly. Figure 1 shows the transition in the num-ber of papers on µ-TAS and lab-on-a-chip. Since the pro-posal in 1990, the number of papers has increased, reflect-ing the growth in research. At the initial stage of researchon µ-TAS, many papers were published on micropumps,valves, and other fluid control elements having movingparts. However, these devices had complicated structuresand so technical problems such as withstanding pressureand long-term stability arose for practical applications.Therefore, the electrophoresis chip and DNA chip/microar-ray which had no moving parts were at first used in prac-tice.

Figure 2 shows the transition in the number of papers onelectrophoresis chips. Papers began to appear at the sametime as the µ-TAS proposal and have increased quicklysince 2000. This is probably because the need for high-throughput DNA analysis rose as the human genome pro-ject progressed. Figures 3 and 4 show the transition in thenumber of papers on DNA microarrays and DNA chips,respectively. In both cases, the number started increasingquickly around 2000 just as DNA microarray and DNAchip technologies started to become established. Researchwas initiated to clarify the genetic functions mainly byexpression analysis and is still continuing. At first, manypapers focused on DNA microarray creation and data pro-cessing methods, but are now turning to applied research,such as research on disease-related genes and the expres-

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05 Biomaterials

Section 2. Bioelectronics

Yuji MiyaharaBioelectronics Group, Biomaterials Center, NIMS

sion analysis of specific genes, for which DNA microarraysand DNA chips are essential tools. In the µ-TAS and lab-on-a-chip fields, research was conducted from the 1990suntil early 2000 mainly in Europe and the US. Especially inthe United States, research spanning from basic to appliedwas conducted, including industrialization. Elementdevices based on various principles were proposed andsome were actually created. In particular, electrophoresischips and DNA chips/microarrays were researched activelyas genetic functional analysis progressed, and are nowessential tools for genetic functional analysis, pharmaceuti-cal creation, and clinical research.

In Japan, systematic research started in the µ-TAS andlab-on-a-chip fields only recently, but is acceleratingthanks to competitive funds from NEDO under the Micro-analysis and Production System Project and the AdvancedNanobiodevice Project. Figure 5 shows the number ofpapers by country accepted at the µ-TAS International Con-ference in the last two years.2, 3) The conference was held inNara in 2003 and in Malmo, Sweden in 2004. The numberof papers from Japan increased quickly in the last two yearsand reached the top in 2004, surpassing the United States.It is noteworthy that the numbers of papers from Korea,Taiwan, and other Asian countries are increasing. Recently,the themes of research are extending from genes to proteinsand even to cell analysis. In addition, device performancehas been evaluated under conditions closer to the actualenvironment of use and many studies geared to practicalapplications have been reported. Meanwhile, nanotechnolo-gy applications are being promoted, and both molecular

measurement and microdroplet operation control are note-worthy new trends.

3. Future outlook

An organism is composed of micrometer-scale cells anda cell is an aggregate of protein, lipid, nucleic acid, andother nanometer structures. Research is underway onachieving target functions and high-sensitivity measure-ment of biomolecules by controlling the structures, forms,and chemical properties of biomaterials at the nanometerlevel. High-sensitivity detection technology is being devel-oped from biomolecular reaction specificity, molecularrecognition, and micromachining to detect biomolecules bycontrolling the surface and interface functions and nanos-tructures. In particular, high-sensitivity biomolecular mea-surement technology using nanomachining technology anddevices is a noteworthy future trend. The author surveyedtechnologies mainly for measuring DNA and proteins withhigh sensitivity by effectively combining the unique prop-erties of biomolecules and the characteristics of nanostruc-tures. Nanopillars, nanopores, cantilevers, nanogaps, thinfilms (field effect), and nanowires and nanotubes have beendeveloped as characteristic nanostructures, and their inter-actions with biomolecular reaction specificity, superstruc-ture, charge, and base sequence are now being studied.

Figure 6 shows the transition in the number of papers onbiomolecular measurement devices using nanotechnolo-gies.

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Fig. 1 Number of papers in the µ-TAS and lab-on-a-chip fields. Fig. 3 Number of papers on DNA microarrays.

Fig. 2 Number of papers on electrophoresis chips. Fig. 4 Number of papers on DNA chips.

A micrometer- to nanometer-scale pole structure havinga large aspect ratio formed on a substrate is called ananopillar. This structure is mainly used in separationanalysis technologies, such as electrophoresis and liquidchromatography. If nanopillars are integrated in a microm-eter-scale channel (µ-fluidics) and biomolecules are letthrough, the biomolecules are sieved by size. In otherwords, small biomolecules can move fast but large ones areslowed down by the steric hindrance effect of the nanopil-lars. This molecule sieving effect of nanopillars spatiallyseparates the biomolecules in a sample by size. Nanopil-lars, which do not require the conventional polymer matrixor similar separation matrix, are being applied to the elec-trophoresis for long-stranded DNA.

A through pore (nanopore) having a nanometer-scaleopening is formed into a thin film and the space is parti-tioned into two chambers. A voltage is then appliedbetween two electrodes installed in each chamber and bio-molecules passing the nanopore are detected as changes incurrent.4) If a phospholipid double layer is used for the thinfilm and a nanopore is formed by using the self-organiza-tion of the α -Hemolysin (α -HL) protein, a channel(nanopore) of 1.8 nm in aperture and 5 nm in length isformed. When a DNA molecule passes through thenanopore, the current flow in the nanopore is blocked andthe current drops quickly. Once the DNA molecule haspassed through, the current flowing through the nanoporerises again to its original value. By analyzing the value ofcurrent and the time of current drop, information can beacquired about the interaction between the DNA moleculeand nanopore and the configuration (secondary structure,length, and base sequence) of the DNA molecule.

By using silicon micromachining technology, the beamthickness was reduced from micrometer to nanometer scale

to fabricate a cantilever that reacts sensitively to surfacestress.5) Silicon or silicon nitride (SiN) is mainly used forthe cantilever. A bio-related material is fixed on the surfaceof the free end of the cantilever and the deflection of thecantilever by the formation of composite containing the tar-get molecule is detected by the light beam deflectionmethod. The biomaterial to be fixed is long-stranded DNAor protein that uses hybridization with complementaryDNA, antigen-antibody reaction, and other specific reac-tions for high-sensitivity biomolecular detection.

Through a nanometer-scale gap, a pair of conductiveelectrodes is fabricated. A biomolecule is trapped betweenthe nanogap electrodes for high-sensitivity biomolecularmeasurement. Electrodes having a gap of 50 nm were fabri-cated from polysilicon and a DNA molecule trapped in thegap was analyzed.6) A single-stranded DNA (poly T or polyG) of 35 bases, composed of thymine or guanine only, wasfixed on the nanogap electrode surface and the inter-elec-trode capacitance was measured. Consequently, hybridiza-tion with complementary DNA was found to reduce theinter-electrode capacitance by 70%. This is because thecomparatively flexible single-stranded DNA gains a doublespiral structure by hybridization and the effective lengthand the dielectric relaxation characteristic change.

Research is now being conducted on using a nanotube ornanowire for high-sensitivity biomolecular detection. Byusing a carbon nanotube as a channel, a back-gate field-effect transistor was fabricated to detect specific biomolec-ular bindings.7) The side of a carbon nanotube was coatedwith a polymer, such as polyethylene glycol (PEG) (< 10nm), and biotin was fixed on the surface to monitorchanges in electrical characteristic due to reaction withstreptoavidin. When biotin was fixed on the carbon nan-otube for reaction with streptoavidin, the current showed anextreme drop in the area of negative gate voltage. Biomole-cular detection using Si nanowire was also reported.6) An

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(b) 2004

2003Contributed

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Adoptedpapers:

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Adoptedpapers:

432

Other83

Other113

UK 19

Korea22

Japan95

USA104

USA117

Germany 20

Sweden23Denmark

33

Japan124

Fig. 5 Number of papers at µ-TAS international conference by country.

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Fig. 6 Number of papers on biomolecular measurement devices usingnanotechnologies.

SiO2/Si substrate was doped with boron and a monocrystalSi nanowire was formed on it. Then metallic electrodeswere connected to both ends to create a field-effect transis-tor structure with the Si substrate as the back gate. The Sinanowire surface was treated with aminosilane and variousbiomolecules were fixed to monitor changes in conductivi-ty of the Si nanowire by the specific biomolecular bindings.

The number of papers on each device above began toincrease around 2003, especially regarding biomolecularmeasurement using nanotubes and nanopores. Since thesetechnologies are effective for high-sensitivity biomolecularmeasurement, single molecule detection, and local mea-surement, new knowledge may emerge and we are moni-toring the future trend.

Since the µ-TAS and lab-on-a-chip technologies areeffective for attaining compact biomolecular detectiontechniques, there are expectations that a portable clinicaltesting system will be developed. By combining these sys-tems with Internet or wireless communication technologies,the concept of remote medicine and home care was pro-posed and demonstrated in some areas. The former Min-istry of Health and Welfare set up a remote medicineresearch group in the information technology developmentresearch project funded by a subsidy for scientific research.The group collected data on the model remote medicine asof 1998. Figure 7 shows the breakdown of the cases ofremote medicine by field,8) although the data is as of 1998,which is somewhat outdated in view of the rapid progressof information communication technologies. However,since the number of cases is as great as 229 and the medicalitems do not change as drastically as communication tech-nologies, the data is still useful for checking the fields ofapplication of remote medicine. Of the 229 cases, 29 are inthe field of pathological diagnosis, 97 in radiological imag-ing, 40 in home care, 6 in ophthalmology, 3 in dentistry, 44in medical imaging, and 10 in other fields. In most cases,excluding those in home care, image information is mutual-ly exchanged between medical institutions. In the field ofhome care, communication is done between medical insti-tution and private home, or between medical institution andaged people’s home. From the patient’s side, images maybe transmitted by the patient or a visiting nurse or automat-ically from a monitor.

For home care, not only images but also various biologi-cal information are collected, including body temperature,pulse, blood pressure, electrocardiogram, body weight,aspiration, pressure in respiratory tract, oxygen saturation,and heart rate (including fetus). Home care is intended foraged people, terminal-care patients, patients undergoingrehabilitation after apoplexy or cardiac infarction, patientsundergoing dialysis for chronic renal failure, and pregnantwomen. Image transmission is used not only for oral med-ical examination or rehabilitation guidance by videophonebut also for monitoring catheter status and observing dia-lyzate.

To meet the growing medical needs in the aged society,home care will become much more important. This style ofhome care is still not popular and its problems are nowbeing studied. To collect information about more biologicalitems, quickly provide information which is useful fordiagnosis, and develop an easy-to-use inspection system,the µ-TAS and lab-on-a-chip technologies hold the key.

4. Conclusion

New technologies of nanometer scale and molecularlevel are quickly emerging to decode all the base sequencesof the human genome in the human genome project, todevelop microfabrication by lithography or self-organiza-tion, and to develop a means of controlling molecules byusing nanotube or nanowire. Technologies are rapidlymerging beyond the existing framework of academic disci-plines. Bioelectronics technologies such as µ-TAS and lab-on-a-chip are applied to various fields and some will beproven while others will be weeded out. The nanobiofusion area has just started, but new breakthrough technolo-gies are expected in the medical and pharmaceutical fieldsin the 21st century. This is an area which is worth keepingan eye on.

References

1) A. Manz, N. Graber, H. M. Widmer, Sensors and Actuators B, 1,244 (1990).

2) S. Shoji, IEEJ Trans. SM, 123, 98 (2003).3) T. Torii, IEEJ Trans. SM, 125, 102 (2005).4) A. Meller, L. Nivon and D. Branton, Phys. Rev. Lett., 86, 3435

(2001).5) J. Fritz, M. K. Baller, H. P. Lang, H. Rothuizen, P. Vettiger, E.

Meyer, H-J. Guntherodt, Ch. Gerber and J. K. Gimzewski, Science,288, 316 (2000).

6) J. S. Lee, S. Oh, Y. K. Choi and L. P. Lee, Micro Total AnalysisSystem, 1, 305 (2002).

7) A. Star, J-C. P. Gabriel, K. Bradley, G. Gruner, Nano Letters, 3, 4,459 (2003).

8) http://square.unim.ac.jp/enkaku/97/Proj/EnkProj-Idx.html (UpdatedAugust 1998).

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Dentistry3Ophthalmology

6Pathological

diagnosis29

Home care40

Medicalimaging

44

Radiologicalimaging

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Fig. 7 Breakdown by fields of remote medicine.

1. Introduction

The global environmental problems and ecologicalchanges in the 20th century were brought by the rapidexpansion of human and industrial activities. In order tosolve them and survive in the 21st century, it is essentialfor us to convert the present society to an environment-friendly sustainable society. Under these circumstances,one of the research targets is the development of environ-mental function materials. Environmental function materi-als are identified newly in the Ecomaterials Center, NIMS,as eco-function materials, which are environment purifica-tion materials with smart functions, that is, high sensitivityand intelligent response to harmful pollutants. The produc-tion of eco-function materials for improving environmentalquality can take two approaches. One strategy is to tailorthe material as a catalyst for decomposing polluting prod-ucts, that is, to make a new photocatalyst. The second oneis to establish an effective adsorbent and separator for theremediation process and correcting already polluted envi-ronments. This section reviews the current status and futureoutlook of photocatalytic materials and other environmentpurification materials.

2. Photocatalytic materials

2.1 IntroductionPhotocatalysts have attracted extensive interest since

Honda and Fujishima introduced the water decompositionphenomenon (Honda-Fujishima Effect) of a photoelectro-chemical cell using a titanium-oxide photo electrode and aPt counter electrode in Nature in 1972.1)

At that time, the Oil Shock and other global energycrises triggered global research on producing hydrogen bydecomposing water using a semiconductor photocatalyst.However, the conversion efficiency remains low and manyhurdles must be overcome before the technology can be putto practical use. Nevertheless, many researchers, especially

those in Japan, are still making continuous efforts towardsachieving the ultimate goal of the chemical conversion ofsolar energy using a photocatalyst.

Meanwhile, a group from the University of Tokyo, incollaboration with many enterprises, began to explore theapplication of a titanium oxide photocatalyst in the field ofenvironmental purification from the 1990s. The photo-induced hydrophilicity2) discovered in 1994 by the grouprevealed promising potential for practical application. Theself-cleaning function, which is combined from the oxi-dization function and hydrophilicity function of titaniumoxide photocatalyst, is now used widely for building walls,window panes, antifogging mirrors, etc. Products using thedeodorizing and antibacterial effects of titanium oxide pho-tocatalyst are also being developed.3)

Photocatalysts are like a magic material that can be usednot only to decompose and remove harmful organic chemi-cal substances, but also to produce hydrogen from water,by the strong oxidizing and reducing power of photo-excit-ed holes and electrons.

2.2 Research trendsFigures 1 and 2 show the transition in the number of

photocatalyst-related papers and patents throughout theworld in the 30 years from 1971 to 2001. The figures showthat Japan is leading the world in both aspects. In contrastto the steady increase of papers, the number of patentsgrew slowly until the 1990s. When the photo-inducedhydrophilicity effect was discovered in 1994, the numberof patent applications jumped. In terms of countries, thenumber of patent applications from Japan is overwhelming,while about half of the patent applications even in the USand Europe are by Japanese people.

Accompanying the development of applications of pho-tocatalysis technology, photocatalytic materials are expect-ed to be highly activated. To decompose and remove vari-ous organic harmful substances quickly under the weakultraviolet rays of natural light and artificial light fromlighting devices, research efforts have been concentrated on

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Chapter 6. Ecomaterials

Section 1. Environmental Function Materials (Photocatalytic

and Environment Purification Materials)

Jinhua Ye and Tetsuya KakoEco-Function Materials Group, Ecomaterials Center, NIMS

Hirohisa YamadaEco-Circulation Processing Group, Ecomaterials Center, NIMS

increasing the specific surface area of titanium oxide, creat-ing a porous structure, and combining with otherabsorbents.4),5) In recent years, research interest is shiftinglargely from the control of ultraviolet-supporting TiO2 pho-tocatalyst to the development of visible light responsivematerials that can utilize more light because the spectra ofsolar light and indoor light (fluorescent lighting) is mostlycomposed of visible light.

Visible light responsive materials can be developed bytwo approaches: one is to convert existing UV sensitivematerials into visible light responsive ones by modification,and the other is to develop new materials. Most researchersare working on the former. The conventional method ofproducing a visible light responsive material is to dope adifferent kind of metal (Cr or V) into TiO2. However, sincephoto-induced electrons and holes tend to re-combinetogether again in the doped level, visible light activationcan seldom be expected. Instead of cation doping, recentresearches showed that partial substitution of oxygen ionsby nitrogen can successfully activate TiO2 to be capable ofdecomposing acetaldehyde or other organic matter under

visible light, as reported by a group from Toyota CentralR&D Labs.6) In addition to N, the doping effects of S and Care now also being researched. Since the doping amountmust be minimal to maintain the crystalline structure oftitanium dioxide, however, the visible-light activationeffect is limited (up to about 500 nm).

For response to a wider range of visible light, a new vis-ible light sensitive photocatalyst should be developedbeyond the framework of titanium oxide. Non-oxide semi-conductors (cadmium sulfide, cadmium selenide, etc.) hav-ing a small band gap and adsorption capability in the visi-ble light area attracted attention but were found to havemany problems such as photo-corrosion caused by thephoto-generated holes in the valence band, and thus pre-vent stable functioning. For practical purposes, a compara-tively stable oxide photocatalyst is required. Recently, agroup from the Tokyo Institute of Technology developedoxynitride7) and a group from the Science University ofTokyo developed BiVO4

8) as new photocatalysts. Thesematerials can generate hydrogen and oxygen from aqueoussolutions containing an electron donor sacrificial agent

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Fig. 2 Number of photocatalyst-related patents in Japan, USA, and Europe (Source: Patent-applied Technology Trend Report 2003 by Patent Office).

(methanol) and an electron acceptor sacrificial agent(AgNO3) under visible light, but fail to decompose purewater. Up to now, only a few materials have been reportedto be capable of splitting pure water under visible light irra-diation. Among them, In1-xNixTaO4 photocatalyst9) jointlydeveloped by the Agency of Industrial Science and Tech-nology (AIST) and the National Institute for Materials Sci-ence (NIMS) attracted much attention for the world’s firstsuccessful decomposition of water into hydrogen and oxy-gen at the stoichiometric ratio of 2:1 under visible light.Recently, NIMS also succeeded in developing several com-posite oxide photocatalysts that could produce hydrogenand decompose various organic harmful substances undervisible light.10)-12)

2.3 Future outlookPhotocatalysis technology is now mainly used for out-

door applications, such as exterior and road materials. Aircleaners using photocatalysts also enjoy strong demand as asolution to “sick house syndrome” in recent years. Themarket is expected to grow continuously for improving theliving environment particularly in the construction materi-als industry. In addition to these products, the fusion ofphotocatalyst technology and environment-related technol-ogy is predicted to produce a large market. For example, anenvironment-related public works technology that decom-poses harmful substances and germs in the atmosphere,water, and soil by solar or indoor light will create a hugemarket for photocatalysts, and the photo-inducedhydrophilicity effect of a photocatalyst will possibly beused for global warming prevention. In the near future,photocatalysis technology will be applied to energy-relatedfields, such as the commercial production of hydrogen bythe photodecomposition of water.

With the expansion of applications, basic research isneeded on clarifying the mechanism of the photocatalyticreaction underlying photocatalyst technology, improvingthe activity, controlling responsiveness to visible light, andstabilizing the reaction. For the time being, the most impor-tant subject is to develop a highly efficient visible light sen-sitive photocatalyst to extend the capabilities of photocatal-ysis technology and bring the material to practical applica-tion.

2.4 ConclusionPhotocatalysis technology originated in Japan, and Japan

leads the world in the number of papers, the number ofpatents, and market scale. However, competition from theUnited States and Europe is growing, as well as from Chinaand Korea. To ensure competitiveness in the internationalmarket, efforts in improving the reliability of photocatalystrelated products while maintaining technological develop-ment superiority are indispensable. Working groups fromindustry, academia, and the government of Japan are nowactively involved in standardization of the performanceevaluation of photocatalysts.

References

1) A. Fujishima and K. Honda, Nature, 238, 37 (1972).2) R. Wang, K. Hashimoto, A. Fujishima, M. Chikuni, E. Kojima, A.

Kitamura, M. Shimohigoshi and T. Watanabe, Nature, 388, 431(1997).

3) A. Fujishima, K. Hashimoto and T. Watanabe: “Mechanism ofPhotocatalyst” (in Japanese), Nippon Jitsugyo Publishing (2000).

4) T. Sasaki, S. Nakano, S. Yamauchi and M. Watanabe, Chem.Mater., 9, 602(1997).

5) S. Chu, K. Wada and S. Inoue, Adv. Mater., 14, 1752 (2002).6) R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki and Y. Taga, Science,

293, 269 (2001).7) M. Hara, K. Domen: Functional Materials (in Japanese), 22, 25

(2002).8) A. Kudo, O. Omori, H. Kato and J. Am. Chem. Soc., 121, 11459

(1999).9) Z. Zou, J. Ye, K. Sayama and H. Arakawa, Nature, 414, 625

(2001).10) J. Yin, Z. Zou, J. Ye and J. Phys. Chem. B., 107, 4936 (2003).11) J. Tang, Z. Zou and J. Ye, Angew. Chem. Int. Ed., 43, 4463 (2004).12) J. Tang, Z. Zou and J. Ye, Chem. Mater., 16, 1644 (2004).

3. Environment purification materials

3.1 IntroductionEnvironmental problems are caused by harmful chemi-

cal substances (dioxins, etc.), harmful heavy metals (Cd-,Cr-ions, etc.), water contaminants (NH4

+, PO43–, A5O3

3–),groundwater contaminants (trichloroethylene and tetra-chloroethylene), volatile organic compounds (VOC),atmospheric contaminants (NOx, SOx, SPM, etc.), andradioactive waste. To solve these problems and create asustainable society, we must remove the contaminantsaccumulated so far and control further contamination.Since even trace quantities of environmental contaminantshave a large impact, a very specific and highly sensitivesensing technology is necessary.

3.2 Research trendsTo promote environmental purification and conserva-

tion, materials have been created to adsorb, separate,decompose, and remove harmful contaminants selectively.Because of organophilic property as well as adsorption andcatalytic capabilities, clay minerals such as smectites havebeen used to adsorb, decompose, and remove harmful sub-stances since ancient times. High selectivity has not beenachieved yet, despite recent reports on the adsorption ofdioxin on pillared smectite and that of aromatics byorganophilic smectite.1)-4) Zeolite is a microporous material,having regular nano-pores, a large specific area, and cation-exchange capacity, and has attracted attention as an adsor-bent or a catalyst support.5, 6) Natural zeolites found inabundance have been used to remove ammonia which isthe main contaminant of closed water systems, lakes andmarshes, and rivers arising from household drainage. How-ever, natural zeolites do not have high selectivity foradsorbing cadmium, arsenic, and other heavy metal ions.Since the 1940s, synthetic zeolites developed by UnionCarbide, Mobil, and others have been used as an industrialcatalyst and a detergent builder. Since the 1970s, the devel-opment of novel zeolites with a unique pore structure have

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enabled many new industrial catalyst processes. However,the synthetic zeolites do not have enough selectivity foradsorbing or removing heavy metal ions and chemical sta-bility. Furthermore, the microporous structure is unsuitablefor adsorbing and fixing large molecules.

In the early 1990s, mesoporous silica was developedindependently by the Waseda University – Toyota CentralR&D Labs group and Mobil. Mesoporous materials withlarge specific surface areas and uniform and regular meso-pores have been greatly expected to adsorb and removeorganic metal complexes and organic matter that cannot beadsorbed by microporous materials.7)-9) However, theirfunctions and chemical stability are not yet adequate forapplications.

Under these circumstances, the development of materi-als to separate, decompose, and remove harmful chemicalsubstances very selectively has been demanded. AIST hasdeveloped mesoporous materials with a selective pore dif-fusion function and inorganic-, organic- and hybrid-typenanospace materials with a high selective adsorption func-tion. AIST has also developed nano-metal particles forhighly active catalysts. By combining these materials,AIST is constructing a multifunctional integrated systemwith catalyst functions for adsorbing and decomposingharmful chemical substances.10, 11) In addition, high-sensi-tivity environmental sensors have been developed by modi-fying the quartz crystal microbalance with biomaterials.12)

NIMS is currently promoting 1) Research on the removalof heavy metals and ammonia and the management ofradioactive waste by using nanopore materials (zeolite,etc.) and nanoparticles (boehmite, etc.),13) 2) Developmentof chemical sensor using ultrathin films prepared by theLangmuir-Blodgett technique,14) 3) Development of a mag-netic separation system using a superconducting magnet forchemical-adsorbing of target substances (arsenic, bisphenolA, dioxin, etc.),15) and 4) Research for fixing biopolymersusing mesoporous silica or mesoporous carbon, and remov-ing VOC and harmful organic substances.16) Mesoporouscarbon is a new material produced by using mesoporoussilica as a template and is expected to be applied to cata-lysts, adsorbents, electrodes, and capacitors.

3.3 Future outlookIn order to separate, decompose and remove the specific

harmful substances, we have to create novel materials withhigh-selectivity and sensing functions by using nanotech-nologies, self-organization, and template reactions. Toapply nanomaterials to environmental purification, we alsoneed to clarify the chemical stability of nanomaterials in

water, soil, and other environments and the desorptioncapability, chemical stability, and catalytic activity ofnanomaterials after fixing harmful chemical substances.This will require the creation of materials by fusion beyondthe traditional frameworks of inorganic, organic, and poly-mer materials.

3.4 ConclusionTo overcome various complex environmental problems,

the technologies should be shifted to be more precise andflexible. It is necessary to improve the functions and char-acteristics of materials through nano-level structural controlutilizing nanotechnologies. It is also important to createenvironment-purifying nanomaterials based on recycling ofresources with less environmental load. This cannot beachieved without widely linked research beyond the fieldsof material science, chemistry, environment science, andbiology. Furthermore it is necessary to develop a new envi-ronment purification system considering the self-cleaningability in nature.

References

1) S. A. Boyd, J. F. Lee and M. M. Mortland, Nature, 333, 345 (1988).2) S. A. Boyd, S. Shaobai, M. M. Mortland, Clays Clay Miner., 36,

125 (1988).3) L. J. Michot and T. J. Pinnavaia, Clays Clay Miner., 38, 634 (1991).4) R. K. Kukkadapu and S. A. Boyd, Clays Clay Miner., 43, 318

(1995).5) J. Weitkamp, Solid State Ionics, 131, 175 (2000).6) K. Meyer, P. Lorenz, B. Bohlkun and P. Klobes, Cryst. Res.

Technol., 29, 903 (1994).7) T. Yanagisawa, T. Shimizu, K. Kuroda and C. Kato, Bull. Chem.

Soc. Jpn., 63, 988 (1990).8) C. T. Kresge, M. E. Leonowicz, W. J. Roth, J. C. Vartuli and J. S.

Beck, Nature, 359, 710 (1992).9) S. Inagaki, Y. Fukushima and K. Kuroda, J. Chem. Soc., Chem.

Commun., 680 (1993).10) K. Kosuge, T. Murakami, N. Kikukawa and M. Takemori, Chem.

Mater., 15, 3184 (2003).11) A. K. Sinha, S. Seelan, S. Tsubota and M. Haruta, Angew. Chem.

Int. Ed., 42, 1546 (2004).12) S. Kurosawa, H. Aizawa, S. Pak, S. Wakita and S. Niki,

“Biosensing Micromachine Using Crystal Resonator” IndustrialTechnology Service Center, p. 542 (2002).

13) Y. Watanabe, H. Yamada, J. Tanaka, Y. Komatsu and Y.Moriyoshi, Sep. Sci. Technol., 39, 2091 (2004).

14) K. Tamura, H. Sato, S. Yamashita, A. Yamagishi and H. Yamada,J. Phys. Chem. B, 108, 8287 (2004).

15) T. Ohara, T. Watanabe, S. Nishijima, H. Okada and N. Saho, OyoButsuri, 171, 57 (2002).

16) M. Miyahara, A. Vinu, T. Nakanishi and K. Ariga, KobunshiRonbunshu, 61, 623 (2004).

1. Introduction

Expectations for the hydrogen energy age are growingand fuel cell technology is progressing rapidly.1) Fuel cellshave more than a 100-year history of research and develop-ment, yet they have been applied to spacecraft and otherlimited uses only. For example, the fuel-cell automobiles ofToyota and Honda were leased to the government inDecember 2002 and a stationary fuel cell was installed inthe Prime Minister’s Office. In reality, however, fuel cellsare still at the prototype stage and there remain many prob-lems concerning output, stability, cost, infrastructure, andso forth. Research and development on conventional largefuel cells and automotive or stationary fuel cells is based onengineering considerations, such as how a system shouldbe created from existing materials. This is the current glob-al trend of fuel cell research and development. However, ifonly this engineering-oriented research toward early appli-cation continues, it will be difficult to use the fuel cells inautomobiles or medium-scale generators. Therefore, thereis a growing perception of the need to return to basics andgive priority to materials research.2)

This report examines the field of materials for hydrogenenergy and fuel cells where research and development isprogressing quickly. To grasp the trends accurately, theauthor investigated the recent transition in the number ofpapers by searching a database of academic papers (SCIExpanded) for the period 1980 to 2004 containing theterms “hydrogen energy,” “fuel cell,” and “hydrogen per-meation” in their titles or keywords, and counting theresulting papers in each year.

2. Research trends

Figure 1 shows the transition in the number of papers onhydrogen energy throughout the world and in each majorcountry. The number started increasing rapidly around1996. It was soon after the 10th World Hydrogen EnergyCongress was held in Cocoa Beach, USA (1994), and WE-

NET I (1993-1998) was started in Japan. Research is nowactive in the United States, Japan, and China, with the

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Fig. 2 Number of papers on polymer electrolyte fuel cells (PEFC).

06 Ecomaterials

Section 2. System Element Type Ecomaterials - Supporting

New Energies and Energy Conservation:

Materials for Hydrogen Energy and Fuel Cells

Chikashi NishimuraEco-Energy Materials Group, Ecomaterials Center, NIMS

growth in China being especially remarkable.Figure 2 shows the transition in the number of papers on

polymer electrolyte fuel cells (PEFC) for which expecta-tions are highest among fuel cells. The total number ofpapers from 1980 to 2004 is about 500. Papers startedincreasing globally around 1990 and reached an annual out-put of 100 in 2004. With about 29% of the world’s totalnumber of papers, Japan holds the lead, far ahead of the US(21%) ranking second and Germany (13%) ranking third.

Figure 3 shows the transition in the number of papers onsolid oxide fuel cells (SOFC). The number in the last 25years was about 1,800, nearly four times that on polymerelectrolyte fuel cells. Papers on solid oxide fuel cells alsostarted increasing rapidly around 1990. Regarding the totalnumber of papers in the last 25 years, Japan accounts for25% of the world’s total, higher than that of the US (21%)ranking second and Germany (10%) ranking third. For thelast decade, the annual number of papers from Japan hasbeen stable at about 50, but the number from the UnitedStates has been increasing and surpassed that of Japan in

2003, and the gap is widening. This may be partly becausethe United States is discussing a combined power genera-tion system with coal fired power at a national level.

So far, we have examined the transition in papers onpolymer electrolyte fuel cells and solid oxide fuel cells. Forcomparison, Figure 4 shows the other main types of fuelcell: molten carbon type (MCFC), phosphoric acid type(PAFC), and alkaline type (AFC). The number of papersalso showed a global rapid increase around 1990. However,the increase leveled off around 1996 and the annual outputhas been stable at about 120 to 140. This is a contrast to thedramatic increase in papers on polymer electrolyte fuelcells (Figure 2) and solid oxide fuel cells (Figure 3).

Fuel cells run on hydrogen, and the trend of hydrogenproduction is as follows. Hydrogen does not exist indepen-dently in nature and is generally produced from fossil fuelsby the steam reforming method, the partial oxidizationmethod, or the auto-thermal method which is a combina-tion of both. Polymer electrolyte fuel cells, which is under-going intensive research for practical application, uses aplatinum-type electrocatalyst. Since the catalyst loses activ-ity in this kind of fuel cell operated at low temperatures, itis necessary to suppress the CO concentration in reformedgas to 10 ppm or less, so a CO removal process is usuallyadded. Metallic membrane materials for hydrogen separa-tion can be laminated up to tens of microns thick with nopinholes. Research is underway on combining these with areforming reaction vessel to produce a new reaction vessel(membrane reformer or membrane reactor) that can concur-rently shift the chemical equilibrium to the product side,lower the reaction temperature, and generate high-purityhydrogen. Figure 5 shows the transition in the number ofpapers. The total in the last 25 years is about 1,500. Thenumber started increasing rapidly around 1990, and for thelast several years the annual output is about 150. Japan isvying for the world’s top position with the United States,Germany, and China.

As the key material for the membrane reformer, mem-brane materials for hydrogen separation are also the subjectof intense research and development. Figure 6 shows theresults of searching papers for the keyword “hydrogen per-meation” with additional conditions “Pd” and “Nb/V oramorphous.” Basic research has been conducted on hydro-gen permeation since around 1980, and on the applicationof hydrogen separating membranes since around 1990. Thenumbers of papers on Pd, Nb/V are increasing in line withthe total number of papers on materials. Papers on non-Pd(Nb/V or amorphous) are increasing slightly faster thanthose on Pd. Figure 7 shows the total number of papers bycountry in the last 25 years. Japan ranks first with about22%, closely followed by the US ranking second with 18%but far ahead of the remaining countries.

In addition to searching papers, the author also investi-gated web pages related to the Ministry of Economy, Tradeand Industry and the Ministry of Education, Culture,Sports, Science and Technology for Japan’s research pro-jects on hydrogen energy and fuel cells.

Concerning projects related to the Ministry of Economy,Trade and Industry (including NEDO), huge research fundshave been invested in projects related to hydrogen and fuel

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cells for over 10 years. R&D was carried out comprehen-sively in WE-NET I (1993-1998, 10 billion yen total) todevelop a large-scale hydrogen infrastructure technologyand WE-NET II (1999-2002, 5.8 billion yen in total) todevelop a hydrogen infrastructure technology mainly forfuel cells. WE-NET was succeeded by “Development ofinfrastructure technology for the safe use of hydrogen.” Inthis project from FY2003 to FY2007, research is focusedon two areas: the safe use of hydrogen, and practical appli-cation. The working expenses in FY2004 were 6 billionyen. Two other projects were carried out simultaneouslyfrom FY2000 to FY2004: “Technical Development Projectfor Polymer Electrolyte Fuel Cell System” aimed atenhancing and systemizing polymer electrolyte fuel cellsfor future full-scale use and dissemination, and “Infrastruc-ture Establishment Project for Polymer Electrolyte FuelCells” aimed at establishing an infrastructure for dissemi-nating polymer electrolyte fuel cells. The working expensesin FY2004 were 4.1 billion and 2.4 billion yen, respective-ly. In FY2005, a 5-year project “Strategic Technical Devel-opment for Practical Polymer Electrolyte Fuel Cells” start-ed, with a first-year budget of 5.5 billion yen, aiming at

developing elemental and systemizing technologies forpractical application and dissemination. To deepen under-standing of the basic mechanisms of fuel cells, the Agencyof Industrial Science and Technology is analyzing phenom-ena and has established a research system for this purpose,“Entrusted Research Expenditures for Fuel Cell AdvancedScience,” with the FY2005 budget of 1 billion yen.

Other projects related to solid oxide fuel cells are“Research and Development of Solid Oxide Fuel Cell(SOFC)” (FY2001-2004, FY2004 budget: 1 billion yen)and “Technical Development of Solid Oxide Fuel Cell(SOFC) System” (FY2004-2007, FY2004 budget: 1.5 bil-lion yen).

Meanwhile, the Japan Science and Technology Agency(JST) is conducting ground-breaking research on develop-ing catalysts and new materials in the Core Research forEnvironmental Science and Technology (CREST) fundedby the Ministry of Education, Culture, Sports, Science andTechnology. The individual topics are “Pseudo 3D Inter-face Design for Electric Energy Conversion” (2000-2005)in the area of resources recycling, “Fabrication of EnergyConversion Device Using Composite Structure of High-level Regular Array” (2002-2007) and “Fabrication ofHigh-function Nanotube Materials and Application toEnergy Conversion Technology” (2002-2007) in the areaof high-level energy use. In the area of nanostructure con-trol catalysts, the topics are “New Environmental CatalystFunction of Surface-optimized Carbon Nanofiber” (2002-2007) and “Fabrication of Nanocatalyst of Precise Univer-sal Control” (2002-2007). The average annual budget isjust under 100 million yen for each topic. The project,“Development of Low-temperature Oxide Electrolyte FuelCell” (2002-2004) was conducted with the FY2004 budgetof 130 million yen funded from promotion and coordina-tion expenses. In the leading project, “Next-generation FuelCell Project” (FY2003-2007, FY2004 budget: 290 millionyen) now in progress, electrode catalysts for polymer elec-trolyte fuel cells are being designed.

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3. Future outlook

As described, huge funds are being invested in research,particularly on the polymer electrolyte fuel cell which isregarded as very promising. Despite the investments, how-ever, fuel cells have not yet reached a practical level interms of cost and lifespan. While considering practical use,we must return to the basics of materials.

Concerning papers on solid oxide fuel cells, Figure 8compares the transition in the number of papers on YSZ(partially stabilized zirconia) which is used in nearly practi-cal systems and papers on non-YSZ materials. A compari-son of the increases in the last three or four years showsthat the number of papers without YSZ is greater, reflectinga return to materials research and basic research.

4. Conclusion

As outlined above, the number of papers on hydrogenenergy, fuel cells, and hydrogen permeation started increas-ing rapidly around 1990. In the last 10 years or more, Japanhas invested heavily in research in this field and ranks firstor near the top in each item in terms of the number ofpapers published. However, large obstacles remain beforefuel cells can enter widespread use. While continuing withresearch toward early application, we must return to thebasics of materials and conduct research on improving thecharacteristics based on fine analysis and tissue and struc-ture control.

References

1) Science and Technology Foresight Center, National Institute ofScience and Technology Policy, Ministry of Education, Culture,Sports, Science and Technology: Forefront of Hydrogen Energy(Illustrated), Kogyo Chosakai (2003).

2) T. Honma and T. Kudo: Ceramics 40, 369-373 (2005).

Num

ber

of p

aper

s (t

otal

)

Year

Fig. 8 Number of papers on solid oxide fuel cells, containing or notcontaining YSZ as a keyword.

1. Introduction

Ecomaterials of lifecycle design refer to materialsdesigned to reduce environmental loads throughout theirlifecycle, from manufacture to disposal. While the afore-mentioned two kinds of ecomaterials address specific envi-ronmental problems by performance, lifecycle design typematerials are based on the design concept “environment-friendly materials (and materials technologies)”.

The environmental load BL of materials is the sum of theenvironmental load BP during production, environmentalload BU during use, and environmental load BE upon dis-posal, minus the value BR upon recycling (BL = BP + BU +BE – BR). The eco-efficiency Ee, which indicates the ratioof service SU provided by the materials to the environmen-tal load, is defined by:

Ee＝ (1)

To create materials of small environmental load, the valuesof BP, BU, and BE must be designed to be small while thoseof SU and BR must be designed to be large. The ecomateri-als of lifecycle design can thus be classified into four cate-gories:1)

1) High materials efficiency (Large SU, small BU)2) Green environmental profile (Small BP)3) Free of hazardous substances (Small BE)4) High recyclability (Large BR)

This classification is certainly not strict, and some ecoma-terials may have characteristics of more than one category.1) and 2) often follow the trend of conventional research(e.g. high specific strength, long life, efficient process,energy-saving, etc.). Since these materials are explained inother chapters, this section discusses the recent trends andfuture outlook for materials free of harmful substances andmaterials of high recycling efficiency. The technique forevaluating lifecycle design conformance is also introduced.

2. Free of hazardous substances

The electronics industry enriches life with products but

also discharges many harmful substances into the environ-ment. It is a typical industry that incurs large environmentalloads. Therefore, much of the research on materials free ofhazardous substances focuses on the electronics industry.In particular, the enforcement of the Home ApplianceRecycling Law in Japan and that of WEEE and ROHS inthe EU made it a matter of urgency to remove heavy metalsand other harmful elements. Since this affects electronicmounting the most, lead-free solder alloys (not containinglead) and electronic mounting techniques using the alloysare being developed throughout the world.

2.1 Global trendsThe National Center for Manufacturing Science (NCM)

of the United States started developing lead-free solder bythe Lead-Free Solder Project in the early 1990s, followedby Improved Design Life and Environmentally AwareManufacturing of Electronics Assemblies by Lead-FreeSoldering (IDEAL) of the EU. This led to active researchand development mainly within industry in Japan. Since itis difficult to make lead-free solder which is able to with-stand high temperatures, this solder was exempted fromlegislation in the United States. Considering the results ofthe WEEE/ROHS bill in the EU and the research for pro-moting practical application in Japan, the United Statesorganized an industry-academia-government research sys-tem again by The National Electronics Manufacturing Ini-tiative (NEMI). In the EU, the practical use of medium-temperature solder (Sn-Ag-Cu solder) was verified in theabove IDEALS Project. In practice, however, the solderhas various problems hindering practical use and theCOST351 Project (EU COST Initiative) and the Intercon-nection Materials for Environmentally Compatible Assem-bly Technologies (IMECAT) Project are now in progress.Figure 1 shows past projects related to lead-free mountingin Europe and the US.

2.2 Domestic trendsStimulated by the NCMS Lead-Free Solder Project,

Japanese industry went ahead with research and develop-ment. NEDO executed a project from 1997 to 2000.Recently, a medium-temperature solder (Sn-Ag-Cu solder)

SU

BP+BU+BE–BR

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06 Ecomaterials

Section 3. Ecomaterials of Lifecycle Design

Hideki KakisawaEco-Circulation Processing Group, Ecomaterials Center, NIMS

Kohmei HaladaEcomaterials Center, NIMS

standardizing project was carried out mainly by The JapanWelding Engineering Society and Japan Electronics andInformation Technology Industry Association (JEITA), thelatter project being followed by a low-temperature solderdevelopment project. These projects in Japan are organizedmainly by industrial groups and not industry-academia-government organizations as in the United States andEurope. The electronic industry is an important pillar ofJapan but academic organs, especially national institutions,are much less aware of problems and less willing to partic-ipate compared with those in Europe and the US. Althoughmuch practical data has been acquired, Europe and the UShave the lead in intellectual property rights because Japanhas no academic infrastructure.

2.3 Current status of NIMS and research by NIMSNIMS has only an individual-level research system for

lead-free mounting and no research system driven by anational laboratory as in the United States. Recently, how-ever, members of the Ecomaterials Center began to partic-ipate in the JEITA project and the industrial sector andorganizations are now expecting the former national labo-ratories to join.

2.4 Noteworthy research outside NIMS and future outlookResearch outside NIMS is mainly conducted between

industry and universities (partially national universities)and the JEITA project of low-temperature lead-free soldertechnology is attracting attention. So far, only the medium-temperature Sn-Ag-Cu solder has entered practical use. Toachieve entirely lead-free mounting, high-temperature andlow-temperature solder alloys and their peripheral tech-nologies are required. In particular, no substitute solder hasbeen found for the high-temperature Pb-5Sn solder that isused for LSI packaging. For future research, an R&D sys-tem led by an academic institute is needed. Bonding with-out solder alloy, such as conductive bonding (already par-tially achieved), will be another research trend. Each coun-try has started work on standardizing lead-free mountingrelated technologies and international competition in stan-dardization will surely become fierce. As a national strate-gy, therefore, industry, academia, and government must

immediately encourage the standardization of technologiesestablished so far and related technologies to be developedin future.

3. Supporting recycling

However far process technologies might advance, it maynever be possible to melt unsorted piles of scrap and toextract the various constituent materials of the same qualityas before disposal. The keys to building a recycling systemare therefore to improve the social system through legisla-tion, establishment of recovery channels, and thoroughsorting, as well as to design products that are easy to disas-semble for recycling. However, approaches based on tech-nology and materials still have a very important role toplay. For example, one technological approach is to devel-op a recycling process that can permit impurities, while amaterials approach is to enhance the recycling efficiency ofmaterials themselves. In addition, materials technologiesmake a significant contribution to product designs thatassist recycling.

3.1 Recycling process technologyThere is no doubt that scraps from used products will

increase in all countries, irrespective of the kind of materi-als. To cope with this problem, we need to develop recy-cling technologies, particularly for plastics, metallic struc-ture materials, and concrete because of the large volumesof such scrap. The United States, Japan, and Europe havemany research projects targeted at the three kinds of scraps,and in the United States there are many FRP recycling pro-jects involving the military.

In most cases, products have already undergone somecompound treatment for usage, but this makes quality con-trol difficult and mixes foreign components. Process tech-nologies for removing artificially mixed impurities are stillnot satisfactory, so cascade recycling of materials of lowergrades than the original ones is unavoidable. Researchshould attempt not only to enhance separation and refiningtechnologies but also to develop processing technologiesthat permit or use impurities. This tendency is evident from

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RQHS Command

Fig. 1 Projects related to lead-free mounting in the world.

the recent international congresses on ecomaterials2), 3) andpapers on ecomaterials in international materials jour-nals.4)5) From this point of view, research on recyclingprocesses can be classified as follows (for details, refer tothe above documents):(1) Making impurities harmless: Clarifying the mechanismof impurities that adversely affect the process and immobi-lizing the impurities during the process(2) Materials design using impurities: Controlling the pre-sent form and distribution of impurities appropriately toutilize them as effective added elements(3) Solid-phase recycling: Recycling scraps in the solidphase, instead of melting and refining.

3.2 Recyclable materials designWhile devising the recycling of scraps, we need to

design marketing materials that are easy to recycle afteruse, especially for composite materials. Recyclable materi-als designs can be classified into:(1) Structure-controlled recyclable design: Design not toenhance properties by added elements but to produce vari-ous properties from materials of simple compositions bycontrolling microstructure.(2) New composite materials: Design combining materialsof the same chemical composition but different propertieswith easy-to-disassemble interfaces.

3.3 Materials technologies for recyclable product designEasy-to-disassemble design is one of the important ele-

ments of product ecodesign (environment-harmoniousdesign) based on lifecycle engineering. The basis of thisdesign is to facilitate separation and its importance is nowwidely recognized. Instead of time-consuming screws, vari-ous quick clamps are being proposed and new types of con-nections such as shape-memory springs6) and shape-memo-ry screws that lose threads, are being developed. Newadhesives for resin bonding include thermoplastic adhe-sives that soften when heated to make separation easy, onesthat are liquefied or produce foams when heated to debondinterfaces, and ones that debond upon absorbing water orreceiving ultraviolet irradiation. It is also proposed to useyeast and biodegradable plastics for connections. In thisunique method, water is added to the plastics to grow yeastfor separation. For metallurgical connections, it is proposedto use materials of low melting points for interfaces, tocondense degraded elements at interfaces by using the dif-fusion of atoms and ions, and to use hydrogen brittleness.Recently, NIMS developed a method of diffusing a low-melting-point metal on an interface for easy separation.Connections designed for easy separation are still at aprimitive stage and future development is expected.

3.4 Future outlookThere is no doubt that materials research conscious of

recycling will increase in future. However, research in thisfield only has value when actually used. As well as R&Dfor the future, it is equally important to develop individualtechnologies jointly with industry from the outset ofresearch by considering various scales of recycling.

4. Technology for evaluating lifecycle materials design

To improve ecomaterials of lifecycle design, not onlythe evaluation of conventional materials characteristics butalso the correct evaluation of lifecycle design compatibilityis important. The representative evaluation indexes are life-cycle assessment (LCA), materials flow accounting (MFA),eco-efficiency, and resource productivity.

4.1 Index by environmental loadLCA is a technique dedicated to the evaluation of prod-

ucts and services from the environmental aspect based onthe concept of lifecycle. A product lifecycle can roughly bedivided into the stages of manufacture, use, and disposal.Environmental loads are accumulated at each stage. Muchresearch on LCA methods and database construction isbeing done worldwide. The main LCA software overseas isthe Bousted Model (http://www.boustead-consulting.co.uk/products.htm). There is sufficient invento-ry data in Japan, and NIMS offers an inventory databasecontaining iron, steel, and nonferrous materials on its web-site (http://www.nims.go.jp/emc/).

4.2 Index by materials flowMFA is a technique of quantifying and grasping system-

atically the materials balance in units of country, area, orindustrial field. Since the late 1990s, surveys and researchhave been particularly active in Europe. In Japan,Moriguchi and co-workers of the National Institute forEnvironmental Studies7) are conducting advanced research.Tohoku University is conducting MFA research in EastAsia with cooperation from Nagoya University, WasedaUniversity, and NIMS, the purpose of which is to proposean MFA technique conforming to overseas trends andavailable for international comparison while compilingexisting MFA results of Japan. [JST RISTEX “Materialsflow as sustainability index”]

Total material requirement (TMR) is a technique focus-ing on hidden flows (or ecological knapsack). This tech-nique was proposed as a powerful means of expressingenvironmental stress factors related to materials use. As thematerial input per service (MIPS), this is given importancealso in “Guideline for Environment-compatible Design”8)

by the US Department of Environment. In Japan, NIMS isperforming approximate calculations of the total materialrequirements of metals.9)

Indexes generally called “recycling rate” are based onmaterials and product flows. However, the definition andmethod of calculating “recycling rate” differ betweenindustries and products, and many indexes focus on part ofrecycling. The Eco Material Forum is proposing a highrecycling index10) based on an overall view of the materialsflow as a guideline, and the index can be regarded as acommon language for discussing recycling. Future discus-sions on the recycling rate are expected to be based on thisguideline.

4.3 Index considering serviceThe above index is attracting attention also from the

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viewpoints of eco-efficiency and resources productivity.On the product level, eco-efficiency is calculated by com-paring the service provided by the product with the envi-ronmental load of the product. Eco-efficiency concernshow the service provided by the product and the environ-mental load of the product should be expressed. The afore-mentioned LCA is one technique of evaluating the environ-mental load. Resources productivity is the eco-efficiencywhen the environmental load is expressed as a function ofthe resources consumed. Japan’s Basic Project for Recy-cling Society divides the gross domestic product (GDP) bythe natural resources input (total amount of domestic andimported natural resources and imported products) to cal-culate the resources productivity. However, this is still atthe research stage and no index definitions or calculationmethods have been established for evaluating materials orproducts.

References

1) K. Halada and R. Yamamoto, Mater. Res. Soc. Bull., 11, 871(2001).

2) J. Adv. Sci. 13 (2002).3) Trans. Mater. Res. Soc. Jpn., 29 (2004).4) Mater. Trans., 43 (2002).5) Mater. Trans., 44 (2003).6) J. D. Chiodo, E. H. Billett and D. J. Harrison, EcoDesign 99: First

Intern. Symp. on Environmentally Conscious Design and InverseManufacturing, 590 (1999).

7) Y. Moriguchi, J. Mater. Cycles and Waste Management, 1, 2(1999).

8) US Environmental Protection Agency, “Design for theEnvironment”, Tomio Umeda, Kogyo Chosakai (1997).

9) K. Halada, K. Ijima, N. Katagiri and T. Okura, Jpn. Inst. Metals,65[7]564-570 (2001).

10) Eco Materials Forum, “High Recycling Index Guideline” (2004).

1. Introduction

To reduce energy-generated CO2 and curb global warm-ing, it is necessary to develop high-efficiency combined-cycle power stations and next-generation jet engines. Themost effective way to raise the efficiency of the thermalengines is to increase the temperature on the high-tempera-ture side of the Carnot cycle. High temperature materialsthat can withstand such temperature increases are nowbeing researched intensively, and platinum-group metalsappear to be the key to development.

This paper introduces research trends in the applicationof platinum-group metals to high temeperature alloys,focusing on Ni-base superalloys with platinum-group met-als additions, and refractory superalloys based on platinum-group metals. It also examines the outlook for traditionalrefractory alloys.

2. The future of refractory materials

At takeoff, the turbine inlet gas temperature of theengines of modern civil aircraft exceeds 1600˚C. Sincenext-generation engines will operate at higher temperaturefor higher efficiency, Ni-base superalloys having greaterheat resistance are required. For the 250-seater Boeing 787to enter service in 2008 and other new models, GE Corpo-ration of the US and Rolls Royce of the UK started to

develop high-efficiency engines (Figure 1) and are nowconsidering using next-generation Ni-base single crystalsuperalloys for the blades and vanes of thier high-tempera-ture turbines.

In Japan, the Ministry of Economy, Trade and Industrystarted developing a regonal jet plane and in 2003 initiateda project to develop an environment-friendly small jetengine. Thus, much work is being done on the developmentof high-performance engines both within and outside Japanand there is growing demand for advanced superalloys thatcould be used in such engines.

In the field of power generation, a combined-cyclepower-generation gas turbine of ultrahigh efficiency isindispensable at a turbine inlet gas temperature of 1700˚Cor higher and higher thermal efficiency of 56% in order tosubstitute coal-firing thermal power plants and to reduceCO2 effectively. Here too, there is a need for high tempera-ture materials for turbine blades and vanes. In addition, thegas turbine needs to be made more efficient in cogenera-tions for local power systems with higher electricity/heatratios.

Turbine blades are manufactured with a hollow interiorby precision investment casting. The metal temperature isadjusted by internal air cooling so that the blades can beused in a gas flow that is hotter than the melting point ofthe metal. Since air cooling lowers the thermal efficiency,however, the temperature capability must be maximizedand the cooling air must be minimized.

3. Development trends for Ni-base superalloys

An Ni-base superalloy can be made to exhibit excellenttemperature resistance by the coherent precipitate of 60 to70 vol% γ’ (L12 ordered phase whose basic composition isNi3Al) in the γ matrix (Ni solid solution) where the inter-phase interface provides a barrier to dislocations, and byincreasing the solution strengthening elements in bothphases by adding Re, W, and Ta. Figure 2 shows a typicalmicrostructure.

Ni-base superalloys have evolved from forged alloys toconventionally cast alloys, directionally solidified alloys,and single-crystal alloys. Single-crystal alloys have alsobeen evolving from first-generation alloys to second-gener-ation alloys containing about 3 wt% rhenium (Re), third-

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Fig. 1 Boeing 787 to enter service in 2008; a new high-efficiency engineunder simultaneous development.

Chapter 7. High Temperature Materials for JetEngines and Gas Turbines

Hiroshi HaradaHigh Temperature Materials Group, Materials Engineering Laboratory, NIMS

generation alloys containing about 5 to 6 wt% Re, andfourth-generation alloys containing a platinum-groupmetal, such as ruthenium (Ru) or iridium (Ir). Figure 3shows the background of enhancement in temperature

capability during this period.1) “Target” in the figure meansthe goal of development in the High Temperature Materials21 Project. Table 1 lists the compositions of typical single-crystal Ni-base superalloys.

The development of fourth-generation single-crystalsuperalloys with platinum-group metals additions is beingundertaken by GE in the US2) and the High TemperatureMaterials 21 Project3) in Japan. The addition of platinumgroup metals can couse the microstructure stability whichis a disadvantage of third-generation single-crystal alloys,thus improving the creep strength. This is a common char-acteristic of fourth-generation alloys.

In the High Temperature Materials 21 Project, thefourth-generation single-crystal alloy TMS-1384) which canwithstand 1083˚C and the fifth-generation single-crystalalloy TMS-1625) which can withstand 1100˚C have beendeveloped. The development methods are to stabilize themicrostructure by adding Ru or Ir and to refine the misfitdislocation networks at the boundary interface by control-ling the γ/γ’ misfit when an element (e.g. Mo) is added.Figure 4 shows a microstructure observed in a transmissionelectron microscope: very fine dislocation networks areformed on the interface.

Regarding the fourth-generation alloy TMS-138 (with 2wt% Ru) developed in the High Temperature Materials 21Project, a demonstration test of the alloy being used as a

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Alloy Composition Generation

Table 1 Compositions (wt%, remaining Ni) of single-crystal (SC) Ni-base superalloys for turbine blades.(The fourth-generation and fifth-generation SC superalloys contain Ru, a platinum-group element.)

Fig. 2 Typical microstructure of Ni-base superalloy.

Tem

per

atu

re fo

r 10

00-h

ou

r cr

eep

at

137

MP

a st

ress

Development goalSingle crystal

Directionally solidified

Year

Common cast

Forged

Fig. 3 Heat resistance improvement of Ni-base superalloy. (: forgedalloy, : conventionally cast alloy, : directionally solidified alloy, :single-crystal alloy; the solid symbols indicate alloys developed by theNational Institute of Materials Science (NIMS) and its joint researchcompanies).

γ phase

γ ’phase

Dislocation networks at γ / γ’ interface

Fig. 4 Misfit dislocation networks formed at the γ/γ’ interface of Ni-basesuperalloy during creep at high temperature.

high-temperature high-pressure turbine blade material wasperformed in the supersonic engine project of the Ministryof Economy, Trade and Industry in collaboration with aJapanese jet engine manufacturer, Ishikawajima-HarimaHeavy Industries. Figure 5 shows the test. The material willbe used in the first-stage turbine blade of Japan’s civil jetengine, an environment-friendly small jet engine now beingdeveloped by the Ministry of Economy, Trade and Indus-try.

Ru costs up to about 5,000 $/kg, lower than other pre-cious metals. If about 2 wt% is added, however, the aver-age cost of raw materials will increase about 50% and thecost of the completed turbine blades will rise by about20%. Nevertheless, the metal will certainly be used in next-generation aircraft engines to improve the engine efficiencyand specific fuel consumption.

If one turbine blade is assumed to weigh 300 g and asuperalloy containing about 2 wt% Ru is used, about 500 gof Ru will be necessary for one engine. If Ru is used fortwin engines on 1,000 planes, the necessary amount of Ruwill be about 1 ton in total. If Ni-base superalloy contain-ing Ru is progressively used on other aircraft engines, thenan even larger amount may be needed. However, the annu-al amount of Ru traded globally is no more than 10 tons, soit will be important to set up a stable supply system byestablishing a technology for recycling used componentsand remaining materials in the manufacturing processes.

As the gas temperature increases and the running condi-tions become severe, turbine blades and vanes, combustors,and other Ni-base superalloy components that are exposedto very high temperatures are usually coated for corrosionresistance, oxidization resistance, and heat shielding. Tradi-tionally, coating against corrosion and oxidation was doneby diffusion coating using chrome or aluminum, but Pt-Alcoating as well as MCrAlY coating are now widely used.

The High Temperature Materials 21 Project developedcoating materials of a new concept6) having long-term sta-bility and compatibility with Ni-base superalloys.

4. Development trends for refractory superalloys

Unlike Ni-base superalloys, refractory metals and theiralloys are expected to be used for turbine blades withoutcooling. Therefore, alloys based on Nb, Mo, W, and Tahave long been developed. However, high-temperaturestrength still cannot be achieved with oxidization resistance

or toughness, so these alloys are limited to applications in aprotective environment such as vacuum or inert gas.

In the High Temperature Materials 21 Project, refractorysuperalloys of the same γ/γ’ stracture as Ni-base superal-loys are being developed based on platinum-group metalshaving excellent oxidation resistance.7) Regarding Ni-basesuperalloys and Ir-base refractory superalloys, Figure 6shows the phase diagrams and typical microstructures oftheir prototype binary alloys (Ni-Al and Ir-Nb). From thefigure, we see that an alloy based on Ir with a melting pointof 2447˚C has crystallographically the same microstruc-tures suitable for enhancing the creep strength as Ni-basesuperalloys. However, the melting points are about 1000˚Chigher than those of Ni-base superalloys.

The resultant Ir-base refracrtory superalloys showedexcellent strength: the 2% deformation time was about 100hours in a compressive creep test at 1800˚C and 137 MPa.8)

Figure 7 compares the creep strength with those of otherrefractory alloys by using the Larson-Miller parameter.From this figure, we see that the Ir-base refractory superal-loys withstand the highest temperature among refractoryalloys, far beyond those of Ni-base superalloys.

The research by the Materials Engineering Laboratoryhas triggered the development of refractory superalloys

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Fig. 5 Single-crystal turbine blade made of a fourth-generation single-crystal superalloy TMS-138 and its ground test on a supersonic engine.

Fig. 6 Phase diagrams and microstructures of Ni-base superalloys andIr-base refractory superalloys.

Stre

ss(M

Pa)

Larson-Miller's parameter

Fig. 7 Comparison of creep strength between Ir-base refractorysuperalloys and other refractory alloys.(The Ir-base superalloys withstand 675˚C higher than the Ni-basesingle-crystal superalloys and have higher creep strength than Nb, Ta,and W alloys.)

130


based on platinum-group metals in South Africa, Germany,the USA, the UK, and other countries.9) Regarding Pt-Altype superalloys, for example, the γ’ phase (L12 phase) isknown to be unstable and transform to a different structureat comparatively low temperature. Therefore, the additionof third and fourth elements is now being attempted to sta-bilize the γ’ phase.

Platinum-group metals generally have much higher oxi-dization resistance than Nb, Mo, W, and Ta, and so refrac-tory superalloys based on them are promising ultra-hightemperature use. However, many issues remain to besolved, such as high cost, large specific gravity (Ir alloys:about 20), and insufficient ductility (Ir-base).

For Ir-base refractory superalloys, new approaches tomaterial design are being attempted. For example, Ni-basesuperalloys are mixed to optimize the cost performance,10)

while Pt-base refractory superalloys are mixed to increasethe ductility.11)

If γ solid solutions produced by mixing Ni, Co, Ir, Rh,Pt, and other FCC-type metallic elements are used as basemetals for refractory superalloys, then Ni-base superalloysto platinum-group refractory superalloys, including theirintermediate products, can be selected for materials accord-ing to cost performance, ductility, and oxidization resis-tance. Therefore, research is expected to proceed in thisdirection.

In the High Temperature Materials 21 Project, researchis being conducted in a wide range of other areas, spanningfrom basic research on refractory materials to practicalresearch through corporate linkage.12) Such researchincludes the development of next-generation turbine diskmaterials, highly ductile chrome alloys, and other newalloys; the development of material design techniques asthe basis for various new materials; microstructure analysisby three-dimensional atom probe and in-situ observation ofcreep deformation under an electron microscope; and thedevelopment of virtual gas turbine/Jet engine systems bylinking materials design and system design.

The overseas bases developing superalloys for jetengines and gas turbines are GE – Michigan University(USA), Rolls Royce – Cambridge University (UK), SNEC-MA (France)-ONERA (France).

5. Conclusion

To save fossil fuels, mitigate CO2 emission, and preventglobal warming, jet engines and various thermal enginesare expected to have higher performance and so thedemand for enhanced high temperature materials is grow-ing.

To meet this demand, fourth and fifth generation Ni-base single-crystal superalloys with platinum-group metalsadditions are starting to be used for jet engines. In addition,refaractory superalloys based on platinum-group metalshave been proposed in NIMS as new materials that maysurpass Ni-base superalloys in future. The new superalloysare now subject to global research and development, andcoating materials are also being developed.

In the field of refractory alloys, the importance of plat-inum-group metals is growing. In future, we expect thatnew superalloys based on platinum-group metals will beincreasingly used through linkage and cooperation in mate-rials research and recycling and other process research tocontribute to global environmental conservation and to theinternational competitiveness of Japanese industry with jetengines and gas turbines of high efficiency.

References

1) H. Harada and T. Yokokawa: MATERIA, 42, No. 9, 621-625(2003).

2) K.S. O’hara, W.S. Walston, E.W. Ross and R. Darolia: U.S. Patent5,482,789A (1996).

3) Y. Koizumi, T. Kobayashi, T. Yokokawa, H. Harada, Y. Aoki, M.Arai, S. Masaki and K. Chikugo, High Temperature Materials 2001,May 31-June 2, 30-31 (2001).

4) J.X. Zhang, T. Murakumo, Y. Koizumi, T. Kobayashi, H. Haradaand S. Masaki, JR: Met. and Mat. Trans. A, 33A, 3741-3749(2002).

5) Y. Koizumi, K. Chou, T. Kobayashi, T. Yokokawa, H. Harada, Y.Aoki and M. Arai: MRS Bulletin, 67, No. 9, 468-471 (2003).

6) H. Harada, A. Sato and K. Kawagishi: Patent pending, a paperaccepted for publication in Met. and Mat. Trans. A.

7) Y. Mitarai, Y. Ro, S. Nakazawa and H. Harada: MRS Bulletin, 64,No. 11, 1068-1075 (2000).

8) Y. Yamabe-Mitarai, Y. Gu and H. Harada, Met. and Mat. Trans. A,34A, No. 10, 2207-2215 (2003).

9) L.A. Cornish, B. Fischer and R. Volkl, MRS Bulletin, 28, No. 9,632-638 (2003).

10) X.H. Yu, Y. Yamabe-Mitarai, Y. Ro and H. Harada, Met. and Mat.Trans. A, 31A, 173-178 (2000).

11) C. Huang, Y. Yamabe-Mitarai, K. Nishida and H. Harada,Intermetallics, 11, 917-926(2003).

12) http://sakimori.nims.go.jp/

1. Global research trends

The demand for steel materials is growing to combatglobal issues such as environmental problems, shortages ofresources and energy, and aging of social infrastructure.Especially in East Asia, the explosive economic develop-ment is stimulating the demand for steel materials that canwithstand earthquakes attributable to geographical factorsand also atmospheric corrosion and so forth. Therefore,steel research in East Asia has been carried out undernational projects. In China, the 10-year NG Steel Project(Fundamental Research on New Generation of Steel Mate-rials in China) was started in 1999. In the first five years,40 organs including many universities conducted steelresearch, with the main themes being ultrafine-grain steel,delayed fracture, and nanodeposition in casting and rolling.In Korea, the 10-year HIPERS21 Project (High Perfor-mance Structural Steels for the 21st Century) was started in1998. In the first five years, basic research was conductedon ultrafine-grain steel, coastal weather resistant steel,ultrahigh-strength bolts, welding technology, and structuraldesign. In China and Korea, the projects have entered thesecond term. Researchers are now shifting the acquiredbasic science technologies toward applications, and aremaking progress in using structural materials designed forhigh strength and safety.

Thus, steel research is particularly active in East Asiaand many international conferences are held in this area.Related to the steel-related projects noted above, theInternational Conference on Advanced Structural Steels(ICASS) provides a forum for academic discussion on steelresearch in Japan, China, and Korea and is growing as aninternational conference to discuss the future of steelresearch. ICASS was held in Tsukuba in 2002 and inShanghai in 2004 and is scheduled to be held in Geongju,Korea in 2006. Many researchers from industry, academia,and the government are planning to participate.

2. Key trends in Japan

The Council for Science and Technology Policyannounced “Promotion of Industrial Exploitation in the

Field of Nanotechnologies and Nanomaterials” in July2003. To develop a bridge structure that is “earthquakeresistant, corrosion resistant, light weight, and low cost” inthe innovative materials industry according to the abovepolicy, ministries and agencies concerned initiated a linkedproject “New bridge structure” in 2004 for the purpose ofconstructing safe social infrastructure and strengthening theinternational competitiveness of the materials industry. Atthe Committee for Surveying the Utilization of Steel inCivil Engineering and Architecture of the Japanese Societyof Steel Construction, many researchers gathered from civilengineering laboratories, architecture laboratories, NIMS,universities, JR, JH, and private enterprises with specificdesign proposals for new structures using steels and theirbonding technologies (welding, bolts, etc.). Based on theresults of surveys conducted by the Japanese Society ofSteel Construction, the Committee will promote the evalua-tion of characteristics of steel structures from FY2005,focusing on automotive road bridges using steel, high-strength bolts, and the corrosion evaluation of weather-resistant steel bridges. Materials and structure researchersshould be encouraged to collaborate on future develop-ments, based on the great vitality of university researchersspecialized in civil engineering and architecture.

3. Research by NIMS

NIMS has long led the world in steel research and is alsohighly respected for its leading position in the Asian pro-ject noted above. The Steel Project is now in its secondterm. Based on the principles of increasing the strength andweather resistance by microcrystallization acquired in thefirst term, steel having high strength and corrosion resis-tance (steel factor of 4) available for use in cities was fabri-cated. Its chemical stability against corrosion was evaluatedby thermodynamic calculation, and Al and Si satisfying thetwo requirements of resource conservation and easy recy-cling were selected as weather-resistant elements to replaceNi and Cu. Since steel having high Al and Si contents isnot tough enough when the grains are of ordinary size, thetoughness was dramatically improved by microcrystalliza-tion. Microcrystallization has an advantage of increasing

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Section 1. Steel - Steel Technology for Strong, Safe

Structures

Toshiyasu Nishimura,Corrosion Resistant Design Group, Steel Research Center, NIMS

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the strength without needing to add special elements. As Aland Si are ferrite generating elements, a ferrite phase wasgenerated at welded sections, which prevented curing andenhanced the weldability. Thus, NIMS successfully devel-oped a material of excellent strength, toughness, and corro-sion resistance, supporting LCA and LCC. For steel struc-tures of high strength and safety, the novel material offersoverall excellence and is highly rated.

The principle of fabrication was established successfullyto enable the production of large or component-shapedsteel materials. NIMS also successfully solved the issue ofcreating steel-welded structures by ultra-narrow bevelGMA welding and large-output pulse-modulated CO2

welding developed in the first term, and the issue of pro-ducing bolts of 2000-MPa class strength. Many of theseachievements have been reported in academic journals andat conventions both within and outside Japan, and haveattracted worldwide respect. Regarding joint work withcivil engineering and architecture researchers on innovativestructural design using steel materials, progress is reportedsystematically at the steel workshop held every year.

4. Future outlook and actions

In the field of structural steel materials, various globalissues remain and can often be solved most efficientlythrough international cooperation. Therefore, it will beincreasingly important to solve specific problems throughlinkage and cooperation by concluding MOUs with theworld’s key research institutes. In China, for example, theSteel Research Center (SRC) concluded an MOU with TheCentral Iron & Steel Research Institute (CISRI) in 2002and with The Institute of Material Research (IMR) in 2004.In India, SRC has already concluded an MOU with AnnaUniversity. In partnership with the institutes, SRC intendsto conduct joint research in the field of corrosion. In 2003,SRC concluded an MOU with MPA (Staatliche Material-prufungsanstalt) of Germany in the field of materials evalu-ation, jointly with the Materials Information TechnologyStation. In 2004, SRC concluded an MOU with MPIE(Max Planck Institut fur Eisenforschung) of Germany toextend the range of cooperation in the field of steel. In2003, SRC concluded an MOU with VUZ (Vyskumny

ústav zváraèsky) of Slovakia in the field of welding. Byconcluding MOUs with research institutes all over theworld, SRC is constructing a global network to solve com-mon problems related to steel.

Meanwhile, it is important to increase international com-petitiveness in the field of steel. SRC is proceeding withstudies to enhance materials characteristics and is commit-ted to grasping characteristics as a practical basis. Next, itis important to exploit technologies for practical utilization.Specifically, we need an environment that enables us to usedeveloped materials in the quickly growing Asian market.Since East Asia is subject to frequent earthquakes and has ahot, humid climate that aggravates corrosion, allresearchers in East Asia need to make steel materials resis-tant to earthquakes and corrosion. As the leader in the fieldof atmospheric corrosion, Japan should guide other coun-tries toward solving the specific problems of high tempera-ture and humidity, coastal environments, and acid rain forthe whole of Asia, and should set up an Asian code onmaximizing the use of high-function materials. Currently,SRC is discussing and creating a specific plan with thoseinstitutes with which it has signed MOUs and other Asianresearch institutes.

Japan has been able to retain its world-leading positionin the field of steel through elemental research. Japan usedto have high levels of research on fracture, welding, andcorrosion, but as no attractive steel materials were pro-posed for a long time, the intellectual curiosity of theyounger generation could not be stimulated, causing uni-versities to lose interest in steel. To solve this great prob-lem, SRC is considering sharing the knowledge obtained sofar by steel research and pending issues with universities tomaintain the basic power of science in steel. For example,we would like to request university researchers to sharesteels and structures and discuss them from their profes-sional points of view to stimulate steel research. SRC hasalready started working toward this goal and will step upsuch activities in future.

References

1) The 9th Steel Workshop Proceedings, 9 (2005) p.1.2) “Survey and Research about New Structural Design for Utilizing

Steel,” FY2004 report by The Iron and Steel Institute of Japan.

1. Introduction

Heat-resistant steel that can be used for a long time athigh temperature is the key to developing thermal andnuclear power generation, chemical plants, power genera-tion from wastes, automobiles, and industries. During thelast decade, great progress was made in developing heat-resistant steels of high strength and corrosion resistance ateven higher temperature, and in evaluating materials interms of the welding joint characteristics necessary for con-structing plants, creep strength, and service life, for exam-ple, under social pressure to reduce CO2 emissions, dioxinsand other environmentally hazardous gases.

In five years from 1999 to 2004, major internationalconferences on heat-resistant steels were held twice in eachof Japan, Europe, and the US, making six times in total.Figure 1 shows the number of reports presented at the con-ferences by countries and the contents presented at theinternational conference held in the United States in 2004.Japan, Europe, and the US are about equal in the number ofreports, which have focused on materials development, oxi-dization, and corrosion.

2. Research trends on heat-resistant steels of highstrength and corrosion resistance

In the field of thermal power generation, the upper limitof temperature was about 620˚C for the conventional ferrit-ic heat-resistant steels. However, Japan, the US, andEurope made progress in the research and development ofhigh-strength 9-12Cr ferrite heat-resistant steels for large-diameter and thick boiler steel pipes and turbines that canbe used for a long time in a 650˚C ultra super critical(USC) power plant. By adding W or other elements,austenitic heat-resistant steels for boiler superheater tubeshas been enhanced from 18Cr-8Ni to 20Cr-25Ni and thento high Cr - high Ni to withstand steam temperatures of upto 700˚C. In the field of nuclear power, oxide dispersionstrengthened 9Cr ferrite steel, which is excellent both inhigh-temperature creep strength and irradiation resistance,was developed for cladding tubes for 650˚C fast breederreactors. Regarding hydrogen refining equipment in chemi-cal plants, the temperature and pressure were 454˚C and 17

MPa in the early 1990s when reaction chambers were madeof 2.25Cr-1Mo steel, but the subsequent development ofhigh-strength 3Cr-1Mo-V steel and 2.25Cr-1Mo-V steelraised the temperature and pressure to 482˚C and 24 MPaby 1995. These figures are now about to reach 510˚C and24 MPa. Regarding power generation from wastes, thedevelopment of austenitic heat-resistant steels having highcorrosion resistance enabled the boiler steam temperatureto be raised from about 300˚C at conventional plants up toabout 500˚C. In the automotive field, exhaust manifoldsused to be made of cast iron to withstand exhaust heat.However, as the exhaust gas temperature rose withimproved engine performance, higher strength wasrequired and so 18Cr-2Mo-Nb and other steels were devel-oped, raising the exhaust gas temperature to 900˚C or high-er.

Recent research on enhancing the creep strength of650˚C class ferritic heat-resistant steels has revealed that:- microstructure observation and creep deformation behav-ior analysis clarified that the formation of even a partiallyweak microstructure near a grain boundary promotes localcreep deformation and causes premature fracture, andsome guidelines on materials design showed that finemicrostructure could be maintained near a grain boundaryfor a long time.

Based on these guidelines, NIMS proposed: a steel forthe long-term stabilization of M23C6 carbides near grainboundaries by adding a high concentration of boron; a steelfor stabilizing microstructure near grain boundaries withnano-size MX-type nitrides only; and a steel having onlyFe2(Mo,W)-Laves phase and other intermetallic com-pounds without using carbonitrides. The world is monitor-ing the results of long-term creep tests which are still con-tinuing and the microstructure stability.

Regarding corrosion resistance, the resistance in high-temperature steam has been increased greatly. This resis-tance depends on the Cr concentration. Since the Cr con-centration of ferritic heat-resistant steels is generally as lowas 12% or less, an oxide scale rich in Fe is generally pro-duced on the surface. Therefore, the main issue used to behow to suppress the growth of this thick oxide scale of Feby adding alloy elements or by other means. On the con-trary, NIMS recently found that, even when the Cr concen-tration is about 9%, by adding about 0.5% Si and perform-

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Section 1. Steel - Steel Technology for High-Efficiency

Energy

Fujio AbeHeat Resistant Design Group, Steel Research Center, NIMS

134


ing pre-oxidation treatment, a nanometer-thick Cr2O3 pro-tective scale can be formed to improve the oxidation resis-tance remarkably. This finding caused great interest inCr2O3 protective scale also in Europe and the US. Regard-ing the exfoliation characteristic of surface scale, a testmethod needs to be established. Surface coatings are alsobeing researched but there are problems of complicatedprocess and cost.

3. Trends of research on the strength of welded joints

If a welded structure made of ferritic heat-resistant steelsis used under high temperature and low stress (about 600˚Cand 100 MPa or less), brittle creep fracture or so-calledType IV fracture progresses at the weld heat-affected zone(HAZ). This causes the serious problem of short creep lifecompared with the base material. In Japan, Europe, and theUS, therefore, 9-12Cr ferritic heat-resistant steels are beingstudied to clarify the mechanism of Type IV fracture, toanalyze the fracture dynamics of brittle creep fracture, andto prevent Type IV fracture.

Regarding the mechanism of Type IV fracture, the HAZgrain refinement model and HAZ softening model wereproposed, of which the former is becoming dominant. Inother words, heating up to about Ac3 changes the HAZregion to fine grains and reduces the life. Regarding frac-ture dynamics analysis, a high-temperature creep crackpropagation test using CT specimens of welded joints wasconducted and the analysis results clarified that high-strength 9-12Cr steels are subject to cracking in HAZregions. By analyzing stresses in welded joints by the finiteelement method (FEM), with the creep strength parametersof the welded metal region, HAZ region, and base material,cracking positions could be accurately predicted. FEMcodes were also developed to simulate the generation of thecreep void ahead of the crack tip and the progress of thecrack. Regarding the prevention of Type IV fracture, theaforementioned high-boron 9Cr steel of NIMS was report-ed to be free of grain refinement in the HAZ region andtherefore resistant to Type IV fracture. This is attractingattention in Europe and the US.

4. Trends of research on predicting long-term creep life

In Japan and Europe, high-strength 9-12Cr steels werefound to suffer quick loss of creep strength at 550˚C orhigher temperature often after prolonged use. This quickloss of creep strength is now actively being analyzed evenwith the latest energy filter type of transmission electronmicroscope to clarify the microstructure degradation fac-tors. High-strength 9-12Cr steels are usually produced bynormalizing-tempering heat treatment. This heat treatmentreforms steel to a microstructure of high precipitationstrength where fine (about 100 nm) M23C6 carbides andnano-size M2X and MX-type carbonitrides are precipitated

in a lath-block microstructure having high dislocation den-sity. Japan and Europe are now competing fiercely to clari-fy the phenomenon in which re-dissolution of nano-sizeM2X and MX during creep promotes the formation of Zphase (Cr(V,Nb)N type composite nitride), which is ther-modynamically more stable and rough, and the creepstrength drops quickly.

For predicting long-term life, the Larson-Miller methodand other time-temperature parameter (TTP) methods usedto be used widely. However, it gradually became clear thatthe conventional TTP methods could not evaluate long-term creep life correctly but tended to overestimate it. Tosolve this problem, new analysis techniques were proposed:- Classifying creep rupture data by temperature dependenceor areas having the same activation energy.- Splitting the area of creep rupture data with half the 0.2%yield strength of the tensile test as the criterion and analyz-ing only data in the low-stress area because time-indepen-dent plastic deformation at loading under high stress affectsgreatly the subsequent creep deformation behavior.These techniques have improved the accuracy of long-termlife prediction to about 100,000 hours.

5. Future outlook

As plant temperatures are raised to improve energy effi-ciency, it is becoming important to establish the foundationof heat-resistant steels that can be used safely for a longtime without showing deterioration of creep strength.Researchers are now interested in clarifying the transitionprocess of nano-precipitates during high-temperature use,the long-term strength at high temperature, the generationand exfoliation of a nanometer-thick surface protectivescale, and the brittle fracture behavior of a welded joint interms of fracture dynamics.

Other countries:28 reports, 8.3%

Life Assessment:7 reports, 12.1%

Weld & Fracture:7 reports, 12.1%

Components:9 reports, 15.5%

Oxidation &Corrosion:

17 reports, 29.3%

Materials &Alloy Development:18 reports, 31.0%

4th EPRI Conf. (2004)(58 reports in total)

USA:75 reports, 22.2%

Japan:115 reports, 34%

Europe:120 reports, 35.5%

Intern. Conf., 1999-2004(338 reports in total)

Fig. 1 Number of reports made at six international conferences on heat-resistant steels in Japan, Europe, and the USA in the 5-year period from1999 to 2004 and the contents of reports made at the conference in theUSA.

1. Introduction - Global trends

There are high expectations worldwide for hydrogenfuel as a clean energy solution to global warming and pol-lution (NOx, particulate matter (PM), etc.). However, thesafety of the entire hydrogen system that produces, stores,transports, and utilizes hydrogen, a material that is explo-sive and not widely used, requires detailed study. Morespecifically, it is important to ensure the safety of materialsused for storage tanks, hydrogen tanks on hydrogen fuelcell cars, pipes, valves, joints, compressors, and so forth.Structural measures to prevent hydrogen leakage and sens-ing technologies are also necessary.

Regarding the global trends in hydrogen fuel cells, theuse of fuel cells on the Apollo and space shuttle while inspace drove technological development in the UnitedStates. In 1993, President Clinton proposed that fuel cellsbe used for vehicles, triggering intensive research on suchapplications. Even after the Bush Administration took over,the policy on fuel cell development was strengthened. InFreedom CAR 9 led by the Department of Energy (indus-try-government partnership between Ford, GM, DaimlerChrysler and the government until 2010),1) technologicaldevelopment is being promoted with an emphasis on tech-nologies related to hydrogen fuel cell cars. In the State ofthe Union address at the end of January 2003, PresidentBush declared that the United States would lead the worldin the development of clean hydrogen fuel cars and pro-posed a total budget of 1,700 million dollars for 5 yearsfrom 2004 to develop a hydrogen cell from the hydrogeninitiative and Freedom CAR, the foundation of the hydro-gen industry, and advanced automotive technologies.2)

In the EU, fuel cells and related technologies are beingdeveloped in the Framework Program,3) which is a compre-hensive R&D project led by the Directorate-General forResearch and (Research DG) and Directorate-General forScience, Research and Development (DG12) at the Euro-pean Commission,4) fuel cell development began in the 3rd

Framework Program (FP3) starting in 1992. From FP5(1998-2002), more than half the budget for fuel cells andhydrogen energy has been allocated to technological devel-opment for transportation. In FP6 for the five years from2002, technologies are being studied to reduce the costs ofstationary and automotive fuel cells, to develop advancematerials for fuel cells, and to construct infrastructure for

producing and supplying hydrogen. In relation to this, theClean Urban Transport System for Europe (CUTE)5) andthe Ecological City Transport System (ECTOS)6) are nowdemonstrating hydrogen fuel cell buses.

Since hydrogen fuel cells are targeted at automobilesthat appear on the international market, Western countriesare keen to have their own standards adopted international-ly.2)

2. Domestic trends

At EXPO 2005 AICHI in Nagoya, hydrogen fuel cellhybrid buses traveled among the pavilions and a hydrogenstation was exhibited. This indicates people’s keen interestin hydrogen infrastructure, such as hydrogen fuel cars andtheir hydrogen stations, in Japan as well as in Europe andAmerica.

Japan’s international clean energy system project forhydrogen utilization “WE-NET”7) was started in 1993under the New Sunshine Project, and the New Energy andIndustrial Technology Development Organization (NEDO)has promoted research.7-9) In the first term (FY1993-1998),the low temperature materials R&D group selected austen-ite stainless steels which are widely used for cryogenic ves-sels and Al alloys used for LNG tankers as candidate mate-rials and tested them as base materials and welded joints inliquid hydrogen and low-temperature hydrogen gas. In thesecond term (FY1999-2002), the development of hydrogensupply stations, automotive hydrogen storage materials,and solid molecular fuel cells with pure hydrogen supply,and hydrogen diesel engines was planned in order to spreadthe hydrogen system in society. The low temperature mate-rials R&D group promoted research with a view to devel-oping elemental technologies for optimum bonding materi-als and methods.

The R&D contents and achievements are summarizedbelow.8,9)

• Selection of candidate materials and welding methods:As candidate materials, the aforementioned austenitestainless steels and Al alloys were selected. For stainlesssteel welding, CO2 laser welding, reduced pressure elec-tron beam welding (RPEB), and friction stir welding(FSW) were used, as well as tungsten inert gas welding,metal inert gas welding, and submerged arc welding.

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08 Metals

Section 1. Steel - Steel Technology for Hydrogen Utilization

Eiji AkiyamaCorrosion Resistant Design Group, Steel Research Center, NIMS

• Introduction of test equipment into liquid nitrogenatmosphere: Test equipment was fabricated for tensilestrength, fracture toughness, and fatigue tests in a cryo-genic atmosphere.

• Large-scale liquid transportation and evaluation of char-acteristics of stored materials: Thick plates of the candi-date materials were welded, and the welded metal jointswere evaluated for their cryogenic characteristics andagain after hydrogen charging of about 10 ppm. TheJapan Atomic Energy Research Institute developed acomplete γ-type welding material (12Cr-14Ni-10Mn-5Mo-N steel) featuring high toughness and excellent sol-derability. When this material was welded by the con-ventional method, the welded joints showed sufficientcryogenic toughness and did not crack at high tempera-ture, showing that the welding method is effective forlarge tankers and tanks. For welding very tough andthick plates, RPEB and FSW are promising. SUS304L,SUS316L, and SUS316LN showed sufficient fatigue lifeboth as base materials and welded joints. For welding Alalloys, FSW and RPEB are effective.

• Research on hydrogen embrittlement: The results of ten-sile tests on austenite stainless steels in a hydrogenatmosphere and a helium gas atmosphere indicated thatbrittleness sensitivity to a hydrogen environmentincreases as the temperature falls below room tempera-ture. After reaching a maximum value at about 200 K,the sensitivity dropped quickly and the influence ofhydrogen was lost at about 150 K or lower. Therefore,criteria for selecting austenite stainless steels could beset from the fact that the phenomenon is related to thegeneration of strain induced martensite and the sensitivi-ty decreases as the austenite phase becomes more stable.In addition, fundamental research was conducted on theconditions of hydrogen permeation into materials andthe local fracture toughness in a hydrogen gas environ-ment, and also on the influences of coolant on mechani-cal properties at 20 K. From the test results, a databasewas constructed.These R&D results were used in the next 5-year project

of NEDO, “Development of Safe Utilization and Infra-structure of Hydrogen” from FY2003 to 2008. In this pro-ject, safety and technologies for implementing hydrogenenergy are being developed to ensure the smooth introduc-tion and implementation of polymer electrolyte fuel cells(PEFC). WE-NET was mainly for materials research at lowtemperature and in a liquid hydrogen atmosphere. Thematerials research in this project, however, is intended toconstruct a safe infrastructure in a liquid hydrogen environ-ment. The research includes further development of hydro-gen stations that supply hydrogen to fuel cell cars by usingPEFC and development of technologies for high-pressurehydrogen tanks to be mounted on cars.9,10)

For fuel cell cars and stationary fuel cells to becomereality, basic safety data needs to be accumulated for re-inspection and standardization, with demonstration tests.Therefore, this is a common basic technology for thehydrogen infrastructure, vehicle-related equipment, andstationary systems. The theme “Basic property research onhydrogen materials” is classified into materials properties

in “Safety technology” above. As common and basic safetymeasures for hydrogen, the basic properties of hydrogenmaterials are being researched. The main candidate materi-als are stainless steel SUS316L and Al alloy A6061T6. InFY2003 and FY2004, strength, fatigue, and other basicproperty data were collected for materials to be used for35-MPa class high-pressure hydrogen equipment. The spe-cific items are as follows:8-11)

• Lining materials for high-pressure hydrogen tanks (Alalloy, stainless steel, etc.)

• Enhancing the durability of high-pressure hydrogenpumps (stainless steel, etc.)

• Materials for high-pressure hydrogen accumulators (Cr-Mo steel, etc.)

• Materials for high-pressure valves and joints (stainlesssteel, etc.)

• Structural materials for liquid hydrogen (stainless steel,etc.)

• Basic properties of nonmetallic materials for hydrogen(FRP, etc.)

• Survey of properties of materials for hydrogen and data-base creation

• Development of hydrogen characteristic test equipmentand basic property evaluation (low strain speed test,fatigue test, and evaluation of fatigue crack propagationcharacteristics) of hydrogen materials with the equip-ment

• Research on materials properties in a cryogenic gasenvironment

• Evaluation of hydrogen-absorbing characteristics• Evaluation of metallic materials for hydrogen stand• Fatigue and tribology evaluation of hydrogen materials

in a hydrogen environmentThe research themes in FY2005 to FY2007 are to extend

the collected basic property data of materials used for auto-motive tanks, stationary tanks, pipes, valves, and other ele-mental equipment and to develop practical materials andtechnologies suitable for use in various high-pressurehydrogen environments. To achieve these themes, industry,academia, and the government set up a linked research sys-tem.

Since the mounting of hydrogen tanks on vehicles wasderegulated in April 2001, the method of storing hydrogenfor fuel cell cars changed from hydrogen absorbing alloy tocompressed hydrogen, and practical fuel cell cars are nowquickly becoming reality. The High Pressure Gas SafetyLaw is now limiting hydrogen tanks to a maximum pres-sure of 350 bars (about 35 MPa). For a hydrogen fuel cellcar to achieve the target cruising distance of 500 km, aboutequal to a gasoline vehicle, the filling pressure will need tobe even higher. Therefore, research is now being conductedon a compressed hydrogen method using a vehicle-mount-ed ultrahigh-pressure tank for up to 700 bars and the liquidhydrogen method. Related technologies being studied forsuch pressure include: hydrogen compressors, dispensers,flowmeters, couplings, and filling control technologies,while technologies for liquid hydrogen include: liquidhydrogen containers, boosters, and pumps.12,13) For thesediverse elemental equipment, new practical steel materialsare needed.

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In the first term of WE-NET (FY1993-1998), theNational Research Institute for Metals (present NationalInstitute for Materials Science: NIMS) evaluated cryogenicmaterials jointly with Chugoku National IndustrialResearch Institute8,9) on the “Development of cryogenicmaterials technologies” related to “Hydrogen transportationand storage technologies,” entrusted by The JapanResearch and Development Center for Metals (JRCM). TheNational Research Institute for Metals conducted researchon low temperature brittleness and the Chugoku NationalIndustrial Research Institute conducted research on hydro-gen embrittlement.

In the second term (FY1999-2002): (1) To clarify themechanisms of hydrogen embrittlement and cryogenicembrittlement, JRCM, the National Institute of AdvancedIndustrial Science and Technology, NIMS, and the Materi-als Testing Institute University of Stuttgart (MPA) con-ducted joint research. (2) Regarding welding technologies,The Welding Institute (TWI) of UK conducted jointresearch with JRCM.

For “Basic property research of hydrogen materials”(from FY2003) in “Development of Safe Utilization andInfrastructure of Hydrogen,” the Hydrogen MaterialsDevelopment Committee was set up in JRCM and aresearch entity was organized consisting of experts fromthe National Institute of Advanced Industrial Science andTechnology, NIMS, Kyushu University, Aichi Steel Corpo-ration, Nippon Steel Corp., and Sumitomo Metal Indus-tries, Ltd.9,10) NIMS is sharing the theme of “Research onmaterials characteristics in a cryogenic gas environment.”The fatigue test, Charpy impact test, and tensile test here ina cryogenic environment are also used to create data sheetson the strength of aeronautical materials.

In addition, NIMS is examining the influence of hydro-gen gas on the fatigue strength of various materials jointlywith Professor Murakami of Kyushu University to confirmthe importance of hydrogen trapped in inclusions for super-long life fatigue fracture, and to ensure the long-term safetyof a fuel cell system. (“Influences of hydrogen on gigacyclefatigue fracture mechanism and establishment of fatiguestrength reliability enhancement method” (FY2002 toFY2006, funded by a science research subsidy and repre-sented by Prof. Yukitaka Murakami, Kyushu University).

Hydrogen can cause delayed fracture of high-strengthsteel, so research is underway to clarify the mechanism ofsuch fracture, to develop a method of evaluating thedelayed fracture characteristics, to study the influences ofmicrostructure on delayed fracture, to fabricate high-strength materials having excellent resistance to delayedfracture characteristics, to clarify the hydrogen trap site insteel, and to study a design guideline for hydrogen traps.Research is currently focusing on high-strength bondingmaterials for architecture and not directly targeted at mate-rials related to hydrogen energy. However, the knowledgeobtained can be applied to materials related to hydrogenenergy. Other activities include joint research with KAIST(Korea) on the hydrogen induced deterioration of low-alloymaterials for pressure vessels14) and research on the hydro-

gen embrittlement of iron-base alloys.15)

4. Key research by organizations other than NIMS andfuture outlook

For “Targeted Support for Creating World-levelResearch and Education Bases” (21st Century COE) inFY2003, the Ministry of Education, Culture, Sports, Sci-ence and Technology selected “Integration Technology ofMechanical System for Hydrogen Utilization” of KyushuUniversity. Accompanying this, the Research Center forHydrogen Utilization Technology was inaugurated.16) Thisis the world’s sole institute for general technologicalresearch on hydrogen utilization, covering a wide range ofresearch from the atomic level to large structures. Regard-ing the strength of metallic materials, for example, the lossof strength caused by hydrogen entry into metal and metalfatigue are being researched. There are also various otherresearch themes, such as bearing damage by wear, friction,seal deterioration, and hydrogen entry and hydrogen leak-age. To take the advantage of the fact that there are manyautomobile manufacturers for producing fuel cell cars andcompanies holding byproduct hydrogen, the Fukuoka Strat-egy Conference for Hydrogen Energy was set up by indus-try, academia, and the government in Fukuoka Prefecturein August 2004. As of February 28, 2005, the conference isparticipated in by 91 corporate members, 78 universitystaff, 12 research and support institutes, and 8 administra-tive organizations. The main activities of this conferenceare to create industry-academia-government projects head-ed by the Research Center for Hydrogen Utilization Tech-nology, to perform various demonstrations with the newcampus (Hydrogen Campus) of Kyushu University andKitakyushu Eco-town District serving as experimentalmini-societies, and to train human resources.

The COE program “Establishment of COE on Sustain-able Energy System” of Kyoto University has four pillars,one of which is “Construction of hydrogen energy technol-ogy”.17) In future, research at such large bases will be thedriving force behind materials research to realize a hydro-gen energy society.

At present, hydrogen fuel cell cars are being demonstrat-ed by test runs and hydrogen stations are being constructedboth within and outside Japan, suggesting that they maysoon enter practical use. It is therefore becoming increas-ingly important to develop and select reliable items andevaluate them accurately. To extend the cruising distanceto the same level as that of a gasoline vehicle, the hydrogenstored in fuel cell cars will be compressed further12,13) andyet the weight of storage tanks and car bodies needs to bereduced. Therefore, a high-strength steel which is safe touse in hydrogen gas environments and which has excellentpressure resistance will need to be developed.

References

1) http://www.eere.energy.gov/vehiclesandfuels/2) Fuel Cell Project Team Report - Japan’s first Project X

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“Developing an engine for earth reproduction” - Fuel Cell ProjectTeam of Vice Ministers’ Conference (2002).

3) http://fp6.cordis.lu/fp6/home.cfm4) NEDO Overseas Report No. 906-908, 910 (2003).5) http://europa.eu.int/comm/energy_transport/en/cut_en.html6) http://www.newenergy.is/7) http://www.enaa.or.jp/WE-NET/8) NEDO Achievement Report Database http://www.tech.nedo.go.jp/9) JRCM News, No. 204, 205 (2003).

10) Polymer Electrolyte Fuel Cell/Hydrogen Energy UtilizationProgram “Basic Plan for Development of Safe Utilization andInfrastructure of Hydrogen” NEDO Hydrogen Energy TechnologyDevelopment Section. http://www.nedo.go.jp/hab/project.html

11) “Development of Safe Utilization and Infrastructure of Hydrogen”(Interim evaluation) Reference material for the first subcommitteemeeting 5-2, 6-4.

12) Y. Tamao and T. Ogata, Science & Technology Trends, Februaryissue (2003).

13) Y. Tamao and R. Omori, Materia., 44, 188 (2005).14) X. Wu, Y. Katada, S. G. Lee and I. S. Kim, Metall. Mater. Trans.

A, 35A, 1477 (2004).15) Y. Tateyama and T. Ohno, Phys. Rev., B67, 174105 (2003).16) http://www.f-suiso.jp/, http://www.kyushu-u.ac.jp/magazine/

kyudai-koho/No. 36/36_18.html17) http://energy.coe21.kyoto-u.ac.jp/

1. Introduction

Before structural materials can be used for machines orplants, the total reliability and safety characteristics of thematerials must be clarified. This makes it necessary toaccumulate an enormous amount of laboratory data, toaccumulate understanding and knowledge about character-istics, and verify the materials by preliminary use. There-fore, it takes a long time from research and development ofmaterials until the materials are actually used in machines,plants, and other products. Since damage still occurs, how-ever, it is necessary to evaluate the strengths of materialsand modify designs to ensure the appropriate use of materi-als.

Structural materials have various characteristics but thecharacteristics must maintain the product performance ofmachines and plants and ensure safe use for a long time.The important characteristics are high-temperature creep,fatigue, and corrosion that depend on time. The time-dependent characteristics are especially important becauseit takes a long time to acquire such data and the characteris-tics are difficult to understand. Based on the results of arecent survey and the reference materials for research andsurvey, this report explains the importance of research onlong-term data accumulation and life evaluation forenhancing the reliability of heat-resistant steels; therequirements for acquiring long-life fatigue data becauselong-life fatigue is related to the development of high-strength materials and clarifying the fracture mechanism; anew metallic structure analysis technique for understandingfatigue characteristics, and a risk-based thinking for mak-ing effective use of optimum materials.

2. Research characteristics

2.1 Creep characteristic of heat-resistant steelSince 1980, the temperatures of thermal power plants

and petrochemical plants have been raised to save energyand mitigate global environmental problems, and so heat-resistant steels have been actively developed. By consider-ing not only high-temperature creep strength but also thesuppression of thermal stress which is generated duringnon-stationary operation, high-Cr ferrite steels having highstrength are attracting attention instead of austenitic stain-

less steels and many materials have been proposed. As datais accumulated from long-term creep tests on high-Cr fer-rite steels, however, researchers are beginning to notice thatthe creep strength remarkably decreases after a long time at550˚C or higher and that the strength value estimated byconventional short-time creep test data is not necessarilyreliable. Damage has also been reported at welded joints ofstructural components made using such materials.

By acquiring long-term creep strength data of high-Crferrite steels, the drop in strength after a long time wasstudied. This research clarified that the recovery of tem-pered martensite differs between high and low stresses andproduces a non-uniform metallic microstructure at lowstress after a long time where only the neighborhood of theprior austenite grain boundary has recovered. In addition,progress has been made in research on the mechanism bywhich the creep strength of high-Cr ferrite steels is mani-fested.1) High-Cr ferrite steels develop high dislocationdensities by thermal treatment and strengthened precipita-tion by the dispersion of fine precipitates. Precipitatesbecome coarse during creep, the pinning force of disloca-tion goes down, and the creep strength drops quickly.

After this mechanism was clarified, a method of predict-ing life modified from the conventional one was proposed.NIMS proposes a method in which the area of creep frac-ture data is split with half the 0.2% proof stress of the ten-sile test as the criterion and only data in the low-stress area

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Fig. 1 Long-life prediction of modified 9Cr-1Mo steel by the areasplitting method.

08 Metals

Section 1. Steel - Reliability of Steel Materials

Koichi YagiMaterials Technology Information Station, NIMS

is analyzed.2) Figure 1 shows the results of applying thearea splitting method to the modified 9Cr-1Mo steel; theexperimental data matches the predicted value well. Thismethod has been used to review the allowable stress ofhigh-Cr ferrite steel for thermal power plants.3)

2.2 Fatigue characteristics of structural materialsFatigue fracture was found to occur even in a long-life

area exceeding 107 cycles which had been considered thefatigue limit of steels; this phenomenon is called gigacyclefatigue. This super-long-life fatigue is unique to high-strength steels and characteristic of the origin of an internalfracture. The influences of various factors on super-long-life and the fracture mechanism are being researched withinand outside Japan.4)

NIMS is also acquiring data on super-long-life fatigueand conducting research based on it. About 20 years ago,NIMS (the former National Research Institute for Metal)started collecting data about up to 108 cycles by consider-ing the problem of fatigue in the long-life area and studiedthe presence or absence of a fatigue limit and also internalfractures. NIMS thus reported that a fatigue limit could notbe determined by 108 cycles. Meanwhile, industry stronglydemanded the collection of long-life fatigue data to ensurereliability in the long-life area for using high-strength mate-rials to reduce weight. Therefore, NIMS initiated a projectto acquire long-life fatigue test data for up to about 1010

cycles from high-strength steels and titanium alloys. Forthe fatigue test of 1010 cycles, it takes three years at thecyclic speed of 100 Hz, so data is being collected simulta-neously by a 20-kHz ultrasonic fatigue test machine.

Figure 2 shows the long-life fatigue test results of springsteel SUP7.5) The results of the rotating bending fatigue testand the ultrasonic fatigue test matched those of the long-life fatigue test. This means that reliable data can beacquired by the ultrasonic fatigue test if care is taken. In thesuper-long-life area, a fracture originates from an internalAl2O3 inclusion. The weak bonding between this inclusionand the matrix is considered to be the cause of internalfracture. The influence of danger volume on the internalfracture characteristic is also studied.

A fatigue fracture often occurs from a crack in a non-

continuous region. Many studies used to follow a mechani-cal engineering approach, but since the super-long-lifefatigue characteristic depends on the metallic microstruc-ture of the material as mentioned above, research on super-long-life fatigue requires a materials approach. Thermaltreatment produces various metallic microstructures fromsteel materials and achieves the requested strength charac-teristic. As metallic microstructures produced by thermaltreatment affect the fatigue characteristic, the characteristicshould be evaluated in relation to fine metallic structureinformation. Therefore, researchers are recently conductingnano level structure analysis by using an intoratomic forcemicroscope (AFM), and nano-meso-macro multilevelstrength analysis linking with nano-level strength andfatigue strength evaluation by ultra-small hardness testingprocedure.

As Figure 3 shows, a high-Cr ferrite steel shows a com-plicated metallic microstructure produced by thermal treat-ment. To evaluate its fatigue characteristic, a quantitativeunderstanding of the metallic microstructure is necessary,and so a nano-scale structure analysis method with AFM isused.6) By this method, the non-uniformity of microstruc-tures was evaluated quantitatively and its relation betweenhigh-temperature fatigue characteristic and metallic struc-ture was clarified.

2.3 Material strength and risk-based engineeringMany of the recently developed structural materials are

used nearly at their strength limits and under extremelysevere conditions for the materials. Therefore, the life eval-uations and deterioration diagnoses of materials need to beeven more accurate. However, it is impossible to reduce thefailure probability to zero because of the dispersions ofmaterial characteristic values and the inaccuracies of lifepredictions and deterioration diagnoses. As long as materi-als are used, therefore, there is always the possibility offracture. When selecting materials, we should not onlydetermine the product, system, technology, or materialsbased on the possibility of an accident by fracture, but alsoby considering the scale of a disaster or damage caused bythe accident or fracture. This is called risk assessment.

To establish risk-based engineering that uses risks as

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Fig. 2 Long-life fatigue strength of spring steel SUP7.

Block boundaryPacket boundary

Lath boundary

Prior γ grain boundary

Fig. 3 Multilevel structure of martensite.

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indexes, we need to create a database or acquire knowledgefrom accident information, to establish a risk evaluationtechnique, and to study risk recognition and communica-tion in society. As well as this research, risk evaluations onactual machines and plants are also often reported.7) Toprovide necessary information for future risk evaluationsfrom the viewpoint of materials, NIMS is proceeding withR&D on creating a materials risk information platform incollaboration with research institutes, universities, andenterprises.8)

3. Future outlook

Research on the reliability of structural materialsrequires a great investment in research equipment and facil-ities. One institute alone cannot tackle such research, butrequires assistance from domestic and overseas researchinstitutes, research groups, and enterprises. NIMS is con-ducting research on the reliability of structural materials bylinking the structural materials data sheet project at theMaterials Information Technology Station with materialscreation at the Steel Research Center. Comprehensiveactivities like this are rare even outside Japan and will needto be expanded in future. In addition, we need to create asystem whereby such activities can be connected to domes-tic and overseas activities physically and effectively to

make best use of research results through informationexchanges. Safety is critical for constructing a societybased on science and technology and it is important toensure that the results of reliability research are of benefitto society. NIMS is expected to strengthen informationexchanges and cooperation with enterprises, to grasp needsappropriately, and to help inform the world of designstrength values derived in Japan.

References

1) F. Abe., Bulletin of The Iron and Steel Institute, Japan, 10, 302(2005).

2) K. Kimura, H. Kushima and T. Abe, Journal of The Society ofMaterials Science, Japan, 52, 57 (2003).

3) Japan Power Engineering and Inspection Corporation: FY2004report “Investigation of Conformance to Technical Standard forLong-term Creep Strength Drop of High-chrome Steel”, March2005.

4) Y. Ochi and T. Sakai, Journal of The Society of Materials Science,Japan, 52, 433 (2003).

5) Y. Furuya, T. Abe and S. Matsuoka, Fatigue Frac. Engin. Mater.Struc., 26, 786 (2003).

6) M. Hayakawa and S. Matsuoka, Materia Japan, 43, 717 (2004).7) K. Yagi, Journal of The Japan Society of Mechanical Engineers,

107, 597 (2004).8) K. Yagi, Journal of The Japan Institute of Metals, 66, 1264 (2002).

1. Aluminum alloys

1.1 IntroductionReducing the weights of aircraft, rolling stock, and auto-

mobiles is effective for saving energy and curbing CO2.Therefore, aluminum alloys are being researched throughboth alloy development and process development and theirapplication areas are expanding.

Aluminum alloys can roughly be classified into rolledmaterials (sheets, foils, sections, tubes, bars, wires, andforging) and cast materials (casting and die casting). Rolledmaterials can further be classified into pure aluminum(1000 series), Al-Mn (3000 series), Al-Si (4000 series), Al-Mg (5000 series), Al-Cu-Mg (2000 series), Al-Mg-Si(6000 series), and Al-Zn-Mg (7000 series). Cast materialscan further be classified into Al-Si, Al-Mg, Al-Cu-Si, Al-Cu-Mg-Si, and Al-Mg-Si.

Alloy development is particularly active for the 2000-series and 7000-series rolled materials, which are mostimportant for transportation equipment such as aircraft.Regarding process development, the application of the6000 series to airframes by laser welding is being studied.In addition, the Friction Stir Welding (FSW) method devel-oped in the UK as a new bonding technique is being usedfor a broadening range of applications. These researchtrends are outlined below.

1.2 Research trendsFigure 1 shows the history of strength improvement of

rolled materials for aircraft.1) Despite the improvementfrom the 2000 series to the 7000 series, even stronger mate-rials are needed to reduce aircraft weight. These alloydevelopment projects are mainly led by US aluminum alloymanufacturers. Since the greater strength of the 7000 seriesis offset by stress corrosion cracking, it is necessary to addmore Zn and other elements to suppress stress corrosioncracking.

Likewise, alloys having a good balance with fracturetoughness are being developed. As Figure 2 shows, newalloys offer both the fracture toughness of the 2000 seriesalloys and excellent proof stress of the 7000 series alloys.2)

Two methods are under research, one is to enhance thetoughness of the 7000 series at the sacrifice of strength, andthe other is to enhance the strength from the 2000 series byincreasing the solute.

For the past 10 years, NIMS has conducted atomistic-level research on the aging and precipitation phenomena,which are crucial for strengthening rolled aluminumalloys.3) The 6000 series is attracting attention as alloys for

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Yie

ld s

tren

gth

(MP

a)

Goal

Aluminum alloy application timing (year)

Fig. 1 History and goal of aluminum alloy development for aircraft.

Fig. 2 Trend of improvements in material characteristics of high-strength Al alloys.

08 Metals

Section 2. Nonferrous Alloys

Hiroshi Harada*, Toshiji Mukai**, Masuo Hagiwara*, Toshiyuki Hirano*,Youko Yamabe-Mitarai*, Satoshi Kishimoto*, Yoshihisa Tanaka*,

Akira Ishida*, Takahiro Sawaguchi**Materials Engineering Laboratory,NIMS

**Ecomaterials Center, NIMS

automotive body panels but the greatest obstacle to practi-cal application is the delay effect of artificial aging by nat-ural aging. To overcome this, the mechanism of the delayeffect has been researched by the 3D atom probe method,the positron annihilation method, and other nano-levelanalysis techniques.4) Based on these results, an importantguideline was created for the heat treatment design for the6000-series alloys. This guideline helped to clarify the age-hardening phenomenon in the mechanism of Mg-Ag addi-tion to Al-Cu-Mg-Ag alloy among the 2000-series materi-als now being used for aircraft5) and to clarify the atomcluster formation, and aging and precipitation of Weldalitealloys which are aeronautical materials having excellentweldability.6) This guideline is now used for alloy designthroughout the world.

NIMS statistically analyzed the alloy compositions andstrength characteristics of the 2000 series and 7000 series.Under the conditions of solution and aging processing (T6),for example, the relationship between alloy compositionand mechanical properties (yield stress, tensile strength,and elongation) was formulated as one equation for boththe 2000-series and 7000-series alloys.7) This equation willbe useful for optimizing alloy compositions.

Since grain refinement is effective for improving bothstrength and toughness, refining processes by liquidquenching and warm rolling have been researched inten-sively in the Supermetal Project and other projects.8) Thisresearch was succeeded by the Nanometal Project and isnow focusing on precipitation control to achieve strengthand ductility at the same time.9)

For the super-large Airbus 380 aircraft due to enter ser-vice in 2006, the 6000-series alloys which are weldable bylaser process were selected instead of the 2000- or 7000-series alloys which need to be riveted. The new process isfaster and is attracting much attention.10)

The Friction Stir Welding (FSW) method11) developedby The Welding Institute on the outskirts of Cambridge inthe UK is being used for an ever-broader range of applica-tions. Compared with the conventional MIG and othermelting methods, this method produces few bondingdefects, and so the method will be applied to vehicles andother fields. It may also be used for aircraft eventually, butstrict reliability evaluations and research on materialstrength are necessary.

1.3 Future outlookThe cost performance of CFRP and other competitive

composite alloys may enable aluminum alloys to be usedfor aircraft and other advanced transportation equipmentdue to the light weight and high specific strength of suchalloys. For the Boeing 787, a next-generation medium-sized civil aircraft now under development, for example,the target weight ratio of composite materials in the air-frame is set to 50% (25% for the Boeing 777). For alu-minum alloys to win the competition and be chosen foradvanced transportation equipment, it is important not onlyto improve the materials property and the processability,but also to make better use of the advantage of aluminumalloys in recycling.

References

1) H. Taira, Materials Science, 35, 220 (1998)2) T. Tsuzuki, Materia, 43, 396 (2004)3) K. Takarano, Metals, 73, 201 (2003)4) M. Murayama and K. Hono, Acta Mater., 47, 1359 (1999)5) L. Reich, M. Murayama and K. Hono, Acta Mater., 46, 6053 (1998)6) T. Honma, S. Yanagita, K. Hono, Y. Nagai and M. Hasegawa, Acta

Mater., 52, 1997 (2004)7) T. Yokokawa, N. Taira and H. Harada, Spring Convention of The

Japan Institute of Metals (2005) 434. (submitted)8) H. Sasaki, K. Kita, J. Nagahora and A. Inoue, Mater. Trans., 42,

1561 (2001)9) T. Sato, Materia., 43, 400 (2004)

10) http://www.airbusjapan.com/media/a380_technical.asp11) http://www.twi.co.uk/j32k/unprotected/band_1/tffricst.html

2. Magnesium alloys

2.1 IntroductionMagnesium has been used mainly for the bodies of

mobile electronic equipment because it is the lightest metalfor structures. To meet the demand for conserving energyand resources and reducing exhaust emissions and otherenvironmental loads, research has started on using magne-sium for automobiles and other moving devices, andindeed, magnesium is now being used for an increasingnumber of automotive parts. Magnesium production hasbeen increasing every year: in 2003, output reached about380,000 tons, up 8% over the previous year. Of the totaloutput, about 40% is used as structural materials, and thispercentage is still increasing every year. This section sum-marizes the recent research trends in magnesium based onthe results of searching an academic paper database (SCIExpanded).

2.2 Research trendsFigure 1 shows the transition in the number of papers on

magnesium worldwide and by major country.Papers are generally increasing although the rate of

increase varies among countries, with a particularly rapidincrease from 2000. There are more papers from Japan thanany other country, with a remarkable increase in 2003probably because it was the last year of national academic

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Tota

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aper

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ber of papers by country

Total number of papers

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Fig. 1 Number of papers in the past 10 years.

project, “Platform Science and Technology for AdvancedMagnesium Alloys”, selected as the priority area of Grant-in-Aid from the Ministry of Education, Science, Sports andCulture, Japan. The number of papers from China is nowgrowing remarkably and reached the top in 2004. This isprobably because the country is not only producing magne-sium metal but also keen to promote research and develop-ment under a national initiative.

Research is mainly focused on so-called cast alloys,including die cast ones, as shown in Figure 2. Since 2002,the ratio of wrought alloys, including rolled, extruded, andsevere-plastically deformed ones, has increasing rapidly.Researchers tend not to be devoted to the research anddevelopment of cast materials not only applicable to actualcasting but to future large members; key research themesare grain refinement, accompanying the increase ofresearch in rolled materials. As to alloy designs, a growingnumber of designs feature the addition of rare earth ele-ments which increase the heat resistance and strength. Thenumber of “nano-aware” research papers is also increasingdramatically. Nanostructured materials made by the addi-tion of rare earth elements is another recent research trend.

Regarding material characteristics, research is focusingon corrosion and corrosion protection as shown in Figure 3,followed by creep. Papers on fracture, bonding, and fatigue

are also increasing, as well as on formability and ductility.Hence, it would appear that materials research is shiftingtoward larger structures and higher safety in line with thegrowing research and development of rolled materials.

2.3 Future outlookFrom the transition in the number of papers, R&D on

magnesium is predicted to keep increasing globallybecause its application to large automotive members willhelp reduce weight. BMW’s announcement of a 6-cylinderengine block made of a magnesium alloy last year mayaccelerate the development of new alloys offering excellenthigh-temperature strength and creep resistance. Like twinroll casting which has been actively researched sincearound 2002, low cost sheet is also expected to be massproduced in future. As an increasing number of new alloysare designed with rare earth elements, R&D on nanostruc-ture analysis and control to optimize the dispersion mayalso increase.

3. Titanium alloys

3.1 Titanium industry within and outside Japan and infor-mation trends

In Japan, the shipment of titanium materials hasincreased steadily for the last 20 years, reaching 13,838tons in 2003 and predicted to reach 30,000 tons in 2009.The world’s shipment in 2003 was 60,601 tons, and soJapan accounted for about 24%. The United States shipped23,600 tons in 2003, about double that of Japan.

At the World Conference on Titanium held in Germanyin July 2003, Japan ranked second with 77 papers after thesponsor nation Germany (89). The United States (62)ranked third and China (51) ranked fourth, followed by theUK (44), France (34), Russia (18), and Korea (17).

3.2 Titanium research and development trendsFor about 10 years after the collapse of the bubble econ-

omy, various ways of reducing cost were studied, such asimproving the efficiency of the manufacturing process,manufacturing parts by powder metallurgy, and developingalloys composed of only low-cost elements such as Al andFe. At that time, new fields of application other than air-craft were sought, and new demand was exploited in con-struction materials, sporting goods, daily necessities, andaccessories. In these latter fields, commercial-grade puretitanium is mainly used.

Fortunately, in recent years in Japan, the situation hasbeen gradually turning more positive. Specifically, thereare some changes being seen which appear to favor a vastexpansion of the usage of titanium alloys. Namely, 1)Japan has plans to produce medium-sized aircrafts usingJapanese own technologies, 2) Adoption of Ti alloy parts incommercial cars (Toyota, VW), 3) Demand for biomedicalapplications due to the growing population of elderly peo-ples.

Under these circumstances, the Titanium Forum of TheIron and Steel Institute of Japan (chaired by M. Hagiwara,NIMS) attempted to identify the main current research

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Num

ber

of p

aper

s Num

ber of papers

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Fig. 2 Number of papers by material types and microstructures.

Num

ber

of p

aper

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Fig. 3 Number of papers by material characteristics.

trends, as well as ones required in future and promisingtrends, in the fields of refining and melting, machiningtechnology, property database, structural alloys, functionalalloys, and uses. Subjects concerning alloy developmentare as follows:

i) Alloy development (structural uses)(1) Titanium alloys having high strength and great

plastic deformation capability for aircraft(2) Heat-resistant titanium alloys having high strength

and toughness for next-generation aircraft engines(3) Titanium alloys having high strength and low elas-

tic modulus for biological uses and automotivesprings

(4) Titanium alloys having low-cost compositions forwelfare equipment and automotive connecting rods

ii) Alloy development (functional uses)(1) Shape memory titanium alloys for high tempera-

ture application (2) Shape memory titanium alloys for biomedical uses

The required characteristics in the new fields of structur-al and functional uses are satisfied by body centered cubic-type titanium alloys (bcc phase or B2 phase) which offersexcellent deformation performance.

3.3 Research by NIMSAs mentioned above, demand for titanium alloys will be

great for next-generation aircraft engines and substitutematerials for biological hard tissues. Since existing titani-um alloys cannot easily satisfy the required characteristicsin these new fields of application, new alloys must bedeveloped.

Therefore, NIMS is now developing new types of bodycentered cubic-type high-strength titanium alloys suitablefor aircraft engines and biomedical applications. For air-craft engines, NIMS focuses on the Ti2AlNb (O phase)-based alloy and its composite materials that shows excel-lent high temperature mechanical properties at 600˚C orhigher. For biomedical uses, NIMS is developing a titani-um alloy having high strength and low Young’s modulusfrom the nanostructured body centered cubic-type Ti-(Ta,Nb)-Cu-Ni-Si alloy by compositional modification,such as substituting harmful Ni with Fe, Co, or Cr.

3.4 Key research by other than NIMSToyota Central Laboratory developed a body centered

cubic-type Ti3(Ta+Nb+V)+(Zr,Hf,O) alloy (named “GumMetal”) showing far superior mechanical properties (highplastic deformation capability, low Young’s modulus, andsuperelasticity) than the conventional titanium alloys, andthe new alloy is expected to be used in other fields. Niino-mi and co-workers of Toyohashi University of Technologyare developing a new titanium alloy having low Young’smodulus and high strength for biomedical uses and pro-posed an alloy of the Ti-29Nb-13Ta-4.6Zr composition.Meanwhile, Ikeda and his group of Kansai University aredeveloping an alloy having low-cost composition for wel-fare equipment. In addition, there is much university-ledresearch on body centered cubic-type shape memory alloysand superelastic alloys.

4. Porous alloys

4.1 IntroductionPorous materials, which have many pores inside, are

used in various fields, such as biotechnology, fuel cells,catalysts, and gas adsorption. Though research field of onporous materials covers very wide fields such as inorganic,organic, and physiochemical fields, solid state physics, etc.,this paper reports on research on mult-functional light-weight porous materials.

4.2 Research trendsPorous materials can be roughly classified into metallic

porous materials, inorganic (ceramics) porous materials,organic porous materials, metallic complex materials,wooden materials and carbon materials. According to func-tion, the materials can be also classified into biomaterials,fuel cell electrodes, catalysts, gas adsorbents and sensorsusing them, solar battery materials, energy absorbing mate-rials, lightweight structural materials, etc. Regarding thestructural materials, solids containing small pores are calledporous materials, and the materials which have high porosi-ty that is actively used are called cellular structural materi-als. Recently, these cellular materials are attracting atten-tion because their uniform-size cells are arranged regularly.

According to the structure, structure materials, it is usingto fabricate lightweight structural materials. Lightweightcell structural materials can be divided into the open cellu-lar material that has no cell walls and the closed cellularmaterial in which each cell is surrounded by cell walls. Theopen-cellular materials include ceramics for filtering mate-rials and open cellular metals for shock absorbing materi-als. The closed cellular structural materials include foamedmetals, sintered hollow shollow spears and honeycombstructure materials. These materials are fabricated by gasfoaming, sintering hollow spears and regularly bondinggeometrically bent plates. These closed-cellular structuresare lightweight and have excellent shock-absorbing capa-bility. So, applications of these cellular materials for shock-absorbing structural materials of automobiles are beingdeveloped.

4.3 Future outlookBecause the safety of transportation equipment is so

important, cellular structural materials are expected to bedeveloped as strong and lightweight structural materials,shock absorbing and damping materials. Structural materi-als having multiple functions are also expected to be devel-oped. Other researches to produce new functional materialsand hybrid materials using cellular structural materials alsoneed to be developed.

4.4 ConclusionMetallic closed cellular materials which are one of

porous materials were introduced. These materials will belightweight structural materials having large shock absorb-ing and damping properties.

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References

1) L. J. Gibson and M. F. Ashby, Cellular Solids, Pergamon Press(1988)

2) Handbook of Cellular Materials, Hans-Peter Degischer andBrigittebKriszt, Wiley-VCH (2002)

5. Intermetallic compounds

5.1 Research trends within and outside JapanAfter several stages of research since 1950, full-scale

research on structural intermetallic compounds started inthe 1980s or later. Research and development are nowfocusing on the aluminide type (TiAl, Ni3Al, FeAl, etc.)and silicide type (Nb3Si, Mo5Si3, etc.) for application to air-craft, automotive engines, power generation turbines, andspace shuttles. This transition is clear from the reportsmade at the 11th MRS Convention in the autumn of 2004, aconvention which has been held every two years since1984.

Regarding TiAl which is lightweight and has excellentheat resistance, Japan, the US, and Europe competed withlarge projects in the 1990s. This fueled research and devel-opment on alloy composition, microstructures, characteris-tics, and manufacturing technology. In 1999, a unique pre-cision casting technology developed in Japan enabled TiAlto be used for turbochargers in actual automotive engineson the market for the first time in the world. The tur-bochargers have reached the production level and Europeanautomobiles are about to follow. The current issues are toenhance the heat resistance and durability for dieselengines. Automotive engine valves and low-pressure tur-bine rotor blades have also been fabricated experimentallyand verified by performance tests, but issues of reliabilityenhancement and cost reduction remain. Compared withthese cast materials, wrought materials are difficult to man-ufacture and expensive, and thus innovative compositions,microstructure control and machining technology are need-ed. Regarding Ni3Al and FeAl, research on the compositionand microstructure control and manufacturing process hasadvanced. In the United States, Ni3Al is now being used inheating element fixtures, high-temperature dices, andvalves for heat treat furnaces, while FeAl is being used inheating elements to some extent. Other materials wereproved to have heat resistance characteristics exceedingthose of Ni-base heat-resistant alloys; basic research isunderway and is expected to progress.

Since intermetallic compounds show peculiar propertiesoriginating from ordered structures, they have beenresearched as thermoelectric materials, catalytic and elec-trode materials, magnetic materials, shape memory materi-als, and superconductive materials. Many of them are inpractical use. These days, intermetallic compounds of Niand Pt are attracting attention and being researched as cat-alytic and electrode materials for fuel cells.

5.2 Current status of NIMS and research by NIMSFor Ni3Al, fabrication technologies of the cold-rolled

foils and honeycomb structures were developed for the first

time in the world and Ni3Al foils were found to have a cat-alytic effect for decomposing methanol and generatinghydrogen. To develop the foils as both a catalyst and astructural vessel, R&D is being promoted to clarify thecharacteristics and create a reformer and an exhaust gaspurifier for fuel cells.

5.3 Future outlookIntermetallic compounds started being used as practical

structural materials at the end of the 20th century, and theapplications and types of intermetallic compounds willexpand. Therefore, cost reduction is essential and techno-logical development is necessary for enhancing the ductili-ty and toughness, and improving and varying the manufac-turing technology.

These days, finely-distinguished characteristics of bothstructural and functional materials are requested, and inter-metallic compounds are expected to satisfy such requests.

While needs-oriented research and development areunderway, there are estimated to be thousands of inter-metallic compounds whose characteristics and functionsare unknown or not used. To use these compounds, basicand fundamental research will continue for seeds research.

6. Refractory alloys

6.1 Research trends within and outside JapanNi-base superalloys are high-temperature materials used

under severe conditions such as in jet and rocket engines.To raise the thermal efficiency of a gas turbine or aircraftengine, a high-temperature material that withstands temper-atures over the temperature capability (1500˚C) of Ni-basesuperalloy is expected. For this, refractory metals (Nb, Mo,etc) and platinum group metals (Ir, Ru, Rh, Pt, etc) havingmelting points of 2000˚C or higher are attracting attention.Researchers are very interested in materials beyond Ni-base superalloys. In 2003, US MRS introduced Pt-Al alloysand Mo and Nb silicides (Si compounds) in a feature“Ultrahigh-Temperature Materials for Jet Engine.1)” TMS,another materials society of the United States, held a sym-posium on the theme of “Beyond Ni-Based Superalloys” inMarch 2004 and published a special issue in an academicjournal in 2004.2) Not only Pt-Al alloys but also the poten-tial of platinum-group metal base alloys using Ir3Nb, RuAl,IrAl, and other platinum-group intermetallic compoundswere introduced in the special issue.

6.2 Current status of NIMS and research by NIMSNIMS is actively researching platinum-group metals. Of

the platinum-group metals, Ir has an especially high melt-ing point, and NIMS is developing Ir- base alloys for usearound 1950˚C. These alloys are expected to be applicablefor very severe aeronautical and space uses, such as theattitude control thrusters of satellites. In addition, PtTi,IrTi, and other intermetallic compounds based on platinum-group metals were found to have potential use as shapememory alloys at 1000˚C or higher. Since the conventionalshape memory alloy NiTi can be used only near room tem-perature, these intermetallic compounds could be used as

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new high-temperature shape memory alloys for gas tur-bines, high-temperature sensors, and actuators.

6.3 Future outlookThese ultrahigh-temperature structural materials are

used only under highly specific condition. However,despite demand, they are not being systematicallyresearched. Then, supply of the ultrahigh-temperaturematerials is insufficient. Such uses require not only ade-quate strength but also oxidization, resistance, corrosionresistance, manufacturability, and various other conditions.Therefore, materials development requires advanced tech-nologies. By clarifying the purposes of application and tar-geting research on them, these materials will start to beused for space and aeronautical applications.

References

1) J-C. Zhao and J. H. Westbrock, Mater. Res. Soc. Bull., 9, 622(2003)

2) D. A. Alven, JOM, 9, 27 (2004)

7. Shape memory alloys

7.1 Research trends within and outside JapanThe TiNi shape memory alloy discovered in the United

States in 1963 spawned many successful products, from thevalves of coffee makers to women’s underwear, thanks tothe production technology established in the 1980s and anew materials boom. In the 1990s, the application rangewas extended to the antennas of cellular materials and bio-materials, riding on the IT wave and high-grade medicaltechnology. With an overwhelming number of researchersand enterprises, Japan has been leading the world in bothbasic and applied research (see Figure 1). Research onshape memory alloys is an important part of domesticmaterials societies. Japan is also playing a leading role ininternational academic societies. In the United States, muchdevelopment is focused on medical applications, withstents used for the treatment of myocardial infarction hav-

ing a market of 3 billion dollars. Research is also beingstepped up in China.

In the field of shape memory alloys, continuous effortsare being made to extend the application range of alloys tomeet emerging needs. New applications for medical materi-als, smart materials, safe materials, MEMS materials, andhigh-temperature shape memory alloys are being studied.As more applications emerge, researchers have started todevelop new shape memory alloys to replace the TiNialloy, such as biologically harmless Ni-free shape memoryalloys, composite materials fusing the functions of differentkinds of materials, thin films made of shape memory alloysby the semiconductor process, iron-base shape memoryalloys that can be mass-produced at low cost, high-temper-ature shape memory alloys for turbines, and ferromagneticshape memory alloys having a quick response by magneticfields.

7.2 Current status of NIMS and research by NIMSNIMS has announced important research results on thin

films of shape memory alloys used for microactuators andiron-base shape memory alloys used for large members.

Thin films of shape memory alloys are expected to beused for as MEMS actuators of great force. The number ofpapers published was about 2 a year around 1990 whenNIMS embarked on research, but began to increase around1995. Now, nearly 50 papers are published a year and thenumber is still rising. The University of California andKarlsruhe are promoting the application of TiNi alloy tomicrodevices. Materials development, however, is led byNIMS which has a wealth of data on characteristics andunique evaluation techniques, as well as Tsukuba Universi-ty.

Meanwhile, the Fe-Mn-Si base alloy discovered in Japanin 1982 is about to be used as a low-cost material for bond-ing large pipes. NIMS recently succeeded in the develop-ment of an NbC-added Fe-Mn-Si base alloy not requiringtraining and is now promoting joint research with domesticand overseas research institutes and enterprises for applica-tion of the alloy to reinforcing bar bonding materials andconcrete reinforcing fibers. NIMS is also studying use ofthe alloy, which has damping properties, as a dampingmaterial.

7.3 Future outlookCompared with other materials, shape memory alloys

are comparatively new. The successful application of TiNialloy triggered new materials development for extendingthe application range of shape memory alloys. With thedevelopment of new industries for which there is greatsocial demand, such as nanotechnologies, biomaterials, andsafe materials, the development of materials and processingmethods is advancing. Shape memory alloys will thereforebe applied to more fields as intelligent materials havingmultiple sensor, actuator, damping, and superelasticityfunctions.

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Other

Other

51 569

9

14

14

16

6842

29

232019

15

13

1211

UK

China

Ukraine

France

Spain

Germany USA

Russia

Japan

Medicalmaterials

TiNi alloy

TiNi base

Febase

Cubase

Microactuators

Dampingmaterials

Compositematerials

Ferromagneticmaterials

Finland

Fig. 1 Number of participants at an international conference onmartensite transformation (ICOMAT ’02) by country (many fromFinland, the sponsor country) and number of reports at an internationalconference on the application of shape memory alloys (SMST ’01) bymaterial.

1. Thermal BarrierCoating

Thermal barrier coating (TBC) is an essential surfacetreatment for the blades and vanes of jet engines and tur-bines for thermal power generation. As Figure (a) shows,TBC produces a multilayer structure consisting of i) a basematerial made of Ni-base superalloy, ii) a metallic bondcoat layer enriched in Al, iii) a thermally grown oxide(TGO) layer formed by the surface oxidization of the bondcoat, and iv) a top coating layer of oxide ceramics with lowthermal conductivity (in general, yttria stabilized zirconia:YSZ).

To meet the recent demand for CO2 reduction, it isimportant to improve the thermal efficiencies of internalcombustion engines or to raise the operating temperatures.In various countries throughout the world, several researchprojects organized by industry, academia, and the govern-ment are in progress to enhance the TBC system for keep-ing the temperature of the substrate material hundreds ofdegrees lower than that of the combustion gas. The mainprojects are the HIPERCOAT Project,1) an internationaljoint program by the NSF in the US and the EC, andJapan’s Nanostructure Coating Project2) following the maintheme of NEDO’s Nanotechnology Program.

The key aspects of TBC technological innovation arehigh temperature operation and long life. Until recently,most researchers had been interested in the design of topcoat materials and the development of coating processes.As Figure (b) shows, however, the life of coated compo-nents greatly depends on i) the peeling of the top coat layeron the bond coat attributable to TGO and ii) the depositionof harmful phase in the substrate material attributable to themutual diffusion of alloying elements between the substratematerial and bond coat. In other words, the highest priorityfor attaining long life is to develop bond coat materialsoffering slow and stable growth of TGO and to suppressmicrostructural changes of the substrate material.Researchers are therefore shifting attention to the bondcoat.

Ahead of these global trends, NIMS has been conduct-ing research since 2000 to develop novel bond-coat alloysusing Ir as a base element, because Ir has low diffusivityinto Ni-base alloys with excellent resistance to high-tem-perature oxidization and corrosion.3-5) In FY2005, NIMSwas appointed as a collaborative institute for the Specially

Promoted Research project “Fabrication of diffusion-barri-er bond coating to realize long-life, high-reliability thermalbarrier coatings” subsidized by Grants-in-Aid for ScientificResearch. Thus, NIMS is attracting national and interna-tional attention for its achievements.

With a research group leading the world in the designand development of Ni-base superalloys, NIMS is the soleresearch institute in Japan that has the full research poten-tial necessary for developing TBC coating materials, suchas the capabilities of developing ceramic top coat materialsand processes. In future, closer linkage between researchersis expected to enable the development of unique turbineblades made entirely within Japan.

References

1) http://www.materials.ucsb.edu/TBC/index.php2) http://www.nedo.go.jp/nanoshitsu/project/pro06/index.htmlFFor

achievement reports by years, search NEDO’s achievement reportdatabase (http://www.tech.nedo.go.jp/Index.htm) with “nanocoat-ing”

3) P. Kuppusami and H. Murakami, Surf. and Coat. Technol., 186,377-388 (2004).

4) P. Kuppusami, H. Murakami and T. Ohnuma, J. Vac. Sci. Technol.,A22, 1208-1217 (2004).

5) H. Murakami, A. Suzuki, F. Wu, P, Kuppusami, H. Harada,Superalloys 2004, Eds. K. A. Green, T. M. Pollock, H. Harada, T.E. Howson, R. C. Reed, J. J. Schirra and S. Walston, TMS (2004),pp. 589-596.

2. Thermal Spraying

Thermal spraying is a surface coating process used toform coatings of 100 micron or thicker. This process canproduce coatings from various materials such as metals,

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Top coat

Bond coat

Substrate (Ni-base superalloy)

TGO growth→Peeling of top coating

Inter diffusion of alloying elements→Precipitation of harmful phase

Fig. (a) Thermal barrier coating and (b) deterioration mechanism.

08 Metals

Section 3. Protective Coating for Severe Environments

Seiji Kuroda, Hideyuki MurakamiThermal Spray Group, Materials Engineering Laboratory, NIMS

149


ceramics, composite materials, and plastics. The process isindustrially very attractive for high-speed large-area coat-ing and field work, and can be classified into various typesby the heat source (combustion flame or electric energy)and the form of raw materials (powder or wire). In the1910s, wire arc spraying and flame spraying were devel-oped and mainly applied to metal spraying. In the 1960s,plasma spraying was put to practical use for coating ceram-ics of high melting points. Low-pressure plasma sprayingdeveloped in the 1970s enabled the formation of a verydense, less oxidized metallic coating. This process becamewidely used for turbine engines and other high-tech fields.High velocity oxy-fuel (HVOF) spraying was developed inthe 1980s. At 500 m/s or higher spray particle speed, thisprocess can stack unmolten spray materials on a substrateby kinetic energy. In particular, the process can form densecoatings of carbide-type cermet materials while suppress-ing decarbonization. Cold spraying and aerosol depositionwere recently developed as other processes using kineticenergy, and are carried out almost at room temperature.The former mainly forms a coating from a metallic powderin the atmosphere while the latter feeds submicron ceram-ics particles into a decompressed chamber and forms acoating by a high-speed impact.

The Thermal Spray Group of NIMS has developed cor-rosion-resistant dense metallic coatings by optimizing thespray particle speed and temperature of the HVOF process,and verified them by demonstration tests in a coastal envi-ronment and the like. These days, it has become possible toform dense coatings of titanium and other materials that areotherwise difficult to make dense in the air atmosphere.NIMS is carrying out basic research on the mechanism ofspray coating adhesion and a method of evaluating it, andthe result is attracting international attention.

The trend toward high speed and low temperature willcontinue in process development because the process canmaintain the microtissues of raw materials and powerfullyform coatings from materials having nanostructures.Regarding nano-structured spray coatings, interestingreports have been published on the enhancement of wearresistance and adhesiveness. For industrial use, the applica-tion of spray coatings to automotive engine blocks is ofparticular interest. Automotive manufacturers worldwideare discussing the replacement of cast-iron cylinder linerswith iron-type sprayed coatings and a manufacturer inEurope has established a production line. This technologyenables weight reduction and greater cooling efficiency byreducing the lining thickness drastically, but the problem ofcontrolling the quality of the coating remains. To solvethis, nondestructive coating inspection is important and amethod using thermography is attracting attention.

As the environment of materials use becomes harsheryear by year, thermal spraying is becoming more recog-nized as an important technology that offers many choicesfor adding environmental performance to the surfaces ofmaterials. Since clarification of the basic phenomena inthese processes has been delayed somewhat, research anddevelopment in advanced countries are often driven byresearch institutes and university laboratories.

References

1) J. Akedo, Surface Science 25, 25 (2004).2) J. Kawakita, S. Kuroda, T. Fukushima and T. Kodama, Sci.

Technol. Adv. Mater., 4, 281 (2003).3) M. Gell, E. H. Jordan, Y. H. Sohn, D. Goberman, L. Shaw and T.

D. Xiao, Surface and Coatings Technol., 146 –147, 48 (2001).

1. Introduction

Upon making bonds with each other, carbon atoms gainvarious structures and become materials having variousproperties. The most typical ones are diamond monocrys-tals consisting of carbon atoms arranged regularly by sp3

bonds and graphite monocrystals arranged regularly by sp2

bonds. Among the many carbon materials, the most famousones recently found are fullerene and nanotube. These haveremarkably extended the world of carbon materials, whichcan be classified by the style of bonds, size, and form asfollows:Diamond type: Monocrystal or polycrystal sintered com-pact, thin film, and nanodiamond. Nanodiamond is ananoparticle of tens of nanometers, which is a form of thinfilm when produced by vapor phase processes or is in dis-persion when produced by the explosion process. Graphite type: Monocrystal, polycrystal, thin film, particu-late, porous form, fiber, nanotube, nanofiber, and fullerene.The graphite-type carbon materials are of sp2 bonds butvary widely from amorphous to highly crystalline ones interms of X-ray diffraction.Between diamond and graphite is diamond-like carbon(DLC). This is an amorphous thin-film material mixed withsp2 bonds and sp3 bonds.

Regarding nanotechnologies now popular, not onlynano-size carbon units but also nano-size voids in porouscarbon are attracting attention.

Modifications with other atoms are also possible. Dia-mond can be doped with impurities and there are also car-bon materials having surfaces modified with hydrogen orother different molecules. Graphite can be intercalated withother atoms or molecules between layers.

Some boron nitrides produced by replacing carbon withboron and nitrogen atoms have structures and forms similarto those of the above carbon materials, and so they mayhave similar characteristics and functions. Here, the boronnitrides are also partly introduced.

These carbon materials of various structures also have awide variety of properties. This section summarizes therecent research trends by properties.

Data on recent research trends was collected from acade-mic journals, particularly the two international academicjournals specializing in carbon materials: “Diamond Relat-

ed Materials” and “Carbon” (both published by Elsevier).In 2004, these journals carried about 300 and 500 papers,respectively. The domestic academic journals “Tanso (Car-bon)” and “NEW DIAMOND” were also referenced.Research achievements may also be reported in magazinesand at academic meetings in the fields of physics, chem-istry, and biology but such areas were not checked.

2. Research trends

2.1 Mechanical propertiesThe most widely-known characteristic of diamond is

that it has the highest hardness of any material. Thanks tothis hardness, diamond is widely used for machining toolsand abrasives. Graphite is also useful as a structural materi-al. As a composite, carbon fiber is widely used for golfclubs, fishing rods, and aircraft. In these fields, carbon fiberis now at the stage of industrialization.

With the emergence of new carbon materials, newresearch on mechanical characteristics has started. Theresearch activities include the synthesis of thin films fromdiamond, DLC, and other amorphous carbon materials byusing plasma technology and also the evaluation of theircharacteristics. The objectives of these activities are toapply the materials to micro electro mechanical systems(MEMS), protective films of magnetic disks and artificialjoints, and bearings and seals for oil-free machines.Research is focused on high hardness, great abrasion resis-tance, and low friction.

The high tensile strength and other mechanical charac-teristics of carbon nanotube are also interesting in the fieldof nanotechnologies.

2.2 Electrical and optical propertiesDiamond is a wide-gap semiconductor having a band-

gap of 5.5 eV; it shows the highest thermal conductivityand excellent light transmittance over a wide range ofwavelength. Active research is underway in expectation ofproducing new electronic devices based on these character-istics. Diamond has the potential to be used for high-fre-quency high-power transistors, ultraviolet light emittersand detectors, thermistors, particle detectors, electron emit-ters, optical windows, X-ray windows, and X-ray mono-

150


Chapter 9. Ceramic Materials

Section 1. Non-oxides - Carbon

Hisao KandaSuper Diamond Group, Advanced Materials Laboratory, NIMS

chromators for synchrotron radiation. Research is currentlyfocused on electron emitting devices. Japan is conducting anational project “Advanced Diamond Device Project”(NEDO: 2003 - 2005) with the goal of developing electronemitting devices. Carbon nanotube, nanodiamond, andDLC are also being studied as electron emitting devices.

To use diamond as a semiconductor, it is essential toproduce p-type and n-type characteristics. This has beendone by doping with boron and phosphorus, respectively,although the characteristics are not yet satisfactory forpractical purposes. Mainly in Japan and Europe, basicresearch on electrical conductivity and mobility is beingcontinued in terms of synthesis and characterization.

Research papers clearly oriented toward specific elec-tronic materials deal with not only electron emittingdevices but also high-frequency transistors, ultraviolet lightemitting devices, ultraviolet light detection devices, andparticle detection devices.

Many papers on graphitic carbon are related to elec-trodes, dealing with negative electrode materials for lithiumbatteries, electrodes for fuel cells, and electrical double-layer capacitors. For these uses, the small pore size andlarge specific area of carbon are important characteristics,in the same way that the characteristics of activated carbonhave long been used. In relation to recent nanotechnolo-gies, research on energy conservation and environmentalproblems has been very active.

Diamond is also useful for electrochemical electrodesbecause it has chemical inertness and wide potential win-dow. Boron-doped semiconducting diamond is now beingapplied to electrodes to decompose waste water. Selectivedetection is now possible for bio-related substances, suchas various molecules (dopamine, uric acid, etc.) containedin body fluid.

2.3 Magnetic propertiesAccording to a paper published several years ago,

pyrolytic graphite and polymerized fullerene show ferro-magnetism. It is interesting to note that magnetic bodies arecomposed of nonmagnetic atoms. However, some ques-tions must be solved to verify the paper, and it was reportedlast year that proton irradiation of carbon produces magnet-ism. This proves that the magnetism of carbon is not attrib-utable to contamination with a magnetic substance.

2.4 Chemical propertiesAs a chemical application of graphite-type carbon, acti-

vated carbon which has long been used as a deodorant iswell known. Graphite-type carbon, however, is still beingresearched intensively for application to many fields relat-ed to nanotechnology by utilizing the characteristics of car-bon, large specific area and small pore size.

Many studies are in progress to purify water and sup-press bacteria generation in water with various kinds ofactivated carbon and to immobilize marine organisms withcarbon fibers. Affinity with blood, such as cohesivenessbetween the DLC surface and blood platelets, is also beingresearched. By nickel or another metal supported on car-bon, hydrogen-added reaction (e.g. reaction from butene tobutane) and other catalytic effects are also being examined.

This may lead to the development of fuel cell electrodes.Technologies for removing NOx and other environmentalcontaminants have also been reported.

Diamond is chemically stable but known to form a p-type semiconducting layer once hydrogen is adsorbed onthe surface. By using this conductive layer, field-effecttransistors (FET) and DNA detectors are being researched.If reduced to nano-size, diamond seems to display specialreactions and has even been reported to acquire the abilityto kill cancer cells.

Although not chemical properties, fine pores may enablecarbon to be used as a molecular sieve to separate hydrogenand carbon monoxide or other substances. The DLC coat-ing of a PET container is also known to suppress gas per-meation.

2.5 JewelryAlthough jewelry may not be directly related to science,

research on diamond is also attracting attention in theworld of jewelry. As jewelry, natural diamond is treasuredbut synthetic diamond has begun to enter the jewelry mar-ket. Jewelry-level synthetic diamond can now be producedfrom gas phase using a chemical vapor deposition (CVD)technique as well as under high pressure, and the CVD syn-thetic diamond is now about to be sold as jewelry. A tech-nology has also been developed to enhance the quality ofbrown low-quality natural diamond by high temperatureand pressure treatment. However, the emergence of thesesynthesizing and processing technologies produces theproblem of how to distinguish natural diamond valuable asjewelry from artificial diamond. A new discriminationtechnology is expected to be established, and research onthe characterization of diamond for raising the level of dis-crimination is underway.

2.6 Thermal propertiesDiamond has the highest thermal conductivity. By using

this characteristic, diamond can be used for heat spreadingboards for laser diodes and other electronics devices. Onthe contrary, a carbon fiber aggregate shows great thermalinsulation and also very high heat resistance. As a heat-insulating material, the carbon fiber composite is applied tothe heat-insulating members of rocket engines. Thus, thethermal characteristics are another excellent advantage ofcarbon but no papers on its thermal characteristics werefound.

2.7 Vibration propertiesDiamond conveys sound at the highest speed, and so has

been applied to thin-film speakers and surface acousticwave devices. However, there have been few researchpapers on this aspect.

2.8 Topics in 2004Last year, the journal “Nature” reported rather unexpect-

ed noteworthy discoveries.One is the superconductivity of diamond. Diamond con-

taining boron has long been known to show electrical con-ductivity. However, the doping of boron as high as 2% wasfound to synthesize superconducting diamond. First, a

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152


Russian research group discovered this phenomenon withhigh-pressure synthetic diamond. The phenomenon wasthen confirmed with CVD diamond in a joint study byNIMS and Waseda University. Although the critical tem-perature is about 10 K, this is interesting because it is dia-mond, which may be in another category of superconduc-tors.

The other is 215-nm deep-ultraviolet laser oscillationfrom hexagonal boron nitride (hBN), which was achievedby NIMS. Ultraviolet light emission of GaN is well knownbut the wavelength of the deep-ultraviolet laser of hBN ismuch shorter. hBN has long been known but never beenconsidered as an electronic material. NIMS successfullysynthesized monocrystals of high purity and crystallinityby using a special solvent, resulting in its success.

3. Conclusion

As outlined above, carbon has a wide range of applica-tions as mechanical and structural materials, electronicmaterials, and chemical materials. Recently, however, car-bon is actively being researched for application to the fieldsof bio and environment from the viewpoint of nanotechnol-ogy, and such research looks set to continue.

Carbon materials for new fields are also expected to bedeveloped. It was only one year ago that the superconduc-tivity of diamond was discovered unexpectedly. The mag-netism of carbon is another interesting subject worthresearching in detail.


Carbides, nitrides, and borides are not produced natural-ly with some exceptions, so powders are synthesized frommetals or oxides and sintered into materials. The mainmaterials are silicon carbide (SiC), silicon nitride (Si3N4)and sialon (Si3N4-AlN-Al2O3 solid solution), aluminumnitride (AlN), boron nitride (BN), boron carbide (B4C), andzirconium boride (ZrB2) and other metallic borides.Because of their excellent heat resistance, strength, elastici-ty and hardness (wear resistance), corrosion resistance, andthermal conductivity, these materials are used for refractoryand structural (engineering) ceramics.

SiC polycrystal materials were developed in the UKaround 1970 as substitute materials for metals in internalcombustion engines to raise the yield temperature andenhance the energy efficiency. This was a pioneeringapproach. Regarding materials development, an SiC pow-der sintering process was developed in the United States in1975 and the Si3N4 sintering process in Japan in 1975 to1977. In 1976, nitride ceramics were developed in the UKand in Japan. These findings had a great impact on scienceand technology and established non-oxide ceramics asmaterials.

With this background, global policies for conservingenergy led to national projects being started in the US,Europe, and Japan. First in the United States, the CeramicApplication in Gas Turbine Engine (CATE) Project (1970-1980) was started and the Department of Energy (DOE)and the Detroit Diesel Allison (DDA) of GM researchedceramics for gas turbines of buses and trucks. This wassucceeded by the Advanced Gas Turbine Project (1979-1987) and then the ATTAP Project (1987-1992). Both pro-jects were carried out by DOE, GM, and Garret Ford.Automotive gas turbine components were developed inWest Germany (1974-1982, by BMFT Ministry ofResearch and Technology, VW, DM, and MTU), the pro-jects for ceramic gas turbines in the UK (1985-1989, byRR), and for ceramic gas turbines aircraft and vehicles inFrance (1985-1989, by ONERA), and the KTT project inSweden (by United Turbine and Volvo).1)

Internal combustion engines made of ceramics becametechnically possible but were not implemented due toissues concerning economy and reliability, since whenR&D on structural ceramics has not been active. In the

United States, however, work on developing aeronautic andspace ceramic materials became very active. Key materialsare Ceramic Matrix Ceramic Fiber Reinforced Materials(CMC) which are composites of carbon (C) fiber reinforcedcarbon matrix and SiC fiber reinforced SiC(Si3N4) matrix.The former is already used for the heat insulation on thespace shuttle. Raw materials in these ceramic products aremostly supplied from Japan. Japan is taking the lead inmanufacturing and the United States in evaluation and uti-lization.

2. Domestic trends

Regarding non-oxide engineering ceramics, the Ministryof International Trade and Industry (MITI) conductedresearch on fine ceramics under the basic technology forfuture industry (1981-1992). Mainly for Si3N4 and SiC,work has focused on developing advanced basic technolo-gies for raw-material powder synthesis, powder processing,and sintering and component creation to raise the efficiencyof internal combustion engines. This boosted the ceramicsmanufacturing technologies of Japan remarkably. MITIthen initiated the Synergy Ceramics Project (1994-2003) todevelop new ceramics by fusing various characteristics andfunctions and started materials development by usingsophisticated nano-micro structure control technologies.This resulted in the development of new Si3N4 and SiC(including oxides) materials featuring high strength, tough-ness, elasticity, thermal shielding, and grinding resistanceand also high (low) thermal conductivity, enabling the nextgeneration of materials to be developed. The concept ofnanoceramics was proposed to strengthen ceramics by dis-persing nanoparticles.

The developed process technologies were inherited bythe Ceramics Gas Turbine Technology Development(CGT) Project of NEDO of MITI (1998-1999) and pro-duced a practical ceramic gas turbine for 300-kW classcogenerators. Eventually, the target thermal efficiency of42% (the world’s highest) could be achieved. For high-temperature regions, Si3N4 ceramics having high strengthand toughness was used.2,3)

Supported by various projects, Japan’s fine ceramicsindustry gained international competitiveness, and current-ly about 70% of the world’s ceramic parts are estimated to

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09 Ceramic Materials

Section 1. Non-oxides -Carbides, Nitrides, and Borides

Hidehiko TanakaNon-oxide ceramics Group, Advanced Materials Laboratory, NIMS

come from Japan. Aluminum nitride (AlN), a material ofhigh thermal conductivity, was developed by enhancedtechnologies of synthesizing and sintering a high-puritypowder, and they were applied to heat sinks for powerdevices. B4C has been used for abrasives. Since the normal-pressure sintering process was developed, B4C is nowattracting attention as a lightweight and very hard material.Other metallic borides and nitrides (TiC, WC, TiN, TiB2,and ZrB2) and their composites (B4C-TiB2, TiB2-CoB6, andTiB2-W2B5) have been well researched as materials havinghigh melting points and great hardness.

Figure 1 shows the market trends in fine ceramics. InJapan, “fine ceramics” means refined functional and struc-tural ceramics. Carbides, nitrides, and borides hold impor-tant positions among fine ceramics.


As the main demand for non-oxide engineering ceramicsin Japanese industry is for precision equipment, semicon-ductor-related equipment, environment and energy, andoptoelectronics, NIMS has been proceeding with materialsdevelopment accordingly.

For application to semiconductor-related equipment,carbides require an easy densification process for obtaininglarge ceramics and cost reduction. Therefore, NIMS devel-

oped a low-cost easy sintering process for SiC ceramics.The Al-B-C phase relation was clarified and the high-tem-perature liquid phase Al8B4C7 was identified. By using thisphase as a sintering additive, NIMS developed a technolo-gy for complete densification at a temperature 200 to250˚C lower than before. Materials having high specificelasticity, specific strength, and resistance applicable tosemiconductor-related equipment will be supplied forwafer tables (Fig. 2, upper). By using high-purity organicmatter as the starting raw materials, an SiC powder ofultrahigh purity was developed through sol-gel precursorsynthesis and organic-inorganic conversion. The powderprovides materials for high-purity reaction furnaces essen-tial in the semiconductor industry. Meanwhile, the effect ofmaterial transportation activated by phase transition andmetallic solution was discovered and applied to graingrowth in manufacturing a porous SiC material, which canbe used for catalytic carriers for environmental purification.

Regarding nitrides, a Lu2O3 added Si3N4 ceramic whichsuffers no loss of strength at 1400 to 1500˚C was manufac-tured for gas turbines in the New Century Heat-resistantMaterials Project. We should also note the discovery of anew sialon phosphor. Sialon easily dissolves other metallicelements. By dissolving optically active rare earth ions insialon, blue, green, yellow, and red phosphor can beobtained (Fig. 2, lower). White LEDs were successfullyproduced by combining the yellow phosphor with the blueLED, and so application to white backlighting is greatlyexpected. The sialon phosphor, which are thermally stable,are also promising for next-generation plasma displays.

Boron nitrides (BN) were mentioned in the section on“Carbons.” Recently, a new material having excellent elec-tron emission performance was found by laser plasmaCVD. CVD under laser emission grew a new needle-like

154


Sin

terin

g te

mpe

ratu

re (

˚C)

Sinteringdensity

AlB2 added amount (mass %, 2%C was added.)

Eu2+ solid-solution sialon

Str

engt

h

Excitation Illumination

Wavelength

Fig. 2 Recent major achievements by NIMS.Upper: Low-temperature SiC sintering process.Lower: Sialon phosphor.

Fine ceramics production(including functional ceramics)

Sal

es (

100

mill

ion

yen)

Year

Market scale by structural material(Total: 116.5 billion yen in 2003)

Alumina

ZirconiaSiliconnitride

Siliconcarbide

Aluminumnitride

Other

Shipment by structural materials(Total: 23 billion yen in 2004)

Catalyticcarriers

Heat-resistantmaterials

Tools

Wear-resistant andcorrosion-resistant materials

Diamondtools

BN toolsOther

Fig. 1 Fine ceramics market trends (Source: References4,5)).

155


material, 5H-BN. The electron emission characteristic wasfound to be 1,000 times or greater than that of nanotube.This material can be applied to RGB displays and DVDrecording devices in combination with phosphor.

The development of single-crystal metallic borides aselectron emission materials was started by the NationalInstitute for Research in Inorganic Materials (present:Advanced Materials Laboratory of NIMS) a long time ago.Recently, NIMS succeeded in synthesizing high-qualitysingle-crystal ZrB2. Since the coefficient of thermal expan-sion is compatible, ZrB2 was found to be the substrate ofGaN-LED. All of the above materials were developed byNIMS and have huge potential markets as electronic andoptical materials.

4. Key research by organizations other than NIMS andfuture outlook

SiC porous honeycomb materials are now used fordiesel engine particle filters (DPF). In Europe, diesel vehi-cles are becoming popular as privately-owned cars, but reg-ulations on graphite particulates are being tightenedaccordingly. The particulates are removed by filtering andburning with SiC porous honeycomb filter already mountedin automobiles. The materials will also have to complywith tougher exhaust gas regulations but demand for themwill grow.

Single-crystal SiC is now undergoing rapid developmentfor semiconductor power devices. Since SiC is a semicon-ductor having a wide band gap, single-crystal SiC can beused for power devices of high frequencies and withstand-ing voltages and large currents. The material can be applied

widely from power generators to automobiles and motorinverters. Since there are still cost and quality problems tobe solved, single-crystal SiC has not yet entered practicaluse but is still an important material as a partial substitutefor Si semiconductor.6)

Sm-Fe-N, Fe-N magnetic substance, and (In)GaN semi-conductor, and other nitride electronic materials arepromising. The use of GaN blue LEDs is growing quick-ly.7) In addition, boride MgB2 superconducting material isattracting attention. Intensive research is now in progresson both materials toward practical use.

The trends in carbide, nitride, and boride ceramics willdepend on peripheral materials for semiconductor manufac-turing, environmental materials, and optical and electronicmaterials.

References

1) Research and development of basic technology for future industry,“Report on the Development of Elemental Technologies forPetroleum Gasifying Ceramics Turbine and Composite FineCeramics Technology”, Shinko Research Co. (2000).

2) Joint research consortium of synergy ceramics, “Synergy CeramicsII,” Gihodo Publishing Co. (2004).

3) NEDO (New Energy and Industrial Technology DevelopmentOrganization), “300kW Class Ceramic Gas Turbine ResearchResults”, (1999).

4) Ceramics Japan, Bull. Ceram, Soc. Japan, 39, 706 (2004).5) FC Report, 23, 44 (2004).6) High-temperature Ceramic Materials 124th Committee of Japan

Society for the Promotion of Science: H. Suzuki, T. Izeki, H.Tanaka, “New Materials of SiC Ceramics”, Uchida Rokakuho Co.(2001).

7) TIC Editing Department, “Nitride Ceramics for New Age”, TICCo., 465 (2001).

1. Introduction

The materials listed in the title are typical fine ceramicsthat are widely used for various machines, chemical plants,that energy equipment such as generators and enginesthanks to their heat resistance, corrosion resistance, highhardness and strength. These materials may thus be regard-ed as “matured” materials. These oxides, however, are stillexpected to have many potential functions that may beexploited through controlling the geometry, size, distribu-tion, localized structures and chemistry of grain bound-aries, inter- and intra-grain particles and pores. To clarifyresearch trends quantitatively, the titles, abstracts and key-words of papers published between 1991 and 2004 weresearched in an academic paper database (SCI Expanded).Of about 45,000 papers concerned with alumina, zirconiaand/or magnesia, 95% or more were written in English.Examination of the searched papers revealed the followingresearch trends on these materials.

2. Research trendsFigure 1 shows the annual number of papers on alumina

(Al2O3), zirconia (ZrO2), and/or magnesia (MgO). Thenumber of papers increases every year, indicating that thesematerials are potential research subjects. In 2004, the totalnumber of papers on the materials became more than dou-ble the number in 1991. Most papers concern Al2O3 thathas often been regarded as the most matured material. Theratio of total paper number is about 68, 29 and 3 for Al2O3,ZrO2 and MgO, and this ratio almost holds true everysearched year.

Figure 2 shows the annual number of papers on typicalresearch subjects for Al2O3, ZrO2, and MgO (black line inFigure 1). Although the data do not distinguish these mate-rials, the ratio of the paper number was similar to that notedabove. The main subjects are catalysts (catalytic functionsand carriers), syntheses (powder processing, molding, andsintering), composite materials (fabrication techniques andproperties), coating (techniques and characteristics), energy(fuel cells and nuclear power plants) and biomaterials (syn-theses and characteristics).

Figure 3 shows the annual number of papers publishedfrom some selected countries. Papers from the US, Europe

156


um

ber

of

pap

ers

(To

tal)

Total

Alumina

Zirconia

Magnesia

Year

Fig. 1 Annual change in the number of papers on alumina, magnesia,zirconia, and magnesia.

Nu

mb

er o

f p

aper

s (T

ota

l)

Catalyst

Synthesis

Compositematerials

Coating

EnergiesOrganisms and bio

Year

Fig. 2 Change in research themes on alumina, zirconia, and magnesia.


Section 2. Oxides - Alumina, Zirconia, and Magnesia

Keijiro HiragaFine Grained Refractory Materials Group, Materials Engineering Laboratory, NIMS

Noriko SaitoElectroceramics Group, Advanced Materials Laboratory, NIMS

1 (Germany, France and the UK) and Japan account for themajority. The total paper number for other EU countries(noted as Europe 2 for Italy, Spain, Austria, Holland, Swe-den, etc.) is about 50% of the number of Japan. Papersfrom Russia (including Ukraine) gradually increases, butthe total number is about one-fifth the number of the Unit-ed States. Since 2000, the paper number of the US, Japan,and Europe tended to saturate, whereas the paper numberof China increased quickly, and caught up with the numberof the United States in 2004. A rapid increase from 2000also appears in Korea.

Of the 45,000 searched papers, about 10% (4,480) ofpapers relate to the nanostructure area that includes rawmaterials, syntheses, characterization and properties. Thefraction of this area increased quickly from 1% in 1991 toabout 10% in 2000 and to about 20% in 2004, indicating ashift to nanostructure-oriented subjects. As shown in Figure4, this tendency appears commonly in all countries exam-ined. In China and Korea, the papers of this area have alsoincreased drastically since 2000, and the paper number ofChina exceeded the number of the US, Europe 1 or Japan.

Figure 5 shows the annual change in typical topicsappearing in the 4,480 papers relating to the nanostructurearea. Most papers focus on the structural characterization

and property evaluation of nanocomposites, porous materi-als and multilayered or oriented materials and on the syn-thesizing processes (powder synthesis, molding and sinter-ing) of these materials. The number of papers in this field isincreasing every year and this tendency has strengthenedparticularly since 2000 for composites, porous materialsand synthesizing processes. As shown in Figure 6, thenumber of papers published from Europe (the sum ofEurope 1 and Europe 2) is the greatest, and the number ofthe United States and Japan follows the former. As shownin Figures 3 and 4, papers from China and Korea increasedquickly since around 2000 and reached a level similar tothe United States and Japan in 2004.

Figure 7 shows the annual number of papers concernedwith basic research on the nanostructure area. Main sub-jects are the experimental analysis of nanostructures, theo-retical evaluations of stable atomic sites and chemicalbonding using molecular dynamics and molecular orbitalcalculations, and the relationships between nanostructuresand electric, magnetic, thermal and mechanical properties.Although the number of papers is less than one-third of thenumber given in Figure 5, the annually increasing numbersuggests strongly that research in this field is essential forexploiting new functions. Figure 8 shows the annual num-

157


Nu

mb

er o

f p

aper

s (T

ota

l)

Nu

mb

er of p

apers (B

y cou

ntry)

Total Europe 1

USA

Japan China

Europe 2Korea

Russia

Year

Fig. 3 Number of papers on alumina, zirconia, and magnesia by country.

Nu

mb

er o

f p

aper

s (T

ota

l)

Nu

mb

er of p

apers (by co

un

try)ChinaNano area (Total)

USAEurope 1

JapanEurope 2

Korea

Russia

Year

Fig. 4 Number of papers in the nano area by country.

Nu

mb

er o

f p

aper

s

Nano area Compositematerials

Synthesesprocesses

Porousmaterials

Multilayer andorientation

Year

Fig. 5 Number of papers on typical research themes in the nano-area.

Nu

mb

er o

f p

aper

s

Nano area (By country)

Europe

China

USA

Japan

Korea

Russia

Year

Fig. 6 Number of research activities in the nano-area by country.

ber of papers relating to research in an incubation stage.The subjects concern multifunctions, namely the combina-tion of such properties as electric conductivity, elasticity,thermal expansion and strength. The subjects also concernmultilayered or oriented structures and superelasticity.Europe, the US and Japan have been ahead of the researchfields shown in Figures 7 and 8: these countries have pub-lished 90% or more of the papers.

In materials relating to Al2O3, ZrO2 or MgO, new func-tions or multifunctions associated with nanostructures havemainly been discovered and developed in Europe, the USand Japan. A typical example of such research in Japan isCuAlO2: the first success in developing a p-type semicon-ductor in transparent oxides.1) This is based on the discov-ery that 12CaO•7Al2O3 (C12A7) has a nanobasket structurethat can include various ions.2) For requirements for multi-functions, typical examples are found in the developmentof a transparent MgO film for plasma display electrodes(requiring translucency, insulation, and durability underdischarge phenomenon) and a transparent Mg2SiO4 sub-strate for microwave (requiring high Q value and lowdielectric constant). Another example is transparent YAGpolycrystals synthesized by using rare-earth elements,3) thetransparency of which enables the polycrystals to be usedfor high-energy lasers and arc tubes.

3. Future outlook and research by NIMS

The searched results described above indicate the impor-tance of designing and controlling the nanometer-sizedstructures of grains, grain boundaries, inter- and intra-grainphases and pores for exploiting new functions and multi-functions in Al2O3, ZrO2, MgO and related complex oxides.This tendency should become stronger in the near future.We should also note that countries achieving success in thisresearch field have simultaneously conducting the basicresearch shown in Figure 7: analysis, characterization andtheoretical calculations of nanometer-sized structures andchemistry, structure–property relationships and new syn-thesizing techniques. This situation indicates that the devel-opment of new functions and basic research are linked and

proceed together.Under such circumstances, NIMS has developed new

functional materials and synthesizing techniques: the syn-thesis of MgO, YAG, Y2O3, ZnO, TiO2,

4) Mg2SiO4, CaZrO3

and other microparticles from water solutions, a newprocess using pulse-modulated RF thermal plasma genera-tion, the synthesis of TiO2 nanoparticles by controlling thesaturation of gas phases,5) the synthesis of highly orientedoxide thin films using symmetric control of a plasma-mag-netic field, colloidal processing that can control the crystalorientation and lamination using an external field6) and thesynthesis and modification of nanometer-sized porousstructures using anode oxidization.7) With the support ofthe synthesizing techniques and the analysis of nanometer-sized structures, NIMS has also synthesized transparentpolycrystals of Mg2SiO4, YAG3), Y2O3,

8) and MgO, sub-stantially superplastic alumina and apatite and high-strain-rate superplastic composites.9) In the next half decade,NIMS will extend the fundamentals relating to theseresearch fields and will develop new processing techniquesand multifunctional materials using electric and magneticfields, thermal plasma, anode oxidation, molecular mixingand superplasticity.

4. Conclusion

Al2O3, ZrO2, and MgO and related complex oxides haveextensively been studied in the last decade, since theseoxides have been expected to possess many potential func-tions. To exploit new functions and optimize the combina-tions of the functions, further research is necessary on thecontrol of nanostructures, theoretical calculations ofnanometer-sized local structures and chemistry and thenanostructure-property relationships. The US, Europe andJapan have been ahead of this research field and are expect-ed to lead the research. NIMS will extend the ability foranalyzing and controlling nanometer-sized local structuresand chemistry in order to develop new functional materialsfor the next generation.

158


Nu

mb

er o

f p

aper

sNanostructure

Structure andstrength, fracture

Structure analysis andcalculation

Structure andphysical characteristics

Year

Fig. 7 Annual change in the number of fundamental papers in thenanostructure area.

Nu

mb

er o

f p

aper

s

Nanostructureandcharacteristics

Superelasticity

Nano-multilayerand orientation

Electric conductivity,elasticity,and strength

Structure, electric conductivity,and thermal expansion

Year

Fig. 8 Annual change in the number of papers on research themes, in anincubation stage.

159


References

1) H. Kawazoe, M. Yasukawa, H. Hyodo, M. Kurita, H. Yanagi, H.Hosono, Nature, 389, 939 (1997).

2) S. Matsuishi, Y. Toda, M. Miyakawa, K. Hayashi, T. Kamiya, M.Hirano, I. Tanaka and H. Hosono, Science, 301, 626 (2003).

3) M. Sekita, H. Haneda, T. Yanagitani and S. Shirasaki, J. Appl.Phys., 67, 453 (1990).

4) D. Li, H. Haneda, N. Ohashi and S. Hishita, Catalysis Today, 95,895 (2004).

5) Y. L. Li and T. Ishigaki, J. Phys. Chem. B, 108, 15536 (2004).6) T. S. Suzuki and Y. Sakka, Jpn. J. Appl. Phys., 41, 11272 (2002).7) S. Z. Chu, S. Inoue, K. Wada, D. Li, H. Haneda and S. Awatsu, J.

Phys. Chem. B, 107, 6586 (2003).8) N. Saito, S. Matsuda and T. Ikegami, J. Am. Ceram. Soc., 81, 2023

(1998).9) B.-N. Kim, K. Hiraga, K. Morita and Y. Sakka, Nature, 413, 288

(2001).

1. Introduction

“3d transition metals” generally refer to the nine ele-ments from Sc to Cu. However, in view of its importanceZn is included here, making 10 elements in total.1)

As representative correlated electron systems, the 3dtransition metal oxides show drastic changes in magneticand electrical properties with temperature, lattice constant,carrier density and so on. Microscopically, the doubleexchange interaction that produces a colossal magnetoresis-tance effect (CMR effect) and the superexchange interac-tion that produces ferromagnetism or antiferromagnetismplay important roles. Spins, charges, and lattices are closelyrelated in the 3d transition metal oxides, and ferromagnet-ism, superconduction, optical response, and other proper-ties appear to have a close relation.

This section describes the recent trends (2000 to 2004)concerning the oxides of individual elements.

2. Trends within and outside Japan

2.1 Scandium oxideSince scandium has the smallest ion radius among the

homologous rare earth elements, it is often used in studiesfor verifying the size effect of added rare earth elements.Furthermore, due to its comparatively high permittivity (ca.13), thermal stability with Si, and large band gap (> 6 eV),the application of scandium oxide for gate insulating filmsand transparent films2) is attracting attention.

2.2 Titanium oxideTitanium oxide is actively being studied as one of the

most important materials for the global effort to create asustainable society and clean environment. Research ontitanium oxide is especially active for photocatalysts andsolar batteries that use light energy. Furthermore, titanatecompounds such as perovskite are the subject of manystudies for application to piezoelectric and ferromagnetic

materials. These trends are evident also in the number ofpapers published. More than 8,000 papers were publishedon titanium oxide in the 5-year period from 2000 to 2004.Of them, more than 2,500 papers were on optical functions,such as photocatalysts and solar batteries. Nearly 2,000papers were on electrical characteristics, such as ferro-electrics, sensors, and electrode materials. There is alsomuch research on titanium oxide as a (thermo)catalyticmaterial. Figure 1 shows the details.

2.3 Vanadium oxideVanadium oxide has been researched traditionally as a

catalytic material, and now it is attracting attention forapplication to sensors and electrode materials.

160


Optics

Solar battery

Catalyst

Dielectrics

Sensor

Electrochemical

Other electronic characteristics

Photocatalyst

Other optical functions

Ferroelectrics

Piezoelectrics

Electrode

Semiconductor

Other

Fig. 1 Research fields of papers on titanium oxide.Breakdown of 7,422 papers published from 2000 to 2004.


Section 2. Oxides - 3d Transition Metal Oxides

Hideo KimuraPiezo Crystals Group, Materials Engineering Laboratory, NIMS

Xiaobing RenMaterials Physics Group, Materials Engineering Laboratory, NIMS

Shunichi HishitaElectroceramics Group, Advanced Materials Laboratory, NIMS

2.4 Chromium oxideChromium oxide is under research not only as an anticor-

rosive material, fuel cell electrode material, and catalyticmaterial but also as a secondary battery electrode material.

2.5 Manganese oxideSince manganate shows a colossal magnetoresistance,

many studies are underway on its electro-magnetism. In the5-year period from 2000 to 2004, over 1,100 papers werepublished on manganese oxide. The number of papers onmagnetism is the greatest with over 300 papers, followedby more than 150 papers on the electrochemical character-istics for electrodes, etc., and more than 120 papers on cat-alytic properties.

2.6 Iron oxideMagnetism is a popular theme of research these days.

More than 2,100 papers were published on iron oxide in the5-year period from 2000 to 2004, of which over 600 wereon magnetism. In particular, papers on superparamagnetismaccounted for the greatest part of about 1/4. There werealso about 200 papers on catalysts, of which about 10%concerned photocatalysts. Figure 2 shows the details. Fromthe viewpoint of structural character, more than one-quarterof the papers were about nanostructures.

2.7 Cobalt oxideCobalt oxide is mainly researched as a magnet, elec-

trode, and catalyst. These days, layered cobalt oxide com-pound is attracting attention as a non-Cu oxide supercon-ducting material.3)

2.8 Nickel oxideNickel oxide is mainly researched as a magnetic materi-

al, electrode material, and catalytic material. In particular,research on nanostructures for electrodes is noteworthy.

2.9 Copper oxideCopper oxide has been researched as a superconducting

material in many projects. Of more than 1,700 papers pub-

lished from 2000 to 2004, over one-quarter were on super-conduction, followed by 20% on electrical and magneticcharacteristics and 10% on catalytic characteristics.

2.10 Zinc oxideAmong more than 3,800 papers published on zinc oxide

from 2000 to 2004, the most popular theme was catalyticeffect (about 6%), followed by varistor (4%), luminescence(4%), photocatalyst (2%), and sensor (1%). As we can see,the target characteristics vary widely. From the viewpointof specimen shapes, over 30% of the papers were on thinfilms, followed by 20% on nanostructures. This indicatesthat function manifestation by shape control is the focus ofzinc oxide research.

3. Research by NIMS

Regarding scandium oxide, NIMS is attempting to syn-thesize a nanopowder for transparent sintered compacts bysolution synthesis.2)

Regarding titanium oxide, NIMS is creating nanostruc-tures such as nanotube,4) nanosheet,5) and nanorod6) andresearching their characteristics. Visible-light driven photo-catalysts7) are also being examined. Regarding titanate,NIMS has proposed a new piezoelectric mechanism basedon the nano-symmetry of point defects and has demonstrat-ed it on BaTiO3.

8) Figure 3 shows its outline. A ferromag-netic material, Pb-free titanate compound,9) is also beingstudied.

As double oxide materials, V, Cr, and Mn oxides havebeen actively researched for lithium secondary battery elec-trode materials.10-12) Manganese oxide is being studied forcreating new nanostructures13) and for creating protein-composite films.14)

Iron oxide is being studied for synthesizing nanocrystalshaving giant coercive force15) and photocatalytic nanorodarrays.16)

Regarding cobalt, the NIMS discovery of a hydratedcobalt oxide superconductor3) is greatly contributing tosuperconductor research. Composite perovskite oxide withNb17) is also under research as a visible-light driven photo-

161


Magnetism

Paramagnetism

Photocatalyst

Ferromagnetism

Spin

Optical functions

Ferrimagnetism

Phase transition

Electronic characteristics

Superparamagnetism

Catalyst

Other

Fig. 2 Research fields of papers on iron oxide .Breakdown of 2,131 papers published from 2000 to 2004.

Fie

ld-in

duce

d st

rain

ε (

%)

1st cycle2nd cycle4th cycle

Aged Fe-BaTiO3 single crystal

PZN-PTsingle crystal

PZTceramics

Electric field (V/mm)

Fig. 3 Giant electro-strain by nano-symmetry property of point defects.

162


catalyst.Regarding nickel oxide, nanoparticles embedded in an

insulator (silica)18) are being synthesized.Copper oxide will be described in a separate section

because many superconducting materials have been creat-ed.

Zinc oxide is now the subject of intensive research byNIMS. From the viewpoint of functions, NIMS is research-ing the electronic,19) catalytic,20) and luminescence charac-teristics.21) From the viewpoint of synthesis, NIMS isresearching the MBE synthesis of thin films,22) self-organi-zation of a zinc oxide mono-particulate film (Figure 4) bythe solution method, and a patterning technique.23) Fordetails on zinc oxide research, refer to the document.24)

4. Conclusion

Because of their various physical and chemical proper-ties, the 3d transition metal oxides are the subject of intenseresearch worldwide as materials for environmental purifi-cation, low environmental load, energy, information &communications, and electronic & optical materials. Underthese circumstances, NIMS is developing new synthesizingtechniques for promoting new applications and clarifyingbasic material properties with enhanced functions andexploited new characteristics.

References

1) Dictionary of Physics and Chemistry (Third enlarged edition),Iwanami Shoten (1981).

2) Ji-Guang Li, T. Ikegami and T. Mori, J. Mater. Res., 19, 733(2004).

3) K. Takada, H. Sakurai, E. Takayama-Muromachi, F. Izumi, R. A.Dilanian and T. Sasaki, Nature, 422, 53 (2003).

4) R. Z. Ma, T. Sasaki and Y. Bando, J. Am. Chem. Soc., 126, 10382(2004).

5) T. Sasaki nad M. Watanabe, J. Am. Chem. Soc., 120, 4682 (1998).6) S. Z. Chu, S. Inoue, K. Wada, S. Hishita and K. Kurashima, J.

Electrochem. Soc., 159, 1 (2005).7) D. Li, H. Haneda, N. K. Labhsetwar, S. Hishita and N. Ohashi,

Chem. Phys. Lett., 401, 579 (2005).8) X. Ren, Nature Mater., 3, 91 (2004).9) Web page of the National Institute for Materials Science, http://

www.nims.go.jp/piezo/10) K. Ozawa, M. Eguchi and Y. Sakka, J. Europ. Ceram. Soc., 24, 405

(2003).11) A. Kajiyama, K. Takada, K. Arihara, T. Inada, H. Sasaki, S. Kondo

and M. Watanabe, J. Electrochem. Soc., 150, A157 (2003).12) L. Q. Zhang, K. Takada, N. Ohta, K. Fukuda, M. Osada, L. Z.

Wang, T. Sasaki and M. Watanabe, J. Electrochem. Soc., 152,A171 (2005).

13) L. Z. Wang, N. Sakai, Y. Ebina, K. Takada and T. Sasaki, Chem.Mater., 17, 1352 (2005).

14) Y. Lvov, B. Munge, O. Giraldo, I. Ichinose, S. L. Suib and J. F.Rusling, Langmuir, 16, 8850 (2000).

15) J. Jin, K. Hashimoto and S. Ohkoshi, J. Mater. Chem., 15, 1067(2005).

16) L. Vayssieres, N. Beermann, S. E. Lindquist and A. Hagfeldt,Chem. Mater., 13, 233 (2001).

17) J. Yin, Z. G. Zou and J. H. Ye, J. Phys. Chem. B, 107, 61 (2003).18) H. Amekura, N. Umeda, Y. Takeda, J. Lu and N. Kishimoto, Appl.

Phys. Lett., 85, 1015 (2004).19) N. Ohashi, K. Kataoka, T. Ohgaki, T. Miyagi, H. Haneda and K.

Morinaga, Appl. Phys. Lett., 83, 4857 (2003).20) D. Li, H. Haneda, N. Ohashi, S. Hishita and Y. Yoshikawa, Catal.

Today, 93-95, 895 (2004).21) I. Sakaguchi, S. Hishita and H. Haneda, Appl. Surf. Sci., 237, 358

(2004).22) T. Ohgaki, N. Ohashi, H. Kakemoto, S. Wada, Y. Adachi, H.

Haneda and T. Tsurumi, J. Appl. Phys., 93, 1961 (2003).23) N. Saito, H. Haneda, W. S. Seo and K. Koumoto, Langmuir, 17,

1461 (2001).24) ISSN 1347-3212. AML/NIMS Reports, No. 8, 2003.

Fig. 4 Zinc oxide mono-particulate film.

1. Introduction

The National Institute for Materials Science (NIMS) iscurrently focusing on lithium niobate (LiNbO3:LN) andlithium tantalate (LiTaO3:LT) which are related to recentinformation & communications and optical technologies.An octahedral structure, composed of six oxygen ions witha d0 ion such as Nb (4d transition metal) or Ta (5d transi-tion metal) at the center, tends to become asymmetric dueto orbital hybridization. This hybridized binding energybecomes low as the octahedron is deformed (low symme-try). When the temperature goes down, therefore, deforma-tion produces a ferroelectric phase having no center ofsymmetry and a spontaneous polarization.

Ferroelectric materials were first applied mainly to sur-face acoustic wave elements as electronic ceramics orpiezoelectric elements, but full-scale development is nowtargeting applying ferroelectric thin films to memory ele-ments and single crystals to optical devices. Applicationsare mostly in the emerging fields of communication andoptical technologies where Japan is again taking the lead inproduction.

The main application of rare earth oxide is crystals forsolid lasers. In 1960, red pulses having a wavelength of694.3 nm were oscillated successfully with a ruby Crystal.Up to 1965, laser oscillations with ions of various rareearth elements (Nd, Pr, Eu, Ho, Er, Tm, Yb, and Gd) werereported, since when almost all candidate materials seem tohave appeared. The development of transparent ceramicsfor solid state laser materials is now attracting global atten-tion, and NIMS was closely involved at the outset of devel-opment.

Due to lack of space, this section focuses on the trendsin research on LN and LT single crystals and ceramics lasermaterials.

2. Research trends

2.1 Research trends in LN and LTLithium niobate (LN) and lithium tantalate (LT) are typ-

ical ferroelectric single crystal materials. According to areport by Matthias and Remeika in 1949,1) both have apseudo-ilmenite structure and show a trigonal ferroelectricphase of space group R3c with no center of symmetry at

room temperature. The successful growth of large singlecrystals by Ballman et al. using the Czochralski (CZ)method2) quickly clarified the properties. There are notmany oxide single crystals that have such excellent piezo-electric, electro-optical, and nonlinear optical characteris-tics and that have been researched in detail in so manyfields.

In general, many ferroelectric crystals show complicatedphase transitions and it is considered difficult to grow largeand homogenous single crystals. In contrast, LN and LTare considered to be stable materials because they haveonly 180-degree polarization and phase transition points athigh temperature. Therefore, research has concentrated onproducing larger and more homogenous crystals from thematerials. During the enhancement of crystal homogeneityby the CZ method, the phase diagrams of LN and LT wereresearched in detail and the [Li]/[Nb] and [Li]/[Ta] ratiosof these crystals were found to show wide ranges of com-position (nonstoichiometry) at high temperature.3-5)

At high temperature, the nonstoichiometry of LN andLT extends mainly to the Nb or Ta component excess sidebut not to the Li component excess side. Therefore, thecongruent composition is on the Nb or Ta componentexcess side and the Li:Nb or Li:Ta ratio is about 48.5:51.5.The ordinary CZ method cannot produce homogenous sin-gle crystals without a melt of congruent composition. Sincegrowth by Ballman, large crystals have always had congru-ent compositions. This indicates that the composition isdetermined by restrictions on growth. In the congruentcomposition, however, as much as a few percent of Nb orTa excess ions substitute Li ions (nonstoichiometric defect)and produce vacancies of several percent at the sites of Liions.6)

To grow and evaluate stoichiometric LN and LT (SLNand SLT; CLN and CLT for congruent LN and LT) by con-trolling the nonstoichimetric defect density, the improve-ments of various characteristics have been reported.7-10)

Once again, NIMS played a major role in this work.Figure 1 shows the transition in the number of papers

with LN in the title (source: Web of Science). Since around1975, more than 100 papers have been published annually.The main application in the 1980s was optical elements,such as optical modulators, optical integrated elements, andholograms, and the number gradually increased until 1990.

From 1990 to 1992, the number of papers started

163



Section 2. Oxides - Niobate, Tantalate, and Rare Earth Oxide

Kenji KitamuraOpto-Single Crystal Group, Advanced Materials Laboratory, NIMS

increasing quickly, partly because the digital hologrambecame available as a means of storing information usingLN and attracted attention. The hologram was mainly usedto store 3D images and execute information processingoperations but was extended to the digital hologram forstoring digital information and triggered a surge in interest.In 1990, it was reported that the inversion of polarizationcan be patterned by an electric field. This enabled applica-tion to wavelength conversion and optical deflection ele-ments and fueled further research. Application to commu-nication devices also increased quickly as investment in theIT revolution boomed.

In 1992, the National Institute for Research in InorganicMaterials (the present NIMS) announced the aforemen-tioned problem of nonstoichiometric defect and the singlecrystal growth method for controlling the problem. Thegreen columns in Figure 1 indicate the transition in thenumber of papers with stoichiometry in the title. Papersdealing with stoichiometry began to appear in 1992 and arenow increasing.

Figure 2 shows the transition in the number of paperswith LT in the title. Up to 1990, the application of LT tooptical elements had been limited mainly to collector sen-sors and some manufacturers’ SAW filters for TV andvideo. Since 1990, however, the number of papers has beenincreasing quickly because the application of LT to SW fil-ters of cellular elements boosted the demand, and wave-length conversion by the inversion of polarization began toattract attention.

The blue columns in Figure 2 indicate the number ofpapers on nonstoichiometry. NIMS has also been publish-ing papers after starting LN research later. Accompanyingthe increase in the total number of papers, papers in thisfield started increasing quickly. Most of these papers dealtwith application to wavelength conversion elements by theperiodic inversion of polarization, and this field may growdramatically in future.

2.2 Research trends in ceramics laserAs already mentioned, crystalline materials for solid

lasers were all identified at a rather early stage. However,the transition in laser use or system to high output, semi-conductor excitation, and microchip processing is changingthe materials of interest. Nd-doped YAG(Y3Al5O12) laser isstill a dominant solid laser but the density to which activat-ed Nd ions can be doped is limited, and so Nd-doped YVO4

was studied. Since Nd-doped YVO4 has a large coefficientof absorption and a large cross section of induced emission,it was developed actively and is already marketed as amicrochip or compact solid laser material.11,12) However,YVO4 has low thermal conductivity, low mechanicalstrength, and short life of fluorescence. The compound alsohas the disadvantage that it is difficult to grow large singlecrystals of high quality.

There has also been research on the application of trans-parent ceramics to laser host systems, which was initiatedby the National Institute for Research in Inorganic Materi-als (the present NIMS).

164


Number of papers

Year

Fig. 1 Number of papers with lithium niobate in the title, by year (Red:Total, Green: Papers on non-stoichiometric defects).

Number of papers

Year

Fig. 2 Number of papers with lithium tantalite in the title, by year(Green: Total, Blue: Nonstoichiometric defects).

Number of papers

Year

Fig. 3 Number of papers with ceramic laser in the title.

165


YAG ceramics produced by the sintering method allowhigh doping of Nd into ceramics to achieve a large absorp-tion characteristic. Since the dispersion of grain boundariescan be almost controlled and the characteristics are moreexcellent than those of the conventional microcrystal, thismaterial is ideal for microchip lasers.

Figure 3 shows the transition in the number of paperswith ceramics laser in the title. The number quickly startedincreasing in 1990. Materials range widely from YAG, andfuture developments should be monitored. The applicationto laser is at a very high level. Once the technology hasbeen established, single crystals will be substituted in manyfields.

References

1) B. T. Matthias and J. P. Remeika, Phys. Rev., 76, 1886 (1949).

2) A. A. Ballman, J. Am. Ceram. Soc., 48, 112 (1965).3) P. Lerner C. Legras and J. P. Duman, J. Crystal Growth, 3/4, 231

(1968).4) L. O. Svaased, M. Eriksrud, G. Nakken and A. P. Grande, J. Crystal

Growth, 22, 230 (1974).5) S. Miyazawa and H. Iwasaki, J. Crystal Growth, 10, 276 (1971).6) N. Iyi, K. Kitamura, F. Izumi, S. Kimura and J. K. Yamamoto, J.

Solid State Chem., 101, 340 (1992).7) K. Kitamura, Y. Furukawa, Y. Ji, M. Zgonik, C. Medrano, G.

Montemezzani and P. Guenter, J. Appl. Phys., 82, 1006 (1997).8) T. Fujiwara, M. Takahashi, M. Ohama, A. J. Ikushima, Y.

Furukawa and K. Kitamura, Electron. Lett., 35, 499 (1999).9) V. Gopalan, T. E. Mitchell, Y. Furukawa and K. Kitamura, Appl.

Phys. Lett., 72, 1981 (1998).10) K. Kitamura, Y. Furukawa and K. Niwa, V. Gopalan, T. E.

Mitchell, Appl. Phys. Lett., 73, 3073 (1998).11) R. A. Fields, M. Birnbaum and C. L. Finchere, Appl. Phys. Lett.,

51, 1885 (1987).12) T. Taira, A. Mukai, Y. Nozawa and T. Kobayashi, Opt. Lett., 16,

1955 (1991).

1. Introduction

Glass materials are used widely for both traditionalwares and products for daily living, such as window panes,bottles, and tableware, and there are also functional glassmaterials which are used for optical equipment lenses,computer hard disks, and computer displays, for example.In particular, a type of glass now the subject of muchresearch is a functional glass called nanoglass, which canbe made to offer new functions by high-grade tissue con-trol.

Figure 1 shows the basic concept of nanoglass. The firstgeneration is ordinary functional glass where atomic orionic active spots are dispersed in the glass matrix at ran-dom. Fluorescent emission materials belong to this group.Research is conducted by varying glass compositions tosearch for new compositions having useful properties. Thesecond generation is nanoglass where particulate activepoints composed of several atoms or ions are dispersed inthe glass matrix at random. The glass properties are domi-nant. Semiconductor particulate dispersed glass, which isexpected to be used as a nonlinear optical material, belongsto this group. The third generation is nanoglass where theactive spots are somewhat larger and are dispersed regular-ly in the glass matrix. With this type, crystal propertiesbegin to appear. This glass manifests the functions of pho-tonics crystals for nonlinear optical materials, and so inten-sive global research is underway on the third generation ofnanoglass. Chemically, the third-generation state is glass

but is about to show crystal-equivalent properties. About18 years ago, glass researchers proposed the concepts ofamostal,1) conjugate glass,1) and polling technology2) to pro-duce glass states of the second and third generations. Thecurrent nanoglass is based on these ideas and research isongoing to achieve higher precision and functionality.

2. Research trends

This section outlines the main functional glass and nano-glass fabrication technologies now being researched world-wide.

2.1 Vapor phase synthesis3)

There are two main gas synthesis processes. The chemi-cal vapor deposition (CVD) process causes a chemicalreaction between raw material gases and deposits the reac-tant on a substrate. The sputtering process makes ionsimpinge upon the same material (target) as the object sub-stance to drive out the target ions and deposit them on thesubstrate. To form active spots or nanostructures, materialsare repetitively deposited by masking or self-cloning. Thisprocess has excellent precision and stability.

2.2 Laser-induced structuring process4)

A femtosecond laser beam is narrowed through a lensinto glass to induce a structural change in the irradiatedregion and to form a region having a high refractive index.Not only spots but also lines or optical waveguides can beformed. This simple process has excellent controllability.Unlike a nanosecond-order pulse laser beam, a femtosec-ond-order laser beam is known to cause a permanent struc-tural change (induced structure) by irradiation into glasswhere electron state changes of ions other than the heatingeffect are involved. This laser is optimum for irradiationbecause high-output irradiation hardly causes irradiationdamage called abrasion on the surface of materials. Todate, ion reduction and ionization of silver and other sub-stances, and diffraction grating by forming an index patternhave been achieved. The possible uses are high-density 3Doptical recording, micro illumination source, and micro dif-fraction grating.

166


1st generation 2nd generation 3rd generation

Active spot sizeSubmicron toseveral nm 1 to 10 nm 10 to 100 nm

Dispersed status

Uniform dispersion Particulate aggregate dispersion High-degree periodicstructure array

Nanoglass Photonic crystals

Fig. 1 Basic concept of nanoglass.


Section 3. Glass

Satoru InoueFunctional Glass Group, Advanced Materials Laboratory, NIMS

2.3 Etching process5)

The etching process, which is used in photolithographyin semiconductor manufacturing, offers excellent precisionand stability. A glass film deposited by vapor phase synthe-sis is bored regularly by precision machining technology tofabricate the world’s first practical photonic crystals. Thecrystal atoms correspond to pneumatic pillars and thematrix corresponds to glass. There is also a technique ofdirect etching by abrasion using an electron beam or high-output excimer laser beam and a technique of etching adamaged region after irradiation by SOR-X-ray or high-speed accelerated baryon ion beam. Pores are used becausethey are very effective for creating a difference in refrac-tive index and the grain boundary can be finished veryneatly.

2.4 Anodic oxidization process6)

Figure 2 shows the formation process. A conductive filmis formed on a glass surface and then an aluminum thinfilm is formed on the conductive film by evaporation orsputtering. This unique process for fabricating functionalglass was developed by NIMS. Anode oxidization changesan aluminum thin film into an amorphous-alumina porousthin film of nanopores vertically arranged on the glass sur-face. The conductive film is an electrode to allow the anodeoxidization of the aluminum to the last. An oxide film on aglass surface has an aluminum film (barrier layer) at thebottom of pores which is thinner than the film on the side,so the barrier layer can be eliminated completely by etch-ing. However, this is not possible for a general anodic-oxi-dized film of aluminum. Since the self-organization processis used, a nanometer-order porous tissue can be formed.Pores of a wide diameter ranging from several to 1000 nm

can be fabricated. Into the pores, a chemical compound ormetal can be entered by the sol-gel process or the elec-trodeposition process to add various functions to the nan-otissue. By using the difference of solubility between theamorphous alumina and the compound which enters thepores, the alumina can be removed to form a nanorod ornanotube array. This process is expected be used for photo-catalysts using titanium dioxide, high-density magneticrecording media using magnetic materials, and pseudo-photonics crystals using dielectrics.

2.5 Crystallization process and phase splitting processThe crystallization process that deposits nanosize crys-

tals in glass is used to manufacture transparent crystallineglass. In general, two-stage heating is used for glass crys-tallization. Glass is heated first in the crystal nucleationtemperature area and then heated to a higher temperature togrow a nucleus of deposition for adjusting the crystal size.In one study, second harmonics were generated from nano-glass using regular crystal deposition7) by a laser beam trig-ger. Another study attempted to deposit crystals and mani-fest functions on a glass surface where deposition is easy.Takahashi8) systematically fabricated transparent crystallineglass by B2O3-GeO2 or other glass formation systems,found that ferromagnetic crystals are orientation-deposited,and thus successfully generated second harmonics.

The phase splitting process9) uses the phenomenon ofliquid-liquid phase splitting that separates a liquid into two(stable immiscible liquids) or the phenomenon of potentialphase splitting at the liquidus temperature. By the nucle-ation and growth mechanism, this process uses the phasesplitting area where phase splitting deposits droplets. Ahomogenous melt is produced by heating beyond the phaseslitting limit called the immiscibility temperature, coolingdown to the immiscibility temperature area, and holding fora specified time to allow phase splitting. Finally, the melt isquickly cooled to produce phase-split grain dispersed nano-glass or nanoglass of the second generation. During quickcooling, the melt may be expanded or compressed to flattenthe phase-split grains and give anisotropy to the properties.This process can be applied to alkali-earth silicates, alkali-

167


An aluminum film is deposited on the glass plate covered with a thin conductive film.

Small pores are bored in the glass surface with the progress of electrolysis

A thin film of aluminum oxide with nanometer-size pores is formed.

When the aluminum oxide is oxidized with an acid, the pores are slightly enlarged and reach the conductive film.

Aluminum

Glass plate

Aluminumoxide

Conductivefilm

Small pore

Throughsmall pore

Fig. 2 Formation of nanostructure on glass surface by anodicoxidization.

High-speedautomatic weighing

Parallel melting

Parallel synthesis

High-speed specimenfabrication and parallelthermal treatment

Crystallizationjudgment

Automaticmeasurement

Quick coolingand observation

Determination of glass forming area

Synthesisresearch

Propertiesresearch

Determination of dependence ofproperties on compositions

Automatic opticalmeasurement

Determination of dependenceon thermal treatment

Fig. 3 Concept of combinatorial glass research system.

168


earth borates, iron silicates, and titanium silicates. A rare-earth oxide, if added as the third component, is condensedin the phase-split grains, so only the compositions of phase-split grains can be varied with priority to manifest func-tions.

2.6 High-speed glass searchTo search for new glasses by varying glass composi-

tions, NIMS is pioneering a glass research system based onthe combinatorial techniques.10) This system can search fornew glasses more than 100 times faster than before. Figure3 shows the concept of the system. Specimen synthesis andproperties measurement are processed at high speed by par-allel operations to increase the speed of research. Compre-hensive research will lead to the discovery of new function-al glass.

3. Future outlook

The functional glass fabrication processes introducedhere have unique characteristics and no single process canbe said to be better; they are used according to the type ofglass to be developed. The vapor synthesis process, laser-induced structuring process, and etching process are suit-able for regular 2D and 3D dispersions but are not good interms of productivity. The anodic oxidization process issuitable for producing comparatively large nanoglass hav-ing a regular structure with high efficiency. The crystalliza-tion process using the deposition phenomenon and thephase splitting method both offer excellent productivity butare not good at regular crystal dispersion.

Materials research and development by the processesintroduced here will proceed in parallel and yield practicalfunctional glass reflecting the features of each process.Combined research techniques will be developed and rolledout to research systems at enterprises to accelerate thedevelopment of new materials.

4. Conclusion

New glass materials will be actively developed by com-bining various synthesizing processes with combinatorialresearch techniques. The demand for glass materials isespecially large in the fields of the environment, energy,and information, and research in these fields will be pro-moted. Since the glass industry consumes large quantitiesof energy, it is a matter of urgency to develop energy-sav-ing production technologies for curtailing CO2 emissions.With the enhancement of recycling technologies, researchand development on industrial glass manufacturingprocesses will proceed based on new ideas.

References

1) H. Yamashita: “Materials and Devices of New Photonics Age” TIC,p. 281 (2000).

2) For example: R. H. Stolen and H. W. K. Tom, Opt. Lett., 12, 585(1987).

3) For example: S. Kawakami, T. Kawashima and T. Sato, Appl. Phys.Lett., 74, 463 (1999).

4) K. Miura: “Materials and Devices of New Photonics Age” TIC, p.284 (2000).

5) For example: M. E. Zoorob, M. D. B. Charlton, G. J. Parker and J.J. Baumberg, M. C. Netti, Nature, 404, 740 (2000).

6) S. Inoue, S. Z. Chu, K. Wada, D. Li and H. Haneda, Sci. Technol.Adv. Mater., 4, 269 (2003).

7) T. Honma, Y. Benino, T. Fujiwara, R. Sato and T. Komatsu, J.Ceram. Soc. Japan, 110, 398 (2002).

8) Y. Takahashi, Y. Benino, T. Fujiwara and T. Komatsu, J. Appl.Phys., 89, 5282 (2001).

9) S. Inoue, A. Makishima, H. Inoue, K. Soga, T. Konishi and T.Asano, J. Non-Cryst. Solids, 247, 1 (1999).

10) S. Inoue, S. Todoroki, T. Konishi, T. Araki and T. Tsuchiya, Appl.Surf. Sci., 223, 233 (2004).


By tracing back the history of R&D on composite mate-rials, we see that the operating temperature has been goingup with the development of composite materials from rub-bers to plastics, metals, and ceramics. In addition toreviewing the history, this section describes the future ofR&D on composite materials focusing on materials charac-teristics. So far, composite materials have been researchedmainly in terms of mechanical properties because compos-ite materials satisfy the requirements of lightweight andhigh strength for aircraft and vehicles. Figure 1 shows therelationship between specific strength and specific modulusfor main metals, ceramics, polymers, and composite mate-rials. Composite materials are the only ones that can haveboth characteristics.

Fiber reinforced plastics (FRP), which are the mostwidely used polymer materials among composite materials,are considered to have almost reached their highest perfor-mance. Figure 2 shows the relationship between the tensilestrength and tensile modulus of carbon fibers. There arehigh-strength carbon fibers of 7000 MPa or greater tensilestrength and high-modulus carbon fibers of 900 GPa orgreater tensile modulus. However, for users, compositematerials require knowledge about how to use them, yettheir practical application range is expanding. There are

various problems that seem to have been solved but haveactually yet to be solved, such as interfacial debonding,joint structure with different materials and its reliability,and the assurance of environmental resistance to shock andwater.

Metal matrix composites have also been the subject ofmuch research, seeking materials that may have high spe-cific modulus and can withstand the high operating temper-ature of a metal which is used as a matrix. Since applica-tions are difficult to find, however, R&D is not so active.Nevertheless, metal matrix composites have a low coeffi-cient of thermal expansion that is not available with metal-only materials. Among ceramic matrix composites, parti-cle-dispersed and whisker-dispersed ones could not achievea fracture toughness of 10 MPam1/2 or higher. Ceramicmatrix composites of a textile type woven from continuousfibers are being studied not to enhance the strength but toproduce high-temperature materials having great fractureresistance.

For all composite materials, it is comparatively easy tounderstand the mechanisms of reinforcement and manifes-tation of functions, because more than 90% of the existingphenomena can be understood based on past knowledge.Macro-mechanical function design and non-mechanicalfunction design do not offer such great potential as newmaterials will be constructed by extension from existing

169


Spe

cific

rig

idity

Specific strength

Fig. 1 Relationship between specific rigidity and specific strength ofvarious materials.

Tens

ile s

tren

gth

[MP

a]

Tensile modulus [GPa]

Fig. 2 Relationship between tensile strength and tensile modulus ofcarbon fibers.

Chapter 10. Composite Materials

Yutaka Kagawa Composite Materials Group, Materials Engineering Laboratory, NIMS

materials and composite guidelines.

2. Trends within and outside Japan

This section summarizes the recent important compositetechnologies.

2.1 Concept of composite materialsResearch on existing composite materials has intensi-

fied, and many reports outlining new composite materialsare being published. In particular, the term “compositematerials” now means nano-order composite and tissuecontrol, far beyond the conventional framework of materi-als. In Japan, no uniform concept has been establishedbecause of the vertical organization of academic societies.

2.2 Metal matrix compositesAbout 30 years ago, metal matrix composites attracted

great attention as a reinforcing mechanism for overcomingthe problem of dislocations. Ceramic fibers and whiskerswere then developed in Japan, and various attempts weremade to use these new materials. However, the materialsfailed to become popular except for particular special uses,because these composite materials offered no advantagesabove those of metallic materials. In the field of metalmatrix composites, it is hard to search for new materials.Further research is necessary in the particular fields of lowthermal expansion and high modulus.

2.3 Polymer matrix compositesFigure 3 shows the demand (including prediction) for

carbon fibers, which are the developing type of reinforcingfibers of FRP. Figure 3 (a) shows the demand by countryand (b) shows the demand by industry. As the space-racetook off in the latter half of the 1960s, carbon fibers beganto emerge, and Japan has an overwhelmingly share of thisfield.

The fields of application of FRP having specific modu-lus and strength are continuing to expand. The ratio of FRP

in aircraft is growing, but neither the universities andresearch institutes are developing the inspection technolo-gies needed for companies to ensure the safety of practicalmaterials nor conducting research on optimum manufactur-ing processes. Although many researchers are examiningIntelligent Materials and Smart Technologies for FRP, thebasic concept has already been developed. In Japan, veryfew researchers are conducting research of the Westerntype where FRP is always being studied as an old yet newsubject whereas the majority of researchers are heading inthe same direction. This is another characteristic of domes-tic research on classic polymer composite materials.

In the world of polymers, nanocomposite materials arealso undergoing active research. Self-organization andnano- structure are the themes of various research activitiesbut not beyond the materials level.

2.4 Ceramic matrix compositesRegarding materials dispersed with particles and ones

dispersed with whiskers, the first stage of research has beencompleted. In particular, fiber-based materials are nowentering practical use because they have high fracture resis-tance that is not available with ceramic materials. However,there are still new issues to be solved before compositematerials can be used in practice, such as surface compositematerials based on a new concept and environmental resis-tance coatings. Due to such delays, Japan may lag farbehind Europe and the US.

All papers published since 1985 in an academic paperdatabase (SCI Expanded) were searched for those contain-ing both the keywords “nano” and “composite materials”.Figure 4 summarizes the number of papers published everyyear by country. The total number of papers started increas-ing in 1993 and has been increasing especially fast since2000. The percentage of papers from Japan is 14%, thegreatest proportion after the United States and China. Thegrowth of China, which is faster than that of the UnitedStates, is noteworthy. In terms of the number of papers,Korea ranks high after France and Germany. Figure 5 clas-sifies the contents of papers published in 2004 into poly-

170


Car

bon

fiber

dem

and

(ton

s)

Asia

Japan

Europe

USA

(a) Demand by country

Fig. 3 Demand for carbon fibers.

Car

bon

fiber

dem

and

(ton

s)

Aeronautics and space

Sports

General industry

(b) Demand by industry

mers, metals, and ceramics. Over 60% of the papers are onpolymer nanocomposite materials. The nanocompositematerials of this type are attracting great attention becausethey not only have enhanced mechanical characteristics butmanifest multiple function, including optical characteris-tics, electrical conductivity, thermal radiation, and attenua-tion characteristics.


The Composite Materials Group of NIMS, which isinvolved in the field of nanocomposite materials, has start-ed researching nanoparticle-dispersed polymer and ceramiccomposite materials. Such nanocomposite materials arebeing studied for composite materials that can not only bedownsized to the nano level but also produce peculiarnanoeffects thanks to composite effects. Our group isexamining whether characteristics such as modulus, ther-mal expansion, electrical conductivity, and thermal conduc-tance can be obtained beyond the conventional range ofmacro-composite effects. Regarding the phenomenon ofinteraction between light and electromagnetic waves,deformation and fracture, we are studying whether unex-pected nano-unique composite effects can be obtained. Inorder to use nano-effects, we also started multiscaling bybiomimetics for hybridization using nanocomposite materi-als.

These procedures are being researched beyond the bor-ders of polymers, metals, and ceramics. We have also start-ed developing measurement and evaluation technologiesfor the nanomaterials technologies. The concept ofnanocomposite materials has expanded widely in the lastfew years and now includes even polymer materials com-posed of different molecular structures. In the field of con-ventional composite materials, however, we have notachieved noteworthy R&D results, but in the field ofnanocomposite materials, we successfully manifested newfunctions and obtained characteristics not available withconventional composite technologies. For example, theinclusion of clay, silica, or other nanoparticles was reportedto increase the modulus of polymer materials by 1.5 to 3

times. These days, composite materials dispersed with car-bon nanotubes are also undergoing active research for verypeculiar mechanical characteristics and low densities.However, these excellent characteristics and the mecha-nisms of nanocomposite effects have yet to be clarified.

Regarding polymer and ceramic composite materialsthat are expected to be applied to a wide range of uses,NIMS is working to secure the necessary human resourcesand to extend the research fields. The first stage of person-nel organization has been completed, and NIMS now plansto initiate full-scale research on composite materials, mak-ing best use of the personnel belonging to the organization.

4. Future outlook

Composite materials are at a turning point in research.Instead of the conventional handling by reinforcing materi-als, matrix, interface, and other parameters, the control anddesign of microstructures of materials themselves and atinterfaces will become necessary, because new develop-ment can no longer be extended from conventional tech-nologies. Great efforts are necessary for composite materi-als research by the nanostructural control of matrix andinterface and by positively employing the nano-order dif-ferences in the modulus and the coefficient of thermalexpansion. As a result, materials research is expected notmerely to downsize the current composite materials butalso to utilize nano-level interactions.

In addition to creating new materials, it is necessary tosolve the problems involving composite materials. Forexample, the tasks of ensuring the quality and reliability ofcomposite materials and inspecting adhesive bonded jointsare addressed by know-how in practical application. Therecent advances in computer and electronic technologieswill enable different approaches even in similar research tothat in the past. As explained above, the following chal-lenges are strongly demanded in composite materialsresearch:(a) Seeking new effects of composites by positively usingnanomaterials technologies,(b) Solving old but new important pending problems, such

171


Tota

l nu

mb

er o

f p

aper

s Total n

um

ber o

f pap

ers

Total numberUSA

China

Japan

Germany

Total numberof papers

Fig. 4 Number of papers on nanocomposite materials.

Total numberof papers:

2,542 PolymersCeramics

Metals

Other

Fig. 5 Breakdown of papers on nanocomposite materials published in2004.

172


as the development of testing and measuring technologiesby positively using recent advances in science and technol-ogy

From the viewpoints of i) Mechanical composite mate-rials and ii) Non-mechanical composite materials, materialsresearch in the future is likely to consider the following.

i) Mechanical composite materials:Composite materials offer the great feature that micro-

fractures can be accumulated in composite materials, irre-spective of the matrix type. The micro-damage of the cur-rent composite materials are fiber breaking, matrix crack-ing, and interfacial debonding but they are of the order oftens of microns. As these micro-fractures accumulate, thecompliance increases, causing dimensional changes of thematerials. The recent materials technologies allow nanome-ter-order tissue control for metallic, ceramic, and polymermaterials. The positive employment of such nanotissuecontrol for composite materials is another subject to besolved. Users of composite materials require a science andtechnology review of the conventional know-how basedsolutions to the subjects of reliability assurance and lifeprediction.

ii) Non-mechanical composite materials:Inclusion of fibers and particles can effectively enhance

the coefficient of thermal expansion. This phenomenon is

already used for many materials but not particularly forcomposites. Theoretical analysis is now almost at the stageof predicting structure-insensitive materials characteristicsfrom the volume fraction ratios of components. Because ofinterface effects, electrical conductivity and thermal con-ductance are difficult to predict accurately but can be esti-mated roughly from the characteristics of components.Regarding functional materials, members employing thematerials will be further downsized in future. In the fieldsof micromachines, bio, and devices, for example, the mate-rials themselves will inevitably be downsized to the micronorder, whereupon the conventional composite materialsmay pose the problems of heterogeneity and anisotropy andbecome inapplicable to these fields. Thus, there are highexpectations for nanometer-order composite technologies.

References

1) The Materials Selector on CD-ROM ver. 2.1, Norman A. Watermanand Michael F. Ashby.

2) Report on “Growth Opportunities in Carbon Fiber Market 2004-2010”, published by E-Composites, Inc. (2004).

3) T. Sun and J. M. Garces, Adv. Mater., 14, 128 (2002).4) On-line Database, Web of Science, Science Citation Index

Expanded (2005).

1. Introduction

In parallel with metallic and inorganic materials, poly-mer materials are playing an important role. As industrialinfrastructure materials, polymers are widely applied toplastics, rubbers, adhesives, photoresists, separation mem-branes, gels, biomaterials, and so forth. If fibers, packagingstyrofoam, and paper are included, it is clear that polymersare closely interwoven with today’s various complicatedindustrial structures.

The global chemical industry, excluding the medicalfield, is estimated to be worth 144 trillion yen and its majorproducts are polymers. Internationally-renowned polymer-related companies are, for example, DuPont, Dow Chemi-cal, Bayer, and BASF.

The annual consumption of plastics per person has nowreached 90 to 100 kg in West Europe, the US, and Japan(statistics of FY2001), while the consumption in Asia (13kg/person in FY2001), including India, is predicted toincrease rapidly in future and cause environmental andenergy related problems.

This section outlines the situation concerning polymerssince 2000 and also the research trends within and outsideJapan.1-3)

2. Global situation concerning polymer materials

The American Chemical Society surveys and publishesthe sales, profits, and R&D expenditure of the 50 top-rank-ing global companies in the chemical industry. First, thejournal of the Society (C&E News, issued on July 18,2005) was checked for the trends. Table 1 gives theFY2004 data of major chemical companies. The top threecompanies by sales are Dow Chemical, BASF, andDuPont, with sales exceeding 30 billion dollars each.BASF spent a total of 1,459 million dollars on R&D, 3.8%of sales. R&D expenditure in FY2004 was 6.2% higherthan in FY2003. Although not shown in Table 1, petro-chemical sales showed a remarkable increase in 2004. Forexample, the sales of Royal Dutch/Shell exceeded 29.4 bil-lion dollars, approaching those of DuPont. The petrochemi-cal industry seems to be raising the profit ratio of the entirechemical industry. From Japan, the four companies of Mit-subishi Chemical, Mitsui Chemicals, Sumitomo Chemical,and Toray rank among the world’s top 20, and their salesincreased from 12% in 2003 to 28%. The world’s top 50

chemical companies include 8 Japanese companies, thetotal sales of which account for 13.2% (78,000 million dol-lars) of the sales of the top 50 companies.

According to C&E News, the profit ratio on chemicalproducts was 8.1% in 2004, up from 5.5% in 2003. Theratio of R&D expenditure to sales is 2.1% on average,down from the past five years.

In the field of polymers, the focus of R&D is changingfrom the provision of general-purpose materials to that offunctional materials and customer-oriented solutions. Inaddition, the most important management strategy is clear-ly shifting from M&A to the expansion of core business(organic growth) and priority investments are extending toAsia including China.

As of the end of March 2005, the price of crude oil onthe NY market was over 55 dollars/barrel. Considering thatthe price was around 32 dollars one year ago and had beenstable around 20 dollars for the last decade, this representsa remarkable sudden rise. The world’s chemical companiesmay be engaged in oil and gas refining or the energy busi-ness, and the dependence on natural gas is high in the US.Under these circumstances, the impact of crude oil priceson polymer research are too complex to be determined, butthere is no doubt that the price is a huge long-term threat,as are environmental problems.

173


CompanyChemical Sales

($ Millions)Chemical R&D

Spending% ofSales

Dow Chem.

BASF

DuPont

Bayer

Mitsui Chem.

Sumitomo Chem.

DSM

Clariant

Rohm & Hass

Ciba Specialties

40161.0

38189.1

30130.0

18088.3

11350.0

9883.0

9641.8

6862.4

6471.0

5653.3

1022.0

1459.0

1333.0

1138.1

322.7

417.9

355.7

220.4

265.0

231.7

2.5

3.8

4.4

6.3

2.8

4.2

3.7

3.2

4.1

4.1

(Source: C&E News, July 18, 2005)

Table 1 Sales and R&D expenditure of polymer-related global companies.

Chapter 11. Polymer Materials

Izumi IchinoseMacromolecular Function Oxides Group, Advanced Materials Laboratory, NIMS

Figure 1 shows the transition in R&D expenditure inJapan’s chemical industry. The data was compiled by TheSociety of Polymer Science, Japan (SPSJ) based on variousstatistical materials of the government. The R&D expendi-ture in FY2000 was 801.8 billion yen, accounting for about4% of total sales. Despite the economic stagnation sinceFY1990, this value has been constant. The facility invest-ment for R&D has been decreasing since peaking inFY1992. The facility investment in FY2000 was not morethan 60% (about 1 trillion yen) of the peak. According todata of the Statistics Bureau of the Ministry of InternalAffairs and Communications, the total sales of Japan’schemical industry in FY2004 were 21.6 trillion yen and theoperating profit was about 1,430 billion yen. The expendi-ture on R&D was 890 billion yen, 4.1% of the total sales.For details, see: http://www.stat.go.jp/data/kagaku/.

3. Environment and polymer materials

In Japan, technological development related to “greensustainable chemistry” is being promoted under the leader-ship of the Japan Chemical Innovation Institute (JCII), andthis is now a global trend of polymer materials research.For example, propanediol synthesized from corn starch isused as a raw material for polyester, and the conversionfrom fossil fuels to cost-competitive biomass materials hasbeen already started. To reduce environmental loads, halo-gen-free fire retardants and water-soluble polymer coatingsnot containing volatile organic compounds (VOC) havebeen developed. Current research ranges widely from watertreatment using polymer membranes and energy-savingtechnologies, such as lightweight polymer composite mate-rials, to polymer membranes for fuel cells and other ener-gy-related purposes and recyclable carpets.

The Society of Polymer Science, Japan featured envi-ronment-supporting polymer technologies in the March2005 issue of its bulletin “KOBUNSHI”. Key technologiesinclude a non-phosgene process for manufacturing polycar-

bonate from CO2 (Asahi Kasei), self-extinguishing epoxyresins (NEC and Sumitomo Bakelite), and a recycle coatingsystem (Nippon Paint).

4. Research trends in Japan and the US

Japan’s polymer research is extremely active andadvanced compared with those of Western countries. Forexample, The Society of Polymer Science, Japan has thelargest number of members (12,500) of any polymer-relat-ed societies in the world, much more than that in the poly-mer chemistry division (7,500) of the American ChemicalSociety.

Figure 2(a) shows the number of papers published in theJanuary to March 2005 issues of the most influential poly-mer-related journal “Macromolecules” (American Chemi-cal Society, IF:3.621) by country. The number of papersfrom Japan is 33, the second highest after the United States.In 2003, the journal carried 240 Japanese papers, 17.5% ofthe total (1372). Figure 2(b) shows the number of paperspublished in the journal “Macromolecular Rapid Commu-nications” (IF:3.236) of Wiley (Germany) in 2004. In termsof the number of papers, Japan ranks third after China andthe United States, above Germany. These results indicatethe advanced level of Japan’s polymer research.

Figure 3 shows the number of papers reported at the54th Annual Meeting of The Society of Polymer Science,Japan (SPSJ) held in May 2005 by field. In this meeting,2,276 general papers were reported. By field, 481 were inthe field of “polymer chemistry” dealing with polymer syn-thesis (radical polymerization and polycondensation), den-drimer and other special structure polymers, polymer reac-tions, and new polymerization processes; 715 in the field of“structures and physics of polymers” dealing with the mol-ecular properties of polymers, solid properties, solutionproperties, surface properties (rheology, gel, and tribology),thin films, and molecular aggregates; 600 in the field of“polymer functions” dealing with optical characteristics,

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Fig. 1 Transition of R&D expenditure in Japan’s chemical industry (excluding the medical field).Statistical data: “Survey Report on Science and Technology Research in Japan”, Statistics Bureau, Ministry of Public Management, HomeAffairs, Posts and Telecommunications; and “Industrial Statistics”, Industry Division, Ministry of Economy, Trade and Industry.

electric, electronic, and magnetic characteristics, separa-tion, recognition, and catalytic characteristics, highlystrong and elastic polymers, properties in ultimate condi-tions, and liquid crystals; 348 in the field of “biopolymersand biomolecules” dealing with proteins, enzymes, DNA,carbohydrate polymers, biomembranes, biomimetics, bio-engineering, DDS, and biomaterials; 113 in the field of“environment and polymers”; and 13 in the field of “poly-mer industry and engineering”.

The number of general papers reported at the SPSJ’sAnnual Meeting was 1,890 in 2000 (Nagoya), 1,940 in2001 (Osaka), 2,028 in 2002 (Yokohama), 2,081 in 2003(Nagoya), and 2,251 in 2004 (Kobe). This annual increaseindicates that polymer materials are closely related to awide range of domestic industries and that researchers’interest is growing.

At the 229th National Meeting (San Diego) of the Amer-ican Chemical Society held in March 2005, 9,200 paperswere reported at 930 chemistry-related sessions. The num-ber of papers was greater than the approximately 8,500papers at the 225th National Meeting (New Orleans) in2003, and 8,000 papers at the 227th National Meeting(Anaheim) in 2004. In relation to polymers, a total of 972papers were reported in the Division of Polymer Chemistry(POLY) and Division of Polymeric Materials: Science &Engineering (PMSE).

For special sessions at POLY, six themes were selected:“Biological and Synthetic Macromolecules for EmergingNanotechnologies”, “Carbon Nanotubes, Polymers, andComplex Fluids”, “Polymer Surfaces and Interfaces”, “Bio-

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Fig. 2 Number of papers published on polymer-related journals by country.(a) Total from January 2005 to March 2005 issues of “Macromolecules”. (b) Total from “Macromolecular Rapid Communications” 2004.

Polymer chemistry (481)

Structures and physics of polymers (715)

Polymer functions (600)

Biopolymers and biomolecules (348)

Environment and polymers (113)

Polymer industry and engineering (19)

Invitations and awards (39)

Fig. 3 Number of papers reported at the 54th Annual Meeting of TheSociety of Polymer Science, Japan, by field.

Special Sessions Papers

POLY

PMSE

Biological and Synthetic Macromolecules for Emerging Nanotechnologies

Carbon Nanotubes, Polymers, and Complex Fluids

General Papers

Polymer Surfaces and Interfaces

Biomimetic Polymers

Degradable Polymers and Materials

Smart Polymer Films, Composites, and Devices

Awards

Others

New Concepts in Polymeric Materials

Polymers and Medical Devices

Application of Polymers in Manufacturing of Integrated Circuits

Polymer Nanocomposites

Polymeric Semiconductors for Thin-Film Electronics

Confinement Effects on Relaxation Properties of Polymers

Bionanotechnology – The Interface Between Biology and Polymer Science

Toward Noninvasive Delivery and Diagnostics: Proteins, Genes and Cells

Awards

Others

74

38

156

85

41

66

42

51

52

33

22

11

33

37

27

31

8

23

142

Table 2 Polymer-related papers reported at ACS National Meeting (San Diego) in March 2005.

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mimetic Polymers”, “Degradable Polymers and Materials”,and “Smart Polymer Films, Composites, and Devices”. Forspecial sessions at PMSE, “New Concepts in PolymetricMaterials”, “Polymers and Medical Devices”, “Applicationof Polymers in Manufacturing of Integrated Circuits”,“Polymer Nanocomposites”, “Polymer Semiconductors forThin-Film Electronics”, “Confinement Effects on Relax-ation Properties of Polymers”, “Bionanotechnology – TheInterface Between Biology and Polymer Science”, and“Toward Noninvasive Delivery and Diagnostics: Proteins,Genes and Cells”. Table 2 lists the numbers of papersreported.

From the titles of the sessions at the POLY divisions,polymer materials are clearly important elements for nan-otechnologies and as infrastructure materials indispensablefor the environment, safety, and medicine. From the ses-sions at the PMSE divisions, polymer materials are closelyrelated to various industries, such as IT, biotechnology, anddevices.

5. Conclusion

Despite several uncertainties regarding the current situa-tion, the numbers of papers reported at R&D sessions ofcompanies and academic societies suggest that polymermaterials are steadily gaining in importance. From the out-set, polymer science has grown in harmony with chemistry

and materials. Before the emergence of biotechnologiesand nanotechnologies, polymer materials spanned manyother fields in order to establish the current solid positionas infrastructure materials. These features of polymer mate-rials will not change regardless of the future direction ofscience and technology. In other words, polymer materialswill remain important for supporting sustainable growth byresolving various problems concerning the environment,safety, health, and energy.

Lastly, the major terms identified in the current surveyof research trends are the following: (1) Bio-based materialdesign, (2) Nanocomposites, (3) Microstructure control ofcapsules and coatings, (4) Optical materials and new cata-lysts, (5) Reduction of environmental load, (6) Organicgrowth, and (7) Quick rise of crude oil price. These will beimportant keywords when considering the future of poly-mers.

References

1) January 2005 and March 2005 issues of “KOBUNSHI” of TheSociety of Polymer Science, Japan (Guide to the 54th AnnualMeeting of The Society of Polymer Science, Japan).

2) January 10, 2005 issue, February 21, 2005 issue, and July 18, 2005issue of “Chemical & Engineering News” of the AmericanChemical Society (Guide to the 229th ACS National Meeting).

3) Statistical materials from “KOBUNSHI DOYUKAI” of TheSociety of Polymer Science, Japan.

1. Introduction

In order to construct nanoelectronics which will supportan advanced information and communications-orientedsociety, nanostructures having atomic-level precision mustbe widely used. To achieve this, it is necessary to addressnot only the locality of measurement but also the enlarge-ment of circuit size as circuit density increases. Nanoscalequantum phenomena need to be detected using advancedinstruments and techniques to support the development ofnanodevices and integrated circuits. Research in an inter-disciplinary field of biotechnology and nanotechnologywill flourish in the future, but its success or failure dependsupon the development of nanoscale measurement technolo-gies which can be applied to biomaterials.

2. Research trends

The widely-used instruments having atomic-level spatialresolution are the electron microscope (EM) and scanningprobe microscope (SPM). Nanomeasurement using an EMhas been established for evaluating synthesized materials,and is also widely used in industries. However, there isnow fierce competition to develop ultrahigh resolutionimaging and elemental analysis at the monoatomic leveland a next-generation nanomeasurement technology con-cerning light elements such as carbon. An SPM-relatedtechnique achieves interesting nanomeasurements, since italso enables us to create ultimate materials by manipulatingatoms one by one (an atom manipulation technology). Thepurposes of nanomeasurement by a proximity probe varywidely, and the detection of electric, magnetic, optical,dynamic and chemical nano-scale properties has been real-ized. Therefore, various probe microscopes such as thescanning tunneling microscope, atomic force microscope,scanning near-field optical microscope and scanning mag-netic-force microscope have been developed. However,SPM technologies for measuring magnetic and chemicalinformation on the nanometer scale have not yet been ade-quately developed, and much R&D in this field is expectedin the future. One of the technological trends is to convertan SPM into a multiple-scanning-probe microscope(MPSPM). SPM manufacturers in Japan and abroad as well

as research groups and organizations around the world suchas IBM, Pittsburgh University, Tokyo University, ToyotaUniversity of Technology, and NIMS are working hard onthis conversion. Since the application of individual nanos-tructures to devices has not reached full-scale practicalimplementation yet, an MPSPM measurement technologyis still at the research stage before practical implementa-tion.

3. Situation and trends of NIMS

Concerning nanomeasurement using an electron micro-scope, NIMS has been carrying out a variety of distinguish-ing development activities, such as the development of anelectron microscope for realizing elemental analysis at theatomic scale, and an ultrahigh resolution electron micro-scope. NIMS is also establishing an Internet electronmicroscope environment. Regarding nanomeasurementrelated to a scanning probe microscope, NIMS has alsoproduced a remarkable outcome in developing and operat-ing an instrument using an extreme field control technolo-gy, as will be described later in this chapter. Moreover,NIMS has succeeded in converting an SPM into a MPSPMahead of any other country, and is the only research insti-tute that has completed several MPSPMs which allowentirely independent driving in two to four scanningprobes, enabling nanomeasurements such as length-depen-dent electrical resistance measurement of individualnanowires, which was impossible in the past. NIMS is alsoconducting research (entrusted by the Ministry of Educa-tion, Culture, Sports, Science and Technology) on an inte-grated control system for multiple-scanning-probe instru-ments that assumes a variety of multiple-scanning-probemeasurements in the future.

4. Conclusion

The scanning tunneling microscope and atomic forcemicroscope have established the basis of nanotechnologytoday because they can deal with various materials. How-ever, the recent nanomeasurement work tends to focus onassessing particular materials and to lack generality. If

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Chapter 12. Analysis and Assessment Technology

Section 1. Nanoscale Measurement

Tomonobu NakayamaElectro-nanocharacterization Group, Nanomaterials Laboratories, NIMS

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researchers continue to develop techniques only for indi-vidual materials, it will become difficult to use researchresources effectively. It is thus necessary to developnanomeasurement instruments and techniques having gen-erality and versatility. Researchers also need to study anddevelop a nanomeasurement technology which can be usedfor assessing a large-scale integrated circuit built up with

precision at the atomic level, and which can be used forassessing biomaterials. The multi-probe measurement tech-nology will become a nano-manufacturing and measure-ment technology that offers even greater precision andscale, beyond the framework of individual nanomeasure-ment, by developing a multiprobe into a superparallellarge-scale multiprobe.

1. Introduction

In recent years, technology for analyzing and assessingthe size effect and quantum effect peculiar to extremelysmall areas has become important as research on sub-stances and materials at the nano-level has stepped up.Much of the new functionality of nanodevices and nanoma-terials is a quantum-mechanical effect that typicallyappears in an extreme-field environment combined with anultralow temperature, a high magnetic field, or an ultrahighvacuum. Since thermal disturbance decreases in an ultralowtemperature environment, a quantum effect in which anelectron wave is involved can be clearly measured. Forexample, the interference of a low-dimensional electronwave, the Kondo effect, a single electron effect, inelastictunneling phenomena, and so forth can be measured. Ahigh magnetic field plays an important role in spin control,superconducting state control, Landau quantization obser-vation, etc. An ultrahigh vacuum environment is essentialfor creating clean surfaces at an atomic level andmonoatomic manipulation. In order to clarify the precisemechanism by which a quantum effect due to an extremelysmall structure appears and to verify new useful functional-ity, a physical-properties measurement technology by ananoprobe in a combined extreme-field environment whichis precisely controlled is required. Physical quantities andnano-information to be measured include: atomic structure,local density of states (LDOS), band structure, a Fermi sur-face, spin, interatomic force, magnetic force, friction force,potential, work function, photon, and atomic vibration.Such measurements of physical quantities and quantum

effects on a nano-scale under such a combined extreme-field environment by means of time resolving are expectedto boost the investigation of new nanofunctionality andphysical properties (Fig. 1).

2. Research trends

Although the transmission electron microscope (TEM)and scanning probe microscope (SPM) are important fornano-analysis, the SPM technique allows a variety of phys-ical properties to be measured and a combined extreme-field environment to be created. This section examines theresearch trend of atomic-resolution SPM measurementtechnology in a combined extreme-field environmentwhere development competition is fierce.

The most important among SPM techniques having awide range of applications are the scanning tunnelingmicroscope (STM) and the non-contact atomic force micro-scope (NCAFM). STM is a probe in a local atomic state,and can measure multiple physical properties such asLDOS, band state, tunneling electron inductive lumines-cence, spin polarization tunnel, and inelastic vibration exci-tation. NCAFM performs imaging by scanning a probe or aspecimen while controlling the approach distance using aprobe top atom and a specimen surface atom. Like STM,NCAFM has true atomic resolution and can also be usedfor insulators. Mainly, the physical quantities of interatom-ic force, magnetic force, friction force, potential, workfunction, etc. can be measured. SPM can be downsizedcomparatively easily, and can measure so many physicalproperties and functions that its application to combinedextreme-field environments has been developed in SPM-leading countries since the latter half of the 1990s.

Japan, the US and Germany are leading other countriesin the development of an ultralow temperature, strong mag-netic field and ultrahigh vacuum STM, and an atomic-reso-lution image in a temperature range of 1 K or less has beenobtained by a 3He cryostat or dilution-refrigerating methodin these countries. In the US, for example, Davis and hisgroup succeeded in developing an ultralow temperature (15mK) and strong magnetic field (9 T) STM based on a dilu-tion-refrigerating method, and has been using it to clarifythe superconducting state. In Germany, Wiesendanger andhis group completed an ultralow temperature (300 mK) and

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Spin controlSuperconducting control

Landau level

Ultraclean surfaceAtomic manipulation

Molecular manipulation

Nanoprobe

Interference of an electron waveKondo effect

Single electron effectInelastic tunneling phenomenon

Photon

Interference effect ofan electron wave

Time axis

Single spin

Fig. 1 Investigation of functional physical-properties by extreme-fieldenvironment nanomeasurement.

12 Analysis and Assessment Technology

Section 2. Extreme Field Measurement

Daisuke FujitaExtreme Field Nano Functionality Group, Nanomaterials Laboratories, NIMS

strong magnetic field (14 T) STM based on a 3He cryostatmethod in 2004, and are using it to clarify spintronics andLandau quantization. In the development of an NCAFM ina combined extreme-field environment, on the other hand,Japan, Switzerland and Germany are leading other coun-tries. An ultralow temperature at a 5 K level, strong mag-netic field and ultrahigh vacuum NCAFM based on a Hecryostat method have been developed. In Switzerland, forexample, Güntherodt and his group of Basel Universityhave succeeded in developing an ultralow temperature (6K) and strong magnetic field (7 T) NCAFM, and haveachieved measurement by an atomic-resolution NCAFMand a magnetic force microscope (MFM). In Germany,Wiesendanger and his group have succeeded in developingan ultralow temperature (5.2 K) and strong magnetic field(5 T) NCAFM.

Concerning Japanese progress in SPM nano-analysis incombined extreme-field environments, STM is introducedbelow first. In Japan, leading research on an atomic-resolu-tion STM technology combined with three extreme-fieldenvironments of ultralow temperature, high magnetic fieldand ultrahigh vacuum is being carried out in Tokyo Univer-sity and NIMS. Fukuyama and his group of Tokyo Univer-sity have developed an ultralow temperature (126 mK) andstrong magnetic field (6 T) UHV-STM based on a dilution-refrigerating method, and have used it to investigate nano-materials at a low temperature level. On the other hand,Morita and Sugawara and their group of Osaka Universityhave been taking the lead in developing an atomic-resolu-tion NCAFM in a combined extreme-field environment,and have successfully developed an ultralow temperature(5 K) UHV-NCAFM and atomic-resolution imaging.Moreover, Sugawara and others started developing anultralow temperature (5 K) and strong magnetic field (10T) UHV-NCAFM in 2001, and recently succeeded in atom-ic-resolution imaging.

The development of an extreme-field environment SPMin NIMS was started from a low temperature atomic-reso-lution UHV-STM in the 1990s. NIMS then began to devel-op an atomic-resolution STM in an extreme-field environ-ment in 2001, and has succeeded in developing an ultralowtemperature (400 mK) / high magnetic field (vertical direc-tion, maximum 11 T) / ultrahigh vacuum (in the order of10-10 Pa) atomic-resolution STM.1) NIMS has its own tech-nology called “ultrahigh vacuum creation technology,” andby combining it with a technique for creating a clean sur-face, has also succeeded in the atomic-resolution measure-ment of a surface that no other groups could observe. Inparticular, it is noteworthy that NIMS has succeeded in theatomic-resolution STM measurement of a Si (100) surfaceand an Au (111) reconstructed surface at an ultralow tem-perature of 1 K or less for the first time. NIMS has thusalready reached world-class standards in the developmentof a combined extreme-field environment STM.


Competition in high-precision SPM nano-analysis inextreme-field environments is expected to intensify in the

future as the investigation of new functionality at the nano-level and the clarification of a quantum effect will becomeimportant.

In combined extreme-field environment STM measure-ment, an atomic-resolution STM technology combinedwith extreme fields of an ultralow temperature of 0.5 K orless, high magnetic field of 10 T or more, and ultrahighvacuum of 10-8 Pa is currently the world’s highest standard.Research groups which have reached this standard exist inJapan, Germany and the US, and they are leading thedevelopment of an extreme-field environment STM mea-surement technology. In particular, the higher the magnet-ic-field intensity, the more likely that new materials andfunctionality will appear, and so development competitionin this area will continue. Since NIMS has a high magneticfield, it is in an advantageous position compared with otherresearch institutes. Another important technology to bedeveloped is an ultrahigh vacuum environment and a high-precision tunneling spectroscopy measurement technology.

Meanwhile, an extreme-field environment NCAFM isbeing developed mainly in Japan, Switzerland and Ger-many, but no research group is currently attempting suchan extreme-field environment that would be required forSTM. This is partly because atomic-resolution measure-ment by an optical method NCAFM involves very complextechnology in an extreme-field environment. If a simplenew high-resolution probe is developed, then developmentof an extreme-field environment NCAFM will surely takeoff. If atomic-resolution measurement similar to that bySTM can be accomplished by a combined extreme-fieldenvironment NCAFM, then it will be possible to measuremultiple physical properties and functionality of the surfaceof various substances including insulators.

4. Conclusion

Concerning measurement technology in extreme-fieldenvironments, this section has outlined mainly an atomic-resolution SPM measurement technology in an ultralowtemperature, high magnetic field and ultrahigh vacuumenvironment where there is global development competi-tion is intense. In order to develop such a highly-advancedmeasurement technology, precision measurement andextreme-field environment creation technologies are indis-pensable, thus testing overall technical capabilities. Such aworld-class measurement technology would be a powerfultool for clarifying how the functions of nanostructuresappear and the mechanisms of their physical properties,and may lead to the discovery of entirely new nano-func-tionality and quantum effects. For such new “creation ofintelligence,” international cooperation is vital, and aninternational core-research institute for substances andmaterials should take the lead in this particular field ofR&D.

References

1) Daisuke Fujita and Keisuke Sagisaka, Microscopy, 40, 14 (2005).

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1. Introduction

In spectroscopies in which electrons are used for theincident probe or detected signals, such as in surface elec-tron spectroscopy (including Auger electron spectroscopy(AES), and X-ray photoelectron spectroscopy (XPS)), elec-tron probe microanalyzer (EPMA), secondaryelectronmicroscope (SEM), many researchers are trying to expandfrom two-dimensional analysis to three-dimensional analy-sis. Depth direction analysis with ion sputtering and speci-men depth analysis in which a cross-section is made byfocused ion-beam (FIB) used to be the mainstream, butnow research is focusing on the method of inferring thethree-dimensional composition and structure of the neigh-borhood of a surface from small changes in an observedspectrum (such as the shape of a peak and background) anda two-dimensional image. While many materials are madein complex shapes at the nano-level today, researchers aretrying to assess the structure and characteristics of materi-als through three-dimensional simulation of spectra andimaging after clarifying the structure and characteristics ofmaterials. In order to identify the two-dimensional andthree-dimensional elemental distribution and structureaccompanied with metrological “uncertainty” from spec-trum measurement, modeling based on precise findings asto the exact physical quantity which describes the interac-tion between electrons and solid, and its transport phenom-enon is required.

2. Present status of physical quantity databases

In spectroscopy using a low-energy electron as an inci-dent probe, it is conventional to trace a multiple scatteringprocess of electrons and to clarify the interaction thereofbased on the Monte Carlo (MC) method. This methodrequires: (a) elastic scattering cross section, (b) inelasticscattering cross section, and (c) stopping power. For EPMAand SEM, (d) inner-shell ionization cross section, (e) fluo-rescence quantum yield, and (f) secondary electron yieldare also required. In reality, the elastic scattering databaseof (a) in which a free atom is calculated using the Dirac-Hartree-Fock potential has been published by NIST, and isreplacing the previous elastic scattering database in which afree atom is calculated using the Thomas-Fermi-Dirac

potential. However, problems remain as to its accuracyunder 1,000 eV. The inelastic scattering database of (b),which is calculated from the general equation TPP – 2M orthe optical dielectric functions, are commonly used, but ithas not yet been fully verified based on comparisons withexperimental values. In particular, the importance ofexchange correction in a low-energy region has been point-ed out, but this has not been taken into consideration in theabove mentioned calculatiens. In the stopping power of (c),the Bethe equation ia used over 10 keV, but there is no def-inite database for the range under 10 keV. Concerning (f)which is important for SEM quantitative analysis, the vari-ation of secondary electron yield is so large (reachingaround 200%) that it has become a serious problem. Otherdatabases for the low-energy range have not been suffi-ciently established either, and so simulations lack accuracy.

3. Development of a simulator

For SEM, the accurate measurement of length is essen-tial in industry. An electron beam of 200 eV or less is con-sidered desirable to reduce the edge effect. Since it is diffi-cult to calculate such a low-energy region with high accu-racy by the MC method, effective modeling of this area hasbeen studied, and it has been pointed out that it would bemore effective to use a elasfic scathering electron whichcan easily control depth than a secondary electron.

On the other hand, the spectrum simulators* of the AESand XPS, which have lately been developed assuming thethree-dimensional structure, can be produced the shapes ofmain peaks and the background of photo-electrons eventhough they could be applied to the limited systems andelements. However, AES spectra have a problem for pre-dicting the shape of a peak. In reality, the surface excitationeffect and elastic scattering effect, which greatly affectspectra, cannot be adequately included for electron trans-port modeling, and it is difficult to use the spectrum simu-lator in practice because the system is limited and quantita-tive accuracy is not enough. At present, the spectrum simu-lator can be used only for depth-direction analysis of ele-ments. It is possible, however, to calculate a combined highlevel of physical quantity of a transport cross section whichis required for electron spectroscopy, and it is useful as adatabase for basic physical quantities of surface analysis.

181



Section 3. Electron Transport Modeling in Surface Analysis

Shigeo TanumaFundamental Chemical Analysis Group, Materials Analysis Station, NIMS

*SESSA (NIST SRD 100), QUASES (http://www.quases.com)

References

“Workshop on Modeling Electron Transport for Applications inElectron and X-ray Analysis and Metrology,” Abstracts, NIST(November 2004).

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1. Introduction

A transmission electron microscope (TEM) is indispens-able and one of the most widely used tools for research onnanomaterials in view of its capability of not only atomicresolution imaging in real space but also simultaneousanalyses of structure and composition in the sub-nanometerarea. One of the key characteristics of nanomaterials is thatthey have unique structures and physical properties differ-ent from those of the bulk, and so analyzing such structuresand physical properties at high resolution and high preci-sion allows nanosubstances and nanomaterials to be accu-rately controlled. Today, the development of next-genera-tion TEM technology is focusing on enhancing the resolu-tion and precision of the TEM itself, adding a function of insitu measurement of nano-physical properties, and develop-ing it into a three-dimensional characterization technology.This section summarizes research and development for:improving the resolution and precision of the TEM; a tech-nology for analyzing in situ nano-physical properties; and atechnology for three-dimensional characterization.

2. Research trends

2.1 Improvement of high resolution and high precision ofTEM

Until around 1990, the main approach to improve theresolution of the TEM was to reduce spherical aberration indesigning the objective lens polepiece, but in the 1990sattempts were made to eliminate the spherical aberration bycomputer processing such as image processing, and anaberration correcting lens was developed around 2000.More recently, since the resolution limits of TEM havefinally reached the information limit of TEM, research onimproving the overall performance of TEM such as stabi-lization of TEM, monochromatization of the electron beam,and correction of aberration of lenses has been carried outas projects among some countries (Table 1).

Concerning the monochromatization of an electronbeam, research and development are being promoted notonly to improve the resolution but also to enhance the pre-

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TEAM project(USA, 2000 –)

Super STEM project(UK, 2000 –)

SESAM project(Germany, 1999 –)

An overall project centering on five US national research institutes (ANL, BNL, LBNL, ORNL, FSMRL). This project is not only developing a TEM but also organizing its industrial applications. The budget for the project is $100 million, and an instrumentation development contract is to be concluded with FEI (USA).

An electron microscope development project centering on a corporation (Carl Zeiss). The project is being promoted in three phases (I, II, and III), and it is in the third phase at present. Resolution of 0.08 nm was announced in 2005.

A project centering on Leeds University, Cambridge University and Liverpool University in the UK concerning enhancing the performance of a scanning TEM (STEM) and it public utilization.

Table 1 High-performance TEM development projects.

Delft University of Technology(Netherlands) + FEI Inc.

Development and application of a mono-chromator for TEM

Application of a monochromator for TEM

Development of a monochromator for TEM

Refer to Table 1.

Development of a monochromator suitablefor a scanning TEM

Tohoku University + JEOL Ltd.

SESAM project (Germany)

IBM (USA) + Delft Universityof Technology (Netherlands)

Graz University of Technology(Austria)

Table 2 Research on electron beam monochromatization.

Electron holography/Lorentz microscopy

SPM in TEM

Cathode luminescence in TEM

High resolutionwavelengthdispersive X-rayspectrometry

Quantitative measurement of electric and magnetic fields inside and outside a specimen is possible. Since the resolution is almost the same as that of a TEM, these techniques are effective for measuring physical properties such as nanodevices.

The probe can be brought into contact with a nanomaterial using piezoelectric driving, and electrical characteristics and mechanical characteristics can be measured while being observed with a TEM. The part of a specimen that is being observed with the TEM can be observed with a STM/AFM at the same time. The use of multiple probes is expected to become possible in future.

It is possible to assess luminescent characteristics while assessing a location and a defect in semiconductor nanomaterials by TEM. One problem is that the lens must contain space to accommodate a condenser mirror.

It is possible to measure valence state density by high resolution Xray emission spectrometry, but the problem of improving detection efficiency remains.

Table 3 Main functions for in situ nano-physical properties measurement.


Section 4. Advancee Transmission Electron Microscope

Masaki TakeguchiIn situ Characterization Group, High Voltage Electron Microscopy Station, NIMS

Koji KimotoHigh-resolution Characterization Group, High Voltage Electron Microscopy Station, NIMS

184


cision of chemical analyses (Table 2). Through the mono-chromatization of an electron beam, it becomes possible toknow the detailed electric state of interatomic bonding innanomaterials.

2.2 In situ nano-physical properties measurement functionMeasuring nano-physical properties inside a TEM in

addition to observing the structure and analyzing the com-position of nanomaterials allows electron microscopy toexplore the appearance of nano-physical properties usingelectron microscopy. Therefore, various functions havebeen added to TEMs in recent years. Table 3 shows themain functions for measurement of nano-physical proper-ties.

2.3 Three-dimensional characterization functionAlthough a projected image of a specimen is observed in

conventional TEM, a three-dimensional image can beobtained by using the tomography technique. Researchersare aiming to apply this TEM tomography technique tonanomaterials research by improving the resolution ofthree-dimensional imaging. Cambridge University (UK)and Arizona State University (USA) are developing the

technology of three-dimensional elemental analysis andthree-dimensional nano-physical property measurement bycombining the tomography technique with a two-dimen-sional composition map and electron holography.

3. Conclusion

High-performance and new-functional TEM willbecome increasingly important in the research of nanoma-terials. New breakthroughs in TEM instrumentation andanalytical technology have been made since 2000, and inorder to take the initiative in the research of nanomaterials,it is important to establish these fundamental and elementaltechnologies of TEM.

References

1) Transmission Electron Energy Loss Spectrometry in MaterialsScience and the EELS Atlas, 2nd ed., Ed. C. C. Ahn, John Wiley&Sons Inc., New Jersey (2004).

1. Introduction

Concerning methods of analyzing and assessing varioussubstances and materials, ISO/IEC provides internationalstandards and JIS (Japanese Industrial Standards) providesnational standards. The “Guideline for Coordinationbetween JIS and International Standards” was revised inaccordance with the revision of the ISO/IEC Guide 21(adoption of international standards as regional nationalstandards) in 1999, and work to coordinate national stan-dards is now underway.

A new criterion called “uncertainty” for indicating thereliability of measured data has been used since the 1990s.Since the concept of error and accuracy was not unifiedamong technical fields and countries, the InternationalCommittee of Weights and Measures unified the method ofassessing and expressing the reliability of measured data.The “Guide to the Expression of Uncertainty in Measure-ment (GUM)” was published in 1993. In the GUM, uncer-tain components are sought either by (1) A-type assessmentbased on ordinary statistical analysis which calculates astandard deviation, or (2) B-type assessment which infersthe size corresponding to a standard deviation from variousinformation other than data, and uncertainty as a whole isthen determined by combining these components. Theassessment of uncertainty is essential in order to complywith the standards of ISO 9000 (quality management sys-tem) and ISO 17025 (general requirements for the ability ofcalibration and testing laboratries).

2. Research trends

A primary standard assessment method is a traceableanalytical method in SI units; such methods for chemicalanalysis include the gravimetric method, coulometry, andisotope dilution-mass spectrometry. The isotope dilution-mass spectrometry adds a spike of an element to be ana-lyzed whose density is already known (which has an iso-tope composition different from the naturally occurringone) to an unknown specimen, and then analyzes its mass.This analysis method, when combined with the barium-sul-fate gravimetric method, can attain accurate results, asshown in the examples of quantitative analysis of sulfur (S)in iron and lead (Pb) in iron. Accurate quantitative analysis

of single ppm content of Si in iron and steels has beenobtained by an inductively-coupled plasma mass spectrom-etry (ICP-MS) using gel absorption and separation and anisotope dilution method. Likewise, determination of Fe andCr, which are the main components of Fe-Cr binary alloy,has also been conducted by ICP-MS. In connection withenvironmental problems, the development of an analyticalmethod without using a chlorine-based organic solventwhich is a harmful reagent has been studied, and work isunderway to develop a coprecipitation separation method,an ion exchange separation method, a solid-phase extrac-tion method, etc., so national and international standardsare being steadily reviewed.

The ISO standards concerning surface analysis were dis-cussed and established in TC201 (surface chemical analy-sis) and TC202 (microbeam analysis). The target of TC201is Auger electron spectroscopy (AES), secondary ion massspectrometry (SIMS), X-ray photoemission spectroscopy(XPS), glow discharge spectroscopy (GDS), scanningprobe microscopy (SPM), and total reflection fluorescentX-ray spectroscopy (TXRF). Not only the definition ofeach method but also the parameters, energy axis, precisionin the x, y and z axes which determine the basic perfor-mance of an instrument, and the standards concerning themethod of calibrating each instrument as well as the stan-dards concerning the method of determining a relative sen-sitivity coefficient and of using it have been drawn up. Thestandards concerning the properties which a specimenshould have and the method of selecting and using themhave also been drawn up. TC201 provides a standard con-cerning the accuracy of quantification of depth profile by asputtering method.

On the other hand, TC202 establishes standards con-cerning procedures for qualitative and quantitative analysisby a wavelength dispersive spectrometer (WDS) electronprobe X-ray microanalyzer (EPMA) and its applicability,the energy calibration and resolution of an electron energyloss spectrometer (EELS) by an analytical electron micro-scope (AES), the magnification calibration and spatial reso-lution of a scanning electron microscope (SEM), and theinstrument specifications and analytical method of an ener-gy dispersive spectrometer (EDS).

185



Section 5. Standardization of Assessment Methods

Takashi Kimura, Shinji ItohFundamental Chemical Analysis Group, Materials Analysis Station, NIMS

3. Conclusion

In recent researches, both speed and accuracy are cru-cial, and the time spent for verification experiments andanalysis has been getting shorter. In order to ensure thereproducibility and traceability of analysis results, it is nec-essary to produce guidelines concerning analysis and toclarify the targets to be analyzed and discussed. Standard-ization and the establishment of standards are thus becom-ing increasingly more important.

References

1) JSCA News, Japanese Industrial Standards, InternationalStandardization Committee for Surface Chemical Analysis (JSCA),17, 2005, pp. 1-22.

186


1. Introduction

Of the various analytical technologies which are expect-ed to greatly assist nanobiology research, national researchinstitutes should put priority on large special instruments,such as a synchrotron radiation system, high-voltage elec-tron microscope, high-field NMR system, and neutron dif-fractometer. Theses instruments have different characteris-tics, and nanobiological analysis will not be completeduntil all of these complementary analytical technologies areprovided.

Concerning the synchrotron radiation system, a high-voltage electron microscope and a neutron diffractometer,their effectiveness is already universally known. The effec-tiveness of high magnetic-field NMR lies in being able toclarify a local three-dimensional chemical structure (thegeometrical structure of a molecule, and the kind and sizeof a chemical bond) even for substances which other ana-lytical technologies are not suitable for, such as amorphousmaterials and compounds. There are many important prob-

lems that can be solved by high magnetic-field NMR insuch fields as catalysts, glasses, slag, fuel cells, solar cells,and living substances.

It has long been known that NMR is theoretically advan-tageous for analyzing amorphous materials and com-pounds. However, since NMR used to have only a lowmagnetic field, its effectiveness was limited to particularsubstances such as organic substances. When a magneticfield of 20 T or more became possible, the effectiveness ofNMR rose dramatically. While NMR should be able to ana-lyze 90% of the elements in the periodic table, its magneticfield was so low in the past that it could not analyze morethan three elements such as hydrogen and carbon (Fig. 1).

2. The trend of high-field NMR

NMR is a striking analytical technology that has pro-duced five Nobel Prize winners, and yet it still involvesmany cutting-edge developments and is still beingimproved. The sixty-year history of NMR is the history ofproducing a high magnetic field with a magnet (Fig. 2), andeach increase in magnetic field has led to an innovation inNMR. When the electromagnet (2 T) was changed to asuperconducting magnet (5 T) about 40 years ago, itbecame possible to use NMR for chemical analysis (struc-tural analysis of low molecules). When the 10 T supercon-ducting magnet based on Nb3Sn was achieved about 20years ago, the structural analysis of protein became possi-ble. In today’s ultra-20T era, even inorganic substances canbe analyzed for the first time. This is because the high reso-lution measurement of quadrupole nuclei which are neces-sary for analyzing inorganic substances can be achieved forthe first time by a high magnetic field of 20 T or more.

Today, 40 T-class magnetic fields are feasible by using ahybrid magnet. In the US, France, and the Netherlands, themain purpose of developing high magnetic-field magnetsincluding hybrid magnets is for the analysis of nanobiologi-cal materials by high magnetic-field NMR.

187


Fig. 1 90% of the elements of the periodic table can be analyzed byNMR (blue, red and yellow in the drawing). However, only threeelements (H, C and N) can be analyzed by conventional NMR. 75% ofthe elements which can be analyzed by NMR are quadrupole nuclei (redin the drawing). Quadrupole nuclei can be analyzed only by highmagnetic-field NMR.

Chapter 13. High Magnetic-Field GenerationTechnology and Its Applications

Section 1. The Aim of Developing a High Magnetic Field

NMR Facility

Tadashi ShimizuNMR & Chemistry Group, High Magnetic Field Center, NIMS

188


A high magnetic field is required not only for NMR butalso for MRI and the analysis of various physical proper-ties. However, since these applications are limited to funda-mental research fields, the market is too small to drive thedevelopment of high magnetic-field magnets. Instead, mag-nets for NMR require higher performance than magnetsused for other purposes, and so if such magnets can bedeveloped, they may be applied to other fields. Developinga high magnetic-field NMR is the most effective way ofpowering the overall development of magnets.

3. Future development and conclusion

General users who require a conventional NMR magnettypically cannot afford to purchase a high magnetic-field

NMR magnet because of the huge costs required for devel-oping and maintaining such magnets. Instead, it would bemore appropriate to install a high magnetic-field NMRmagnet in one or two research facilities in Japan and makethem available to domestic users.

The highest-risk technology in developing high magnet-ic-field NMR is the magnet. The High Magnetic Center ofNIMS is the only high magnetic-field institution having allkinds of magnetic-field generation instruments such asultra-20 T superconducting magnets (930 MHz, 920 MHz)and a 40 T-class hybrid magnet. In order to develop thetechnical basis of NIMS in the most efficient manner,NIMS needs to develop a system including a group ofdevices based on the magnets as a core. The NMR facilitieswith high magnetic-field magnets of NIMS are expected tobe useful for researchers engaged in nano-research in uni-versities and industry.

The main magnet to be developed is a high magnetic-field magnet such as a power-source driving type supercon-ducting magnet (1.2 GHz class) and a hybrid magnet (1.5GHz class). In terms of the strength of magnetic field, ahybrid magnet is more advantageous, but in terms of thedevelopment and maintenance cost, a power-source drivingtype superconducting magnet is more suitable when usedexclusively for NMR for a long time. Hybrid magnets willlikely be used only for materials which cannot be analyzedin a lower magnetic field.

Since the magnetic field of these new-type NMR mag-nets is less stable than that of superconducting magnets ofpersistent-current operation by at least one order of magni-tude, it is necessary to develop a technology that allowshigh resolution NMR measurement even when the magnet-ic field is not so stable. Such a technology has two aspects,that is, developing equipment for making a magnetic fieldstable, and the software aspect of developing the measuringtechnique. As these peripheral technologies are notrequired for low magnetic-field magnets which are wide-spread among general users, they must be independentlydeveloped in NIMS.

High magnetic-field NMR may soon become as wide-spread as today’s synchrotron radiation and neutron dif-fraction.

1000

Hybrid magnetUSA – 40 TNIMS – 35 T

17.5T magnetin NIMS

920 MHz,21.6 T magnet

in NIMS

Superconductingmagnet

Electromagnet

5.5 T magnet in the US

100

Mag

netic

fiel

d (N

MR

freq

uenc

y M

Hz)

Year1950 1960 1970 1980 1990 2000 2010

Fig. 2 History of NMR magnet.

1. Introduction

MRI (Magnetic Resonance Imaging) uses an NMR phe-nomenon, and by dividing an object to be analyzed intosmall volume elements and incorporating a technique forsimultaneously analyzing from which element a signal isobtained, MRI carries out imaging at an arbitrary slicedplane of the object. The Nobel Prize in Physiology or Med-icine of 2003 was awarded to P. Lauterbur and P. Mans-field for their development of the magnetic resonanceimaging technique.

MRI has the advantage that the inside of the brain,spinal cord, etc. can be clearly diagnosed because MRIcauses no radiation exposure and is not affected by bone orair. In Japan, more than 500 MRI instruments are at workin hospitals and the like. Today, there is a trend toward spe-cialization in two types of MRI. One type uses a donut-shaped superconducting magnet which generates 1.5 T, andthe other type is called “open MRI” and uses an inexpen-sive permanent magnet of about 0.3 T, which is designed toavoid stress during diagnosis.

2. Merits of high magnetic fields

Theoretically, the sensitivity of NMR increases in pro-portion to the power of 3/2 of the magnetic field. It is pos-sible to improve the S/N ratio of an image and make animage finer by increasing the magnetic field. Accordingly,the Ministry of Health, Labor and Welfare has alreadygiven its approval for an MRI instrument using a 3 T mag-net, which is now being introduced for clinical diagnosis.

Almost all conventional MRI instruments are used foranatomical morphological measurement (distribution ofwater states by measurement of 1H), but MRI is expected tobe used for functional measurement as well in the future,and so the development of a high magnetic-field MRIinstrument is now being promoted. In MRS (Magnetic Res-onance Spectroscopy) which analyzes metabolism usinginformation concerning chemical shifts, the nuclei that playan important role for metabolism such as 31P and 13C can bemeasured as the magnetic field increases. In fMRI (func-tional MRI) which is used to observe susceptibility changes

in blood flow in the brain occurring due to a stimulus, amap of the active part of the brain is made. The susceptibil-ity effect increases with magnetic fields. High-field MRI isbeing used mainly to clarify brain functions at present.

3. Global trend

A 7 T whole-body MRI instrument has been installed inthe Brain Research Institute of Niigata University in Japan.In the US, high-field MRI instruments have been activelyintroduced, and 7 to 8 T whole-body MRI instruments havealready been installed in a number of leading institutes. A9.4 T (400 MHz in the resonance frequency of 1H) MRIinstrument that features the highest magnetic field availabletoday has been installed in the University of Illinois andUniversity of Minnesota.

In France, the construction of “NeuroSpin” (IntenseField Neuro-Imaging Center) is being promoted by CEA(Commissariat à l’énergie atomique).1) Under this plan, theIntense Field Neuro-Imaging Center is built within thepremises of CEA Saclay near Paris, in which today’s highest-level MRI technologies including magnets are to beinstalled, and these MRI technologies will be used forresearch of human brain functions. Although the plan isflexible, the original plan includes the following.• 3 T wide bore MRI for clinical studies• 11.7 T (500 MHz) wide bore MRI for clinical studies• 11.7 T MRI for anaesthetized and awake monkey studies• 17 T small bore MRI for rodent studies

4. Materials development for high-field MRI

The field quality almost equivalent to that of an NMRspectrometer is required for the superconducting magnet ofwhole-body MRI, but the space required to generate a mag-netic field quite differs between the two. An NMR spec-trometer generates a magnetic field in a space of 51 to 89mm in diameter, whereas a whole-body MRI instrumentneeds to generate a magnetic field in a space of 0.7 to 1 min diameter, which is about ten times as large. As a result,the stress applied to the superconducting conductor increas-

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13 High Magnetic-Field Generation Technology and Its Applications

Section 2. Development of High-Field Whole-Body MRI

Tsukasa KiyoshiMagnet Development Group, High Magnetic Field Center, NIMS

es. NMR spectrometers had reached a turning point for the11.7 T (500 MHz) NMR spectrometer, by using Nb3Snconductor which has excellent high-field characteristics inaddition to NbTi conductor which has excellent mechanicalcharacteristics. For the 11.7 T MRI instrument, it has yet tobe decided whether to use only NbTi conductor by employ-ing superfluid helium cooling, or a combination of otherconductors such as Nb3Sn conductor. However, NbTi con-ductor cannot be used in magnetic fields over 12 T byitself, so Nb3Sn and Nb3Al conductors which haveimproved mechanical characteristics need to be developed.

References

1) http://www.meteoreservice.com/neurospin/

190


1. Introduction

Mass spectrometry is a fundamental analytical techniquethat has been used in a wide range of research fields suchas atomic and molecular science and gas analysis. In recentyears, it has been used for the analysis of biological mole-cules such as proteins and nano-clusters such as fullerene,and has become an indispensable analytical technique inthe fields of biological science and nanotechnology. Thissection describes mass spectroscopy as an application of ahigh magnetic field.

2. Research trends

As the applicability of mass spectrometry expands tosubstances whose mass is large and which have a compli-cated structure, the mass resolution and mass range whichcan be analyzed need to be improved. In mass spectrome-try, a gas substance to be analyzed is ionized and mass isdetermined from its mass-to-charge ratio (m/z). For themeasurement of mass-to-charge ratio, various techniquessuch as time-of-flight mass spectrometry (TOF-MS) andquadrupole mass spectrometry (Q-MS) are used, but thedevelopment of Fourier transform ion cyclotron resonancemass spectrometry (FT-ICR) has been promoted in recentyears because it can, theoretically, obtain high mass resolu-tion in comparison with other techniques. In FT-ICR, anionized gas sample is introduced into a magnetic field andis run under cyclotron motion (circular motion). When ahigh-frequency voltage conforming to the frequency ofcyclotron motion is applied from outside, the ion absorbsenergy, and the revolution radius of the motion increases.Since the frequency of cyclotron motion differs accordingto the mass-to-charge ratio of the ion, the mass-to-chargeratio can be measured by detecting the absorption of thehigh frequency voltage. The mass resolution in FT-ICRimproves in accordance with the increase in strength of themagnetic field used. Mass spectrometers using 5 T to 10 T-class superconducting magnets have been developed inJapan and the US and are already in use.1), 2)


As the importance of mass spectrometry in biologicalscience and nanotechnology has rapidly risen, manyattempts will be made to improve the performance of FT-ICR. In fact, the Korean Basic Science Institute hasannounced the joint development of an FT-ICR spectrome-ter using a 15 T-class superconducting magnet (aiming atcompletion by 2007) with the US National High MagneticField Laboratory (in Tallahassee, Florida).3)

Meanwhile, the High Magnetic Field Center of NIMShas developed a high-magnetic-field TOF-MS spectrometerwhich is a TOF-MS spectrometer built into the bore of asuperconducting magnet. FT-ICR is mass spectrometryusing a magnetic field, whereas high-magnetic-field TOF-MS is mass spectrometry of a substance under a magneticfield. Since this spectrometer (TOF-MS spectrometer) cancarry out both mass spectrometry and spectroscopic mea-surement in a high magnetic field at the same time, it ispossible to perform mass-selected spectroscopy of a sub-stance in a high field. The high-magnetic-field TOF-MS isexpected to be developed further as a new measuring tech-nology for observing a high-magnetic-field effect on bio-logical molecules and nanomaterials.

4. Conclusion

The importance of mass spectrometry in fundamentalscience is clear from the fact that two Nobel Prizes wereawarded for research achievements in this field in the pastten years.4), 5) Mass spectrometry is considered to be one ofthe most important applications of a high magnetic field toanalytical technology.

References

1) S. Maruyama, L. R. Anderson, R. E. Smalley and Rev. Sci.Instrum., 61, 3686 (1990).

2) A. G. Marshall and Int. J. Mass Spectro., 200, 331 (2000).3) Homepage of National High Magnetic Field Laboratory

(http://www.magnet.fsu.edu/).4) 1996 Nobel Prize in Chemistry (Discovery of fullerene).5) 2002 Nobel Prize in Chemistry (Analytical method of

biomolecules).

191


13 High Magnetic-Field Generation Technology and Its Applications

Section 3. Mass Spectrometry

Ken TakazawaNMR & Chemistry Group, High Magnetic Field Center, NIMS

1. Introduction

The peak performance of the Earth Simulator, the fastestcomputer in Japan, is 40 TFLOPS (40 tera floating opera-tions per second). It was ranked as the fastest computer inthe world, but recently fell to the third following the BlueGene (91 TFlops) and Columbia (60 TFlops) in the US.Such rapid increase of the computer speed makes us possi-ble to perform larger and more accurate simulations in thecomputational materials science, and our targets are nownot only simple atoms, molecules or solids, but also morecomplicated systems having so-called “nano-scaled” struc-tures.

In Fig. 1, several computational methods in materialsscience are shown and categorized with respect to the sys-tem size and time-scale of the phenomena of our targets.They are first-principles calculations, which consider theelectronic structures as well as the atom movements; classi-cal molecular dynamics (MD) and Monte Carlo simulations(MC), which treat the collective motion of the atom or mol-ecules; finite element methods (FEM) and statistical ther-modynamics calculations, whose targets are bulk materials;and the phase-field method which deals with meso-scalesystems connecting between micro and macro.

Today’s information and communications based societyis built on silicon technologies. Many researchers predictthat we will have a problem of reaching the limit of down-sizing in the near future. The target we need to work on isin the nano-scale region, which requires micro analysis and

control and in which unknown functions are being investi-gated. As the phenomena in this area cannot be clarified byexperiments only, there are great expectations for computa-tional science to employ the efficient way of research. It isexpected that simulations would first predict the phenome-na in this region, and then, for selected targets, experimen-tal verification would be made. This section describes thepresent situation and outlook for simulation techniqueswhich are the key to the computational science.

2. First-principles simulation

The electron wave function, which determines the natureof a material, is governed by Schrödinger’s equation. Itused to be difficult to solve Schrödinger’s equation of amulti-electron system numerically. The Density FunctionTheory (DFT) proposed by Hohenberg and Kohn in 1964,shows that the ground state of a system can be described bya total electron density instead of multi-electron wave func-tions and that the problem can be ascribed to a single elec-tron problem.1), 2) DFT enables us to get the electronicstructure from the atomic information alone, and calcula-tions based on this theory are called first-principles simula-tions. Due to the development of a linearization technique,pseudopotential methods, etc. and the improvement ofcomputing power in recent years, it has become possible toprecisely calculate the electronic structures of several hun-dred atom systems. For the exchange-correlation part, amore accurate method such as the Generalized GradientApproximation3) (GGA) has been developed instead of theoriginal Local Density Approximation (LDA) from about1990, and theoretical predictions have become possible forstrongly correlated systems, such as ferromagnetic materi-als, molecules and so on.

For strongly correlated systems, quantum Monte Carlomethods which directly solve multi-electron wave func-tions numerically using Schrödinger’s equation have beenproposed, and the variational Monte Carlo method, the dif-fusion Monte Carlo method, etc. have been developed. Inthe variational Monte Carlo method,4) the electronic struc-ture of a multi-electron system is approximated by a wavefunction including an adjustment parameter, and the adjust-ment parameter is optimized by the variational method tocalculate the total energy. The diffusion Monte Carlomethod deals with Schrödinger’s equation of a multi-elec-tron system with an imaginary time. In the time evolution

192


Tim

e

Macro-scaleFinite element methodStatistical thermodynamics method

Meso-scalePhase-field method

Cellular automaton method

Atomic-scaleMolecular dynamics methodMonte Carlo method

Atomic stateQuantum mechanics

Space

Fig. 1 Time and space scales of computational science.

Chapter 14. Nanosimulation Science

Takahisa Ohno, Xiao Hu and Hidehiro OnoderaComputational Materials Science Center, NIMS

of an imaginary time, the ground state of the multi-electronsystem is obtained using the fact that any arbitrary initialwave functions converge to the ground state after a longtime simulation. Maezono and co-workers5) have appliedthis technique to the metallic Na and obtained more accu-rate cohesive energy and the bandwidth than those obtainedby the LDA calculation.

Towards the large-scale simulations, order-N methods,hybrid methods, and so forth have been proposed since the1990s. Nano-scaled materials, such as DNA and biomole-cules, contain several thousand atoms or more. However, itwas difficult to apply conventional first-principles simula-tion techniques to such a large system including more thanseveral hundred atoms because the computational timeincreases as N3 with the number of atoms N in the system.The order-N method is a computational technique in whichthe computational cost is proportional to the number ofatoms N, and so offers great potential for large-scale simu-lations. Order-N methods can be classified into two kinds.One is the moment expansion method, which includes theFermi operator expansion method and the Bond orderpotential method, and the linearity of computational cost isachieved by using a finite number in the moment expansionof energy or force. The other is based on the variationalprinciple, which includes the density matrix method6) andthe localized orbital method.7) Linear scaling is achieved byusing localization of a density matrix and the Wannierfunction. Recently, Miyazaki and Ohno have started toapply the order-N method based on the density matrixmethod to an actual system, and proved the possibility ofits application to a Ge cluster-system (including about10,000 atoms) on the surface of Si (001). We expect theorder-N method can be used for various fields such as thesurface nanostructures, catalytic activity of a metallic clus-ter, and oxygen reaction of a biomolecule.

The hybrid method is one of the multi-scale techniques.The method divides a large system into several regions spa-tially, applies a most suitable technique for each region,and analyzes the whole system simultaneously. For aregion requiring analysis of electronic state, we apply thefirst-principles MD or the Tight Binding (TB) MD meth-ods. For a region in which there is little change in electron-ic state and sufficient description by classical interatomicpotential is possible, the classical MD method is applied.We can use the finite element method for a macro regionwhere the continuum approximation is sufficient. In orderto seamlessly merge the different techniques at the bound-ary of different regions, several connecting schemes have

been proposed. The hybrid methods have been applied tovarious systems, such as the mechanical characteristics ofcrack propagation, dynamical process to the surface, oxy-gen reaction in a biomolecule system, etc. Ohno andTateyama recently made public their Quantum – ClassicalHybrid Method Program, CAMUS.

For nano-scaled materials, it is extremely important toanalyze and predict the physical properties and their func-tionalities, and to clarify the relationship between the struc-tures and the functionalities. This is the key for the advanceof the nanotechnologies. Electron transport is one of theimportant functions displayed by nanomaterials. In aCMOS transistor, the thickness of the SiO2 insulating gatefilm is only several nm (nanometer), and leakage currentthrough the film causes a serious problem. In addition, theuse of single molecules or atomic wires has been proposedto make electronic devices smaller. For the numericalanalysis of electron transport, we need a theoretical tech-nique to treat the electronic structure in an open system,which is different from the usual one for periodic systems.For this, the method using the Lippmann-Schwinger equa-tion and the method using the Non Equilibrium GreenFunction (NEGF) have been proposed. Nara and Ohnodeveloped the Lippmann-Schwinger method8) and theNEGF method,9) and have investigated the properties ofelectron transport in an atomic wire, nanotube, organicmolecule, and so on. They have clarified the dependence ofthe conductance upon the point-of-contact structure as wellas on the electrode materials. On the other hand, Kino andOhno10) calculated the electronic state of DNA and haveshown theoretically that when hydrating water is removed(dried) from metallic ions, such as Mg and Zn around aDNA chain, positive-hole carriers are introduced into theDNA chain, resulting in electronic conduction. From theresult, they have proposed the possibility of a next-genera-tion nano device using DNA.

The dielectric response of a material changes dependingupon its frequency, and in the operating frequency area (1MHz to several hundred GHz) of CMOS, both electronicstates and phonons contribute to the polarization of thematerials. Most of the high-dielectric materials studied as acandidate of the insulating gate film for the next-generationCMOS, are highly-ionic materials, like metal oxides andmetal silicates. The polarization due to the phonons is largefor these materials. Thus, we need to analyze both contri-butions from the electronic part and phonon part to calcu-late the dielectric response of the materials. We can calcu-late the contribution from the electronic part using the

193


Fig. 2 Ge cluster on Si (001) (calculated up to atom 9263 maximum).

Fig. 3 Transfer of hole from metallic ions to DNA chain.

time-dependent perturbation method, and the contributionfrom the phonon part by calculating the phonon frequenciesand by using the Berry phase polarization theory.11)

In principle, DFT can describe the ground states ofmaterials correctly, and has been highly successful with theuse of LDA or GGA. However, one of its major drawbacksis that the energy gaps of semiconductors or insulators areunderestimated by about 50%. In the GW method proposedby Louie et al. in 1985, quasiparticle energies are calculat-ed by evaluating the self-energy with the screenedCoulomb interaction, and the energy gaps can be calculatedmore accurately.12) However, as the computational cost isvery large, this method can be applied only to small sys-tems with a few tens of atoms. The Time-Dependent DFT(TDDFT) method formulated by Gross in 1984 has beenapplied with the linear response theory to the calculation ofthe adsorption spectra of various gas molecules, and theresults turned out to be very accurate.13) Moreover, usingTDDFT, we can calculate the real-time dynamics of a sys-tem after an electron excitation, including both electronicand atomic dynamics. Tateyama, Oyama and Ohno appliedthis method to the photoisomerization reaction of a pho-tochromic molecule, which is a candidate for a future opti-cal switch or memory. The results agree well with experi-mental results.

Some of the calculation techniques to analyze the struc-ture and functionality of materials shown in the above areopen to public as the outcomes of the IT program project“Frontier Simulation Software for Industrial Science” ofthe Ministry of Education, Culture, Sports, Science andTechnology.

References

1) P. Hohenberg and W. Kohn, Phys. Rev., 136, B864 (1964).2) W. Kohn and L. J. Sham, Phys. Rev., 140, A1133 (1965).3) J. P. Perdew, K. Burke and M. Ernzerhof, Phys. Rev. Lett., 77,

3865 (1996).4) W. M. C. Foulkes, L. Mitas, R. J. Needs and G. Rajagopal, Rev. of

Modern Phys., 73, 33 (2001).5) R. Maezono, M. D. Towlor, Y. Lee and R. J. Needs, Phys. Rev., B

68, 165103 (2003).6) T. Miyazaki, D. R. Bowler, R. Choudhury and M. J. Gillan, J.

Chem. Phys., 121, 6186 (2004).7) T. Ozaki and H. Kino, Phys. Rev., B 69, 195113 (2004).8) J. Nara, W. T. Geng, H. Kino, N. Kobayashi and T. Ohno, J. Chem.

Phys., 121, 6485 (2004).9) H. Kondo, H. Kino and T. Ohno, Phys. Rev., B 71, 115413 (2005).

10) H. Kino, M. Tateno, M. Boero, J. A. Torres, T. Ohno, K. Terakuraand H. Fukuyama, J. Phys. Soc. Jpn., 73, 2089 (2004).

11) T. Yamamoto, H. Momida, T. Hamada, T. Uda and T. Ohno, ThinSolid films, 2005 (in press).

12) M. S. Hybertsen and S. G. Louie, Phys. Rev. Lett., 55, 1418 (1985).13) E. Runge and E. K. U. Gross, Phys. Rev. Lett. 52, 997 (1984)

3. Strong coupling modeling

Much recent attention has been focused on the investiga-tion of strongly correlated systems. Because of the effectsof many-body correlations, a system may exhibit a largeresponse to a small variation of external conditions, such as

electric and magnetic fields, density and temperature,which are crucial for nano technologies with low energyconsumption. The search and control of these systems aretherefore not only of academic interests but also of applica-tion importance. Hot topics include studies on new super-conductivity phenomena, nano-ferromagnetism, spintron-ics, and polymer-based materials.1)-13)

As a macroscopic quantum phenomenon, superconduc-tivity has remained a central subject in condensed matterphysics since its discovery. The well-known equipmentMRI (magnetic resonance imaging) for observing intobrains in clinical practice is actually based on the advan-tage of the quantum interference property of superconduc-tivity in measuring a tiny magnetic field. Today, researcheson making full usage of the potential of superconductivityphenomenon are going on worldwide. For example, theimplementation of quantum bits and quantum calculationusing the so-called Josephson junctions offers a better scal-ability than other competing techniques.2) Another effort isto excite laser of tunable terahertz frequency based on sin-gle crystals of the so-called high-Tc cuprate superconduc-tors.3)

The clarification of the thermodynamically stable statesof interlayer Josephson vortices is an important researchtheme since it lays the basis for the above-mentioned laserradiation. In superconductivity state, the magnetic fieldpenetrating into the sample is quantized into tiny pieces,known as the flux quantum or quantum vortex. Flexibilityof Josephson vortex lines because of thermal fluctuations,anisotropic interaction between vortex lines and the com-mensuration effect between the vortex alignment and theunderlying layer structure of high-Tc cuprate superconduc-tors produce rich physics, which is not experienced in con-ventional systems. Hu and Tachiki were the first to find anovel thermodynamic state of interlayer Josephson vor-tices, in which vortex lines within same layers exhibitquasi-long-range order, while those in different layers showshort-range order (Fig. 4).5), 10)

Japan is one of the top runners in the pace of developingquantum bits and quantum calculation using Josephsonjunctions as well as terahertz laser radiation based on high-Tc superconductors. In the former topic, NEC and NTT

194


Fig. 4: Left-top: schematics of interlayer Josephson vortex line. Left-bottom: Structure factors for the lattice and the novel phases. Right:Magnetic field vs. temperature phase diagram of interlayer Josephsonvortices obtained by large-scale Monte Carlo simulations.

have succeeded in the implementation and control of twoquantum bits. In the latter topic, a theoretical proposal wasmade by Tachiki et al., and research based on large-scalenumerical calculation by the Earth Simulator is going on.Concerning the new state of the interlayer Josephson vor-tices proposed by Hu and Tachiki, two research groups inthe US and France are planning to carry out experiments inorder to confirm the theoretical proposal and to map out thetotal phase diagram.

References

1) S. Murakami, N. Nagaosa and S. C. Zhang, Science, 301, 1348(2003).

2) Y. Nakamura et al., Nature, 398, 786 (1999).3) M. Tachiki et al., Phys. Rev. B, 71, 134515 (2005).4) X. Hu, S. Miyashita and M. Tachiki, Phys. Rev. Lett., 79, 3498

(1997).5) X. Hu, M. Tachiki, Phys. Rev. Lett., 85, 2577 (2000).6) X. Hu, Phys. Rev. Lett., 87, 057004 (2001).7) Y. Nonomura and X. Hu, Phys. Rev. Lett., 86, 5140 (2001).8) A. Tanaka and X. Hu, Phys. Rev. Lett., 88, 127004 (2002).9) A. Tanaka and X. Hu, Phys. Rev. Lett., 91, 257006 (2003).

10) X. Hu and M. Tachiki, Phys. Rev. B, 70, 064506 (2004).11) X.G. Wan, M. Kohno and X. Hu, Phys. Rev. Lett., 94, 087205

(2005).12) X. G. Wan, M. Kohno and X. Hu, Phys. Rev. Lett., 95, 146602

(2005).13) A. Tanaka and X. Hu, Phys. Rev. Lett., 95, 036402 (2005).

4. Prediction of nano-structures and properties

Phase diagrams are indispensable for materials develop-ment, and they have been determined by experiments formany systems. Because it is not possible to determine allphase diagrams of multi-component systems by experi-ments, a phase-diagram calculation technique called CAL-PHAD (CALculation of PHAse Diagram) has greatlyadvanced in recent years owing to the sophistication ofthermodynamic modeling1) and the higher performance ofcomputers. Commercial software packages such as Ther-mo-calc,2) ChemSage, P*A*C*T, and Pandat are sold assystems equipped with a thermodynamic database, an equi-librium calculation function, and a construction function,and such software is being used for the development andanalysis of materials because they can reproduce, with highprecision, phase diagrams of complicated multi-componentalloy systems for practical use.

Now, one of the important targets here is to expand thethermodynamic database, and a database indispensable fordeveloping advanced materials such as Pb-free solderalloys3) has been developed. Great advances have beenmade concerning thermodynamic modeling. Kikuchi4)

developed the Cluster Variation Method (CVM) in whichthe distribution of atoms is considered not as a point but asa pair of atoms and units of a triangular cluster. The CVMcan deal with the short range order existing in a solid solu-tion alloy. The phase diagram calculation based on firstprinciples is academically important but requires enormouscomputation. Therefore, when there is no measured value

of thermodynamic data, the realistic approach is to predictthe thermodynamic parameters based on the first principlescalculation which can be used as a part of the database ofthe CALPHAD method.5)

Concerning a stable phase in an equilibrium state, accu-rate prediction has become possible. However, for the pre-diction and control of materials microstructure, informationon the equilibrium structures based on a phase diagram isinsufficient, and we need a technique for predicting timedependent microstructure evolution. The phase-fieldmethod6) is a hopeful technique to analyze the time depen-dent process of the microstructure formation. Here, theshape of microstructure is expressed by variables such asthe chemical compositions and the order parameters andthe time development of microstructure is obtained by solv-ing their evolution equations. Koyama7)-10) and his grouphave successively clarified the dynamics of variousmicrostructure-forming processes in real materials based onthe phase field method, and it is becoming possible to pre-dict microstructure in practical alloy systems (Fig. 5).

The phase-field method can handle sizes from nano to

meso scale, and in order to handle the scale of an actualproducts, it must be coupled with some other techniquessuch as the finite element method. In NAREGI, which is anational project of the Ministry of Education, Culture,Sports, Science and Technology, a multi-scale simulationtechnique is now being developed.

In analyzing changes of internal microstructure usingFEM as the core method, materials parameters such asrecrystallization rate constant and the recovery velocity aremissing. If these materials parameters can be theoreticallyobtained as a function of chemical compositions based onthe phase-field method, the MD method, etc., then the pre-diction of macro-structure will progress dramatically. Con-cerning the prediction of mechanical properties, too, vari-ous techniques have been developed in order to model thedeformation process after describing the elementaryprocess of plastic deformation, and it is possible to analyzethe deformation process of polycrystalline materials includ-ing the dislocation distribution inside a grain and the for-mation of sub-grains by the homogenization method, thecrystal plasticity theory, and the diffusion equation of dis-

195


Fig. 5 Two-dimensional simulation of γ’ precipitation process in Ni-Alalloy based on phase-field method (973 K isothermal aging).

locations.

5. Conclusion

The ultimate goal for nano-bio materials is to achieveinnovative functions and to design and control such func-tionalities. It is necessary to develop advanced nano-simu-lation techniques which enable us to clarify the relation-ships between the electronic structures, physical propertiesand functions of these materials. Developments andimprovements of the simulation techniques for very large-scale simulations, multifunctional analysis (multi-physics),strongly-correlated modeling and multi-scale techniquesare urgently needed.

References

1) T. Abe and B. Sundman, CALPHAD, 27, 403 (2003).2) B. Sundman, B. Jansson and J. O. Andersson, CALPHAD, 9, 153

(1985).3) I. Ohnuma, M. Miyashita, K. Anzai, X. J. Liu, H. Ohtani, R.

Kainuma and K. Ishida, J. Electron Mater., 29, 1137 (2000).4) R. Kikuchi, Phys. Rev., 81, 998 (1951).5) H. Ohtani, Y. Takeshita and M. Hasebe, Mater. Trans., 45, 1499

(2004).6) R. Kobayashi and Bull. Jpn. Sco. Ind. Appl. Math., 1, 22 (1991).7) M. Ode, S. G. Kim, W. T. Kim and T. Suzuki, ISIJ Int., 45, 147

(2005).8) T. Koyama and H. Onodera, Metals and Mater. Int., 10, 321 (2004).9) T. Koyama and H. Onodera, Mater. Trans., JIM, 44, 1523 (2003).

10) T. Koyama and H. Onodera, Mater. Trans., JIM, 44, 2503 (2003).

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1. Introduction, world trend

Particle-beam technologies with ions, electrons and neu-tral atoms for creating nanostructures have greatlyadvanced in recent years. This section starts with ionimplantation and irradiation technology. The authors ana-lyzed the recent research trend by counting papers devotedto various topics at the IBMM-14 (conference on Ion BeamModification of Materials, US in September 2004) 1) whichis one of the most important international conferences inthis field. Among 343 papers in total, the largest numberwas on radiation damage (22.7%), followed by semicon-ductor applications (20.7%), nanoparticles and nanostruc-tures (16.6%), plasma-immersion implantation (16.3%),biological applications (6.4%), high-energy ions (5.2%),and beam lithography. Other papers, such as beam-solidinteractions (2.9%) and magnetism applications (2.3%),were reported but in small numbers. It is not surprising thatradiation damage and semiconductor applications dominat-ed, occupying first and second place in the number ofpapers, because of their long history. What is noteworthy isthe third place occupied by the field of nanoparticles andnanostructures, which has rapidly advanced in the last 5 to10 years. This rising field offers the potential of using thenonequilibrium processes and excellent controllability ofion implantation. Research institutes active in this field areOak Ridge National Laboratory, Vanderbilt University,Alabama A & M University (all in the US), FOM (theNetherlands), FZ Rossendorf (Germany), Padova Universi-ty (Italy), Australian National University (Australia), andNIMS. Plasma-immersion implantation in fourth place isan emerging field, but it should be regarded as a processingtechnology or a parts-making technology which is differentfrom a genuine technology for creating new materials andwill not be considered further in this section.

One technology which has attracted attention in recentyears is beam-induced chemical vapor deposition which isadvantageous for creation of nanostructures. The techniquefor introducing a precursor gas such as an organic metalinto the neighborhood of a specimen and irradiating afocused beam onto it 2)-5) enables three-dimensional nanos-

tructures to be made with a high degree of freedom, withlow penetrability of ions. In this technique, structures suchas a wineglass of about 2 µm in diameter and a nanobel-lows have been made. A structure with a minimum size ofabout 100 nm has been achieved by a ion beam whosediameter is about 7 nm.6) Electron beam-induced depositionaims to make even finer structures by using an electronbeam which can be focused more finely, and this techniquehas been widely studied for various gases based on themethod of introducing a gas into a scanning electron micro-scope.7)-10) In this technique, structures such as a nanodot ofabout 10 nm and a needle-like structure of about 15 nmhave been made using an electron beam of about 1 nm. Aresearch group at Delft University of Technology in theNetherlands has recently been carrying out both theoreticaland experimental research in this area.11)

Lithography is an excellent technology for mass-produc-ing nanometer elements, but conventional exposure sourcesconcerning an electron beam are subjected to various prob-lems such as transmission and scattering, diffraction, andspace charge. On the contrary, a low-speed atom beamsuch as metastable atoms (He*, Ne*, Ar*) has no problemswith transmission; its limit of diffraction as a material waveis very small as the mass is large; and it is neutral and hasno divergence without the space charge effect. Therefore, ithas ideal characteristics as an exposure source for nanolith-ography. Since Berggren and other researchers 12) proposedneutral atom-beam lithography in 1995, research on it hasbeen advancing in the US, Germany and Australia. A self-assembled monolayer film (SAM), a hydrocarbon or siliconpolymerized film, and a passivation layer on the substratesurface are used as a resist.

2. Domestic trend

Ion implantation technology: The main application issurface modification of materials. Research reports onimproving adaptability of artificial biological materials to aliving body 13) have been published, in addition to industrialapplications such as (a) improvement of crystallinity of

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Chapter 15. Technologies New Materials Creation

Section 1. Particle-Beam Technologies

Naoki KishimotoNanofunction Group, Nanomaterials Laboratory, NIMS

Kazutaka MitsuishiIn-situ Characterization Group, High Voltage Electron Microscopy Station, NIMS

YBCO and DLC films by plasma-immersion implantationin the case of inorganic materials and (b) improvement ofgas barrier properties in the case of organic materials. Con-cerning nanoparticles, attempts have been made to createmetal nanoparticle (Au, Ag) monolayers in a silicon oxidefilm with the aim of making a single electron device.14)

Beam induced vapor deposition: Matsui and his groupare studying creating nanostructures by ions, and haveactually made structures such as a switch and a coil.6) Inmaking nanostructures using an electron beam, Hiroshimaand his group have made nanostructures using a scanningelectron microscope of up to 30 kV.10)

Atomic beam lithography: In Japan, only the atomicbeam lithography system is developed at NIMS, but cre-ative research on the related technology of atom-beamholography is underway.15) This technology forms a patternwith an ultra-slow Ne* atom beam whose monochromatici-ty is increased by laser cooling passes through a hologram,and is a promising technique for maskless lithography.

3. Current status and research activities of NIMS

Ion implantation technology: NIMS is promoting thecreation, control, and evaluation of nanoparticles in insula-tors using a high-current/heavy-ion accelerator. NIMS hassucceeded in controlling nanoparticle precipitation bywavelength-selective laser irradiation after ion implanta-tion, and in creating oxide nanoparticles, such as ZnO, withthermal oxidation of implanted substrates. In-situ opticalspectroscopy during formation of nanoparticles, evaluationof the optical nonlinearity of metal nanoparticles, and theapplication to an optical device are in progress.

Beam induced vapor deposition: NIMS has made a finerstructure using a scanning transmission electron micro-scope (STEM) of 200 kV, which has triggered interestworldwide.16) With such a powerful electron microscope,NIMS has succeeded not only in making a nanodot of 4 nmor less and a three-dimensional structure of 10 nm or lessby an electron beam of 1 nm or less, but also in making ananodot of 1.5 nm by controlling the degree of vacuum.17)

Atom-beam lithography: NIMS has succeeded in trans-ferring a pattern onto a gold thin film with the edge widthof 40 nm using an alkanethiol SAM as a resist and using aHe* atom beam as an exposure source.18) Researchers atNIMS are systematically studying optimum conditions inaccordance with the difference in the length of a normalchain, and evaluating the transferred pattern. They havefound solarization of the contrast of a transferred pattern inthe process of such research, and clarified that the contrastof a transferred pattern depends on the length of a normalchain. They are currently working to clarify the exposureprocess by observing desorbed ions by He* irradiation.19)

Moreover, since the spin dependence of desorption proba-bility has been clarified by a spin polarized He* atomicbeam, they are examining the behavior of surface electronspin.

4. Future trend

Concerning the creation of nanoparticles and nanostruc-tures using nonequilibrium processes and good spatial con-trollability inherent in ion implantation technology, it isexpected that various new nanostructures including notonly metal nanoparticles but also metal oxides andnanorods will continue to be created. To enhance function-ality of the nanomaterials, development of (one- or twodimensional) nanoparticle-array structures, instead of ran-domly distributed nanoparticle structures, is indispensable.Hybridization of beam technology with micro-scale pro-cesing or laser treatment is very important.

Electron-beam induced vapor deposition has adequatecapability for making nanostructures in terms of size andposition controllability, but it is also necessary to develop atechnology for identifying the structures obtained and toimprove physical properties such as crystallinity of nano-materials obtained.

In atom-beam lithography, a report has been publishedconcerning a method of depositing an evaporated atombeam on a substrate while controlling its position and form-ing structures without a mask or etching treatment, which isentirely different from conventional lithography. An evapo-rated atom beam of Na, Cr, Al, etc. is focused by dipoleinteraction with the electric field of a standing wave oflight which deviates slightly from the absorption line of theevaporated atom. Three-dimensional doping has been alsoproposed,20) and it is predicted that this technique will bedeveloped to cover all the elements constituting devices.

References

1) Abstract book, 14th Intern. Conf. on Ion Beam Modification ofMater., Monterey, California, USA, (2005) Sept.

2) T. Minafuji, Mater. Sci., 38, 184 (2001).3) J. Fujita, M. Ishida, T. Sakamoto, Y. Ochiai, T. Kaito and S.

Matsui, J. Vac. Sci. Technol., B19, 2834 (2001).4) G. M. Shedd, H. Lezec, A. D. Dubner and J. Melngailis, Appl.

Phys. Lett., 49, 1584 (1986).5) S. Matsui, T. Kaito, J. Fujita, M. Komuro, K. Kanda and Y.

Haruyama, J. Vac. Sci. Technol. B., 18, 3181 (2000).6) S. Matsui, Appl. Phys., 73, 445 (2005).7) H. W. P. Koops, J. Kretz, M. Rudolph, M. Weber, G. Dahm and K.

L. Lee, Jpn. J. Appl. Phys., 33, 7099 (1994).8) H. W. P. Koops, R. Weiel, D. P. Kern and T. H. Baum, J. Vac. Sci.

Technol. B., 6, 477 (1988).9) P.C. Hoyle, J. R. A. Cleaver and H. Ahmed, J. Vac. Sci. Technol.

B., 14, 662 (1996).10) H. Hiroshima, N. Suzuki, N. Ogawa and M. Komuro, Jpn. J. Appl.

Phys., 38, 7135 (1999).11) N. Silivis-Cividjian, C. W. Hagen, P. Kruit, M. A. J. v.d. Stam and

H. B. Groen, Appl. Phys. Lett., 82, 3514 (2003).12) K. K. Berggren, A. Bard, J. L. Wilbur, J. D. Gillaspy, A. G. Helg, J.

J. McClelland, S. L. Rolston, W. D. Phillips, M. Prentiss and G. M.Whitesides, Science, 269, 1255 (1995).

13) F. Saito, T. Yotoriyama, Y. Nagashima, Y. Suzuki, Y. Itoh, A.Goto, M. Iwaki, I. Nishiyama and T. Hyodo, Proc. Mater. Sci.Forum, 445-6, 340 (2004).

14) H. Tsuji, N. Arai, T. Matsumoto, K. Ueno, Y. Gotoh, K. Adachi, H.Kotaki and J. Ishikawa, Appl. Surf. Sci., 238, 132 (2004).

15) J. Fujita, S. Mitake and F. Shimizu, Phys. Rev. Lett., 84, 4027(2000).

16) K. Mitsuishi, M. Shimojo, M. Han and K. Furuya, Appl. Phys.

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199


Lett., 83, 2064 (2003).17) M. Tanaka, M. Shimojo, M. Han, K. Mitsuishi and K. Furuya,

Surface and Interface Analysis, 37, 261 (2005).18) X. Ju, M. Kurahashi, T. Suzuki and Y. Yamauchi, Jpn. J. Appl.

Phys., 42, 4767 (2003).

19) Y. Yamauchi, T. Suzuki, M. Kurahashi and X. Ju, J. Phys. Chem.B., 107, 4107 (2003).

20) T. Schulze, T. Muther, D. Jurgens, B. Brezger, M. K. Oberthaler, T.Pfau and J. Mlynek, Appl. Phys. Lett., 78, 1781 (2001).

1. Introduction

Fabrication of a new material by controlling the configu-ration and structure of atoms constituting the material at theatomic level based on a design drawing is one of the ulti-mate approaches. In order to treat a material at amonoatomic or monomolecular level it is necessary to min-imize the absorption of gaseous molecules which causecontamination at the same level. By using an extremelyhigh vacuum (atmospheric pressure of 10-10 Pa or less) inwhich only a few to tens of gaseous molecules exist per 1mm3, an ultraclean ultimate environment is generated inwhich contamination due to surface absorption can beneglected even at a monoatomic size. Moreover, by con-structing an extremely highly integrated process whichconsecutively carries out all the multistage operations suchas making the surface of the sample substrate ultraclean,preparing the film, processing, analyzing the characteris-tics, and evaluating the performance in an extremely high,ultraclean vacuum, it is expected to lead to a materialdevelopment process which can fabricate new materials atthe atomic or molecular level.

In such a large-type vacuum process, however, thereexist many gas desorption sources which deteriorate theultraclean vacuum atmosphere, such as the walls of thevacuum chamber, the filaments of the vacuum gauge elec-tron system, and the evacuation system. In particular, in asample movement-based source in a meter, not only gasdesorption but also generation of dust such as microparti-cles might occur due to the increase of friction and abrasionpeculiar to a vacuum environment, and in the worst case,the driving mechanism might seize up by friction andbecome inoperable.

To eliminate the friction which can contaminate thisultraclean space during sliding, it is essential to develop anon-contact floating transport system which is not accom-panied by sliding for a substrate transport-based source, forwhich long-haul high-speed transportation is required.

The next section looks at research on the construction ofa magnetic-levitation type extremely highly integratedprocess that NIMS is working on to achieve an extremelyhigh, ultraclean vacuum space for fabrication of materialsat the atomic level.

2. Research trend

Japanese universities and research institutes have outdis-tanced many other countries in research on an ultrahighvacuum which is the key technology of an extremely highvacuum process, especially research on a high-performanceevacuation technology for generating an extremely highvacuum environment, a technology for reforming a materi-al whose gas absorption is hard and its surface, and an ele-mental technology for measuring ultra-low atmosphericpressure with high precision. The results of these studieshave been widely used for the development, etc. of single-function measuring and analyzing equipment such as vari-ous electron microscopes and surface analyzers as well as alarge high energy accelerator system.

A multi-chamber integrated process has been much usedfor developing semiconductors, analyzing the surface ofcompounds, etc. However, as a contact-type driving systemwas used for moving a substrate in all of the processes,contamination of the surface of a substrate due to gas des-orption following sliding could not be avoided.

In recent years, NIMS has developed a magnetic-levita-tion type of mechanism for transport in an extremely highvacuum, as shown in the photo. In this transport system,the movable body which carries a substrate is made to floatusing electromagnetic force and so can travel long dis-tances by using a driving mechanism with a linear motor.Since there exists no contact part that suffers friction orseizing up during driving, almost no dust particles and nogas desorption are generated that would damage the ultra-clean, extremely high vacuum environment and ultracleansubstrate surface. By installation of an electromagnetic-lev-itation type transportation mechanism which can performlong-distance levitation transportation in a main line as atransportation device, and also by installation of an oxidesuperconductive levitation transportation mechanism offer-ing tough positioning power required for a branch line thatreceives and delivers substrates between the main linetransportation system and a vacuum apparatus to be con-nected, it is possible to receive and deliver substrates whilekeeping the substrate surface ultraclean at an atomic andmolecular level between each vacuum apparatus connectedsuch as film-preparation apparatus and surface analysisapparatus. This system is the extremely high vacuum inte-grated process unprecedented in the world.

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15 Technologies New Materials Creation

Section 2. Applied Technology of Vacuum Process

Masahiro TosaMicro-nano Component Materials Group, Materials Engineering Laboratory, NIMS

201


3. Future trend

Although the extremely high vacuum integrated processdeveloped by NIMS receives and delivers ultraclean sub-strates, control of the transportation positioning is some-times not so accurate, and so reliability of the system needsto be improved. In fabrication of next-generation LSIdevices, research will focus on downsizing from a semi-conductor-based material in which gas absorption on thesurface of a substrate is hard, to a metal-based material inwhich such gas absorption is easy, or from a micron scale

to a nano scale. This will be highly promoted by theincrease in performance of the extremely high vacuum inte-grated process that provides consistent operations at eachprocess in an extremely high, ultraclean vacuum environ-ment at the atomic or molecular level, which will con-tribute to the fabrication of next-generation new advancedmaterials and micro-nano devices.

4. Conclusion

Elemental technologies which can use an extremely highvacuum or an ultraclean environment at an atomic levelhave almost fully come out, and the extremely high vacu-um integrated process which has been constructed by inte-grating the elemental technologies is expected to exhibit itstrue value in the creation and fabrication of new advancedmaterials and devices by establishing transportation accura-cy and reliability.

References

1) M. Tosa and K. Yoshihara, J.Vacuum Society of Japan, 40, 156(1997).

2) M. Tosa, A. Kasahara, K. Lee and K. Yoshihara, J.Vacuum Societyof Japan, 42, 443 (1999).

3) M. Tosa, K. S. Lee, A. Kasahara and K. Yoshihara, Vacuum, 60,167 (2001).

4) M. Tosa, K. S. Lee, Y. S. Kim, A. Kasahara and K. Yoshihara,Appl. Surf. Sci., 169, 689 (2001).

Electromagnetic-levitationtransportation system.

Superconducting magnetic-levitation transportation.

Photo: Extremely high vacuum integrated process equipped withmagnetic levitation type transportation systems.

1. Introduction

In order to secure the reliability of machines, structures,plants, etc., materials data are indispensable. NIMS hasaccumulated materials data related to creep, fatigue, corro-sion, and space use; publishes about ten data sheets everyyear; and has distributed them to about 1,000 organizationsinside and outside Japan. NIMS has almost a 40-year histo-ry of working on creep and fatigue data sheets, and its datasheets including those on corrosion and space use materialsare highly valued inside and outside Japan. These datasheets are based on ISO9001 “Quality Management Sys-tem”. The achievements of each data sheet and researchtrend are summarized below.

2. Creep data sheets

We published three volumes of creep data sheets inFY2004, which are 1) base metal, weld metal and weldedjoint of hot rolled stainless steel SUS316-HP (18Cr-12Ni-Mo-middle N-low C) (No.45A), 2) alloy steel tube for apower boiler KA-STBA27 (9Cr-2Mo) (No.46A), and 3)metallographic atlas of long-term crept materials on threetypes of 2.25Cr-1Mo steels (No. M-4). By FY2004, we hadpublished 132 volumes of creep data sheets, including fourvolumes of metallographic atlas. We have also obtained708 creep test data for long durations exceeding 100,000hours (about 11.4 years) including data for which experi-ments are still underway.

We clarify the mechanism of degradation occurring inaccordance with prolonged use at high temperature, andstudy methods of predicting long-term creep strength usingthe valuable long-term creep test data which we have accu-mulated over about 40 years. Regarding high-strength high-Cr ferrite heat-resistant steel which has recently been usedto improve the efficiency of thermal-power generationplants, a drop in strength was found with long-term use thatcould not have been predicted based on past knowledge,

and in fact an accident occurred. Based on creep datasheets, we therefore proposed an easy and precise methodfor predicting long-term creep strength (NIMS method) andfor analyzing and evaluating long-term creep strength usinghalf of the 0.2% offset yield stress as an index. In FY2004,based on long-term creep strength analysis by the NIMSmethod, we reviewed the allowable tensile stress regulatedin the national standard. The creep data sheets have con-tributed greatly to improved safety in high-temperatureplants such as power generation and petrochemical plants.We have focused on creep fracture in the past creep datasheets, but will systematically acquire creep deformationdata and publish creep deformation data sheets in thefuture. We are also planning to acquire creep data on an Alalloy, Mg alloy, etc. which is in great demand for energysaving in transportation equipment such as automobiles aswell as creep data on light-weight nonferrous metals.

3. Fatigue data sheets

In FY2004 we published 1) giga-cycle fatigue datasheets (No. 97) for carbon steel S40C (0.4C), and 2) giga-cycle fatigue data sheets (No. 98) for a titanium alloy Ti-6Al-4V (1100-MPa class). Among 98 volumes of fatiguedata sheets, there have been as many as 14 volumes ofhigh-cycle fatigue data sheets which we started publishingin 1997 on high-temperature fatigue and welded jointfatigue characteristics in addition to room-temperaturefatigue and titanium-alloy fatigue.

In recent years, the issues of long-term use of structuresand extension of life have emerged as problems to besolved, and the trend of fatigue research has been shiftingtoward clarifying fatigue fracture at ultrahigh cycle of 107

or more, especially internal fractures, for which data havenot been obtained to date. Therefore, the published long-term fatigue data sheets are well-timed data sheets. In par-ticular, NIMS has developed an ultrahigh cycle fatigue test-ing method using a 20-kHz ultrasonic fatigue tester for

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Chapter 16. Acquisition and Transmission ofMaterials Information Data andInformation

Section 1. Structural Materials Data Sheets

Saburo MatsuokaMaterials Information Technology Station, NIMS

203


accelerated fatigue testing, and has developed a test methodwhich can obtain data on fractures of up to 1010 cycles in ashort time. These data sheets, which focus on fatigue thatcauses internal fracture to occur from an intermediary as astarting point newly named “giga-cycle fatigue”, are veryuseful for engineering and are highly valued in industry.Concerning welded joints, we have also obtained data of upto 108 cycles in a large-type joint test, and are striving tointerpret a new welded joint fatigue strength that has notexisted before. In addition, we are undertaking epoch-mak-ing research, for example, on a new method of observingmetallic structures using an atomic force microscope(AFM) and associating micro and macro structures andhardness based on the measurement of nano-hardness.

High-cycle fatigue data sheets are well underway anddata have been steadily published, but we are planning toadvance toward new materials and fields of new test condi-tions such as: giga-cycle characteristics in an average stressstate and a thickness effect in welded joints; systematicstudy of notch effects; and high-temperature characteristicsof Ni-base superalloys.

4. Corrosion data sheets

Corrosion is a chemical phenomenon which changesendlessly according to the combination of material andenvironment. NIMS’s corrosion data sheets cover atmos-pheric corrosion phenomena among a variety of corrosionphenomena available at the moment. About seven yearshave passed since we started an atmospheric exposure teston the binary alloys of Fe-Ni and Fe-Cr systems in 1998 inorder to acquire basic data on corrosion-resistant low-alloysteel in a coastal environment and establish developmentguidelines for it. Concerning the atmospheric corrosion ofthese steel materials, we gathered all data together threeyears after starting the exposure test, and published corro-sion data sheets No. 1A in FY2002. We collected data onthe atmospheric corrosion of binary alloys of Fe-Al and Fe-Si systems and published corrosion data sheets No. 2 inFY2004.

We are also working toward issuing corrosion data sheetmaterials in March 2006 which will include photographs onthe external appearance of test pieces, influences of alloyelements and weather factors upon durability, etc. that wecould not include in No. 1A and No. 2.

There has been an immense reaction since corrosiondata sheets No. 1A was issued, and we have since receivedopinions from many people requesting us to issue corrosiondata concerning various materials and environments. Wewill positively study these opinions, reflect them in futureresearch for corrosion data sheets, and aim to issue corro-

sion data sheets that will be increasingly useful.From now on, we will evaluate the corrosiveness of var-

ious materials including practical materials in an atmos-pheric corrosive environment, and enrich basic data con-cerning atmospheric corrosion phenomena.

5. Data sheets on strength of materials for space use

We started to produce data sheets on the strength ofmaterials for space use after the LE-7 engine of H-II Rock-et No. 8 was raised from 3,000 meters down on the seabedwest of the Bonin Islands in January 2000. It was pointedout while searching for the cause of the accident that therewas almost no strength data on the materials of domestical-ly-made rockets, that data of NASA in the US had beenused to design the rocket, and that information aboutmicrostructure and fracture surface, which were indispens-able for analyzing the accident and resolving defects duringall development stage, had not been well prepared. AsNIMS had developed test technologies concerning thesematters, NIMS was requested to prepare data. While NIMSprepared materials strength characteristics data jointly withthe Japan Aerospace Exploration Agency, NIMS publisheddata sheets on the strength of materials for space use basedon the past data sheet results, with the aim of not onlyobtaining data and providing it for the design, but also pro-viding data to the public to be widely used and to helpthose who handle similar materials, thus improving the reli-ability of materials themselves.

Starting with the data sheets from the liquid hydrogenfuel turbo pump (FTP) and engine materials of the H-IIARocket, we published data sheets one after another for tita-nium alloys, Alloy 718, and superalloys, and we published1) data sheets (No. 5) on the destruction toughness of anAlloy 718 forged material and high-cycle fatigue character-istics, and 2) data sheets (No. 6) on the destruction tough-ness of an A286 forged material and high-cycle fatiguecharacteristics, thus contributing to the successful launch ofthe H-IIA.

In the process of acquiring the materials strength datafor publication of such data sheets, we obtained many use-ful findings for improving the characteristics and reliabilityof future materials such as the influence of grain size uponfatigue characteristics at low temperature, the occurrence ofaccompanying internal cracks, and the influence of notcheffects.

We will continue to publish collections of data sheets onfractures and fatigue crack progress characteristics forwhich demand is strong, in addition to strength characteris-tics data, and will study the acquisition of other enginematerials and important structural materials.

1. Introduction

Basic data and information on science and technologyhave been edited in the form such as dictionaries, encyclo-pedia, handbooks, manuals, and data books, which havebeen in general use for a long time. When large general-purpose computers became widespread in the 1990s, thepossibility of digitizing huge quantities of data was studied,and a wide variety of databases have since been construct-ed as information processing equipment has progressed.Since the 1990s, people around the world have been able toshare data and information over the Internet thanks to therapid diffusion of the world wide web.

Materials data can be classified into the following twocategories: 1) High-quality basic data whose universality ishigh (such as physical constants, spectrum information,nuclear data, structure-independent characteristics, crystalstructures, and phase diagrams), and 2) Fundamental engi-neering data (various characteristics on practical materialswhich are the basis of design and safety assessment). High-quality basic data is made useful data by linking it withengineering data.

This section describes the situation of the materials data-bases made public on the Internet at present, as well asassociated problems.

2. Research trends

As an example of high-quality basic data, basic physicalconstants were revised greatly and officially announcedtoward the end of 1999 after a lapse of over ten years bythe Task Group on Fundamental Constants which wasfounded under the Committee on Data for Science andTechnology of the International Council for Science(CODATA) of the International Council of ScientificUnions (ICSU).1) The corresponding organization in Japanis the CODATA sectional meeting of the Science Councilof Japan and the CODATA sectional meeting of the JapanSociety of Information and Knowledge. In Japan, theNational Institute of Advanced Industrial Science andTechnology, an independent administrative institution, hasmade spectrum data of organic compounds available to the

public.2) Nuclear data is included in the nuclear materialsdatabase of the National Institute for Materials Science,another independent administrative institution, and crystalstructure information and phase diagrams are included inthe basic crystal structure database (Pauling file) and elec-tronic structure database.3) Concerning such database-mak-ing activity, it is important to construct databases efficient-ly through international tie-ups while avoiding the duplica-tion of similar work, and to establish databases as publicgoods to be used all over the world.

Fundamental engineering data and information are indis-pensable not only for researchers and technical experts butalso for designers of equipment. Such data is used formaterials design and various simulations. It is also used forselecting materials for equipment design and optimum useof materials. There are two ways of gathering fundamentalengineering data. One is to collect brochures of materialsmanufacturers, make a database of the data, and distributeit. The other is to accumulate measured data obtained byvarious research institutes by carrying out materials tests ordata collected from scientific reference materials and com-pile them into a database. Therefore, a database containingcharacteristic values as well as information on the manu-facturing process of a material, measuring equipment,shape, size and test conditions of a test sample, and testorganizations needs to be constructed to enable fundamen-tal engineering data to be used in industry. However, thereis no research institute in the world that collects data sys-tematically, compiles databases therefrom and makes thedatabases publicly available. The only data available in theworld is data on creep, fatigue, corrosion, and space usematerials strength in the structural materials databases ofNIMS. The largest database of brochures of materials man-ufacturers is MatWeb, which is the most popular and isaccessed by 16,000 persons a day.4) In Europe, handbooksand databooks published by publishers are the traditionalformat, but CD-ROM versions have been made recently.As a database on structural materials, the European Com-mission Joint Research Center (JRC) gathers data of theEU countries together and distributes it.5)

Reliability (quality) is crucial in a materials database,but comprehensiveness (quantity) is necessary, too. More-over, a database must not only gather data but also offer a

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16 Acquisition and Transmission of Materials Information Data andInformation

Section 2. Materials Databases

Masayoshi YamazakiMaterials Database Group, Materials Information Technology Station, NIMS

retrieval function which can promptly display the data andinformation required by a user. However, there is a limit tothe volume of data and information which one organizationcan transmit, so Granta Design Ltd. of the UK has devel-oped and made public MATDATA.net, which combinespublicly available databases on substances and materials onthe Internet, and the data of each database can be retrievedby category of material (ceramic, composite, fiber & partic-ulate, foam, metal, natural and polymer).6) At present, 12database sites are connected to MATDATA.net, of whichthe substances and materials database of NIMS is one. Fig-ure 1 shows the top page of the substances and materials

database of NIMS, and Table 1 shows the materials data-base connected to MATDATA.net.7)


Concerning universal and high-quality basic data onmaterials, research which promotes the accumulation ofdata in international tie-ups in order to discover substancesand materials through data informatics will be actively pro-moted. Accordingly, the representatives of database con-struction organizations in Japan, the US, and Europe willstudy the standardization of XML and MatML to enabledata-sharing, at the materials sectional meeting of theCODATA.

Concerning fundamental engineering databases, strate-gic development investment by the government (nationalinstitute) is required. The materials procurement and glob-alization of manufacturing factories in industry isinevitable in Asia as seen in the EU. It will become increas-ingly important to collect, accumulate and transmit dataand fundamental information concerning materials to main-tain the quality of products.

4. Conclusion

Past databases were used only by groups engaged indevelopment, and many of them disappeared as the devel-opment budget was curtailed and no data was added whenthe R&D period came to an end. Databases must be contin-uously accumulated by grasping the needs of users and“usable databases” must be constructed.

References

1) 1) http://physics.nist.gov/cuu/Constants/Citations/Search.html2) http://www.aist.go.jp/RIODB/riohomej.html3) http://mits.nims.go.jp4) http://www.matweb.com/index.asp?ckck=15) http://odin.jrc.nl/6) http://matdata.net/index.jsp7) K. Yagi, Problems and Future Perspectives of Materials Database,

Sci. &Tech. Tendency, No. 42, pp. 22 to 33 (2004).

205


Fig. 1 Materials Databases of NIMS. http://mits.nims.go.jp

DatabaseSource

ASM Handbook

ASM Alloy Center

ASM Micrograph Center

PGM Database

IDES Resin Source

MatWeb

Metals Universe.com

MIL-HDBK-5H

NIMS Materials Database

NPL MIDS

Steel Spec II

TWI JoinIT

Organization Country

USA/UK

USA/UK

USA/UK

USA/UK

USA

USA

UK

UK

Japan

UK

UK

UK

ASM International/Granta Design

Ltd.


Ltd.


Ltd.

Platinum group metals (PGMs)

IDES Inc.

Automation Creations, Inc.

National Metals Technology Center

Granta Design Ltd.

NIMS

National Physical Laboratory

UK Steel

The Welding Institute

Table 1 Databases Connected to MATDATA.net.

1. Introduction

In order to promote fair and smooth national trade, it isnecessary to quantitatively evaluate the international equiv-alence of measured and analyzed values of substances andmaterials, and their reliability. In people’s daily lives, theequivalence and reliability of analyzed values in the fieldsof environment, food, health, and so are also very impor-tant. This requires the traceability of those values to bekept. Traceability is called “sourceability” or “retroactivi-ty,” and means “the ability to trace the source of some-thing.” In other words, it means that a measured value isassociated with an international standard or can be traced toan international standard with some degree of uncertainty.That is, the accuracy and trueness of standard equipmentused to perform a test or a standard substance on which atest is performed are associated with international measure-ment standards and whether they can be traced to theInternational System of Units (SI) based on the internation-al definition in the Meter Convention.

2. Certified standard materials and development trend

Standard materials are developed to adjust the needs ofcommunities, social structures, corporations, organizations,etc., but ultimately they should also be valid globally.Therefore, “certified” standard materials or high-rankingstandard materials are important. The strict definition ofthese standard materials is described in ISO Guide 30, butfor certified values of characteristics, international equiva-lence based upon traceability is the most important, and soit is necessary to make traceability to the SI units as certainas possible.

As described above, it is indispensable to be able tomutually validate analyzed and measured values on a glob-al basis, and the International Committee of Weights andMeasures (CIPM) has 10 consultative committees in addi-tion to the International Bureau of Weights and Measures(BIPM), and its mission is to unify international unit sys-tems and measurement standards (standard materials andstandard measurements methods) of basic quantities ineach field. The fields with which the consultative commit-tees deals are as follows: 1) Electricity and Magnetism

(CCEM), 2) Photometry and radiometry (CCPR), 3) Tem-perature scale (CCT), 4) Length (CCL), 5) Time and fre-quency (CCTF), 6) Ionizing Radiation (CCRI), 7) Unit(CCU), 8) Mass and Related Quantities (CCM), 9) Amountof a Substance (CCQM), and 10) Acoustics, ultrasound,and vibration (CCAUV). Of these fields, CCQM deals withchemical quantity standards using an amount of a substance(mol) as a basic unit, and is closely related to the material.The consultative committees develop various standard sam-ples which serve as a scale for measurement chemical sub-stances and component standards which are used to cali-brate measument methods and measument equipments. Inrecent years the consultative committees have been ener-getically preparing standard materials and standard measu-ment methods jointly with the World Health Organizationand the International Food Standards Committee. Mean-while, as the field of materials (particularly including themeasurement and analysis of substances on the nano scale)cannot be covered by the ten fields specified above, it hasbeen proposed that a Consultative Committee on MaterialsMetrology (CCMM) be newly established.

3. Certified standard materials for surface and micro-area analysis

Standard materials are used in such a wide range offields that it is difficult to give an overview of all fields.Thus, this section describes only certified standard samplesin nano-scale analysis (which is limited to the method ofmeasument a substance of 100 nm even in one axis out ofthree-dimensional measurement). Table 1 shows these cer-tified standard materials. As can be seen, the number ofcertified high-ranking standard materials in this particularfield is very small. It is hoped that secondary standards andpractical standards to enable materials measurement on sitewill be promptly developed in this field.

References

1) Masaaki Kubota, “Standard Substances – For Securing Reliabilityof Analysis and Measurement”, Kagaku Nipposha (1998).

2) ISO Guide 30, 31; ISO 14606, 156969.

206


Chapter 17. International Standard

Section 1. Standard Materials

Shigeo TanumaFundamental Chemical Analysis Group, Materials Analysis Station, CNIMS

3) Koichi Chiba, Bunseki, 125 (2005).4) “Auger Electron Spectroscopy” ed., J. Japanese Society of Surface

Science, Maruzen (2001).

207


Name ofmaterial

Thickness(mm)

Certifyingorganization

Name ofproduct

Distributingorganization

Ta2O5/TaNi/Cr multilayer filmAlAs/GaAs multilayerCr/CrOTa2O5/Ta multilayer film

30 and 100 (4)66/53 (8)

25/25 (4)

29 – 30 30/30 (6)

IRMM1

NIST3

NIMC4

NISTKRISS6

No. 2612135c

213603-04-10

BCR2

NIST

SASJ5

NISTKRISS5

Certified values are thickness. Numerical values in ( ) are the number of layers.1: Institute for Reference Materials and Measurements2: Community Bureau of Reference3: National Institute for Standards and Technology4: National Institute of Materials and Chemical Research5: Surface Analysis Society of Japan6: Korea Research Institute of Standards and Science

Table 1. Examples of certified standard substances in surface analysis.

1. Introduction

International standardization research in NIMS aims atdeveloping new evaluation methods required for the appli-cation and practical implementation of new materialsthrough a pre-standardization activity and promotinginternational standardization thereof. In particular, the fol-lowing are important in international standardizationresearch: 1) making newly-developed materials and newevaluation methods known to the public, 2) increasingJapan’s contribution to international standardization activi-ties, and 3) contributing to the general public throughinternationalization activities.

VAMAS (Versailles Project on Advanced Materials andStandards) is one of the international research cooperationprojects agreed upon at the 1982 Group of Seven summit,and its purpose is to promote international standardization

through international cooperation concerning advancedmaterials and to stimulate foreign trade in advanced techni-cal products.1), 2) The steering committee of VAMAS ismade up of senior officials of governmental organizationsin the seven summit countries and ISO who are engaged inmaterials and standards. VAMAS, which currently has 30technical working areas (TWA, experts’ sectional meet-ings), terminates the activities of the TWA once it hasachieved its goal, and continually keeps its activities up todate in line with the needs agreed upon by each country.Each TWA is composed of national research institutes, uni-versities, and private enterprises of each country. Concern-ing the TWA sectional meeting marked with an asterisk (*)shown in Fig. 1, a researcher at NIMS acts as chairman ofthat TWA sectional meeting, thus taking the leadership inthat field.

2. Merits and outcomes of VAMAS

Much remains to be established in the evaluation ofadvanced materials and there are major differences amongorganizations, so the first mission of VAMAS is to deter-mine measuring and evaluating methods which can be used

208


Japan VAMAS Committee

Steering CommitteeSeven summit countries + EU (Director General-class officials of research institutes)

UK (chairman), Japan, USA, Canada, France, Germany, Italy, EU, and ISO (observer)

Technical Working Areas (TWA)

01 Wear test methods02 Surface chemical

analysis03 Ceramics for structural

applications05 Polymer composites10 Computerised

materials data*13 Low-cycle fatigue16 Superconducting

materials*17 Cryogenic structural

materials*18 Statistical techniques

for interlaboratory studies and related projects

20 Measurement of residual stress

21 Mechanical measurement for hard metals

22 Mechanical property measurements of thin films and coatings

24 Performance related properties for electro-ceramics

25 Creep/fatigue crack growth in components

26 Optical measurement of stress and distortion

27 Characterization methods for ceramic powders and green bodies

28 Quantitative mass spectrometry of synthetic polymers

29 Nanomaterials30 Tissue engineering*

Fig. 1 Organization and Technical Working Areas of VAMAS.

ISO International Standards ProcedureVAMAS activities

Technical transfer assessment report (proposal of tests and measuring methods)

1st Committee draft (CD)

Final committee draft (FCD)

Draft of international standards (DIS)

Proposal of new work items (NWIP)

Final working draft

Working draft (WD)

Partially agreedstandards (PAS)

Technicalstandards

Final draft of international standards (FDIS)

Internationalstandards

Fig. 2 International Standards Process of ISO and Liaison withVAMAS.

17 International Standard

Section 2. International Standardization Research, VAMAS

Toshio OgataCryogenic Materials Group, Materials Information Technology Station, NIMS

as standard ones. By participating in an internationalround-robin test of VAMAS and comparing measuredresults obtained on common samples with the results ofother organizations, it is possible to improve the evaluationtechnology and reliability of the participating organiza-tions.

The achievements obtained through VAMAS activitiesbecome international standards by being submitted to ISOand IEC. It takes several years to establish internationalstandards, so some successes first emerged ten years afteractivities on them first started. These have contributed tothe creation of about 60 standards of the ISO and theAmerican Association of Test and Materials (ASTM).Since the international round-robin test is held at the con-venience of the organization which carries out the test, it isnot easy to collect the results as scheduled. Moreover, ittakes a long time to gather international standards togetherbecause the opinions of people in many countries aresolicited, collected by each country, and are then distrib-uted and adjusted. Although circumstances differ accordingto each TWA, the steady establishment of internationalstandards is one of the great achievements of VAMAS.

In recent years, as VAMAS has gained internationalrepute, its liaison with ISO has been strengthened, and theirrespective achievements are now mutually respected.Under such circumstances, the registration of achievementsof VAMAS in the ISO standards has been promoted, andby collecting and organizing the results of the internationalround-robin test of VAMAS (a test in which common sam-ples are distributed to each participating organization andtest results are compared) and proposing the organizedresults as technical transfer assessment documents (TTAdocuments), it has become possible to speed up the discus-sions, as shown in Fig. 2.

NIMS has organized a Domestic VAMAS Committeeconsisting of a VAMAS steering committee member andexperts involved in international standards, and NIMS willarrange domestic standardization activities, deliberateJapan’s contribution in the field of VAMAS internationaljoint research, and propose new TWA(s). Researchachievements and cooperative relationships obtained frompositive activities toward new materials and internationalstandardization of the methods of testing them in coopera-tion with VAMAS will boost Japan’s influence in ISO andIEC, thus enabling Japan to easily propose standards ofwhich it takes the lead. This is because in order to proposeinternational standards, adequate supporting research dataand the development of international cooperative relation-ships are necessary; even if an international standard issuddenly proposed to the ISO, it will be difficult to gainconsent even to consider the proposal.

3. Importance of VAMAS international standardizationactivities

One of the clear means of using the achievementsobtained in substances and materials research for the com-mon good of society is to establish international standards(an international law) which have binding power interna-

tionally, but this requires the accumulation of data as thebasis of standards through the international round-robin testin cooperation with researchers both inside and outsideJapan. It is also necessary to obtain the understanding andapproval of many people concerning the proposed testmethod.

Since international standards are established by obtain-ing positive approval through lengthy discussions and thework of many countries, such standards have a greaterimpact than is generally imagined, and can trigger the pro-posal of other standards. The larger the impact of interna-tional standards, the more difficult it is to balance the mer-its and demerits of many countries. Moreover, since thenumber of proposal achievement is related to the appoint-ment (or acceptance) of a lead manager country, and thisincreases the power of persuasion in the ISO and IEC andmakes it easy to arrange a prior agreement, it is necessaryto emphasize and highly appreciate steady activities.

International standards of materials evaluation areimportant technologies pertaining to not only the promo-tion of foreign trade related to shipment inspections butalso the safety and reliability evaluation of materials andthe prediction of remaining life of existing infrastructuresfrom a national interest point of view. If foreign technologyand standards are introduced too easily, then the peopleengaged in such work may use the technology or standardswithout knowing the basis of them; they may not know thetechnology which is involved until the technology or stan-dards are established, or techniques for evaluating the tech-nology or standards may disappear. Unless Japaneseresearchers have underlying data for standards and thepotential to counter foreign researchers, and promoteinternational standardization activities positively, then vari-ous standards including design standards and safety stan-dards will be dominated by other countries, and Japan willnot be able to leave technologies and markets to the nextgeneration. By promoting international standardizationactivities positively and proposing international standards,the research institutes and industrial world that participatetherein can maintain the same technical level as in othercountries.

Judging from the fact that many countries include nano-materials in their national policies and are beginning tocompete in international standardization, the internationalstandardization activities of VAMAS will clearly rise inimportance in government and industry. Since it takes fiveto ten years to propose and establish international standardswhich are binding internationally starting from the proposi-tion and verification of our own method of assessing char-acteristics, it is essential to increase the appreciation ofresearch in order to foster successors.

References

1) Tetsuya Saito, VAMAS in International Standardization, Bulletin ofJpn. Soc. of Machin., 102, 302 (1999).

2) Toshio Ogata, Yoshitaka Tamao, Current Conditions and Issues ofInternational Strategy from the Viewpoint of InternationalStandardization of Materials, Science and Technology Trend, No.28, 19 (2003).

209


1. Introduction

As investment in nanotechnology R&D has grownrapidly worldwide, it has become crucial to secure the per-manence of nanotechnology as a basic industrial technolo-gy for the next generation. Accordingly, public trust in nan-otechnology must be gained by scientifically evaluatingboth the positive and negative aspects of nanotechnologies.To avoid the risks of nanotechnology and secure interna-tional competitiveness, a movement toward internationalstandardization of nanotechnology became conspicuous inthe US and leading European countries in 2004, and movestoward nanotechnology standardization simultaneouslystarted in Japan, too. One often-cited example of the risksof nanotechnology is carbon nanomaterials. The technolo-gy of mass-synthesizing nanometer-scale new-functionalsubstances such as carbon nanotubes and fullerene has late-ly been developed, and these nanomaterials will start beingused in various products in large quantities. The main enti-ty of such carbon-based nanostructures is a fine powdersimilar to soot. However, the main component of dieselexhaust particles (DEP) contained in the exhaust gas fromdiesel engines is carbon and is of a nanoscale size. Sincethere are concerns over the harmful health effects of DEP,it is necessary to scientifically evaluate the toxicity andrisks to the human body of fullerene and carbon nanotubeswhich are carbon-based substances of a similar size. Thetoxicity of nanoparticles is deemed to be the main potentialrisk of nanotechnology, but various other social influenceshave been also raised.

As the application of nanotechnology in industry hasadvanced, the necessity of international standardization ofnanotechnology has become clear in order to maintain theindustrial competitiveness of nanotechnology in the sameway as in other existing industries. Japan is highly depen-dent on foreign trade, so industrial competitiveness andinternational standardization are closely related to eachother. For products to gain international market share, glob-al product compatibility is essential and standardization ofthe product by the manufacturer itself is important. TheWTO/TBT (Trade Barrier Treaty) came into force in 1995,and the treaty member countries were obligated to useinternational standards when establishing technical criteria

(such as standards). As a result, establishing internationalstandards and international specifications in favor of indus-trial technologies of one’s own country is linked to thehigher competitiveness of products in the world market. Asa natural consequence, the importance of acquiring interna-tional standards (de jure standards) in the ISO and IEC,which are organizations establishing international stan-dards, is now recognized. In fact, for strengthening indus-trial competitiveness, European countries have rapidlybegun to reflect the predominance of their industrial tech-nologies to international standards such as ISO and IEC.

2. Research trends

This section describes world and domestic trends in thestandardization of nanotechnology. Efforts toward the stan-dardization of nanotechnology have started not only inEurope and the US but also in Japan and Asia. As aninternational framework, the International Dialogue onResponsibility for Research and Development of Nanotech-nology, which has the mission of promoting the researchand development of nanotechnology as a national policy,has been held since 2004.

In the US, ANSI (American National Standard Institute)and ASTM International have begun to tackle the standard-ization of nanotechnology. ANSI established the Nanotech-nology Standard Panel (ANSI-NSP) in 2004, and ANSI-NSP has determined the following order of priority for thestandardization of nanotechnology:

(1) Generic terminology in nanotechnology science(2) Systematic terminology concerning the composition

and characteristics of materials(3) Evaluation of influence and risks of toxic effect on

the environment(4) Measuring methods, analyzing methods and standard

testing methodsVarious risks of nanotechnology are cited as important

priorities in this list. On the other hand, ASTM agreed inOctober 2004 to promote the standardization of nanotech-nology, and Nanotechnology Committee (E56) was estab-lished in 2005. E56 consists of industrial, governmentaland academic people, particularly in the US, who are

210


17 International Standard

Section 3. Standardization of Nanotechnology and Risk

Management

Daisuke FujitaExtreme Field Nano Functionality Group, Nanomaterials Laboratory, NIMS

211


actively involved in the field of nanotechnology. E56 issupposed to develop concrete standards and guidelines andadjust various matters with relevant organizations with aview to international cooperation.

In Europe, CEN (European Committee for Standardiza-tion) has begun a new movement of promoting the stan-dardization of nanotechnology. The technical board (BT) ofCEN decided to establish a working group concerning nan-otechnology (CEN/BTWG 166) in March 2004. The maintask of this group is to analyze the necessity of standardiza-tion activities in this new field, develop strategies, and startvarious related activities.

In Asia, the Asia Nanotech Forum (ANF) summit washeld in 2004 under the initiative of the Ministry of Econo-my, Trade and Industry and the National Institute ofAdvanced Industrial Science and Technology (AIST) ofJapan as a common ground to discuss the research anddevelopment of nanotechnology among Asian countries.ANF is considered to be a common ground for comprehen-sive discussions including on the social influences of nan-otechnology at the moment, and ANF is important as acommon ground for discussing nanotechnology in Asia as awhole from the viewpoint of promoting national policies.In the ISO, which is an international standardization orga-nization, a committee concerning nanotechnology (TC: Forexample, TC201 Surface Chemical Analysis) has carriedout standardization activities individually, but the UK hasnow proposed that a new TC concerning nanotechnologybe established.

The movement toward the standardization of nanotech-nology in Japan started promptly in 2004 in accordancewith the trend in Europe and the US. The NanotechnologyStandardization Survey Committee was established withthe Japanese Standards Association as its secretariat underthe initiative of the Ministry of Economy, Trade and Indus-try in November 2004. The purpose of this committee is topresent a policy for drawing up specifications for the stan-dardization of nanotechnology in Japan and a policy forsubmitting proposals to the ISO.

Concerning the nanotechnology standardization activi-ties in NIMS, both ISO activities as international standard-ization and VAMAS as international joint research surveyactivities for standardization are being promoted in parallel.In the ISO activities, NIMS is working closely with TC201(surface chemical analysis). It was decided in 2004 toestablish a subcommittee concerning a scanning probemicroscope which is particularly important for nano analy-sis (SC9), and accordingly NIMS provided committeemembers and has proposed new working items, etc. Mean-while, in the ISO activities, an independent administrative

institution as a neutral organization should gather the opin-ions of experts from private enterprises and universities,and in the case of ISO/TC201, NIMS is positively cooper-ating with AIST to promote standardization. Regarding theVAMAS activities, on the other hand, NIMS promotesinternational joint research for pre-standardization in coop-eration with the international standardization activities ofthe ISO. The VAMAS has decided to establish a new com-mittee concerning nanomaterials measurement (TWA29).These actions demonstrate that standardization is beingactively studied.

3. Future trend

Standardization of nanotechnology is indispensable toguarantee the permanence of the nanotechnology industry,and standardization activities are set to make rapid progressfor several years to come. Speed is of the essence. Beforethe US and European countries solidify the general frame-works and important matters, Japan should take the initia-tive in the international standardization activities of theISO, etc. to take the lead in the standardization of nan-otechnology. Concerning the position of NIMS, it is impor-tant for NIMS to get involved in formulating de jure stan-dards which Japan is promoting because this will yieldmany benefits for NIMS. By strategically combining intel-lectual property rights such as patent rights and standard-ization, various effects can be expected such as thestrengthening of tie-ups between industrial enterprises, uni-versities and NIMS, and the promotion of intellectualinternational contribution by NIMS’ fundamental research.

4. Conclusion

Nanotechnology is expected to boost international com-petitiveness and new industries as a key technology for cre-ating a society in the 21st century. In the second-term sci-ence and technology basic plan, national resources havebeen allocated preferentially to nanotechnology, and theindustrialization and practical implementation of researchachievements are strongly desired. Accordingly, it is vitalto promote the industrialization of nanotechnology in closecooperation with industry, universities and the government,as well as standardization for securing international com-petitiveness ahead of the US and European countries. As aneutral and core independent administrative research insti-tution, NIMS has a major role to play in leading the stan-dardization of nanotechnology.

Acknowledgements

We would like to acknowledge that some of the articles published in this book refer to database

products of Web of Science® which is published by Thomson Corporation Ltd. and ScienceDirect®

which is published by Elsevier Science Ltd.

Web of Science® was used as a source for the following figures:

Yoshio Bando, Fig. 1, p. 74, Fig. 2, p. 75

Nobuyuki Koguchi, Figs. 1-2, p. 79, Figs. 3-5, p. 80, Figs. 6-9, p. 81

Hiroyuki Kumakura, Fig.1, p. 87

Takao Takeuchi, Fig. 1, p. 91

Toyohiro Chikyow, Figs. 1-4, p. 103, Fig. 5-6, p. 104

Hisatoshi Kobayashi, Fig. 1, p. 106, Figs. 2-3, p. 107, Figs. 4-7, p. 108, Fig. 8, p. 109

Yuji Miyahara, Figs. 1-4, p. 112, Fig. 6, p. 113

Chikashi Nishimura, Figs. 1-2, p. 119, Figs. 3-4, p. 120, Figs. 5-7, p. 121, Fig. 8, p. 122

Hiroshi Harada, Toshiji Mukai, Masuo Hagiwara, Toshiyuki Hirano, Youko Yamabe-Mitarai,

Satoshi Kishimoto, Yoshihisa Tanaka, Akira Ishida, Takahiro Sawaguchi,

Fig. 1, p. 143, Figs. 2-3, p. 144

Keijiro Hiraga, Noriko Saito, Figs. 1-2, p. 156, Fig. 3-6, p. 157, Fig. 7-8, p. 158

Hideo Kimura, Xiaobing Ren, Shuichi Hishita, Fig. 1, p. 160, Fig. 2, p. 161

Kenji Kitamura, Figs. 1-3, p. 164

Yutaka Kagawa, Figs. 4-5, p. 171

ScienceDirect® was used as a source for the following figures:

Yoshio Sakka, Figs. 1-2, p. 77


Date of publication: March 1, 2006Tomoaki HyodoPublication Secretariat of the Materials Science OutlookInternational Affairs OfficeNational Institute for Materials Science1-2-1 Sengen, Tsukuba, Ibaraki 305-0047, JapanTel: 81-29-859-2749Fax: 81-29-859-2049E-mail: [email protected]://www.nims.go.jp

S If you have any opinions or questions about this book, please contact the above.

© 2005 National Institute for Materials Science, Printed in Japan. All rights reserved.

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