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Page 1: Present Status of Neutron Instruments - KEK

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Present Status of Neutron Instruments

Neutron Science Section, Materials and Life Science Division,

J-PARC CenterJapan Atomic Energy Agency

Yukinobu Kawakita

Page 2: Present Status of Neutron Instruments - KEK

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23 Neutron Beam Ports

Operation: 21 (April, 2018)

Commissioning:0

4SEASONS (JAEA)

HRC (KEK)

ANNRI(Tokyo Tech. U., JAEA,, Hokkaido U.)

SHRPD(KEK)

NOBORU (JAEA)

SOFIA (KEK)

iBIX (Ibraki Pref.)

iMATERIA (Ibraki Pref..)TAKUMI (JAEA)

NOVA (NEDO, KEK)

AMATERAS(JAEA)

PLANET (JAEA, U. of Tokyo)

DNA (JAEA)

SENJU (JAEA)SHARAKU(JAEA)

SPICA(NEDO, KEK)

Operation Operation

Operation

Operation

Operation

OperationOperation

Operation

Operation

NOP(KEK)

OperationOperation

Operation

Operation

Operation

Operation

Operation

VIN_ROSE(KEK, Kyoto Univ.)

RADEN (JAEA)

POLANO (Tohoku Univ,, KEK)

Neutron Instruments in MLF

Operation

Operation

Operation

TAIKAN(JAEA)

VIN-ROSE (NSE): opened to users @2017B

Operation

POLANO(Polarization Analysis Spect.)

Opened to users @2019A

Operation

Page 3: Present Status of Neutron Instruments - KEK

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MLF Percentile Top 10 2019

Source data @ 2021-01-08Citation data @ 2021-01-13Figure revision @ 2021-02-08

Rank被引用回数

CNCI Percentile タイトル 雑誌名 ESI22分野 Inst.

1 42 12.25 0.38 Colossal barocaloric effects in plastic crystals NATURE PHYSICS BL14

2 34 9.91 0.63A new approach for measuring the muon anomalous

magnetic moment and electric dipole momentPROGRESS OF THEORETICAL AND EXPERIMENTAL PHYSICS

PHYSICS D2

3 22 6.41 1.71Topological transitions among skyrmion- and hedgehog-

lattice states in cubic chiral magnetsNATURE COMMUNICATIONS PHYSICS BL15

4 19 5.54 2.28Skyrmion phase and competing magnetic orders on a

breathing kagome latticeNATURE COMMUNICATIONS PHYSICS BL15

5 15 4.37 3.64Large Anomalous Hall Effect in Topological Insulators with

Proximitized Ferromagnetic InsulatorsPHYSICAL REVIEW LETTERS PHYSICS BL17

6 14 4.08 4.16Unique Helical Magnetic Order and Field-Induced Phase in

Trillium Lattice Antiferromagnet EuPtSiJOURNAL OF THE PHYSICAL

SOCIETY OF JAPANPHYSICS BL18

7 12 3.50 5.68Characteristic fast H- ion conduction in oxygen-substituted

lanthanum hydrideNATURE COMMUNICATIONS PHYSICS BL21

8 12 2.32 10.85Reversible elastocaloric effect at ultra-low temperatures in

nanocrystalline shape memory alloysACTA MATERIALIA

MATERIALS SCIENCE

BL19

9 8 2.33 11.27Coexisting spin resonance and long-range magnetic order

of Eu in EuRbFe4As4PHYSICAL REVIEW B PHYSICS

BL01, BL18,

LabCROSS

10 11 2.13 12.50Plastic anisotropy and deformation-induced phase

transformation of additive manufactured stainless steelMATER SCI ENG A STRUCT

MATERMATERIALS

SCIENCEBL19

◼ Worlds' leading high quality scientific papers were published from MLF.

◼ The 1st Nature from MLF published in 2019.

◼ MLF high quality papers cover issues from functional materials to basic solid-state physics.

Page 4: Present Status of Neutron Instruments - KEK

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MLF Percentile Top 10 2018

Source data @ 2021-01-08Citation data @ 2021-01-13Figure revision @ 2021-02-08

Rank被引用回数

CNCI Percentile タイトル 雑誌名 ESI22分野 Inst.

1 49 4.60 3.00Liquid-like thermal conduction in intercalated layered

crystalline solidsNATURE MATERIALS

MATERIALS SCIENCE

BL02, BL14

2 34 3.19 5.83Exceptional phase-transformation strengthening of

ferrous medium entropy alloys at cryogenic temperaturesACTA MATERIALIA

MATERIALS SCIENCE

BL19

3 20 2.98 6.70Topological spin excitations in a three-dimensional

antiferromagnetNATURE PHYSICS PHYSICS BL01

4 23 2.65 7.52Graphene-based ordered framework with a diverse range

of carbon polygons formed in zeolite nanochannelsCARBON CHEMISTRY BL21

5 28 2.63 8.08 Retreat from Stress: Rattling in a Planar Coordination ADVANCED MATERIALSMATERIALS

SCIENCEBL14

6 18 2.68 8.11Effect of rattling motion without cage structure on lattice

thermal conductivity in LaOBiS2-xSexAPPLIED PHYSICS LETTERS PHYSICS BL14

7 17 2.53 8.91Three-Dimensional Fermi Surface of Overdoped La-Based

CupratesPHYSICAL REVIEW LETTERS PHYSICS LabCROSS

8 25 2.35 9.66Lithium-ion conducting oxide single crystal as solid electrolyte for advanced lithium battery application

SCIENTIFIC REPORTSMATERIALS

SCIENCEBL18

9 15 2.23 10.91Three Dimensional Polarimetric Neutron Tomography of

Magnetic FieldsSCIENTIFIC REPORTS PHYSICS BL22

10 18 2.07 11.65Elucidating the Solvent Effect on the Switch of the Helicity of Poly(quinoxaline-2,3-diyl)s: A Conformational Analysis

by Small-Angle Neutron Scattering

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY

CHEMISTRY BL15

Page 5: Present Status of Neutron Instruments - KEK

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Outcomes from MLF (publications)

0

100

200

300

400

500

600MLF

SNS

ISIS

Annual trend of publications

◼ Number of publications are increasing steadily.*Rapid increase at '14, '15 and '18 were caused by work shopproceedings.

◼ PP10% is keeping ~5%.

Comparison with other pulsed neutron facilities

◼ Still we are rather behind SNS & ISIS.

◼ Increasing rate is smaller than that of SNS.

Publication year

Num

ber

of publications

Pro

portio

n o

f the to

p 1

0%

public

atio

ns0%

5%

10%

15%

20%

25%

30%

0

50

100

150

200

250

300Others

Dr. thesis

Proceedings

Paper

PP10%

Page 6: Present Status of Neutron Instruments - KEK

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Num

ber

of publications

Num. pubs. (paper & proc.) Source data @ 2021-01-08

Figure revision @ 2021-01-13 2006-2020

0

20

40

60

80

100

120

140

160

Proceedings Paper

Page 7: Present Status of Neutron Instruments - KEK

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0.0%

10.0%

20.0%

30.0%

40.0%

50.0%

60.0%

70.0%

80.0%

90.0%

100.0%

0

50

100

150

200

250

Public

atio

nra

teN

um

ber

ofpro

posa

ls

Proposal round

Conducted

Published

Publication rate

Publication rate (2008B-2020A)◼ Publication rate for proposals before 2016 is ~40%, which is close to the

worlds' standard (?) value 50%.

Page 8: Present Status of Neutron Instruments - KEK

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MLF general proposal

0

100

200

300

400

500

600

700

➢ Number of Proposals & Performed Experiments in 2009A to 2020B+2021A

Term

Adopted Reserved & unadopted Conducted

Hadron accident

Target trouble

Earthquake

Fire in MLF

Page 9: Present Status of Neutron Instruments - KEK

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Page 10: Present Status of Neutron Instruments - KEK

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Scientific Outcomes in 2020

Page 11: Present Status of Neutron Instruments - KEK

BL03 iBIX

Fukuda et al., PNAS, 117, 4071–4077(2020)

His244

Asp96 Hydroxide ion

Neutron crystal structure of CuNiR

High-resolution neutron crystallographyvisualizes an OH-bound resting state of acopper-containing nitrite reductase (CuNIRs)

CuNIRs transform nitrite togaseous nitric oxide, which is akey process in the globalnitrogen cycle

A hydroxide ion can exist as a ligand to the catalytic Cuatom in the resting state even at a low pH.

OH-bound Cu site is unexpected from previously given X-ray structures but consistent with a reaction intermediatesuggested by computational chemistry.

Dynamics of proteins with different molecularstructures under solution condition

Folded(globular)

Unfolded(Intrinsically Disordered Protein(IDP))

FWHM

FWH

M (

meV

)

Folded

Unfolded

The internal dynamics were related to the highlysolvent exposed amino acid residues depending uponprotein’s structure. The dynamical prosperitiesdependent on structure should be essential forprotein function.

Rigid Flexible

IDP is characterized bysolvent exposed flexibleamino acid, which shouldcontribute the recruitingthe target molecule.

QENS spectra of proteinin diluted solvent can beobtained.

Q-dependence of FWHMindicates that amino acidchain is more diffusive inunfolded than folded.

BL02 DNALife Science

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Page 12: Present Status of Neutron Instruments - KEK

Experimental Visualization of InterstitialcyDiffusion Pathways in Fast-Fluoride-Ion-conducting Solid Electrolyte Ba0.6La0.4F2.4

305 K

512 K

NPD patterns and crystal structure of Ba0.6La0.4F2.4

obtained by Rietveld refinement.

MEM nuclear density distribution at 512 K and electrical conductivity of Ba0.6La0.4F2.4 .

K. Mori, et al., ACS Appl. Energy Mater. 3, 2873 (2020).

F- diffusion in solid electrolyte Ba0.6La0.4F2.4 was investigated by MEM analysis and was found to be based on an interstitialcy diffusion mechanism.

BL09 SPICA BL08 SuperHRPD

Getting through the bottleneck—A new class of layered perovskite with high oxygen-ion conductivity

Crystal structure and oxide-ion diffusion pathway of tetragonal CsBi2Ti2NbO9.80(2) at 973 K.

Comparison of bulk conductivityσb of CsBi2Ti2NbO10−δ (CBTN) oncooling with those of best oxide-ion conductors.

M. Yashima, et al. (Tokyo Tech)Nature Communications 11, 1224 (2020).

Crystal Structure and Ion Diffusion Path Analysis using SuperHRPD Reveals Cause of High Oxygen Ion Conductivity.

Battery Science

11/34

Page 13: Present Status of Neutron Instruments - KEK

Topological transitions among skyrmion-And hedgehog-lattice states

Fig 5. Schematics of topological multiple-q spin textures and two-step magnetic transitions in MnSi1−xGex.Y. Fujishiro, et al., Nature Commun. (2019).

It was observed three different topological spin textures with variation of the lattice constant controlled by Si/Ge substitution: two-dimensional skyrmion lattice and two distinct three-dimensional hedgehog lattices.

BL15 TAIKANCooperative deformation in high-entropy

alloys at ultralow temperatures

At ultralow temperature, the increase in the num-ber of grains with (111) orientation to the loa-ding dir. becomes slower due to the occurrence of stacking faults

At ultralow temperature, dislocation glides and stacking faults mutually occur

M. Naeem et al., Science Advances 6 (2020) eaax4002

CoCrFeMnNi alloy

At ultralow temperature, high entropy alloy shows in-creases in the strength and ductility → in situ loading at ultralow temperature

BL19 TAKUMI

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Page 14: Present Status of Neutron Instruments - KEK

Origin of the Difference in Ion-Water Distances for Aqueous NaCl and KCl SolutionsSimultaneous least squares fitting procedures wereperformed for X-ray and neutron interference termsobserved for (NaCl)x(

*H2O)1-x and (KCl)x(*H2O)1-x.

The difference in ion-water distance observed from X-rayand neutron diffraction studies mainly arises from theunited atom model of X-ray diffraction data analysisassuming a spherical electron density around oxygenatom within the water molecules..

Kameda et al., Bull. Chem. Soc. Jpn. (2019)

BL21 NOVA

Y. Higuchi et al, Phys.Chem.Chem.Phys., 2021, 23, 1062

Water/ice identification by energy selective imaging for fuel cell application.

Difference in the energy dependent cross section between liquid water and ice enables us to distinguish them.

Energy dependence of the cross sectionratio a between ice and water

Image of the cross sectionratio b between ice and water during thawing process.

BL22 RADEN

13/34

Page 15: Present Status of Neutron Instruments - KEK

Identification of hydrogen species on Pt/Al2O3 by INS measurement

Hydrogen (H) species adsorbed on catalyst surfaces are key intermediates in catalytic hydrogenation reactions over supported metal catalysts.

➢ However, individual identification of H species on the metal catalysts was not clear…

Successfully elucidated the H species on Pt/Al2O3 by the combination of INS and DFT

S. Yamazoe et al.,Catalysis Science & Technology 11 (2021) 116

(Kyoto U., TMU, TUT, JAEA, CROSS, U. Tokyo)

In C2H4 hydrogenation reaction

- hydride/atop Pt–H- bridged perimeter/terrace

Pt–H–Pt- threefold Pt3–H

- edge Pt–H–Pt

BL01 4SEASONS

Magnetic excitation in spin-1/2 anisotropic triangular lattice antiferromagnet Ca3ReO5Cl2

✓ magnetic ground state and excitation in frustrated spin systems

✓ anisotropic triangular lattice antiferromagnet with interactions J and J’

K. Nawa et al., Phys. Rev. Res. 2, 043121 (2020)

2D1D

J’/J = 0 J’/J = 1wellunderstood

BL14 AMATERAS

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Page 16: Present Status of Neutron Instruments - KEK

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Instruments

Please see our web page https://mlfinfo.jp/en/beamlines.htmlto find specification of each instrument.

Commissioning of New Instruments

POLANOVIN ROSE

Page 17: Present Status of Neutron Instruments - KEK

POLANO enables polarization analysis of inelastic scattering in the dynamics of multiple degrees of freedom

summary

BL23 POLANO (Polarized Neutron Spectrometer)

Although the polarized neutron technique has been developed and used for many years, the application of the time-of-flight (TOF) method has only been realized in recent years. In the light of recent discoveries in material science, many of the observed complex phenomena are largely due to the entangled physical degrees of freedom of spins, charges, orbitals, and even lattice vibration. In neutron scattering experiments, a unique, effective, and direct way to observe these properties separately via the polarization analysis. The POLANO enables polarization analysis of inelastic scattering experiments to investigate the dynamical properties of the above mentioned multiple degrees of freedom.

Research: Dynamics of spin, orbital, charge, and lattice in magnetic, superconducting, functional materialsFeatures: POLANO is a direct geometry spectrometer with middle energy and spatial resolution. Combination of SEOP 3He gas spin filter and 5.5 Qc bending mirror analyzer makes it possible higher-energy polarization experiment.

16/34

Page 18: Present Status of Neutron Instruments - KEK

Helium spin filter polarizer SEOP Magnetic system for polarization

BL23 POLANO (Polarized Neutron Spectrometer)

Development of spin polarizer, spin exchange optical pumping on-beam SEOP

guide field system

asymmetric Helmholtz-coil

Figure of merit P x sqrt(T) optimized for 100 meV neutron energy

Development of magnetic devices for polarimetry at POLANO

Helmholtz coil used in vacuum chamber has to be effectively cooled down to reasonable temperature. Cooling system with flange was developed.

220K -> 55K

SEOP system including controlling system have been developed, manufactured and tested (off-beam). Now installing in the BL

30 atm cmK & Rb hybrid cellGE180 Cell

60 (100) mm φL = 60 (100) mm

3He = 3.5 atmlong life timeappropriate K/Rb ratio

small “X” factor

fun-shaped magnet (permanent 30 G)

SEOP solenoid coils and guide fields

Helmholtz coil

supermirror analyzer(400 G)

In addition to the Helmholtz coil, SEOP solenoid, permanent magnet guide field,Helmholtz coil,fun-shaped guide field,analyzer mirror

17/34

Page 19: Present Status of Neutron Instruments - KEK

BL23 POLANO (Polarized Neutron Spectrometer)

Commissioning with "unpolarized" neutron is nearly completed

High-energy neutron spectroscopy in hydrogen material ZrH2

Incident neutron energy: Ei = 485 meV

Clear incoherent spectra originated from hydrogen atoms are ob-served. This experiment has been done under a part of the KEKsummer student program.

POLANO beam time has been opened to a part of user program

Absolute flux value from Au-foil [email protected]✕ 10^8 [n/cm2/s@1MW] (below Cd cut-off energy)corrections of, self-shielding, efficiency of Ge-detector, irradiation & cooling

3He [email protected]✕ 10^8 [n/cm2/s@1MW] (below Cd cut-off energy)efficiency, frame-overlap

evaluation of neutron flux

first inelastic signal at POLANOcross-section of neutron beam

left:Simulated beam cross-section at sample position. Some energy range are integrated. (top: 2d, bottom: 1d cut)

right:Observed beam cross-section at near sample position. Integrated energy range is little bit different from simulation.

high-energy excitation in hydrogen material

Experiments with “unpolarized” neutron on 1D material CsVCl3

show palm tree structure at 1 Å-1 originated from magnetic spin fluctuation. (also, Q=3 Å-1)

S = 3/2TN = 13.3 Kmeasured at T = 20 Kbackground subtracted

1D AFM spin chain

18/34

Page 20: Present Status of Neutron Instruments - KEK

Dynamical behaviors from ps to sub-µs

Research: Relaxation properties of small molecules such as water, etc. Diffusion of liquid molecules and assembly. Slow dynamics of glass and large scale structures of magnetic materials and ferroelectrics.Features: Intermediate structure factor I(Q, t) could be observed directly. The highest energy resolution without losing intensity.

summary

BL06 VIN ROSE (Neutron Resonance Spin Echo Spectrometers)

The neutron spin echo (NSE) technique is an essential spectroscopic method, which has achieved the highest neutron energy resolution at the present moment. NSE with a pulsed neutron source makes it possible to scan a wide spatiotemporal space very efficiently. Kyoto University and KEK are jointly installing two types of NSE spectrometers at BL06, that is, a neutron resonance spin echo (NRSE) instrument and a modulated intensity by zero effort (MIEZE) instrument. Both NRSE and MIEZE make use of neutron resonance spin flippers, which made it possible to design and install compact and multiple spectrometers machines in a narrow space. We named the beam line “VIN ROSE” (VIllage of Neutron ResOnance Spin Echo spectrometers), which will spawn a new field of spectroscopic methods.

19/34

Page 21: Present Status of Neutron Instruments - KEK

BL06 VIN ROSE

Sample Environments

(Neutron Resonance Spin Echo Spectrometers)

Large 2D detector “MPix”

Elliptic focusing mirrors

4K GM Cryostat

Max. 0.6T Electromagnet

32cm × 32cm large2D detector withMPPC sensors.

Sensitivity ofthe detector.

Scattering profile of astandard sample (GlassyCarbon) and comparisonwith the result given by NIST.

Extremely large ellipsoidal mirrors (900mmlength) to focus neutron beam have beendeveloped for BL06. The ellipsoid are 1250mm and 65.4 mm, respectively. The interior ofthe ellipsoid is coated with m = 6 NiC/Tisupermirror.

6Qc

10mm

20/34

Page 22: Present Status of Neutron Instruments - KEK

Spin dynamics of skyrmions in MnSiFormulation of TOF MIEZE

BL06 VIN ROSE (Neutron Resonance Spin Echo Spectrometers)

The phase and frequency of TOF-MIEZE signal are affected bythe two factors, namely, the MIEZE condition (distancerestriction) & wavelength distribution.

Phase shifts due to different wavelengthswith different energy distributions.

Phase and frequency shiftsdue to the distance condition(the MIEZE condition).

Phase correction can be realized with a2D-detector. ↓

Oda et al., Phys. Rev. Applied 14, 054032 (2020).

NSE experiments with magneticfield at the sample position can berealized with the MIEZE technique.

Nakajima et al., Phys. Rev. Research 2, 043393 (2020).

Very high q resolution can beachieved in combination withTOF method and a RPMT 2Ddetector, which contributes toexplore the phase transitiondynamics in detail.

21/34

Page 23: Present Status of Neutron Instruments - KEK

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Progress in Instrumentation

Page 24: Present Status of Neutron Instruments - KEK

The new T0 chopper doubled the intensity compared with a previous experiment

Replacement of the T0 chopper:Max. speed 25 Hz → 100 Hz

Installation of the new T0 chopper →

← Transmission of the new T0 chopper as a function of neutron energy

Iron-based superconductor Ba0.75K0.25Fe2As2

ħω = 200 meV

Magnetic excitations at ħω = 200 meV

by using Ei = 500 meV →

High-energy magnetic excitations originating from the electronic band structure

By the Technology Development Section

BL01 4SEASONS4D-Space Access Neutron Spectrometer

InstalledAgingSi111

-30<2q<150

Si311-150<2q<-42(-126<2q<-54 in 2020) Upgrade

Analyzer mirror aging of Si111

& grade-up of Si311

The banks with

damaged Si111

mirrors with Gd

back coating will be

replaced to the

refabricated Si111

mirrors with Gd2O3

back coating.

Single crystal QENS

Diffusion

paths of

Li ions

Garnet type Li conductor7Li6.5La3Zr1.5Nb0.5O12

(LLZNO)

(hhl)

plane

[h-h0]

direction

single crystal

Simulation of QENS width

QENS width

Si111 Si311

BL02 DNABiomolecular Dynamics Spectrometer

23/34

Page 25: Present Status of Neutron Instruments - KEK

Addition of new area-detectors

㊵ ㊴㊳

Direct beam

㊴ ㊳

Four area-detectors were added in the obliquely downward direction of the sample position.

Sample:Ruby

R(I>5s(I):0.0519

BL18 SENJUVersatile Single-Crystal Diffractometer

Testing of new 2D detectorWSLF

➢ One candidate of future detectors for materials engineering diffractometer has been developed and the operation has been tested

➢ Set at the bottom of 90° scattering detector bank to observe and compare with the present detectors (ENGIN-X type detectors)

Prototype scin-tillator 2D detec-tor with WSLF(made by Neutron Device Sect.)

Pixel size: 3 by 3 mm2

@~45 deg scattering angle

BL19 TAKUMIEngineering Materials Diffractometer

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Page 26: Present Status of Neutron Instruments - KEK

Ultra-precise focusing mirror

0.13 mm in FWHM, 0.3mm in full width was achieved!

Collaboration with RIKEN and Kyoto Univ.

Open for uses!

x2

BL16 SOFIA Horizontal-type reflectometer

Development of spatially resolved neutron reflectometry technique

Spatially resolved neutron reflectometry (NR) measurement with sheet-shaped beam and tomographic reconstruction enabled to obtain the direct imaging of the lateral structure and the local analysis of the depth distribution of SLD.

Langmuir, 37, 196 (2021)

This method allow the NR analysis for a local are as small as 0.001 cm2.

BL17 SHARAKU Polarized Neutron Reflectometer

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Page 27: Present Status of Neutron Instruments - KEK

BL21 NOVAHigh Intensity Total Diffractometer

SiO2

capillary3D radial

collimatorCd coated plates

Background reduction effect by 2D collimatorwas verified by refinements of S(Q) and G(r).S/N will be improved even for mg order of samples.

High S/N sample environments for small amounts of samples

6

80.01

2

4

6

80.1

2

4

6

81

Re

liabili

ty f

acto

r

100

101

102

103

104

Time / sec

Si (NIST SRM 640d) − 500 kW − 900 kW

Z-Rietveld Rwp

Re

PDFgui Rw

Required measurement time

5-min measurement of Si powder at 900 kW operationis enough to refine the diffraction pattern, but PDFanalysis needs 1 h.The coordination numbers of SiO2 glass rod wereconverged for 200 sec or more at 900 kW.

High Resolution Imaging

2.3

mm

High spatial resolution of ~10µm has been achieved using a new apparatus.

MTF = 10.5µm

Improve temporal limitTOF gate of Image Intensifier improved exposure time texp of energy selective imaging.

Energy selection by disc chopper:

texp=6min

Energy selection by Image Intensifier:

texp=50sec

• 短波長(1st frame),長波長(2nd frame)について,それぞれ撮像条件を探索した

光IIのgainは900,積算は10枚

以下「delay(ms)-width(ms)-pulse数」と表記

12

高速撮像試験

長波長-0-17.8-75. 短波長-3.88-7.82-10.

水入りキャピラリー 空キャピラリー

石英セル

Water in capillaries f1

100 mm

With water Empty

Quartz cell

Upgrade

BL22 RADEN Energy-Resolved Neutron Imaging System

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Page 28: Present Status of Neutron Instruments - KEK

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Sample Environment

Page 29: Present Status of Neutron Instruments - KEK

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Trends for remote & automation PRISM budget from the government(public-private investment promotion

for research development ) 55M¥

Adding remote func.

Communication toolsDesktop sharing software

PC for data analysis

Data storage

Portalserver

Device controlling

PC

Adding Automation for Exp. Process

Gas gene. w. control.

Humidity & HW/LW ratio

Sample Changer w. control. T

Rapid cooling sample stick

Standard sample cells

LN automatic supplier for pulse mag.

N. Camera for sample

positioning

Low T system for loading

machine

Page 30: Present Status of Neutron Instruments - KEK

Automated Measurement and Batch Processing of Data Reduction

The maximum sample number will be increased up to more than 40.

The large number of the observed data is converted to the neutron reflectivity profiles in a batch process. The parameters such as the normalization factor and divergence correction is automatically optimized.

The automatic sample changer and auto-alignment was implemented. The sample up to 16 samples are automatically observed.

BL17 SHARAKU Polarized Neutron Reflectometer

SE automation & remote

Auto sample-changer (20 samples for biomatters, commissioning)

Sample stick with three cells holding PEACE (3 samples, wide T range 5K-400K) DNA vacuum chamber

Cryostat

TM

P

TMP

DIC

EDICE Automatic IVC atmosphere controlling device

Blue cryostat(1.5K-300K) Maintenance free for 4days. 100 mK with a dilution stick.

Oscillating radial collimator

direct beam

motor

Others (planed)Furnace <1100⁰C Magnet 3.5 TeslaA new convergence guide mirror

BL02 DNABiomolecular Dynamics Spectrometer

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Page 31: Present Status of Neutron Instruments - KEK

3He Cryostat

LA bank 1.10 K- 1.00 K

c2 = 1.39

QA bank 1.10 K- 1.00 K

c2 = 1.26

The 3He cryostat (the lowest temp is 0.9 K) was commissioned and released for general user from 2020B cycle.

The high resolution of profile using the cryostat can detect very tiny lattice change caused by magnetic transition.

Magnetic structure analysis can be performed using the data collected by the multidirector banks.

BL08 SuperHRPDSuper High Resolution Powder Diffractometer

Superconducting Magnet

H =5 T

H =0 T H =3 T

A superconducting magnet is available at H ≤ 5T after long commissioning due to vacuum leak.

Ba2MnGe2O7

single crystal 1.85 g

BL12 HRCHigh Resolution Chopper Spectrometer

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Page 32: Present Status of Neutron Instruments - KEK

Improvement on CCR

➢ To improve performance of CCR and reduce the BG, a slimmer and lighter thermal shield was adopted

After

Before

➢ To suppress a slow increase in T due to outgas adsorption, a room-temperature shield was tested

Before

After

Achievement

cooling time and the lowest temperature were successfully improved

Future plans

room-temperature shield / cryocoil & polycoldsystem will be installed

BL14 AMATERAS Cold-Neutron Disk-Chopper Spectrometer

Temp. range spec.4.2K-800K(Reached ~3.5K in commissioning.)

0 1 2 3 4 5 6 7 80

1

2

3

4

5

6

7

0

200

400

600

800

1000

1st test (moderate)

2nd test (excess gas)

4 K Cryostat

Avg. Sample T (K)

103

1st test (moderate)

2nd test (excess gas)

4 K Cryostat

Inte

g.

inte

nsi

ty (

arb

. u

nit

s)

(1/2 0 1/2)

(0 1 5/2)

Co2(OD)3Br

5.19

5.22

5.25

6.2

6.3

6.4

6.5

560 600 640 680 720 760 800

90

93

96

99

bm

am/√3

ah

T ~ 736 K

(Tref ~ 750 K)

Na2CO3

cm

Lat

tice

par

amet

ers

(Å)

ch

betam

bet

a an

gle

(°)

T (K)

betah

Low & high temp. commissioning

Calibration of sample temperature and determination of PID and other conditions are in progress.

Commissioning of Cryo-furnace

BL08 SuperHRPDSuper High Resolution Powder Diffractometer

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Page 33: Present Status of Neutron Instruments - KEK

Commissioning of Cryofurnace Commissioning of Cryostat

SE automation & remote

- Beamline dedicated to the next generation battery.- Optimized for operando observations of working batteries. - Cryostat and cryofurnace have been commissioned to meet

the requirements for various temperature environments from wide research fields.

Sequential Phase transitions of BaTiO3

- Sample exchange : Top-loading- Temperature range : 20 ~ 600 K- Sample holder: V-Ni alloy can, φ 6 mm- Beam height : max. 20 mm- New sample rod under development, to increase maximum

temperature and to improve temperature precision.

- Sample exchange : Top-loading- Temperature range : 4 ~ 300 K- Sample holder: V-Ni alloy can, φ 6 mm- Beam height : max. 20 mm

Cryofurnace & Cryostat

- Automation of temperature control and measurement sequences.

- Remote operation of temperature-controlled measurements (Access to JLAN network required)

- Sample exchange procedures : Development for partial automation underway (ex. vacuum valves or temperature controls).

Time dependence of the temperature at sample position

Cryoufurnace

Cryostat

Standard setting

NPD patterns of NIST-Si powder

BL09 SPICA Special Environment Powder Diffractometer

BL09 SPICA Special Environment Powder Diffractometer

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Page 34: Present Status of Neutron Instruments - KEK

Starting to use the loading machine with induction heating in user program

Crosshead speed< 1000 mm/min

A Fe-C-Mn alloy was heated to 1273 K with 5 K/s, held for 300 s (single austenite temp), then rapid cooled to

938 K (pearlitic transformation temp) and subsequently compressed with a strain rate of 0.0004 s-1 down to 50%

Highest temp: 1573 K

Heating/cooling rate < 30 K/s

BL19 TAKUMIEngineering Materials Diffractometer

BL20 iMATERIAIBARAKI Material Design Diffractometer

Maximum loading 50 kN

Temp range:RT – 1273 K

The texture changes corresponding to stress vibrations during high-T tensile deformation was observed.

The universal deformation testing machine

In-situ neutron diffraction environment simulating the microstructure control process of metallic materials

Temp range:RT – 1273 KHeating Speed: 10 K/sCooling Speed:>20 K/s

When bainite transformation occurs during

isothermal holding at 673 K, austenite with

low carbon concentration is gradually

consumed, and austenite with high carbon

concentration appears.

The rapid heating/quenching furnace with an automatic sample changer

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Page 35: Present Status of Neutron Instruments - KEK

Summary

Publication number keeps increasing.

Although average paper quality must be improved, many

exciting results outcome.

For instrumentation, we are making effort to improve

optics.

Automation of sample environment and remote access

are key functions to make neutron science sustainable

even under the pandemic situation, which may change

future utilization way of large facilities.

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