structure processing properties - ku leuven · ceramics research group ... •colloidal processing...

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Dept. Metallurgy and Materials Engineering, K.U.Leuven

The MTM triangle

Processing Properties

Structure

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ZAP (Professors): ATP (Technical support):Prof. Omer Van der Biest Joop VandeursenProf. Jef Vleugels Wout Veulemans

Olivier Van RoeyMohammed Abid

Postdoctoral Researchers: Visiting scientists:Dr. Bernd BaufeldDr. Shuigen HuangDr. Kim VanmeenselDr. Songlin RanDr. Bram Neirinck

PhD students: PhD students:Tina Mattheys Annabel BraemSwarnakar Akhilesh Kumar Olivier MalekLi Zhang Ezhil JothinathanKhuram Shahzad

Ceramics research group


Activities ceramics research group

• Powder synthesis (sol-gel, carbo- and borothermal reduction)• Powder metallurgical shaping•Colloïdal shaping by electrophoretic deposition (EPD)•Sintering (pressureless, hot pressing, microwave, SPS)

Processing of ceramics

Microstructural analysis and functional properties•Microstructural analysis (SEM, EPMA, XRD, TEM)•Mechanical properties (hardness, toughness, strength, etc.)•Elastic and damping properties at room and elevated temperature•Chemical compatibility

Modelling•Electrophoretic deposition (EPD)•Functionally graded materials (FGM)•Damping•Field assisted sintering technology (FAST, SPS, PECS)


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Ceramic Materials under investigation

Gra ded mate rials

Reinforce d ceramicCompo sitesMatrix: Y-TZP,C e-TZP,SiN,AlOAd dition: AlO,TiB ,TiN,TiCN,TiC,W C,...342323 2 B orosilicate, MA S and BMAS witSiC f ibresC eramic mat rix composite s

Cerm etsGlass-ce ramicsBariumalumin osilicates (BAS)M agnesiumalum inosilicates (MA S)WC/Co -based

Fibre-rei nforcedPlatelet-r einforcedSiAlON,mullite and AlO withAlOpl atelets2323

MonolithsOxides

SiAlON, Si3N4SiC, TiB2, TiN, TiCN,

WC, ZrB2, B4C,etc

Composites

Ceramic matrix compositesMatrix: Si3N4, ZrO2, Al2O3, ZrB2, TiB2Additive: Al2O3, TiB2, TiN, TiC, TiCN,

WC, NbC, ZrC, HfC, HfTiC, ZrN,B4C, SiC, etc.

Glass-ceramicsBariumaluminosilicate (BAS)

Magnesiumaluminosilicate (MAS)

CermetsWC-Co, TiCN-based

NbC-based

Reinforcedceramics

Fibre reinforced

Platelet reinforced

Borosilicate, MAS & BMAS with SiC fibres

Sialon, Al2O3, mullitewith Al2O3 platelets

GradedMaterials

Functionally graded (FGM)

Laminates

Coatings

ZrO2/Al2O3 & ZrO2/WCWC-Co/WC-Co

TiCN-based/WC-CoCe-TZP/Y-TZP

SiC / graphite & SiC / porous SiC

Metal / ZrO2WC-Co / steel

Non-oxides

Mullite, Al2O3Y-TZP & Ce-TZP

Mixed stabiliser ZrO2


Research Topics

• Processing and characterisation of functionally graded materials (FGM)

• Colloidal processing by means of electrophoretic deposition (DC & AC-EPD)

• Development and characterisation of ceramic, CMC’s and cermets

• Modelling and application of field assisted sintering (FAST, SPS, PECS)

• Investigation of elastic and damping properties of materials

• Cutting tool development and chemical compatibility assessment

• Nanomaterials and nanocomposites (biomaterials, photovoltaics, batteries)

• Processing of Porous materials (ceramics, glass & metals)

• Mechanical alloying

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Cutting tool development and chemical compatibility studies

DEVELOPMENT OF NEW CUTTING MATERIALS, TOOLS, MACHINE CONCEPTSAND TECHNOLOGIES FOR DRY HIGH SPEED CUTTING


• New composites• Chemical wear assesment• Gradient materials

Cutting tool development


Dry machining of cast iron with siliconnitride tools

Dry drilling of cast iron at 450 m/min

Dry machining of cast iron with ceramic composite tools

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Chemical compatibility assessment


Workpiecematerial

Ni-Cr or Ni-Al wire

Tool material

Drill core

Coating

WorkpieceExperimental parametersTemperatureHolding timeMechanical load

Al2O3

WorkpieceToolNimonic 105

Fixed


K40

E

Steel

Temperature (°C)300 350 400 450 500 550 600 650 700

Log

solu

bilit

y (lo

g(cm

3 /m

ole)

)

-20-18-16-14-12-10

-8-6-4-202

ZrO2

TiN

TiCTiB2

Al2O3

Si3N4

WCSiC

Ni3Al

CoNiTi

C

Chemical compatibility assessment

Interaction couples Equilibrium solubility calculations

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Fracture toughness

The

rmal

resi

stan

ceW

ear

resi

stan

ce (

Har

dnes

s)

Functionally graded materials (FGM)

To combine irreconcilable properties in the same component by engineering a gradient in composition and concomitant properties

Electrophoretic deposition (EPD)


Colloidal processing technique in an electric field_

electrode

+

• Particles are charged by interactionwith the solvent and additives

• Charged particles move under the influence of an applied electric field (electrophoresis)

• Partices form a growing deposit onthe deposition electrode (deposition)

+Charged particlesCationsAnions

suspensionelectrode

++

+

+

_

_

_+

_

_

V

_

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Electrophoretic deposition (EPD) of FGM


+ -FGM set-up

Gradient profile

Thickness gradient

100%

Composition

Applications:

• Gradient materials• Laminates• Coatings (nm-mm)• Infiltration• Textured materials• Save processing of nanopowders

Graded Tribological Materials Formed by Electrophoresis

EPD of FGM and coatings


20 µm

0

1

2

3

4

5

6

7

0 1 2 3 4 5 6

distance from electrode surface side (mm)

Ti(C

,N) c

onte

nt (w

t%)

12131415161718192021

HV

(GPa

)

experimental

theoretical

Ti(C,N) ↑ Ti(C,N) ↑

Cutting tool inserts : WC-Co-Ti(C,N)/ WC-Co/ WC-Co-Ti(C,N)

WC-Co-Ti(C,N)

WC-Co

WC-Co-Ti(C,N)

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EPD of FGM and coatings


HSS taps with carbidecoating

HSS substrate

EPD-coated

Sintered

Final machined

EPD of FGM

Increasing the Performance of Total Hip Replacement Prosthesesthrough Functionally Graded Material Innovation and Design


• Gradient in properties• Residual thermal stresses• improved strength and wear resistance

Gradient in composition resulting in:

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Symmetrical Al2O3/Al2O3-ZrO2/Al2O3 FGM

measuredpredicted

EPD of plate shaped FGM


Near-net-shape processing (max + 100 µm)

EPD of complex shaped FGM


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EPD of complex shaped FGM


EPD of coatings

Texturing ofmaterials

ZrO2 coating onmetal substrates


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Fundamentals of AC electrophoretic deposition (AC-EPD)

Aqueous electrophoretic deposition in asymmetric AC electric fields

Alumina powder deposit formed by unbalanced AC (a) and DC (b) electric fields from a water-based suspension

How does this work ?

Basic science on EPD


Electrophoretic forming of functionally graded materials and coatings

GOA-TBA 2005-2008 K.U.LeuvenHydrodynamic layerdeposit

+_

_

_

_

+

+

+

Adso

rp-

tion

Desorp-

tion

Dep

osi

-tion L

iqui

dflo

wlin

es

Felectroforetic

Region of surface forces

• Suspension stability studies

• Charging mechanisms and particle-additive interactions

• Electrophoretic mobility and zetapotential measurements

• Study of the deposition process

• AFM of particle-electrode interaction

• Electrochemical reactions

• Fluid dynamic interactions during EPD

• Modelling of the EPD kinetics

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Modelling of EPD


- --

---

- -

+

-

+

+ -

- -

V

-

- ++++

+

- +++ +

- +++ +++

-

-

-

-

--

+ +

+

+

+

d - dl dl

Rldep

Rpdep

Rlsus

Rpsus

∆1 ∆2

Va

The currents and voltages during EPDare calculated from the equivalent electric

circuit shown

To calculate the composition gradient in the FGM material from the starting composition of the suspensions, the EPD operating parameters and the powder-specific EPD characteristics.


GOA-TBA 2008-2011 K.U.Leuven

Nanocomposite < 100 nm !

?

Conventional composite

Colloidal processing

of nanopowders

Shaping of Coatings

CompositesGradient materials

Densificationwith limited grain growth

Characterisation:microstructural

physicalmechanical

Processing flowchart

Nanomaterials and Nanocomposites

GOA 2008-2011 K.U.Leuven

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Development of biocompatible coatings

2006-2010

6th Framework Project

Project Coordinator: K.U.Leuven

Meddelcoat

Multifunctional bioresorbable biocompatible coatings with biofilminhibition and optimal implant fixation


to be coated

www.meddelcoat.eu

Development of Porous Materials


Development of porous glass, ceramic and metalstructures and coatings

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Processing of materials using a strong magnetic field

2007-2010

SBO

Project Coordinator K.U.Leuven

PROMAG

Development of textured materials by EPD

Plane parallel and perpendicular to electrode

EBSD

10 µm 70 µmcolour coded map


EPD of SOFC

Novel Materials for Silicate-Based Fuel Cells

Processing of Solid Oxide Fuel Cells

• Nanopowder synthesis• Colloidal processing of half cells• Sintering of half cells

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Field Assisted Sintering Technology (FAST)

Field assisted sintering technology for the densification of nanostructured powders and fabrication of functionally graded materials


• Technology development• Experimentation• Thermo-electrical modelling• Thermo-electrical-mechanical modelling• Superplastic deformation



Ceramic and ceramic-metal nanocomposites (cermets)

fabricated from nanopowders

Nanostructured aluminium based alloys from rapid solidification or

mechanical alloying

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FE-modelling of the temperature distribution during FAST

Temperaturedistribution in

sample & die set-up

die

punch

sample

High temperature equipment


SPS Equipment Properties:

pulsed electric current: 0 – 8000 Apulse/pause time combinations:

0 - 255 msforce: max. 250 kNheating rate: up to 1000°C/minheating cycle duration: 10 -30 min

(incl. heating-cooling)max temperature > 2200°Cmin controllable temperature = 150°C

Materials : Al-alloys, intermetallics, steel, ZnSe, ITO, borides, carbides, nitrides,Cu3Sn, oxides, electroceramics, BaTiO3, cermets, cemented carbides,ceramic composites, tungsten, etc.

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Electro-conductive ceramic composites

For electrical discharge machining (EDM) and wear applications


http://www.moncerat.org

http://www.mtm.kuleuven.be/Research/GBOU-IWT/spark/index.html

Development of ceramic composites


Electrical discharge machined new composites

Gears Attritor disc

Fine blanking tool

Extrusion die insert

Injection moulding toolLens mould insert

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Elastic and internal friction properties of materials

ImpulseExcitationTechnique

(IET)


⇒ Measurement of E, G, ν, and Q-1 at RT⇒ Measurement of E and Q-1 at elevated temp.Applicable to monoliths, coatings and laminates

Measuring of resonance frequency and damping

Elastic and damping properties of materials


Schematic of an IET-furnace

Si3N4 result : fr or E (T) and Q-1(T)

Test specimenCeramic ball

Ceramic tube

Pneumatictapping device

Furnace

Microphone

160

190

220

250

280

310

0 200 400 600 800 1000 1200 1400Temperature (°C)

You

ng's

mod

ulus

(GPa

)

0

0.02

0.04

0.06

0.08

0.1

Inte

rnal

fric

tion

(Q-1

)

Test in N2 (1 atm)heating at 2°C/minfr (25°C) = 8.7 kHz

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0.6

0.7

0.8

0.9

1

900 1000 1100 1200 1300 1400Temperature (°C)

E/E

RT

0

0.01

0.02

0.03

0.04

Inte

rnal

fric

tion

SiC, 2.7Al-3.5YSiC, 2.7Al-3.5Y + annealSiC, 6Al-4YSiC, 6Al-4Y + anneal

0

0.005

0.01

300 400 500 600 700 800 900 1000Temperature (K)

inte

rnal

fric

tion measured IF

broad Debyemeasured - Debye

0.0

0.4

0.8

1.2

1.6

2.0

0 200 400 600 800 1000Temperature (°C)

E/E

o

0.00

0.01

0.02

0.03

Inte

rnal

fric

tion

Q-1

E/Eo HeatingE/Eo cooling

Q-1 heatingQ-1 cooling

γ ⇒α

Hot pressed SiC Sintered 2Y-TZP

Sintering PM steel


Structural Integrity of Ceramic Multilayers and Coatings”


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Selective laser sintering and melting


Direct rapid manufacturing of metallic and ceramic parts

SBO project: DiRaMaP (2008-2012)Project Coordinator:

PMA, K.U.Leuven


Solution Deposition Technologies for CIGS and TCO

Powder-based opposed to vacuum sputtered photovoltaics

Selenisation studies of Cu(In,Ga)-Selenides

Assessment of fast selenisation processes

Rapid annealing processes of transparent conductive oxides (TCO)

Cross-section of Cu(In,Ga)Se2 solar cell

SIM project: SoPPoM (2010-2014)

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Publications ceramics research group


0510152025303540

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Ceramics research group

structure processing properties - ku leuven · ceramics research group ... •colloidal processing...

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