The MTM triangle

Structure

Properties
Processing

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

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 Ceramics research group

ZAP (Professors): ATP (Technical support):

Prof. Omer Van der Biest Joop Vandeursen
Prof. Jef Vleugels Wout Veulemans
Olivier Van Roey
Mohammed Abid

Postdoctoral Researchers: Visiting scientists:

Dr. Bernd Baufeld
Dr. Shuigen Huang
Dr. Kim Vanmeensel
Dr. Songlin Ran
Dr. Bram Neirinck

PhD students: PhD students:

Tina Mattheys Annabel Braem
Swarnakar Akhilesh Kumar Olivier Malek
Li Zhang Ezhil Jothinathan
Khuram Shahzad

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

Activities ceramics research group

Processing of ceramics
• Powder synthesis (sol-gel, carbo- and borothermal reduction)
• Powder metallurgical shaping
• Colloïdal shaping by electrophoretic deposition (EPD)
• Sintering (pressureless, hot pressing, microwave, SPS)
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)
Dept. Metallurgy and Materials Engineering, K.U.Leuven

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 Ceramic Materials under investigation

Composites Reinforced
Glass-ceramics ceramics
Bariumaluminosilicate (BAS)
Magnesiumaluminosilicate (MAS) Fibre reinforced
Ceramic matrix composites Borosilicate, MAS & BMAS
Matrix: Si3N4, ZrO2, Al2O3, ZrB2, TiB2 with SiC fibres
Additive: Al2O3, TiB2, TiN, TiC, TiCN,
WC, NbC, ZrC, HfC, HfTiC, ZrN, Platelet reinforced
B4C, SiC, etc. Sialon, Al2O3, mullite
Cermets with Al2O3 platelets
WC-Co, TiCN-based C

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NbC-based Graded
Monoliths
Oxides
Materials
Functionally graded (FGM)
Mullite, Al2O3
ZrO2/Al2O3 & ZrO2/WC
Y-TZP & Ce-TZP
WC-Co/WC-Co
Mixed stabiliser ZrO2
TiCN-based/WC-Co
Ce-TZP/Y-TZP
Non-oxides
Laminates
SiAlON, Si3N4 SiC / graphite & SiC / porous SiC
SiC, TiB2, TiN, TiCN, Coatings
WC, ZrB2, B4C,etc Metal / ZrO2
WC-Co / steel

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

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

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Cutting tool development and chemical compatibility studies

DEVELOPMENT OF NEW CUTTING MATERIALS, TOOLS, MACHINE CONCEPTS

AND TECHNOLOGIES FOR DRY HIGH SPEED CUTTING

• New composites
• Chemical wear assesment
• Gradient materials

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

Cutting tool development

Dry machining of cast iron with siliconnitride tools

Dry machining of cast iron with ceramic composite tools

Dry drilling of cast

iron at 450 m/min

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

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 Chemical compatibility assessment

Ni-Cr or Ni-Al wire

Workpiece
material

Al2O3
Tool material Workpiece
Tool
Experimental parameters Workpiece Nimonic 105
Temperature
Holding time Drill core
Mechanical load

Coating
Fixed

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

Chemical compatibility assessment

Equilibrium solubility calculations

Interaction couples 2
Ni3Al
Log solubility (log(cm3/mole))

0 WC
-2 SiC
K40 Steel Ti
-4 Ni
Co
-6 TiC
TiB2
-8 Si3N4
-10 TiN
E -12
C
-14
-16 ZrO2
-18 Al2O3
-20
300 350 400 450 500 550 600 650 700
Temperature (°C)

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

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 Functionally graded materials (FGM)
To combine irreconcilable properties in the same component
by engineering a gradient in composition and concomitant properties

Wear resistance (Hardness)

Thermal resistance

Fracture toughness

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

Electrophoretic deposition (EPD)

Colloidal processing technique in an electric field

_
+
V

_ • Particles are charged by interaction

+
+ with the solvent and additives
_
+ • Charged particles move under the
_ influence of an applied electric field
_ (electrophoresis)
+
+
_ • Partices form a growing deposit on
the deposition electrode (deposition)

electrode suspension electrode

Charged particles
+ Cations
_ Anions

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

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 Electrophoretic deposition (EPD) of FGM

FGM set-up Applications:

+ -

• Gradient materials
• Laminates
• Coatings (nm-mm)
• Infiltration
Gradient profile • Textured materials
Composition
100
% • Save processing of
nanopowders
Thickness gradient

Graded Tribological Materials Formed by Electrophoresis

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

EPD of FGM and coatings

Cutting tool inserts : WC-Co-Ti(C,N)/ WC-Co/ WC-Co-Ti(C,N)
7 21

6 20
Ti(C,N) content (wt%)

19
5
18
HV (GPa)

4 17
3 experimental 16
theoretical 15
2
14
1 13
0 12
WC-Co-Ti(C,N) 0 1 2 3 4 5 6
distance from electrode surface side (mm)

WC-Co

WC-Co-Ti(C,N)

20 µm

Ti(C,N) ↑ Ti(C,N) ↑

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

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 EPD of FGM and coatings

HSS substrate

EPD-coated

Sintered

Final machined

HSS taps with carbide

coating

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

EPD of FGM

Increasing the Performance of Total Hip Replacement Prostheses

through Functionally Graded Material Innovation and Design

Gradient in composition resulting in:

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

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

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 EPD of plate shaped FGM

Symmetrical Al2O3/Al2O3-ZrO2/Al2O3 FGM

predicted
measured

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

EPD of complex shaped FGM

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

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

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 EPD of complex shaped FGM

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

EPD of coatings

ZrO2 coating on
metal substrates

Texturing of
materials

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

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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 ?

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

Basic science on EPD

Electrophoretic forming of functionally graded materials and coatings

Region of surface forces

+ _ • Suspension stability studies

• Charging mechanisms and particle-
-
tio orp

_ additive interactions
s

Liquid flow
n
tio orp-
Ad

lines
n
es

• Electrophoretic mobility and zeta

D

+ potential measurements
Deposi
-tion

• Study of the deposition process

+
• AFM of particle-electrode interaction
_
+ • Electrochemical reactions
_ Felectroforetic
• Fluid dynamic interactions during EPD
• Modelling of the EPD kinetics

deposit Hydrodynamic layer

GOA-TBA 2005-2008 K.U.Leuven

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

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 Modelling of EPD

dl d - dl

V
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.
+ + - + +
+

R pdep R psus

R ldep R lsus
∆1 ∆2

Va
The currents and voltages during EPD
are calculated from the equivalent electric
circuit shown

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

Nanomaterials and Nanocomposites

Conventional composite Nanocomposite < 100 nm !

Shaping of Characterisation:
Colloidal Densification
Coatings microstructural
processing with limited
Composites physical
of grain growth
Gradient mechanical
nanopowders
materials
GOA-TBA
Processing flowchart
2008-2011 K.U.Leuven
GOA 2008-2011 K.U.Leuven
Dept. Metallurgy and Materials Engineering, K.U.Leuven

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 Development of biocompatible coatings

Multifunctional bioresorbable biocompatible coatings with biofilm

inhibition and optimal implant fixation

to be coated

6th Framework Project

Meddelcoat
2006-2010
Project Coordinator:
K.U.Leuven
www.meddelcoat.eu
Dept. Metallurgy and Materials Engineering, K.U.Leuven

Development of Porous Materials

Development of porous glass, ceramic and metal

structures and coatings

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

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 Development of textured materials by EPD

Processing of materials using a strong magnetic field

EBSD

SBO
10 µm colour coded map 70 µm

Plane parallel and perpendicular to electrode

PROMAG Project Coordinator
2007-2010 K.U.Leuven

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

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

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

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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

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

Field Assisted Sintering Technology (FAST)

Ceramic and ceramic-metal

nanocomposites (cermets)
fabricated from nanopowders

Nanostructured aluminium based

alloys from rapid solidification or
mechanical alloying

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

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 Field Assisted Sintering Technology (FAST)
FE-modelling of the temperature distribution during FAST

sample

die

Temperature
punch
distribution in
sample & die set-up

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

High temperature equipment

SPS Equipment Properties:

pulsed electric current: 0 – 8000 A

pulse/pause time combinations:
0 - 255 ms
force: max. 250 kN
heating rate: up to 1000°C/min
heating cycle duration: 10 -30 min
(incl. heating-cooling)
max temperature > 2200°C
min 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.

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

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 Electro-conductive ceramic composites

For electrical discharge machining (EDM) and wear applications

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

http://www.moncerat.org

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

Development of ceramic composites

Electrical discharge machined new composites

Gears Extrusion die insert Attritor disc

Lens mould insert Injection moulding tool Fine blanking tool

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

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 Elastic and internal friction properties of materials

Measuring of resonance frequency and damping

Impulse
Excitation ⇒ Measurement of E, G, ν, -1and Q at RT
-1

Technique ⇒ Measurement of E and Q at elevated temp.

(IET) Applicable to monoliths, coatings and laminates

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

Elastic and damping properties of materials

Schematic of an IET-furnace
Microphone

Furnace

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

Test specimen 310 0.1

Ceramic ball
Young's modulus (GPa)

Internal friction (Q-1)

280 0.08
Ceramic tube 250 0.06

Pneumatic 220 Test in N2 (1 atm) 0.04

tapping device heating at 2°C/min
190 fr (25°C) = 8.7 kHz 0.02

160 0
0 200 400 600 800 1000 1200 1400
Temperature (°C)

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

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 Elastic and damping properties of materials
1 0.04

0.9 0.03 0.01

internal friction
measured IF

Internal friction
SiC, 2.7Al-3.5Y broad Debye
RT

SiC, 2.7Al-3.5Y + anneal

0.8 SiC, 6Al-4Y 0.02 measured - Debye
E/E

SiC, 6Al-4Y + anneal

0.005
0.7 0.01

0.6 0 0
900 1000 1100 1200 1300 1400 300 400 500 600 700 800 900 1000
Temperature (°C) Temperature (K)

Hot pressed SiC E/Eo Heating Q-1 heating

Q-1 cooling Sintered 2Y-TZP
2.0 E/Eo cooling 0.03

1.6 γ ⇒α

Internal friction Q-1

0.02
1.2
E/Eo

0.8
0.01
0.4

0.0
0 200 400 600 800 1000
0.00 Sintering PM steel
Temperature (°C)

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

Elastic and damping properties of materials

Structural Integrity of Ceramic Multilayers and Coatings”

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

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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

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

Solution Deposition Technologies for CIGS and TCO

ƒ Powder-based opposed to vacuum sputtered photovoltaics

ƒ Selenisation studies of Cu(In,Ga)-Selenides

ƒ Assessment of fast selenisation processes

ƒ Rapid annealing processes of transparent conductive oxides (TCO)

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

SIM project: SoPPoM (2010-2014)

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

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 Publications ceramics research group

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35 Journals
30 Proceedings
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Dept. Metallurgy and Materials Engineering, K.U.Leuven

Ceramics research group

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

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