Ceramics research group

1.

2.

The MTM triangle
Structure
Processing
Properties
Dept. Metallurgy and Materials Engineering, K.U.Leuven

3.

Ceramics research group
ZAP (Professors):
ATP (Technical support):
Postdoctoral Researchers:
Visiting scientists:
PhD students:
PhD students:
Prof. Omer Van der Biest
Prof. Jef Vleugels
Dr.
Dr.
Dr.
Dr.
Dr.
Bernd Baufeld
Shuigen Huang
Kim Vanmeensel
Songlin Ran
Bram Neirinck
Tina Mattheys
Swarnakar Akhilesh Kumar
Li Zhang
Khuram Shahzad
Joop Vandeursen
Wout Veulemans
Olivier Van Roey
Mohammed Abid
Annabel Braem
Olivier Malek
Ezhil Jothinathan
Dept. Metallurgy and Materials Engineering, K.U.Leuven

4.

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

5.

Ceramic Materials under investigation
Composites
Reinforced
ceramics
Glass-ceramics
Bariumaluminosilicate (BAS)
Magnesiumaluminosilicate (MAS)
Ceramic matrix composites
Matrix: Si3N4, ZrO2, Al2O3, ZrB2, TiB2
Additive: Al2O3, TiB2, TiN, TiC, TiCN,
WC, NbC, ZrC, HfC, HfTiC, ZrN,
B4C, SiC, etc.
Fibre reinforced
Borosilicate, MAS & BMAS
with SiC fibres
Platelet reinforced
Cermets
WC-Co, TiCN-based
NbC-based
Sialon, Al2O3, mullite
with Al2O3 platelets
Composites
Reinforced ceramic
Ceramic matrix composites
Matrix: Y-TZP,Ce-TZP,Si3N4,Al2O3
Addition: Al2O3,TiB,TiN,TiCN,TiC,WC,...
2
Glass-ceramics
Bariumaluminosilicates (BAS)
Magnesiumaluminosilicates (MAS)
Cermets
Fibre-reinforced
Borosilicate, MAS and BMAS with
SiC fibres
Platelet-reinforced
SiAlON, mullite and Al2O3 with
Al2O3 platelets
WC/Co-based
Graded materials
Monoliths
Oxides
Mullite, Al2O3
Y-TZP & Ce-TZP
Mixed stabiliser ZrO2
Non-oxides
SiAlON, Si3N4
SiC, TiB2, TiN, TiCN,
WC, ZrB2, B4C,etc
Graded
Materials
Functionally graded (FGM)
ZrO2/Al2O3 & ZrO2/WC
WC-Co/WC-Co
TiCN-based/WC-Co
Ce-TZP/Y-TZP
Laminates
SiC / graphite & SiC / porous SiC
Coatings
Metal / ZrO2
WC-Co / steel

6.

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

7.

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

8.

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

9.

Chemical compatibility assessment
Ni-Cr or Ni-Al wire
Workpiece
material
Al2O3
Tool material
Experimental parameters
Temperature
Holding time
Mechanical load
Workpiece
Tool
Nimonic 105
Workpiece
Drill core
Coating
Fixed
Dept. Metallurgy and Materials Engineering, K.U.Leuven

10.

Chemical compatibility assessment
Equilibrium solubility calculations
Interaction couples
Steel
E
Logslubity(logcm
3/mole)
K40
2
0
2
4
6
8
1
0
1
2
1
4
1
6
1
8
2
0
3
0
0
3
5
0
4
0
0
4
5
0
5
0
0
5
5
0
6
0
0
6
5
0
7
0
0
N
i
A
l
3
W
C
S
i
C
T
i
N
i
C
o
T
i
C
T
i
B
2
S
i
N
3
4
T
i
N
C
Z
r
O
2
A
l
O
2
3
T
e
m
p
e
r
a
t
u
r
e
(
°
C
)
Dept. Metallurgy and Materials Engineering, K.U.Leuven

11.

Functionally graded materials (FGM)
Thermal resistance
Wear resistance (Hardness)
To combine irreconcilable properties in the same component
by engineering a gradient in composition and concomitant properties
Fracture toughness
Dept. Metallurgy and Materials Engineering, K.U.Leuven

12.

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)
+
_
_
+
+
electrode
• Partices form a growing deposit on
the deposition electrode (deposition)
_
suspension
electrode
Charged particles
+ Cations
_ Anions
Dept. Metallurgy and Materials Engineering, K.U.Leuven

13.

Electrophoretic deposition (EPD) of FGM
FGM set-up
+
-
Applications:
• Gradient materials
• Laminates
• Coatings (nm-mm)
Gradient profile
Composition
• Infiltration
• Textured materials
• Save processing of
nanopowders
100
%
Thickness gradient
Graded Tribological Materials Formed by Electrophoresis
Dept. Metallurgy and Materials Engineering, K.U.Leuven

14.

EPD of FGM and coatings
WC-Co-Ti(C,N)
7
21
6
20
19
5
18
4
17
3
experimental
16
2
theoretical
15
HV (GPa)
Ti(C,N) content (wt%)
Cutting tool inserts : WC-Co-Ti(C,N)/ WC-Co/ WC-Co-Ti(C,N)
14
1
13
0
12
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

15.

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

16.

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

17.

EPD of plate shaped FGM
Symmetrical Al2O3/Al2O3-ZrO2/Al2O3 FGM
predicted
measured
Dept. Metallurgy and Materials Engineering, K.U.Leuven

18.

EPD of complex shaped FGM
Near-net-shape processing (max + 100 µm)
Dept. Metallurgy and Materials Engineering, K.U.Leuven

19.

EPD of complex shaped FGM
Dept. Metallurgy and Materials Engineering, K.U.Leuven

20.

EPD of coatings
ZrO2 coating on
metal substrates
Texturing of
materials
Dept. Metallurgy and Materials Engineering, K.U.Leuven

21.

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

22.

Basic science on EPD
Electrophoretic forming of functionally graded materials and coatings
Region of surface forces
+
_
Liquid flow
lines
_
+
• Electrophoretic mobility and zeta
potential measurements
• AFM of particle-electrode interaction
_
+
deposit
• Charging mechanisms and particleadditive interactions
• Study of the deposition process
+
_
• Suspension stability studies
Felectroforetic
Hydrodynamic layer
• Electrochemical reactions
• Fluid dynamic interactions during EPD
• Modelling of the EPD kinetics
GOA-TBA 2005-2008 K.U.Leuven
Dept. Metallurgy and Materials Engineering, K.U.Leuven

23.

Modelling of EPD
dl
d - dl
V
+
- + - - +
- - + - - - -
-
-
+ - + ++
+
+
-
+
+ - + +
+
Rpdep
Rpsus
Rldep
Rlsus
+
+
+ +
+ - + +
+
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.
2
1
Va
The currents and voltages during EPD
are calculated from the equivalent electric
circuit shown
Dept. Metallurgy and Materials Engineering, K.U.Leuven

24.

Nanomaterials and Nanocomposites
Nanocomposite < 100 nm !
Conventional composite
?
Colloidal
processing
of
nanopowders
Shaping of
Coatings
Composites
Gradient
materials
Densification
with limited
grain growth
Characterisation:
microstructural
physical
mechanical
Processing
flowchart
GOA-TBA
2008-2011
K.U.Leuven
GOA 2008-2011 K.U.Leuven
Dept. Metallurgy and Materials Engineering, K.U.Leuven

25.

Development of biocompatible coatings
Multifunctional bioresorbable biocompatible coatings with biofilm
inhibition and optimal implant fixation
to be coated
6th Framework Project
Meddelcoat
2006-2010
www.meddelcoat.eu
Project Coordinator:
K.U.Leuven
Dept. Metallurgy and Materials Engineering, K.U.Leuven

26.

Development of Porous Materials
Development of porous glass, ceramic and metal
structures and coatings
Dept. Metallurgy and Materials Engineering, K.U.Leuven

27.

Development of textured materials by EPD
Processing of materials using a strong magnetic field
EBSD
SBO
10 µm
colour coded map
PROMAG Project Coordinator
2007-2010
70 µm
Plane parallel and perpendicular to electrode
K.U.Leuven
Dept. Metallurgy and Materials Engineering, K.U.Leuven

28.

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

29.

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

30.

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

31.

Field Assisted Sintering Technology (FAST)
FE-modelling of the temperature distribution during FAST
sample
die
punch
Temperature
distribution in
sample & die set-up
Dept. Metallurgy and Materials Engineering, K.U.Leuven

32.

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

33.

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

34.

Development of ceramic composites
Electrical discharge machined new composites
Gears
Lens mould insert
Extrusion die insert
Injection moulding tool
Attritor disc
Fine blanking tool
Dept. Metallurgy and Materials Engineering, K.U.Leuven

35.

Elastic and internal friction properties of materials
Measuring of resonance frequency and damping
Impulse
Measurement of E, G, , and Q-1 at RT
Excitation
Measurement of E and Q-1 at elevated temp.
Technique
Applicable to monoliths, coatings and laminates
(IET)
Dept. Metallurgy and Materials Engineering, K.U.Leuven

36.

Elastic and damping properties of materials
Schematic of an IET-furnace
Microphone
Furnace
Ceramic tube
Pneumatic
tapping device
310
0.1
280
0.08
250
0.06
Test in N2 (1 atm)
heating at 2°C/min
fr (25°C) = 8.7 kHz
220
190
160
0
200
400
0.04
0.02
Internal friction (Q-1)
Ceramic ball
Test specimen
Young's modulus (GPa)
Si3N4 result : fr or E (T) and Q-1(T)
0
600 800 1000 1200 1400
Temperature (°C)
Dept. Metallurgy and Materials Engineering, K.U.Leuven

37.

0.04
0.9
0.03
E/E
RT
SiC, 2.7Al-3.5Y
SiC, 2.7Al-3.5Y + anneal
SiC, 6Al-4Y
SiC, 6Al-4Y + anneal
0.8
0.02
0.7
0.01
0.6
0
900
1000
1100
1200
Temperature (°C)
Hot pressed SiC
1300
2.0
E/Eo Heating
E/Eo cooling
measured IF
broad Debye
measured - Debye
0.005
0
300
1400
400
Q-1 heating
Q-1 cooling
500
0.02
1.2
0.8
0.01
0.4
0.0
0
200
400
600
800
Temperature (°C)
600
700
800
Temperature (K)
1000
0.00
900
1000
Sintered 2Y-TZP
0.03
g a
1.6
E/Eo
0.01
Internal friction Q-1
1
Internal friction
internal friction
Elastic and damping properties of materials
Sintering PM steel
Dept. Metallurgy and Materials Engineering, K.U.Leuven

38.

Elastic and damping properties of materials
Structural Integrity of Ceramic Multilayers and Coatings”
Dept. Metallurgy and Materials Engineering, K.U.Leuven

39.

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

40.

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

41.

Publications ceramics research group
40
35
30
25
20
15
10
5
0
Journals
2010
2009
2008
2007
2006
2005
2004
2003
2002
2001
2000
1999
1998
1997
1996
1995
Proceedings
Dept. Metallurgy and Materials Engineering, K.U.Leuven

42.

Ceramics research group
Dept. Metallurgy and Materials Engineering, K.U.Leuven