Post on 13-Oct-2020
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Spring School, Darmstadt March 2011 1
R. Kirchner
FCT Systeme GmbH, Rauenstein – Germany
„FAST“ - Field Assisted Sintering Technology
Basics, State of the Art and Future Aspects
1
www.fct-systeme.de
2
FCT Systeme - company profile
Development of innovative concepts as well as
design and construction of high - temperature furnaces for
technical ceramics, powder metallurgy and solar industry.
from small lab – furnace to turn - key - production plant
Spring School, Darmstadt March 2011
0
10
20
30
40
2004 2005 2006 2007 2008 2009 2010
EMPLOYEES
TURNOVER / MioEuro
www.fct-systeme.de
Spring School, Darmstadt March 2011 3 3 3
EU-project “FAST”
“Field Assisted Sintering Technology
for the Densification of Nanostructured Powders
and Fabrication of Functionally Graded Materials” FP5–“GROWTH”–Project N° GRD1-2001-40737
www.fct-systeme.de
Spring School, Darmstadt March 2011 4 4
Spark Plasma Sintering (SPS) – Principle
dS/dt
Hydraulic
system
V
P
Power
Supply
System Temp.
U
Vacuum chamber
I
t
Vacuum,
Ar / N2 / H2
S
Q
Field
Assisted
Sintering
Technology
Spark
Plasma
Sintering
SPS
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Spring School, Darmstadt March 2011 5
Pulse form modulation
High flexibility from pure DC to almost any pulse burst
Pulse duration ton = 1…255 ms
Pause duration toff = 0…255 ms
Pulse number n = 1…255
Extra pause tp = 0…255 ms
G 2.2D - tO N=2m s tO FF=1m s n PULS=12 tPAUSE=6m s - P=100%
0
-50 -40 -30 -20 -10 0 10 20 30 40 50
Tim e / m s
Current
/ kA
ton=2ms toff=1ms n=12 tp=6ms
corr. to SCM „12:2“
0
-50 -40 -30 -20 -10 0 10 20 30 40 50
Tim e / s
Cur
rent
/ kA
C urrent at 1500°C / 10/5m s
K U L26 - SN 5Y5A - 14 Apr 04
G raphite D um m y at 150°C - C urrent 100%
0
2
4
6
8
10
-25 -20 -15 -10 -5 0 5 10 15 20 25
Tim e / m s
Curre
nt / k
A
G raphite D um m y at 150°C - C urrent 100%
0
2
4
6
8
10
-25 -20 -15 -10 -5 0 5 10 15 20 25
Tim e / m s
Curre
nt / k
A
TIME / ms
ton=3ms toff=3ms n=1 tp=0ms
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
0.0
2.0
4.0
6.0
0.000 0.005 0.010 0.015 0.020
ton=15ms toff=5ms n=1 tp=0ms
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Spring School, Darmstadt March 2011 6
Temperature difference (∆T) mould to sample
internal pyrometer
-50
0
50
100
150
200
250
0 200 400 600 800 1000 1200
Tim e, sec
Te
mp
era
ture
, C
Controlled sample temperature < 4°C
die
pyrometer
T(mould) – T(sample) = - 210 °C
Sample: TiN Ø50 x 10 mm (97 % theo. density) Sample temperature 1500°C
-
-
-
-
-
+
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Spring School, Darmstadt March 2011 7
Simulation of FAST/SPS heating process
FEM calculation of
experiment
FEM = Finite Element Method
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Spring School, Darmstadt March 2011 8
Number of FCT FAST/SPS facilities worldwide
0
5
10
15
20
25
30
35
40
45
50
2003 2004 2005 2006 2007 2008 2009 2010 2011
www.fct-systeme.de
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FAST/SPS series
32 kW - 50 kN 60 kW - 250 kN
www.fct-systeme.de
FAST/SPS series
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60 kW - 250 kN 180 kW - 1.250 kN
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FAST/SPS series
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360 kW - 2.500 kN 360 kW - 2.500 kN
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FAST/SPS series
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360 kW - 2.500 kN 360 kW - 2.500 kN Semi-Conti
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360 kW - 2.500 kN
Industrial Applications already in operation:
☺ Tungsten Carbide 175x150 : teff = 35 min
☺ Noble Metal D200 : teff = 20 min
☺ Chromium D60: teff = 10 min
☺ Ti / Al D100: teff = 4 min
Semi–continuous FAST/SPS–system
Spring School, Darmstadt March 2011
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Spring School, Darmstadt March 2011 14
Pressing tool Pressing tool parts
Electrical Conductivity
Thermal Conductivity
Thermal Expansion
Bending Strength
Fracture Toughness
Creep Resistance
Hardness
Wear Resistance
Electrical Conductivity
Thermal Conductivity
Thermal Expansion
Bending Strength
Fracture Toughness
Creep Resistance
Hardness
Wear Resistance
= f (T) ?
Electrical conductivity
Thermal conductivity
Thermal expansion
Bending strength
Fracture toughness
Sample
Electrical conductivity
Thermal conductivity
Thermal expansion
Bending strength
Fracture toughness
Creep resistance
Hardness
Wear resistance
= f (T) ? = f () ?? Degree of sintering
(Density, microstructure, phase comp.)
Important material properties
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Spring School, Darmstadt March 2011 15 15
Finite element simulation of FAST/SPS heating process
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Spring School, Darmstadt March 2011 16
Temperature distribution in Ø200mm sample after heating to 2100
C - 100K/min
Standard tool design Optimized tool design ΔT > 250K ΔT < 70K
Finite element simulation of FAST/SPS heating process
www.fct-systeme.de
0
200
400
600
800
1000
1200
0
200
400
600
800
1000
1200
1400
1600
1800
2000
2200
2400
00:00 00:10 00:20 00:30 00:40 00:50 01:00 01:10 01:20
den
sif
icati
on
[0.0
4*m
m];
den
sif
icati
on
sp
eed
[0.0
05*m
m/m
in]
tem
pera
ture
[°C
]; p
ressin
g f
orc
e [
kN
]
time [hh:mm]
temperature
pressing force
densification (x25)
densification speed (x200)
SPS cycle of binderless WC using the HP D 250
60 min
sample: sputter target (Ø200 x 13 mm) density: 15,51g/cm3 (99,3% th. d.)
17 Spring School, Darmstadt March 2011
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Spring School, Darmstadt March 2011 18
SPS process of a Al/Si alloy; using HP D 250
90 sec.
Goal: 60 sec. (FAST2)
Density: 2,85g/cm3, >99% th.D. Sample: piston, pre-shaped (dia. 82 x 25 mm)
00:00 [h : min] 00:01 [h : min] 00:03 [h : min] 00:04 [h : min] 00:02 [h : min]
PWS = constant
Stellgröße
Ds/dt [mal 10]
Position rel. [mal 10]
Presskraft
Pre
sskra
ft [
kN
]; L
eis
tun
g [
kW
]
s/d
t [m
m/m
in];
Verd
ich
tun
g [
mm
] P
ressin
g f
orc
e [
kN
];
Set
valu
e P
WS
in
%
Set value [x 5]
Ds/dt [x 10]
Position rel. [mal 10]
Pressing force
Time
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Spring School, Darmstadt March 2011 19
Samples made of different materials by SPS
Fig. 1
Fig. 2
Fig. 3
Fig. 4 Fig. 5
Fig. 6
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Spring School, Darmstadt March 2011 20
6-fold SPS-mold Ø63x34 Cr-cathodes
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Spring School, Darmstadt March 2011 21
Hydraulic
System
Vacuum
& Gas
Pyro
Induction
Heating
System
FAST
Heating
System
FAST/SPS Hybrid – technology for sintering of large parts
made from electroconductive powders
www.fct-systeme.de
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1000 kW - 6.000 kN
Spring School, Darmstadt March 2011
FAST/Hybrid system HHPD 600 (under construction by FCT Systeme GmbH)
www.fct-systeme.de
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Filling Covering Pressing/Dwell Ejecting
VISION: Fully automatic powder press
Producing parts, which are net shaped and readily sintered
High speed FAST/SPS – dry press technology
Spring School, Darmstadt March 2011
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• Cycle time: 10 – 30 sec / pc
• Pressing force: 200 kN
• Dimension: 1 … 5 cm2
• Fully automatic operation
Spring School, Darmstadt March 2011
High speed FAST/SPS – dry press technology
www.fct-systeme.de
25
Typical PIM – part of FAST-Sint®
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Spring School, Darmstadt March 2011 26
Metals: W, Mo, Cr, Ru, Si, Cu, Cu (+W / Cr)
Intermetallics: TiAl, Ni3Al, PbTe, SmCo5
Carbides: WC, B4C, SiC, TiC, ZrC
Nitrides: AlN, TiN, Si3N4 (+TiN), hBN (+TiB2)
MMC / CMC: Al / Ti (+ SiC / Al2O3), Steel (+ TiC/N),
Co / Cr / Pt (+ Oxides)
Cutting Tools: WC-Co/Ni/Steel (+cBN, +Diam.), Al2O3-Ti(C,N)
Armor materials: B4C, SiC, ZrB2, TiB2, Al2O3 (+CNT)
Functional / Functionally Graded Materials („FGM“)
Transparent: Spinel, Al2O3,
Nanostructured Materials
FAST/SPS material examples
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PRODUCTION
COSTS
MATERIAL
PROPERTIES
NEW
POSSIBILITIES
Goal of FAST/SPS developments at FCT
Spring School, Darmstadt March 2011
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Thank You For Your Attention
Merci De Votre Attention
Gracias por su Atención
Grazie per la vostra attenzione
Obrigado para sua atenção
Σας εσταριστώ για την προσοτή σας
Danke für Ihre Aufmerksamkeit
Dank u voor uw aandacht
TEŞEKKÜR
谢 谢 您 的 注 意
Спасибо за внимание
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Tack för Uppmärksamheten
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Spring School, Darmstadt March 2011