institut für materialforschung i what a wonderful world
TRANSCRIPT
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distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 1
Institut für Materialforschung I
What a wonderful world !
http://w1.siemens.com
www.donci.de
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distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 2
Institut für Materialforschung I
Hydrogen-Free Hard Amorphous Carbon Coatings: Properties by
Cathodic Vacuum Arc Evaporation and Magnetron Sputter Deposition
Forschungszentrum Karlsruhe, Germany
Sulzer Metaplas GmbH, Germany
M. Stueber, J. Vetter, H. Leiste, S. Ulrich, C. Ziebert ,J. Mueller, G. Erkens
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distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 3
Institut für Materialforschung I
1. Introduction
2. Experimental SET UP – sputtering/ arc
3. Sputtered and arc coatings
4. Coating properties (concentration at arc)
5. Summary
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Institut für Materialforschung I
www.damasko.de
lever
escapement
DLC a wonderful world of coating solutions
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distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 5
Institut für Materialforschung I
DLC
Me; N;O;Si ...
Source: FhG Freiburg
DIAMOND
GRAPHITE POLYMERS
sp3 sp3
C content higher
H lower
DLC: amorphous material
All DLC variants are amorphous !
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Institut für Materialforschung I
E-Modulus versus density
0100200300400500600700800900
100011001200
1 1,25 1,5 1,75 2 2,25 2,5 2,75 3 3,25 3,5 3,75 4
Density [g/cm3]
E-M
od
ulu
s [G
Pa]
a-C:H:Me
t-a-C
Diamant
graphite 2,26
diamond 3,52
sp3 content
E-Modulus
Hardness = ----------------
10
a-C a-C:H
Investigation of hydrogen "free" types
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 7
Institut für Materialforschung I
Industrial aspects of DLC synthesis
Demands on
DLC
technology
for
components
and
tools
Functionality & Performance
hardness – toughness
thermal & chemical stability
wear resistance
friction properties
multi-purpose coatings
Production technology
process stability & reliability
target materials
processing costs
high volume deposition
high DLC growth rates
Technology development
high density plasma processes
low temperature deposition
multi-capability coating systems
SPUTTERING
ARC
PE-CVD
Coating design
sufficient thick coatings
adhesion – stress management
interface engineering
Smooth, dense structures
amorphous – columnar growth
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 8
Institut für Materialforschung I
Experimental set up
PVD-SYSTEM
and
working hypothesis
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distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 9
Institut für Materialforschung I
DC/RF-magnetrons
with variable
magnetic field
DC+RF parallel
C-sputtering
APA-Arc evaporators
with variable
magnetic field
operation under RF
C-arcing
DC/RF-Bias: etching and a-C:H:X- PE-CVD
Enforced chamber cooling for low coating temperature
Universal R&D and industrial DLC-coater
"TRIPLE" HYBRID
Sputtering DC/RF + Arc + PE-CVD(RF) MZR304RF
Individual shutters
Experimental set up
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 10
Institut für Materialforschung I
Experimental set up
ARC by APA
DC arc 100 mm
with adapted
magnetic field
for carbon
DC-Sputtering
3 time rotation
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 11
Institut für Materialforschung I
d.c./r.f.
magnetron
graphite target
d.c./r.f.
magnetron
graphite target
flexible flange position
(i.e. pulsed magnetron)
advanced d.c. arc module
graphite cathode
Metaplas MZR 304/RF system at FZK
modular PVD/PE-CVD system
reactive d.c./r.f. magnetron sputtering
d.c. cathodic arc evaporation
magnetic field configuration tuning
d.c./r.f. substrate bias
low temperature deposition
large variation in modification of
plasma density
plasma particle energies
substrate current density
growth conditions for
hard a-C and a-C:H films
Hard a-C and ta-C films in novel hybrid PVD system
L = 450 mm
W = 130 mm
100 mm
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 12
Institut für Materialforschung I
Best : small lab unit LEYBOLD
50 GPa, 10 mm
Sputtering MZR304RF APA-Arc MZR304RF -distance 5 cm
- d.c./r.f. bias gradient
-temperature < 100 °C
- 11 W/cm2
"Upscaling " of best LAB-RESULT into MZR304RF
by sputtering and arc
? ? What we can achieve in
„industrial like“ equipments
by DC sputtering ?
Question 1 Question 2
What we can achieve by
APA arc evaporators
in DC-mode ?
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 13
Institut für Materialforschung I
Arc
Laser
Graphite
C+ C+ C+
C+
C+
C+
C+
Plasma
C+ C+ C+
C+
p ~ 10-4 Pa
Laser Arc Filtered Arc
Enhanced Arc
Modified DC Methods
Pulsed Arc
COMPLEX ARC DEPOSITION METHODES
What can be achieved by simple APA arc
evaporators in comparison to more complex
evaporation types ? Question 3
Inovap
Dresden US6139664
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 14
Institut für Materialforschung I
optimized target material
optimized magnetic field
Example of a Graphite type:
not useful for ARC
Investigation of graphite types and magnetic field set up
Example of a magnetic field:
not useful for graphite arc
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 15
Institut für Materialforschung I
Growth Rate of investigated coatings
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
2
Magnetron ARC
stationary
3 time rotation
0.4
1.0
growth rate
µm/h
stationary not used:
"over" heating due to ion flux
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 16
Institut für Materialforschung I
Thickness/ hardness range of a-C and ta-C coatings
Coating thickness
Coating hardness
10 GPa 60 GPa
5 µm
10 µm
30 GPa
ARC
ta-C
a-C:H:Me
industrial
Sputtering
a-C
industrial
a-C:H:X
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 17
Institut für Materialforschung I
Structure and properties of a-C and ta-C coatings
BEST LAB: magnetron sputtering result
temperature < 100°C, d.c./r.f. bias gradient
cathodic arc evaporation
temperature < 100°C, d.c. bias gradient
lab-scale process
stationary
target: 11 W/cm2
50 GPa, 10 mm
upscaled process
3-fold rotation
target: 4 W/cm2 25 GPa, 7 mm
Atarget/Atable ~ 1
Dtarget-table >> 10 cm
27 GPa, 2 mm
high current arc
start pressure: high
end pressure: low
58 GPa, 1 mm
lower current arc
low pressure d
eve
lop
me
nt
Atarget/Atable < 0,1
Dtarget-table < 10 cm
LEYBOLD
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 18
Institut für Materialforschung I
M08C37_ab3
0
200
400
600
800
1000
1200
900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900
Raman-Shift / cm-1
Co
un
ts
m08c37_ab.spc
Peak Fitting
Peak1
Peak2
Peak3
Baseline
Residuum
a
0
100
200
300
400
500
600
700
800
900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900
Raman-Shift / cm-1
Inte
ns
ity /
Cn
ts
D-peak
G-peak
Typical RAMAN SPECTRA
a-C sputtered
hardness ca. 15 +/- 5 GPa
ta-C arc
hardness ca. 55 +/- 10 GPa
ID/IG.= 0.44 ID/IG.= 1.54
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 19
Institut für Materialforschung I
Hardness
PIN-ON-DISC
mechanical
tribological
characterization
Tribological and mechanical characterization
Abrasive wear rate
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 20
Institut für Materialforschung I
Hardness
PIN-ON-DISC
mechanical
tribological
characterization
Tribological and mechanical characterization
Abrasive wear rate
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 21
Institut für Materialforschung I
Hardness of DLC deposited by different methods
12,0
25
38
58
45
51
10,00
20,00
30,00
40,00
50,00
60,00
70,00
a-C.H:W a-C:H LinearFilter APA ArcVersX ArCVersY
Hardness GPa
Types of coatings
Industrial
a-C:H:X
=
MZR304RF
sputtered
Industrial
a-C:H:´W
Different Arc: non or partially filtered
Hardness
typical
field
arc coatings
40 -60 GPa
LAB SCREENING RESULT: different carbon coatings
+/- 5 +/- 10 +/- 8 +/- 9 +/- 6
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 22
Institut für Materialforschung I
Hardness
PIN-ON-DISC
mechanical
tribological
characterization
Tribological and mechanical characterization
Abrasive wear rate
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 23
Institut für Materialforschung I
KALOMAX: 3 Body Abrasion Test
diamond
suspension
Coating
27 min ta-C APA-ArC evaporator
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 24
Institut für Materialforschung I
3
15
0,6
1,5
0,250,35
0,12
0,2
0,1
1
10
100
a-C.H:W a-C:H:X ARCVersY APA
10-15
[m3*m-1*N-1]
Kalomax wear rate: different carbon coatings
from 10 to 0.2
ca. factor 50 !
Industrial
a-C:H:X
Industrial
a-C:H:´W
Different Arc:
non filtered
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 25
Institut für Materialforschung I
Hardness
mechanical
tribological
characterization
Tribological and mechanical characterization
Abrasive wear rate PIN-ON-DISC
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 26
Institut für Materialforschung I
Ball 100 Cr6 Ball , R =3 mm
Coating/Substrate : wear properties pin on disc
moderate hard/"smooth" and hard/ "rough"
5,32 x 10 -15 m 3/Nm
1120 µm
F =4,9 N, v = 0.274 m/s, s = 1000 m
0.4
Tribotest DLC:
FN = 4,9N ; s = 1000m (R=3 / 53052U) ; v = 0,164m/s ; Integrator 1
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0.4
0.45
0.5
0 600 1200 1800 2400 3000 3600 4200 4800 5400 6000 6600
Zeit [ sec ]
Reib
wert
230 µm
9,35 x 10 -17 m 3/Nm
F =4,9 N, v = 0.164 m/s, s = 1000 m
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 27
Institut für Materialforschung I
Structure and "roughness" management
"ideal":
- no substrate effects
- no growth defects
sputtered
or
filtered arc coating
Rough
ness
DEPOSITION
METHODS
"POLISHING"
TREATMENT
PROCESS
OPTIMIZATION
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Ra [um] Rz[um]
0.1 0.02
0.9
0.2
thickness 1µm
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 28
Institut für Materialforschung I
1) The sputtering process were optimized to deposit very smooth a-C coatings
with a hardness of 25 +/- 5 GPa comparable to industrial applied
a-C:H:X coatings: up to 7 µm coating thickness (low stress).
2) An DC arc process was developed to deposit super hard ta-C coatings with
a hardness of 58 +/-10 GPa comparable to industrial applied
ta-C coatings deposited by more complex arc methods
with a thickness of about 1 µm.
3) The arc coatings were deposited with a higher growth rate (1 µm/h) than the
sputtered coatings.
4) The deposited arc coatings show a low 3body wear rate (KALOMAX)
comparable to other industrial used arc coatings deposited by more
complex deposition methods.
5) The hybrid PVD-system allowed to open process windows for thick moderate hard
(7µm) and super hard thin (1 µm) hydrogen free DLC coatings.
SUMMARY
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Unless prior written agreement has been received from Sulzer Metco, no part of this presentation may be reproduced,
distributed, or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording. R&D/ICMCTF2009vom240409/Dr. Jörg Vetter slide 29
Institut für Materialforschung I
What a wonderful world !
http://w1.siemens.com
www.donci.de
Wondering is the starting point to make things new !
Thanks for your attention