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Carbon-Based Nanostructured Composite and Nanolaminated Films. Carbon-based nanocomposite thin films – deposition , structure and properties. W itold Gulbiński Institute of Mechatronics, Nanotechnology and Vacuum Technique Koszalin University of Technology, PL. - PowerPoint PPT Presentation
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Witold Gulbiński Institute of Mechatronics, Nanotechnology and Vacuum Technique
Koszalin University of Technology, PL
Carbon-based nanocomposite thin films – deposition, structure and properties
Carbon-Based Nanostructured Composite and Nanolaminated Films
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Carbon-based nanocomposite thin films – deposition, structure and properties
OUTLINE
Carbon films – DLC: taC, aC, aC:H
Carbon-based nanocomposite thin films (CBNTF) – the design concept
Deposition methods
Structure and properties of nanocomposite thin films Carbide containing MeCx-taC and MeCx-aC:H films (Me = Si,
Ti, V, W, Mo…)
Metal containing Me-taC:H and Me-aC:H (Me=Co, Ni, Cu, Ag, Au…)
Comments on applications
Concluding remarks
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A.C. Ferrari, J. Robertson, Interpretation of Raman spectra of disordered and amorphous carbon, Phys. Rev. B 61 (20) (2000) 14095.
Carbon-based nanocomposite thin films – deposition, structure and properties
The bombardment of energetic carbon speciesduring deposition is critical for the growth of DLC films.
The ion energy is the most important parameter for determining the characteristics of DLC films.
The ion bombardment tends to result in thehighly-dense packing of carbon atoms in the film, yielding a very high compressive stress therein.
A very high compressive stress tends to detach the film from the substrate, when the film thickness increases above a critical value.
The internal stress can be reduced by different mechanisms.
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A.C. Ferrari, J. Robertson, Interpretation of Raman spectra of disordered and amorphous carbon, Phys. Rev. B 61 (20) (2000) 14095.
G peak position and I(D)/I(G) ratio vs sp3 fraction for as-deposited a-C:H.
Carbon-based nanocomposite thin films – deposition, structure and properties
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Carbon-based nanocomposite thin films – deposition, structure and properties
taC
Al Ni Co Cu Ag, Au
Ti Cr V Mo Ta Zr W
MeCx-taC Me-taC
Si
taC:H aC:H
Ti Cr V Mo Ta Zr W
Me-taC:HMeCx-taC:H
Me-aC:HMeCx-aC:H
Al Ni Co Cu Ag, Au
Si
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Carbon-based nanocomposite thin films – deposition, structure and properties
REQUIREMENTS for tribological coatings- high toughness (high strength + ductility): ability to
support high loads in sliding/rolling contact
- low friction
- high hardness
- high adhesion
- chemical and tribochemical stability
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Carbon-based nanocomposite thin films – deposition, structure and properties
How to do that?
- Embed grains of hard phase (TM carbides) in a softer matrix (aC or aC:H), allowing for high ductility due to grain boundary sliding
Carbon based nanocomposite coatings- the way to increase
toughness and wear resistance accompanied by low friction
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Carbon-based nanocomposite thin films – deposition, structure and properties
Design concepts of tough nanocomposite coatings:
Encapsulation of 3-10 nm sized hard crystalline grains in an amorphous matrix restricts dislocation activity, diverts and arrests macro-crack development.
A large volume fraction of grain boundaries provides ductility through grain boundary sliding and nano-cracking along grain/matrix interfaces.
A graded interface layer is usually applied between the substrate and crystalline/amorphous composite coating to enhance adhesion strength and relieve stresses (combination of functional gradient and nanocomposite design)
A.A. Voevodin, Tsinghua Science and Technology, 10 (2005) 665-679
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Carbon-based nanocomposite thin films – deposition, structure and properties
(111)(200)(220)(311)(222)(400)(420)(422)
(111)(200)(220)(311)(222)(400)(420)
Nanocrystalline MeCxx
crystallites < 20 nm
Nanocomposite MeC-aC;Hx
crystallites < 10 nm
Nanocomposite MeC-aC;Hx
crystallites < 4 nm
Powłoki nanokompozytowe typu XC/a-C:H krystality < 10 nm
b) d)c)
a)
Up to 10 % a-C:H 10- 70 % a-C:H 70- 95 % a-C:H
MeCxaC:H
TiC d = 8-10nm
TiC-aC:Hd = 4-6nm
H = 32 GPa, μ = 0.35
Ti48C40H9(O,N.Ar)3
TiC-aC:Hd = <4nm
H = 42 GPa, μ = 0.26
Ti38C52H6(O,N.Ar)4
H = 15 GPa, μ = 0.06
Ti6C72H21(O,N.Ar)1
A. Czyżniewski et al., Journal of Materials Processing Technology 157–158 (2004) 274–283
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Carbon-based nanocomposite thin films – deposition, structure and properties
3-10 nm crystalline grains (TiC) embedded in an amorphous matrix (aC).The grains are separated by 1-3 nm.
A.A. Voevodin, Tsinghua Science and Technology, 10 (2005) 665-679
From scratch test Film thickness: 1μm
Load: 10N!
Indentation depth: 9μm!
TiC-aC
restriction of dislocation activity, macro-cracking blocked,ductility through grain boundary sliding,nanocracking along grain-matrix interfaces
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Carbon-based nanocomposite thin films – deposition, structure and properties
MeCx- or Me-taC Magnetron sputtering
(multisource: Me & C or segment targets)
Ion beam sputtering (multitarget)
Filtered cathodic vacuum arc
Pulsed laser (ns, fs) - segment targets or multitarget geometries
taC
Al Ni Co Cu Ag, Au
Ti Cr V Mo Ta Zr W
MeCx-taC Me-taC
SiDeposition of CBNTF
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Carbon-based nanocomposite thin films – deposition, structure and properties
MeCx- or Me-aC:H CVD, PECVD (RF, MV-ECR)
Reactive magnetron sputtering (multisource: Me targets)
Other techniques usually linking two or more techniques listed above (DMWECR + Sputtering)
taC:H aC:H
Ti Cr V Mo Ta Zr W
Me-taC:HMeCx-taC:H
Me-aC:HMeCx-aC:H
Al Ni Co Cu Ag, Au
SiDeposition of CBNTF
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Carbon-based nanocomposite thin films – deposition, structure and properties
Filtered vacuum arc of graphite with simultaneous magnetron sputtering of Si.
Si-taC films
Churl Seung Lee et al., Diamond and Related Materials 11 (2002) 198–203
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Si incorporated into tetrahedral amorphous carbon (aSiC-taC)
Churl Seung Lee et al., Diamond and Related Materials 11 (2002) 198–203
sp3/sp2
Carbon-based nanocomposite thin films – deposition, structure and properties
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B.K. Tay et al., Diamond and Related Materials 10 (2001) 1082-1087 (Al or Ti – taC)
D. Sheeja et al., Diamond and Related Materials 12 (2003) 2032–2036 (Al -taC)S. Zhang et al., Thin Solid Films 482 (2005) 138– 144 (Ti+Al – taC)
Me-taC, Me =Al, Ti films
Carbon films were deposited by the off-plane double-bend filtered cathodic vacuum arc from metal doped graphite target.
sp3/sp2
ncTiC-taCAl-taC
Carbon-based nanocomposite thin films – deposition, structure and properties
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WCx-WS2-aC adaptive nanocomposite films(for vacuum applications)
Andrey A. Voevodin et al., Surface and Coatings Technology 116–119 (1999) 36–45
KrF excimer laser + MS
S - 0 at.%
S - 15 at.%
S - 29 at.%
PLD: Graphite + MS: (W, WS2)
Carbon-based nanocomposite thin films – deposition, structure and properties
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WS2 lubrication
Graphite
lubrication
Carbon-based nanocomposite thin films – deposition, structure and properties
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A. Czyżniewski et al., Journal of Materials Processing Technology 157–158 (2004) 274–283
Ti, W, Si – aC:H nanocomposite films
Carbon-based nanocomposite thin films – deposition, structure and properties
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19A. Czyżniewski et al., Journal of Materials Processing Technology 157–158 (2004) 274–283
Ti, W, Si – aC:H nanocomposite films
Carbon-based nanocomposite thin films – deposition, structure and properties
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C1s
C-C
C-Ti
W. Gulbiński et al., Applied Surface Science 239 (2005) 302–310
TiC– aC:H nanocomposite films
Carbon-based nanocomposite thin films – deposition, structure and properties
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W. Gulbiński et al., Applied Surface Science 239 (2005) 302–310
Carbon-based nanocomposite thin films – deposition, structure and properties
TiC– aC:H nanocomposite films
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22P. Zhang, Diamond and Related Materials 13 (2004) 459–464
Me-aC where Me = Al, Ti, Ni, Si, were prepared by the filtered cathodic vacuum arc technique with metal-carbon (5 at.% metal) composite targets.
HydrophobicΘ>700
HydrophilicΘ<700
aC
Carbon-based nanocomposite thin films – deposition, structure and properties
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23Q.F. Huang et al., Diamond and Related Materials 9 (2000) 534–538
MoCx-aC:H nanocomposite films
Carbon-based nanocomposite thin films – deposition, structure and properties
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Ion beam co-sputtering of graphite target having a nickel chip attached to its surface.
F. C. Fonseca et al., JOURNAL OF APPLIED PHYSICS 97 (2005) 044313
Films were deposited on polished Si wafers heated to 350 °C. (above Ni3C decomposition temperature)Ni concentration: 5 to 22 wt %
Ni-aC films with superparamagnetic properties
Carbon-based nanocomposite thin films – deposition, structure and properties
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F. C. Fonseca et al., JOURNAL OF APPLIED PHYSICS 97 (2005) 044313
Normalized magnetization as a function of H/T at temperatures of 100, 150, 200, 250 and 300 K
Ni grain size distribution
Carbon-based nanocomposite thin films – deposition, structure and properties
TB = 13K
Hc=0
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The films deposited below 400 C showed acolumnar structure of hexagonal Ni3C type crystallinegrains embedded in a matrix consisting of an amorphousand/or graphite-like carbon.
Ts = 200C
K. Sedlackova, P. Lobotka, I . Vavra, G. Radnoczi, Carbon 43 (2005) 2192–2198
Ni3C-aC films by DC MS of Ni and C
30 at% Ni
18 at% Ni
Carbon-based nanocomposite thin films – deposition, structure and properties
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Above TS = 400 C the composite consists of globular fcc Ni grains sized between 50 and 100 nm that were separated by the Fullerene-like carbon phase.
Ts = 4000C
K. Sedlackova, P. Lobotka, I . Vavra, G. Radnoczi, Carbon 43 (2005) 2192–2198
Ni-aC films30 at% Ni
Carbon-based nanocomposite thin films – deposition, structure and properties
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Co-taC nanocomposite films (Co 65 at.% -taC) with ferromagnetic properties
Hao Wang et al., Materials Science and Engineering C 16 (2001) 147–151
Carbon-based nanocomposite thin films – deposition, structure and properties
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Co-taC nanocomposite films (Co: 65 at.%) with ferromagnetic properties
The most important advantage of carbon encapsulation is the increase of the effective distance of neighbouring magnetic grains so that the exchange coupling between them is weakened or eliminated.
As dep.
3500
C
4000
C
Hao Wang et al., Materials Science and Engineering C 16 (2001) 147–151
C1sXPS
Carbon-based nanocomposite thin films – deposition, structure and properties
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As deposited
3000C
3500C 4000
C
Magnetic Force Microscopy
Hao Wang et al., Materials Science and Engineering C 16 (2001) 147–151
Co-taC nanocomposite films
Magnetization loop
Carbon-based nanocomposite thin films – deposition, structure and properties
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0 at.% Cuσ = 2.9 GPaμH = 22 GPa
0.7 GPa16 GPa 11 at.% Cu C.-C. Chen, F.C.-N. Hong, Applied Surface
Science 242 (2005) 261–269
Cu-aC:H nc thin films(RF PECVD + Cu sputtering)
Copper was used to:
- prevent the formation of bonds between the nanocrystallite and the carbon matrix,
- facilitate grain–matrix interface sliding, which increases the film’s ductility.
Carbon-based nanocomposite thin films – deposition, structure and properties
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Cu-aC:H
16 at.% Cu
C.-C. Chen, F.C.-N. Hong, Applied Surface Science 242 (2005) 261–269
Carbon-based nanocomposite thin films – deposition, structure and properties
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Ag-aC:H nanocomposite films
Silver within a diamondlike carbon–silver nanocomposite film may provide antimicrobial functionality to a medical devices.
Silver nanoparticles are highly toxic to microorganisms, and demonstrate biocidal effects against:
Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Listeria monocytogenes and other species of bacteria.
The exact mechanism of action of silver is unknown, but it is believed that silver ions act by binding to DNA, interfering with electron transport within cells, and injuring bacterial enzymes.
R.B. Thurman, C.P. Gerba, CRC Crit. Rev. Environ. Control 18 (2000) 295
Carbon-based nanocomposite thin films – deposition, structure and properties
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34R.J. Narayan, Diamond & Related Materials 14 (2005) 1319–1330
10 nm
self-assembled morphology
Ag-taC
TiC-taC
32 GPa
μ = 0.15
29 GPa
μ = 0.10
Excimer laser KrF, 248nm, 25ns, 10Hz, 5J/cm2
Ag
Ti
Coalescence of
Ag clusters
Carbon-based nanocomposite thin films – deposition, structure and properties
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Pulsed laser deposition of Ag-taC nanocomposites
Graphite
Ag
Laser beam
P.A. Patsalas, ESF Exploratory Workshop, ‘Carbon-based nanostructured composite films’ August 2006, Gdansk, Poland
Carbon-based nanocomposite thin films – deposition, structure and properties
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P.A. Patsalas, ESF Exploratory Workshop, ‘Carbon-based nanostructured composite films’ August 2006, Gdansk, Poland
Pulsed laser deposition of Ag-taC nanocomposites
Ag
_
+
Carbon-based nanocomposite thin films – deposition, structure and properties
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Ag
2
4
6
8
0 100 200 300 400 500 6001.0
1.5
2.0
2.5
(a)
Negative DC-Voltage (V)
=532 nm
(b)
Gro
wth
Rat
e (n
m/m
in)
=355 nm
P.A. Patsalas, ESF Exploratory Workshop, ‘Carbon-based nanostructured composite films’ August 2006, Gdansk, Poland
Pulsed laser deposition of Ag-taC nanocomposites
Carbon-based nanocomposite thin films – deposition, structure and properties
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Ag
18
19
20
21
22
23
0 1 2 3 4 5 6 7 8
0
20
40
60
80
(a)
[Ag] (% at.)
CK
LL W
idth
(eV
)
(b)
Con
cent
ratio
n (%
at.)
sp2
sp3
4
6
8
0 50 100 150 200 2500
10
20
30
4
5
6
7
[Ag]
(%
at.
)
Negative Bias Voltage (V)
[sp
3 ] (%
at.
)
GA
g (nm
)
30 35 40 45 50 55 60
(a) 25% Ag Target V
b=-250 V(200)
(111)
(b) 12.5% Ag Target V
b=-250 V
Inte
nsity
(A
rb. U
nits
)
(c)
12.5% Ag Target V
b=-125 V
(d)
Angle 2 (deg)
12.5% Ag Target V
b=0V
P.A. Patsalas, ESF Exploratory Workshop, ‘Carbon-based nanostructured composite films’ August 2006, Gdansk, Poland
Pulsed laser deposition of Ag-taC nanocomposites
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MeSi-aC:H; Me=Mo, Cr
V.K. Dmitriev et al.. Diamond and Related Materials 10 (2001) 1007-1010
Silicon-organic liquid – Plasma Polymerized Methyl Silane (PPMS) was used as a plasma-forming substance of the open plasmatron.
(C2H5)3SiO[CH3C6H5SiO]3Si(CH3)
3
Mo, Cr
IR radiation source or thermostable resistors
CrSi-aC:H
Carbon-based nanocomposite thin films – deposition, structure and properties
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MeSi-aC:H; Me=Mo, Cr
V.K. Dmitriev et al., Diamond and Related Materials 10 (2001) 1007-1010
Mo, Cr
Stability test:
1 year at 8000C in air
Carbon-based nanocomposite thin films – deposition, structure and properties
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SEM micrograph of two-level Cu wiring with DLC dielectric
ρ = 1016 Ωcm
ULSI chipsFilms with dielectric constant values between 3.3 and 2.7.
Incorporation of fluorine in FDLC films produces a material of apparently higher thermal stability and further reduced dielectric constant, to values even lower then 2.4
A. Grill, Diamond and Related Materials 10 (2001) 234-239
R.F. plasma-assisted PACVD in a parallel plate reactor.
P = CV 2f
Low-k interconnect dielectric
Carbon-based nanocomposite thin films – deposition, structure and properties
a-C:(H+F)
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Microwave radiation absorption
Co-aC:H films deposited by magnetron sputtering on aramide tissue (20-61 at.% Co) up to percolation threshold.
Superparamagnetic state at RT
Co-aC:H sputtering on aramide (aromatic polymer - polyamide) tissues provides flexible and durable electromagnetic absorption coverings.
L.V. Lutsev et al., JOURNAL OF APPLIED PHYSICS 97 (2005) 104327
Al2O3 Substrate
aramide tissueCo(60 at.%)-aC:H
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Concluding remarksCBNTF can be deposited by well known PVD (MS, VArc, PLD) and CVD (PACVD)
methods
In tribological applications CBNTF show:
• friction coefficient below 0.1 - can be achieved in vacuum and under humid conditions,
• low wear,
• hardness in the range from 10-40GPa,
• low residual stresses and good adhesion,
• high cohesive toughness.For CBNTF containing ferromagnetic metals (Ni, Co), superparamagnetic as well
asferromagnetic behaviour is observed dependent on metal cluster size.
Dielectric properties of CBNTF can be tuned form low to high k values.
Surface wetting properties of CBNTF can be modified by metal doping.
Silver conataining CBNTF show a potential for antibacterial applications.
Due to chemical inertness and biocompatibility, CBNTF are candidates for medical applications.
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Thank you for your kind
attention
Carbon-based nanocomposite thin films – deposition, structure and properties