carbon-based nanocomposite thin films – deposition , structure and properties

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3Koszalin University

of Technology

1

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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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.


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.


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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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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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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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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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(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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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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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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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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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


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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


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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)


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WS2 lubrication

Graphite

lubrication


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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


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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


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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


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W. Gulbiński et al., Applied Surface Science 239 (2005) 302–310


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


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23Q.F. Huang et al., Diamond and Related Materials 9 (2000) 534–538

MoCx-aC:H nanocomposite films


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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


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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


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


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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


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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


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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


C1sXPS


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As deposited

3000C

3500C 4000

C

Magnetic Force Microscopy


Co-taC nanocomposite films

Magnetization loop


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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.


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Cu-aC:H

16 at.% Cu

C.-C. Chen, F.C.-N. Hong, Applied Surface Science 242 (2005) 261–269


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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


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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


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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


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Ag

_

+


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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




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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




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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


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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


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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


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

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