Study of MoS2/SiC thin films on GCr15 steel substrate

d b Jiaming Je, Xiaojing WANO , Honghong SHAOe, Ji WANO Jiangsu University School of Material Science and Engineering

Zhenjiang, China ajijiaming@126.com, bhellomot085105@126.com, Chjgshh@ujs.edu.cn, dendeavor good@126.com

Abstract-The

MoSiSiC thin films were deposited on

Silicon carbide (SiC) has remarkbale thermal stability, chemical inertness and optical property. These days, researches at home and abroad are mainly about optical property of SiC thin films on single crystal silicon, diamond and so on [7-10]. SiC is considered to be an important high temperature structural material because of its outstanding mechanical properties, such as extreme hardness, high resistance to corrosion and wear, excellent high-temperatuer strength and good temperature

GCr15 steel substrate using radio frequency magnetron sputtering technique. Surface morphology, components and mechanical properties of the films were investigated by scanning electron microscopy, energy spectrometer, friction and wear tester and scratch tester, respectively. It was found that the surface morphology of the MoS2/SiC films prepared on GCr15 steel substrate was vermicular. The SiC inner layer and the MoS2 outer layer were binded tightly with a smooth interface and the thickness of the films was about 0.8 11m. The films-substrate system exhibited

conductivity. In fields like aerospace and electronic industries, SiC coating has been applied widely for antioxidation at high temperature [11,12]. Magnetron sputtering
IS

excellent friction and wear properties with a mean friction coefficient of about 0.11. Interlayers added into the films can improve the cohesion from 21 N to 26 N.

the

most

important

technology for the deposition of thin films. Today it has conquered all industrial branches needing high-quality coatings for realization of new or improvement of existing products. The main advantages of magnetron

Keywords- MoSjSiCfilms; magnetron sputtering; microstructure; mechanical properties; cohesion I.

INTRODUCTION

sputtering are as follows:

1 ) low plasma impedance

Molybdenum disulfide (MoS2) is one of typical layered compounds, which is particularly important for solid lubrication or as an additive for lubricating oils and greases. The laminar structure of MoS2 is made of layers, each of which comprises a plane of Mo atoms arranged in hexagonal array situated between two hexagonal layers of S atoms. The S-Mo-S covalent bonds inside layers are strong, providing excellent load capacity. However, the force between layers is weak

and thus high discharge currents from 1 A to 100 A (depending on cathode length) at typical voltages around 500V; 2 ) deposition rates in the range from 1 nmls to 10 nmls; 3 ) low thermal load to the substrate; 4 ) coating uniformity in the range of a few percent even for several meters long cathodes; 5 ) easy to scale up; 6 ) dense and well adherent coatings; 7 ) large variety of film materials available (nearly all metals and compounds); 8 ) broadly tunable film properties [13,14]. In this work MoS2/SiC thin films were deposited on OCr15 steel substrate using radio frequency magnetron sputtering technique. While MoS2 provides the

van-der-waals, so the interfacial shear strength is low. The easy sliding between MoS2 layers is generally regarded as a significant feature for its excellent lubricity [1]. As a promising solid lubricant, it has been of great interest for aerospace applications, commercial

lubrication, the existence of SiC as a inner layer is thought to improve the endurance lifetime of the films. Until now, such studies have been reported rarely at
1932

manufacturing and so on [2-6].

978-1-61284-752-8/11/$26.00 2011 IEEE

home and abroad, therefore investigations in this paper can provide basises for engineering applications of thin film materials in industry in the future.

argon pressure changed to 3 Pa. Process flow: deoil (ultrasonic cleaning with acetone and absolute alcohol) rust cleaning (10 % dilute sulfuric sputter acid)

II.
A

EXPERIMENT DETAILS

vacuum-pumping

substrate

cleaning

(magnetron power: 100 W, argon pressure: 3-5 Pa, deposition time: 20 min) target sputter cleaning deposition.

Sample preparation.
The sintered MoS2 and SiC targets with diameters of

60

mm

had a purity of 99% and the substrate to target

distance was 80 mm. As substrate material, hardened and lonnealed discs (30 mm diameter, I mm thickness) of GCr15 steel was used. Both the targets and the substrate were cooled by water and argon plasma was used for all depositions. In addition, single crystal silicon was also used as subatrate in order to test the components and the thickness of the films. Fig. I shows the micrograph of
A

III.

RESULTS

Microstructure analysis.
Scanning electron microscopy (SEM) was used to

study the surface morphology of coated GCr15 steel substrate. As shown in Fig. 2, surface morphology of the MoS2/SiC films was vermicular. Since MoS2 was

deposited on the residual heat of preparing SiC film and the temperature decreased so fast that atoms in the films can't diffuse adequately.

the GCr15 steel substrate.

Fig. 1 Micrograph of the GCr15 steel substrate

B

Film design.
The MoS2/SiC thin films, with the inner layer of

Fig.2

SEM image of the GCr15 steel substrate coated with MoSh/SiC films

ultrahard material SiC and the MoS2 antifriction outer layer, were deposited on GCr15 steel substrate, first the SiC layer and than theMoS2 layer, not to forget changing the target. Generally speaking, the inner layer is thicker than the outer layer. That is because the inner layer played the role of support and protection, while the outer layer was for lubricating. The procedure was carried out on JGP560CVI type ultra-high vacuum multifunction magnetron sputtering equipment, using radio frequency magnetron sputtering technique. The argon flow rate was 60 sccm during the deposition, with a background 5 vacuum level of less than 5x 10- Pa. The SiC film was deposited at the applied power of 200 W for 2 hours, with the argon pressure of 0.1 Pa. For the MoS2 film, the

The

components

of

the

MoS2/SiC

films

were

investigated by energy spectrometer. Fig. 3 reveals the cross-sectional SEM images and their EDS analysis of the GCr15 steel substrate and the MoS2/SiC films. From those pictures, we can see that the inner layer was SiC and the outer layer was MoS2 The two layers were binded tightly with a flat interface and the thickness of the films was about 0.8 /lm.

1933

2000

Me S

1000 '"

fr

Si

5 keV

10

(a) MoS2 outer layer

3000

Si

2000

1000

Me 5 keV 10

(b) SiC inner layer Fig.3 Cross-sectional SEM images and their EDS analysis of the MoS2/SiC films speed was 200 r/min, with a test diameter of
B

3 mm. For

Mechanical properties.
The friction coefficient of the substrate and the

accurate comparisons, each sample was tested under the same condition. Plots of the friction coefficient as a function of elapsed time were obtained for both the substrate and the MoS2/SiC films, such as those shown in Fig. 4.

MoS2/SiC films were tested with friction and wear tester at ambient temperature. A load of 0.49 N was applied to the surface of the samples during the test and the rotation

1934

1.1 1.0 0.9

1.0 0.9 0.8 0.7

<I> 0 if: <I> a <.> c .Q 13

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0 20 40 60 Time/min 80 100 120

== .,
c

., u 0.6 0 0.5 (J 0.4 0.3 0.2 0.1

U:

.!1

10 Time/min

(a) GCr15 steel substrate Fig.4 Friction curves of the substrate and the films

(b) MoS2/SiC films

It can be seen from the plots that the MoS2/SiC films-substrate system had a low and stable friction coefficient, with a mean magnitude of about 0.11 (Fig.4 (b)). Compare to the MoS2/SiC films, the friction

It was found that the MoS2 outer layer was scratched up at the load of 9 N, where there was a inflection point in the graph. When the load increased to 21 N, there was another inflection point with a sound signal,

coefficient of the substrate was much higher and unstable, about 0.9 (Fig.4 (a)). Therefore, MoS2/SiC films can reduce friction coefficient efficiently. In order to provide a intuitionistic and quantitative assessment of critical 10ad(Lc) of the films to the substrate, we investigated the coated samples with

characterizing the cohesion curve of hard coating under dual-mode. It indicated that SiC inner layer was failed at the load of 21 N. In other words, the cohesion between the substrate and the MoS2/SiC films was 21N.

scratch tester. The loading speed was

20 N/min and

the scratch length was 5 mm, with a final load of 60 N. All tests were conducted at ambient temperature. A sound emission and circumferential force dual-mode was adopted. Fig. 5 shows the cohesion curves of the MoS2/SiC films.

Influence of interlayers on the cohesion.

The mismatch of the coefficient of the thermal

expansion and the lattice parameter between GCr15 and

100 sound 80

SiC, SiC and MoS2, may result in unsatisfied cohesion (Fig. 5). In addition, films prepared using magnetron sputtering by high-energy particle bombardment and

::>

60

friction

2S
iii $ .!:
c

.;

energy transformation had a high residual stress, which will lead to the protection failure of the films. To solve

40

these problems, interlayers were designed to be added

20

into the films, which will considerably increase the cohesion between the films and the substrate.
10 20 30 Load/N 40 50 60

In order to play the role of transition layer, interlayer must meet two requirements [15]. Firstly, interlayer should have a good adhesion to the substrate or the film;

Fig.5

Cohesion curves of the GCr15 steel substrate coated with MoSiiSiC films

secondly, the coefficient of the thermal expansion of the interlayer must between the film and the substrate or between the two films.
1935

In line with those principles, a Ti interlayer deposited by DC magnetron sputtering and a Ni-P interlayer using Tab. I

electroless plating were added into the substrate and SiC, SiC and MoS2, respectively.

The thermal expansion coefficient of the substrate, the films and the interlayers materials MoS2
1 0. 7 Ti 8.2

SiC 4.6

Ni-P
9.1

GCrl5 14

thermal expansion coefficient Ix 1 0-6CC)

was vermicular. The inner layer of SiC and the outer layer The thermal expansion coefficient of interlayers, the substrate and the films are given in Table 1. From the table, it can be seen that the Ni-P electroless deposit and the DC magnetron sputtering Ti film meet those two requirements of interlayers. The process of Ni-P chemical plating was as follows: pretreatment (deoil) washing

of MoS2 were binded tightly with a smooth interface and the surface of the MoS2/SiC thin films was flat. The films-substrate system exhibited excellent friction and wear properties with a low friction coefficient. Interlayers added into the films can improve the cohesion between the substrate and the MoS2/SiC film. REFERENCES [1] K. H. Hu, 1. Wang, S. Schraube, Y. F. Xu, X. G. Hu, R. Stengler. Wear. 266 (2009) 1198. [2] J. X. Deng, W. L. Song, H. Zhang, 1. L. Zhao. International Journal of Machine Tools and

water

Ni-P chemical plating

water washing

drying. The coating time was 20 min and the thickness was about 3-4 f..Ul1, with a content of P of about 8.2%. Cohesion curves of the MoS2/SiC films with Ti and Ni-P inter-layer are shown in Figure 6.

100

Manufacture. 48 (2008) 1546.

sound

[3] B. Podgornik, J. Vifintin. Vacuum. 68 (2003) 39. [4] A. M. Merlo. Surface and Coatings Technology. 21 (2003)

80

U Iv
20 10

I\.

j\

174. [5] S. Voronin, O. Smorygo, P. Bertrand. Surface and

Coatings Technology. 180 (2004) 113. [6] S. Carrera, O. Salas, 1. 1. Moore. Surface and Coatings Technology. 167 (2003) 25. [7] G. Pandraud, H. T. M. Pham, P. J. French, P. M. Sarro.

?1
20

30 Load/N

40

50

60

Optics & Laser Technology. 39 (2007) 532. [8] P. S. Xu, C. K. Xie, H. B. Pan, F. Q. XU. Journal of Electron Spectroscopy and Related Phenomena. 144 (2005)

Fig.6

Cohesion curves of the MoS2/SiC films with Ti and Ni-P inter-layer

593. [9] Z. D. Sha, X. M. Wu, L. 1. Zhuge. Physics Letters A. 355 (2006) 228. [10] A. Le Donne, S. Binetti, S. Pizzini. Diamond and Related Materials. 14 (2005) 1150. [11] C. A. A. Cairo, M. L. A. Graca, C. R. M. Silva, J. C. Bressiani. Journal of the European Ceramic Society. 21 (2001) 325. [12] T. Aoki, H. Hatta, T. Hitomi, H. Fukuda, I. Shiota. Carbon. 39 (2001) 1477. [13] G. Brauer, B. Szyszka, M. Vergohl, R. Bandorf. Vacuum. 84 (2010) 1354. [14] P. J. Kelly, R. D. Arnell. Vacuum. 56 (2000) 159. [15] B. Rother, H. A. Jehn. Surface and Coatings Technology. 85 (1996) 183.
1936

From the curves we can see that the first inflection point appeared at the load of 10 N, at this point, MoS2 outer layer was scratched up. When the load added to 26 N, a strong sound signal appeared, SiC film was failed. Compare to the curves in Fig. 5, Cohesion between the substrate and the MoS2/SiC films after adding interlayers was improved from 21 N to 26 N.

IV.

SUMMARY

In this work MoS2/SiC films were deposited on the GCr15 steel substrate using radio frequency magnetron sputtering technique. Surface morphology of the films