磁控溅射WS_2、WS_2-C固体润滑薄膜的制备与性能研究
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摘要
作为固体润滑材料,WS2以其优异的摩擦学性能在航空航天、机械加工、微电子等领域有广泛的应用价值。但是纯WS2薄膜的承载能力较低、且易在潮湿空气中吸潮氧化,从而缩短了其使用寿命。为提高纯WS2薄膜的承载能力及服役寿命,本研究以WS2、石墨和纯Ti为靶材,采用孪生靶中频磁控溅射、直流磁控溅射结合离子增强的方法,在单晶硅片及TC4合金(Ti6A14V)基体表面制备了WS2和WS2-C复合薄膜。通过扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)、Raman光谱仪、金相显微镜(OM)、显微硬度仪、划痕仪和球盘式摩擦磨损试验机对薄膜的微观组织、物相结构、力学性能及摩擦磨损性能进行了研究。结果表明：
通过中频磁控溅射方法制备的WS2薄膜有不同程度的S元素损失现象,其S/W原子比与工作气压密切相关,受沉积温度的影响不太明显；WS2薄膜呈现明显的(002)晶面择优生长,随着沉积温度的升高,薄膜的(002)衍射峰逐渐减弱；纯WS2薄膜的显微硬度较低,膜/基结合强度较好；较低温度条件下制备的WS2薄膜具有较低的的摩擦系数,减摩效果良好,升高沉积温度,薄膜的摩擦系数有所提高。
共溅射WS2靶和石墨靶制备的WS2-C复合薄膜结构致密,S/W原子比接近于同条件下的WS2薄膜；随着碳含量的增加,复合薄膜的WS2(002)晶面衍射峰逐渐减弱；碳钨化合物的出现使得薄膜的硬度有了一定程度的提高；添加碳元素,复合薄膜的膜/基结合强度有降低的趋势；随着碳含量的增加,复合薄膜的摩擦系数逐渐升高,其减摩效果不如纯WS2薄膜,但是其耐磨寿命有了很大程度的提高；纯WS2膜及低碳含量复合薄膜的摩擦系数随载荷的增加而有所降低,对于较高碳含量的复合薄膜,摩擦系数受载荷的影响不太明显,载荷变大时薄膜的摩擦过程基本上都逐渐趋于稳定。
As a kind of solid lubrication materials, tungsten disulphide (WS2) with perfect tribological properties is very practical in these fields such as aerospace, mechanical manufacturing and micro-electron. But WS2 film will react with oxygen in humid environment forming WO3 that has a high friction coefficient and poor wear behavior. To improve its bearing capacity and tribological behavior, we deposited pure WS2 films and WS2-C composite films using WS2, graphite and pure titanium targets on silicon and Ti6A14V (TC4) alloy substrates by twin-target MF magnetron sputtering and DC magnetron sputtering combined with ion source. Their surface morphology, phase structure, mechanical and tribological properties were investigated via SEM, EDX, Raman spectroscopy, OM, microhardness gauge, scratch tester and ball-on-disk friction/wear test machine. The results showed that:
The films depodited by twin-target MF magnetron sputtering was deficient in sulfer element, the S/W atomic ratio of the tungsten disulfide films was more obviously related to the working pressure than the deposition temperature. The films showed the strongest (002) crystal plane at fifty degree, and the diffraction peak decreased as improving the deposition temperature. The micro-hardness of the films was low, but the adhesion force between the substrate and the film was high. The tungsten disulfide films deposited at lower temperatures exhibited much better tribological properties, and the friction coefficient of the films grudurally went up as increasing the deposition temperature.
The S/W ratio of the WS2-C composite films was close to the pure films, and the structure was much denser than pure films. The WS2 (002) diffraction peak weakened as increasing the carbon content, but the hardness of WS2-C composite films become much higher because of the presence of carbide phases. The critical load values, Lc2, of the composite films obtained by scratch testing varied from 50N to 70N, and it gradurally decreased with incrementing the carbon content. Compared with the pure films, the anti-wear life of the composite films were much longer, though the friction coefficient was a little higher. The friction coefficient of the pure WS2 film and low carbon content films were observed to decrease continuously with increasing load. It could be concluded that the friction mechanisms of high carbon content films fundamentally differ from those of low carbon content films and pure films.
通过中频磁控溅射方法制备的WS2薄膜有不同程度的S元素损失现象,其S/W原子比与工作气压密切相关,受沉积温度的影响不太明显；WS2薄膜呈现明显的(002)晶面择优生长,随着沉积温度的升高,薄膜的(002)衍射峰逐渐减弱；纯WS2薄膜的显微硬度较低,膜/基结合强度较好；较低温度条件下制备的WS2薄膜具有较低的的摩擦系数,减摩效果良好,升高沉积温度,薄膜的摩擦系数有所提高。
共溅射WS2靶和石墨靶制备的WS2-C复合薄膜结构致密,S/W原子比接近于同条件下的WS2薄膜；随着碳含量的增加,复合薄膜的WS2(002)晶面衍射峰逐渐减弱；碳钨化合物的出现使得薄膜的硬度有了一定程度的提高；添加碳元素,复合薄膜的膜/基结合强度有降低的趋势；随着碳含量的增加,复合薄膜的摩擦系数逐渐升高,其减摩效果不如纯WS2薄膜,但是其耐磨寿命有了很大程度的提高；纯WS2膜及低碳含量复合薄膜的摩擦系数随载荷的增加而有所降低,对于较高碳含量的复合薄膜,摩擦系数受载荷的影响不太明显,载荷变大时薄膜的摩擦过程基本上都逐渐趋于稳定。
As a kind of solid lubrication materials, tungsten disulphide (WS2) with perfect tribological properties is very practical in these fields such as aerospace, mechanical manufacturing and micro-electron. But WS2 film will react with oxygen in humid environment forming WO3 that has a high friction coefficient and poor wear behavior. To improve its bearing capacity and tribological behavior, we deposited pure WS2 films and WS2-C composite films using WS2, graphite and pure titanium targets on silicon and Ti6A14V (TC4) alloy substrates by twin-target MF magnetron sputtering and DC magnetron sputtering combined with ion source. Their surface morphology, phase structure, mechanical and tribological properties were investigated via SEM, EDX, Raman spectroscopy, OM, microhardness gauge, scratch tester and ball-on-disk friction/wear test machine. The results showed that:
The films depodited by twin-target MF magnetron sputtering was deficient in sulfer element, the S/W atomic ratio of the tungsten disulfide films was more obviously related to the working pressure than the deposition temperature. The films showed the strongest (002) crystal plane at fifty degree, and the diffraction peak decreased as improving the deposition temperature. The micro-hardness of the films was low, but the adhesion force between the substrate and the film was high. The tungsten disulfide films deposited at lower temperatures exhibited much better tribological properties, and the friction coefficient of the films grudurally went up as increasing the deposition temperature.
The S/W ratio of the WS2-C composite films was close to the pure films, and the structure was much denser than pure films. The WS2 (002) diffraction peak weakened as increasing the carbon content, but the hardness of WS2-C composite films become much higher because of the presence of carbide phases. The critical load values, Lc2, of the composite films obtained by scratch testing varied from 50N to 70N, and it gradurally decreased with incrementing the carbon content. Compared with the pure films, the anti-wear life of the composite films were much longer, though the friction coefficient was a little higher. The friction coefficient of the pure WS2 film and low carbon content films were observed to decrease continuously with increasing load. It could be concluded that the friction mechanisms of high carbon content films fundamentally differ from those of low carbon content films and pure films.
引文
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