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磁控溅射制备MoS2基复合薄膜的结构与性能研究
Investigation of Microstructure and Properties of Molybdenum Disulfide Based Composite Films Deposited by Magnetron Sputtering
【作者】 李倩倩;
【导师】 何丹农;
【作者基本信息】 上海交通大学 , 材料学, 2011, 硕士
【摘要】 为了提高MoS2薄膜在室温潮湿大气条件下的摩擦磨损性能,本文采用磁控溅射方法制备了MoS2-Ti-WS2、MoS2-Ti-C和MoS2-TiN复合薄膜,作为比较在相同实验条件下制备了纯MoS2和MoS2-Ti薄膜。采用能谱仪(EDS)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)等对薄膜的成分、结构和形貌进行表征,采用纳米压痕仪、UMT-2多功能微摩擦磨损试验机等测试薄膜与基体的结合力、纳米压痕硬度以及摩擦系数,并观察薄膜的磨损形貌,评价薄膜在室温潮湿大气条件下的摩擦磨损性能。在溅射气压0.3 Pa条件下,采用磁控共溅射方法制备了MoS2-Ti-WS2复合薄膜,对薄膜的结构进行表征并测试其性能。研究结果表明:MoS2-Ti薄膜和MoS2-Ti-WS2复合薄膜均未出现(100)晶面衍射峰,结构致密,表面没有空洞,呈现纳米晶粒聚集的岛状结构,未观察到纯MoS2薄膜的蠕虫状疏松结构。与纯MoS2和MoS2-Ti薄膜相比,MoS2-Ti-WS2复合薄膜具有更高的纳米压痕硬度,更长的稳态摩擦时间,更低的摩擦系数,且摩擦系数波动范围更小。对薄膜的表面磨损形貌进行测试,发现MoS2-Ti-WS2复合薄膜的磨痕深度和宽度小,磨损率更低,复合薄膜的耐磨性能明显改善。在溅射气压1 Pa条件下,采用反应磁控溅射方法分别制备了MoS2-Ti-C和MoS2-TiN复合薄膜,对薄膜结构进行表征并测试其性能。研究结果表明:纯MoS2薄膜(100)晶面择优取向,为典型的第一类疏松多孔柱状晶结构薄膜;MoS2-Ti薄膜具有(002)、(100)混合晶面取向,薄膜中存在疏松结构;而MoS2-Ti-C和MoS2-TiN复合薄膜(002)晶面择优取向,属于第二类薄膜,薄膜结构致密,未发现疏松结构,与基体的结合力及纳米压痕硬度明显提高。在摩擦过程中,纯MoS2、MoS2-Ti薄膜的摩擦系数波动大,摩擦系数较高,分别约为0.35和0.22;而MoS2-Ti-C和MoS2-TiN复合薄膜的摩擦系数稳定,约为0.1。与纯MoS2和MoS2-Ti薄膜相比,MoS2-Ti-C和MoS2-TiN复合薄膜的磨损率更低,说明薄膜具有更优异的减摩和耐磨性能。
【Abstract】 In order to improve friction and wear properties of MoS2 films in humid air at room temperature, MoS2-Ti-WS2, MoS2-Ti-C and MoS2-TiN composite films were prepared by magnetron sputtering. For comparison, pure MoS2 and MoS2-Ti films were deposited under the same conditions. The composition, microstructure and morphology of the films were analysed by X-ray diffraction, energy dispersive X-ray spectroscopy and scanning electron microscope. The adhesion to substrate, nanoindentation hardness and friction coefficient of the films were tested by nanoindenter and UMT-2 multi-functional tribometer tester, respectively. In addition, worn surfaces of films were characterized. The friction and wear properties were investigated in humid air at room temperature.The microstructure and properties of MoS2-Ti-WS2 composite films, which were prepared by magnetron co-sputtering at a working pressure of 0.3 Pa, were investigated. It has been observed that, no (100) diffraction peaks appear for both MoS2-Ti and MoS2-Ti-WS2 films, which exhibit granular structure, agglomerated nanosized grains and are more compact than pure MoS2 film; while pure MoS2 film has typical porous and worm-like surface structure. Compared with pure MoS2 and MoS2-Ti films, the MoS2-Ti-WS2 composite films have higher nanoindentation hardness, longer steady-state friction time, lower friction coefficient and smaller fluctuation range. The worn surfaces show MoS2-Ti-WS2 composite film has smaller depth and width. The wear rate value for MoS2-Ti-WS2 composite film is much lower, which means it has much better wear resistance.MoS2-Ti-C and MoS2-TiN composite films were deposited by reactive magnetron sputtering at a working pressure of 1 Pa. The study of microstructure and properties shows that, pure MoS2 film has preferred orientation of (100) plane and columnar plate morphology with inherent porosity, called type I film. MoS2-Ti film has mixture of (002) and (100) crystal orientation with loose construction. MoS2-Ti-C and MoS2-TiN composite films have strong basal orientation of (002) crystal plane and compact microstructure, called type II films. The adhesion to substrate and nanoindentation hardness were improved significantly for the composite films. Pure MoS2 and MoS2-Ti films are shown to have larger fluctuation and higher friction coefficient, that is, about 0.35 and 0.22, respectively; while it is steady, about 0.1 for the MoS2-Ti-C and MoS2-TiN films. The wear rate values for MoS2-Ti-C and MoS2-TiN composite films are much lower than those of pure MoS2 and MoS2-Ti films, which shows that MoS2-Ti-C and MoS2-TiN composite films have much superior friction reducing and anti-wear properties.
【Key words】 magnetron sputtering; MoS2-Ti-WS2; MoS2-Ti-C; MoS2-TiN; composite film; friction and wear;