WS_2薄膜制备工艺及其摩擦学性能的实验研究
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摘要
近年来随着科学技术的发展,特别是空间技术的迅猛发展,人们对润滑材料的要求不断提高,研制高性能的固体润滑材料就成为目前迫切需要解决的问题。WS2作为一种新型的优秀固体润滑材料在某些方面的表现要优于传统的MoS2薄膜,因此人们开始越来越多地关注WS2在摩擦学方面的应用。同国外相比国内对于WS2的研究起步较晚,对于WS2薄膜的润滑机理仍有待研究,仍有许多新现象有待发现,在实际应用中更没有形成产品规模。我国W、Mo矿储量非常丰富,而我国在工业中所使用固体润滑产品的份额,仍不足美国、日本等国家的一半,显然对于WS2薄膜的研究具有尤为重要的意义。
本文研究了在3Crl3马氏体不锈钢基底上,分别利用硫化法和射频溅射法两种方法制备WS2薄膜。通过对薄膜结构、表面形貌、化学成分以及摩擦磨损等方面的表征测试,研究了工艺条件对WS2薄膜性能的影响,为WS2薄膜在国内相关领域的应用及推广提供了有益参考。
研究表明,采用硫粉硫化氧化钨薄膜的方法可以在3Cr13马氏体不锈钢基体表面上获得WS2薄膜,温度对硫化钨薄膜的表面形貌和结晶率有明显的影响,对膜层的化学成分影响不大,薄膜能够有效地改善不锈钢基体的摩擦学性能,随着硫化温度的升高,摩擦系数降低,同时测试环境和测试条件对薄膜的摩擦系数也会产生影响。
利用射频溅射法制备WS2薄膜时,溅射气压、溅射功率和沉积时间三种工艺参数的变化也会对薄膜的性能产生一定影响。薄膜的化学成分即S/W原子比,受工艺参数变化影响较为明显,通过对比可以发现,射频溅射所获得薄膜的摩擦系数在一定范围内与其硫钨比成反比。
本文还研究了利用射频溅射法制备WS2薄膜时,预先沉积Ti、Ni两种过渡层及成膜后真空退火对薄膜性能的影响。结果表明,Ti过渡层对硫化钨薄膜结构和S/W原子比没有明显的影响,对膜层的摩擦系数影响也不大,但薄膜耐磨性有所提高。而Ni过渡层虽对S/W原子比无明显影响,但却明显地提高薄膜Ⅱ型织构(基面取向)的强度,从而降低了薄膜的摩擦系数,提高了薄膜耐磨性。而适当的后续真空退火处理可以对由射频溅射所获得的WS2薄膜的结构和表面形貌产生一定影响,可以促进薄膜的晶化进程,但有时也会使薄膜发生脆化,导致薄膜的破损、脱落。
As the development of science and technology, especially flourishing development of space technology, the requirement of lubricating material has been increasing accordingly. Development high-performance solid lubricating material has been exigent problem. As a late-model excellent solid lubrication films tungsten disulfide films performance is better than classical molybdenum disulfide films in some aspects. So the tribological behavior of WS2 films has been paid more and more attention. Comparing with foreign study, the domestic research of WS2 films was carried out later. The lubricating mechanics of WS2 films still needs discussing, some new phenomenon needs discovering and the WS2 films are not extensive used in practical application now. The mineral reserves of W, Mo in our country is abundant, but according to some countries like USA, Japan, etc, the quotient of solid lubricant application has not reached moiety. So research of WS2 films is significant.
In this paper, tungsten disulfide thin films were prepared by sulfuration method and RF sputtering on 3Cr13 martensite restless steel. The effects of process parameters on the properties of WS2 films were investigated by characterization and testing on film structural, surface topography, chemical constitution, friction wear properties, etc. It offers a useful reference for generalizing of WS2 films in correlative fields.
The research showed that WS2 films could be obtained by sulfured tungsten oxide thin films on 3Cr13 martensite restless steel. Sulfurizing temperatures influenced surface topography and crystallization obviously. But the influence on chemical constitution was not obvious. The frictional behaviour of stain less steel basal plant was improved by these films. When sulfurizing temperature raised the fiction coefficient of the films reduced and the fiction coefficient were also influenced by testing environment and conditions.
When the WS2 films deposited by RF sputtering, the performance of films would be influenced by the changes of power, pressure and deposition time. The chemical constitution namely S/W ratio were impacted by sputter technological parameter obviously. The coefficient of friction of the sample prepared by RF sputter had inversely-proportional relationship with S/W ratio in definitive range.
The effects of Ti and Ni transition layers and vacuum annealing on frictional behavior of tungsten disulfide thin film preparation with RF sputtering on substrate was also researched in this paper. The results showed that Ti transition layer didn't influence tungsten disulfide films'structure, S/W ratio and frictional coefficient observably, but the abradability of this film was enhanced. The S/W ratio of tungsten disulfide film was not influenced observably by Ni transition layer, but the intensity of textureⅡ(basal plane orientation)of tungsten disulfide thin film was strengthen obviously by Ni transition layer, then the frictional coefficient of this film was reduced and the abradability of the film was enhanced. And suitable vacuum annealing was able to promote crystallization and improve tribological performance of RF sputtering WS2 films. But sometimes the films could be desquamated from substrate because of embrittlement.
本文研究了在3Crl3马氏体不锈钢基底上,分别利用硫化法和射频溅射法两种方法制备WS2薄膜。通过对薄膜结构、表面形貌、化学成分以及摩擦磨损等方面的表征测试,研究了工艺条件对WS2薄膜性能的影响,为WS2薄膜在国内相关领域的应用及推广提供了有益参考。
研究表明,采用硫粉硫化氧化钨薄膜的方法可以在3Cr13马氏体不锈钢基体表面上获得WS2薄膜,温度对硫化钨薄膜的表面形貌和结晶率有明显的影响,对膜层的化学成分影响不大,薄膜能够有效地改善不锈钢基体的摩擦学性能,随着硫化温度的升高,摩擦系数降低,同时测试环境和测试条件对薄膜的摩擦系数也会产生影响。
利用射频溅射法制备WS2薄膜时,溅射气压、溅射功率和沉积时间三种工艺参数的变化也会对薄膜的性能产生一定影响。薄膜的化学成分即S/W原子比,受工艺参数变化影响较为明显,通过对比可以发现,射频溅射所获得薄膜的摩擦系数在一定范围内与其硫钨比成反比。
本文还研究了利用射频溅射法制备WS2薄膜时,预先沉积Ti、Ni两种过渡层及成膜后真空退火对薄膜性能的影响。结果表明,Ti过渡层对硫化钨薄膜结构和S/W原子比没有明显的影响,对膜层的摩擦系数影响也不大,但薄膜耐磨性有所提高。而Ni过渡层虽对S/W原子比无明显影响,但却明显地提高薄膜Ⅱ型织构(基面取向)的强度,从而降低了薄膜的摩擦系数,提高了薄膜耐磨性。而适当的后续真空退火处理可以对由射频溅射所获得的WS2薄膜的结构和表面形貌产生一定影响,可以促进薄膜的晶化进程,但有时也会使薄膜发生脆化,导致薄膜的破损、脱落。
As the development of science and technology, especially flourishing development of space technology, the requirement of lubricating material has been increasing accordingly. Development high-performance solid lubricating material has been exigent problem. As a late-model excellent solid lubrication films tungsten disulfide films performance is better than classical molybdenum disulfide films in some aspects. So the tribological behavior of WS2 films has been paid more and more attention. Comparing with foreign study, the domestic research of WS2 films was carried out later. The lubricating mechanics of WS2 films still needs discussing, some new phenomenon needs discovering and the WS2 films are not extensive used in practical application now. The mineral reserves of W, Mo in our country is abundant, but according to some countries like USA, Japan, etc, the quotient of solid lubricant application has not reached moiety. So research of WS2 films is significant.
In this paper, tungsten disulfide thin films were prepared by sulfuration method and RF sputtering on 3Cr13 martensite restless steel. The effects of process parameters on the properties of WS2 films were investigated by characterization and testing on film structural, surface topography, chemical constitution, friction wear properties, etc. It offers a useful reference for generalizing of WS2 films in correlative fields.
The research showed that WS2 films could be obtained by sulfured tungsten oxide thin films on 3Cr13 martensite restless steel. Sulfurizing temperatures influenced surface topography and crystallization obviously. But the influence on chemical constitution was not obvious. The frictional behaviour of stain less steel basal plant was improved by these films. When sulfurizing temperature raised the fiction coefficient of the films reduced and the fiction coefficient were also influenced by testing environment and conditions.
When the WS2 films deposited by RF sputtering, the performance of films would be influenced by the changes of power, pressure and deposition time. The chemical constitution namely S/W ratio were impacted by sputter technological parameter obviously. The coefficient of friction of the sample prepared by RF sputter had inversely-proportional relationship with S/W ratio in definitive range.
The effects of Ti and Ni transition layers and vacuum annealing on frictional behavior of tungsten disulfide thin film preparation with RF sputtering on substrate was also researched in this paper. The results showed that Ti transition layer didn't influence tungsten disulfide films'structure, S/W ratio and frictional coefficient observably, but the abradability of this film was enhanced. The S/W ratio of tungsten disulfide film was not influenced observably by Ni transition layer, but the intensity of textureⅡ(basal plane orientation)of tungsten disulfide thin film was strengthen obviously by Ni transition layer, then the frictional coefficient of this film was reduced and the abradability of the film was enhanced. And suitable vacuum annealing was able to promote crystallization and improve tribological performance of RF sputtering WS2 films. But sometimes the films could be desquamated from substrate because of embrittlement.
引文
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