刘进龙,李红轩,吉利,刘晓红,张定军.TiB2掺杂WS2复合薄膜的宽温域摩擦学性能研究[J].表面技术,2023,52(6):235-245.
LIU Jin-long,LI Hong-xuan,JI Li,LIU Xiao-hong,ZHANG Ding-jun.Tribological Properties of TiB2 Doped WS2 Composite Films in Wide Temperature Range[J].Surface Technology,2023,52(6):235-245
TiB2掺杂WS2复合薄膜的宽温域摩擦学性能研究
Tribological Properties of TiB2 Doped WS2 Composite Films in Wide Temperature Range
  
DOI:10.16490/j.cnki.issn.1001-3660.2023.06.020
中文关键词:  WS2/TiB2复合薄膜  宽温域  机械性能  摩擦磨损  晶体取向
英文关键词:WS2/TiB2 composite film  wide temperature range  mechanical properties  friction and wear  crystal orientation
基金项目:国家自然科学基金(U2141210,51975561);中国科学院青年创新促进会优秀会员计划(Y202084)
作者单位
刘进龙 兰州理工大学 材料科学与工程学院,兰州 730030;中国科学院兰州化学物理研究所 固体润滑国家重点实验室,兰州 730000 
李红轩 中国科学院兰州化学物理研究所 固体润滑国家重点实验室,兰州 730000 
吉利 中国科学院兰州化学物理研究所 固体润滑国家重点实验室,兰州 730000 
刘晓红 中国科学院兰州化学物理研究所 固体润滑国家重点实验室,兰州 730000 
张定军 兰州理工大学 材料科学与工程学院,兰州 730030 
AuthorInstitution
LIU Jin-long School of Material Science and Engineering, Lanzhou University of Technology, Lanzhou 730030, China;State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China 
LI Hong-xuan State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China 
JI Li State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China 
LIU Xiao-hong State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China 
ZHANG Ding-jun School of Material Science and Engineering, Lanzhou University of Technology, Lanzhou 730030, China 
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中文摘要:
      目的 探究TiB2溅射电流(即TiB2含量)对WS2/TiB2复合薄膜在宽温域(25~500 ℃)下摩擦学性能的影响。方法 采用非平衡磁控溅射技术制备WS2/TiB2复合薄膜。通过场发射扫描电子显微镜(FESEM)、高分辨率透射电子显微镜(HRTEM)观察薄膜的形貌及结构;通过X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)表征薄膜结构;通过纳米压痕仪(Anton Paar,NHT2)评价薄膜的机械性能;利用高温球盘摩擦磨损试验机(THT01,03591)测试薄膜的摩擦学性能;采用光学显微镜(Olympus,STM6)、三维轮廓仪(Micro XAM–800)观察磨痕及磨斑形貌,通过HRTEM分析磨痕和磨斑的结构。结果 TiB2掺杂使WS2薄膜由高度结晶态向非晶态转变,增大了薄膜的致密度并提高了其机械性能。随着TiB2溅射电流的增大,复合薄膜的摩擦因数和磨损率呈先下降后上升的趋势。随着试验温度的升高,复合薄膜的摩擦因数先降低后升高,但磨损率一直逐渐升高。TiB2溅射电流为1.5 A时,制备的复合薄膜在宽温域(25~500 ℃)具有较低的摩擦因数和磨损率。300 ℃条件下,TiB2溅射电流为1.5 A时制备的复合薄膜在摩擦剪切力作用下重新定向形成了TiB2(101)晶体取向和平行于滑动方向的WS2(002)晶体取向,并在高环境温度和摩擦热作用下氧化形成了润滑相TiO2(001)晶体结构。结论 TiB2溅射电流为1.5 A时制备的复合薄膜具有优异的宽温域摩擦学性能。薄膜致密的非晶结构、高的硬度和弹性模量,以及在摩擦剪切力和高温氧化作用下重新结晶取向是低摩擦磨损的关键。
英文摘要:
      The work aims to investigate the effect of TiB2 sputtering current (the content of TiB2) on tribological properties of WS2/TiB2 composite films in wide temperature range (25-500 ℃). WS2/TiB2 composite films were prepared by non-equilibrium magnetron sputtering. The morphology and structure of the films were observed by field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscope (HRTEM). The structure of the films was characterized by X-ray diffractometer (XRD) and X-ray photoelectron spectrometer (XPS). The mechanical properties of the films were evaluated by nanoindentation instrument (Anton Paar, NHT2). The tribological properties of the films were tested by a high temperature ball disc friction and wear tester (THT01, 03591). Optical microscope (Olympus, STM6) and three- dimensional profilometer (Micro XAM-800) were used to observe the morphology of wear tracks and wear scars, and HRTEM was used to analyze the structure of wear tracks and wear scars. TiB2 doped WS2 films changed from highly crystalline to amorphous state, and the surface morphology of composite films changed from "worm-like" to "island-like", improving the density and mechanical properties. With the increase of TiB2 sputtering current, the friction coefficient and wear rate of the composite films decreased firstly and then increased. In addition, as the test temperature rose, the friction coefficient of the composite films firstly decreased and then increased, but the wear rate was gradually increasing. Among them, sputtering current of TiB2 with 1.5 A contributed to the lowest friction coefficient and wear rate in wide temperature range (25-500 ℃). The friction coefficients of composite films at 100 and 300 ℃ at sputtering current with 0-2.5 A were lower than those at 25 and 500 ℃, while the friction coefficient of composite film prepared with TiB2 sputtering current of 4.0 A was opposite. By analyzing the wear tracks and corresponding wear scars of composite films prepared with sputtering current of 1.5 A at different experimental temperature, it was found that the furrow on the surface of wear tracks was obvious at 25 ℃. When the temperature rose to 100 and 300 ℃, the furrow on the surface of the wear tracks became shallow, and the friction coefficient decreased and remained stable, respectively to about 0.015 and 0.021. However, the depth, width and wear rate of wear tracks slightly increased, and the friction mechanism was mainly abrasive wear and adhesive wear. When the experimental temperature reached 500 ℃, the plastic deformation of the film surface and subsurface increased, the damage was serious, there was a wide furrow, and the film was basically invalidated. However, the friction coefficient was kept at about 0.08, which was typical of the transfer film lubrication, occurring in part of the oxidation wear during friction. With the increase of the experimental temperature, the size of the debris on the pair ball became larger, the transfer film on the pair ball moved from the edge of the wear scars to the center gradually, and a continuous and dense transfer film was formed at 300 ℃. In order to further investigate the structure evolution of composite films at high temperature, the wear tracks and wear scars of composite film with TiB2 sputtering current of 1.5 A at 300 ℃ were prepared by FIB and observed by transmission electron microscope. Under the frictional shear force, the crystal plane orientation of WS2(002) parallel to the sliding direction and the crystal plane orientation of TiB2(101) was formed. Meanwhile, the crystal plane structure of lubricated TiO2(001) was formed by oxidation under high ambient temperature and frictional heat. The composite films prepared at TiB2 sputtering current of 1.5 A have excellent tribological properties in wide temperature range. The dense amorphous structure, high hardness and elastic modulus, and recrystallization orientation under frictional shear force and high temperature oxidation are the key factors for low frictional wear.
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