WS_2/W-DLC复合固体润滑薄膜的制备与组织性能研究
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摘要
本论文以改善掺钨类金刚石（W-DLC）膜的摩擦学性能为出发点，以多层膜技术为主导，利用复合沉积技术结合低温离子渗硫技术制备了含氢和无氢的WS2/W-DLC复合固体润滑薄膜。在MS-T3000球盘摩擦磨损实验机上对比研究了在离子渗硫处理前后薄膜的摩擦磨损性能。利用扫描电子显微镜、三维白光形貌仪、X射线衍射仪、拉曼光谱、X射线光电子能谱等微观分析仪器全面观察分析了薄膜的形貌、组织结构、元素原子价态与元素分布等，研究了薄膜中钨含量对于WS2/W-DLC复合固体润滑薄膜的微观形貌、成分、结构、力学性能、摩擦学性能的影响，结果表明：
（1）利用阴极电弧+直流磁控溅射技术结合离子渗硫技术制备了含氢的WS2/W-DLC复合固体润滑薄膜。薄膜表面光滑，仅存在少量纳米级颗粒。薄膜的微观形貌、成分、力学及摩擦学性能均受到W含量的影响。随着W含量增加，薄膜中sp2含量增多，并促使WXC纳米晶生成，薄膜硬度之增大。渗硫处理后，由于石墨化和表层生成软质相WS2，造成薄膜硬度下降。其中渗硫处理W含量为27.7%的薄膜具有最优的摩擦学性能，摩擦系数为0.19，磨损率为1.65×10-7mm3/Nm。
（2）利用离子束辅助沉积技术结合离子渗硫制备了无氢的WS2/W-DLC复合固体润滑薄膜。薄膜具有纳米尺度光滑表面，无任何缺陷，渗硫处理后表面粗糙度小于30nm。随着W靶束流增大，薄膜硬度和弹性模量增大。渗硫处理后，由于表面生成金属硫化物和富石墨的复合固体润滑层，导致薄膜硬度值下降。渗硫处理W靶束流为75mA的薄膜具有最优的性能，摩擦系数为0.107，磨损率为2.37×10-7mm3/Nm。
（3）离子渗硫处理后的W-DLC膜，薄膜表层软质金属硫化物和富石墨层，是减摩抗磨主要原因。渗硫处理后，高钨含量的薄膜，为软质表层提高了良好的支撑。在干摩擦条件下，减小了摩擦接触面积和塑性变形，有效地改善了摩擦学性能。
With the purpose of improving the tribological property of W doped diamondlike carbon (W-DLC) film, on the basis of the coating concept of multilayer, twoseries of WS2/W-DLC composite solid lubrication films were prepared using hybriddeposition techniques in combination with low temperature ion sulfurizationtechnique, including hydrogenated and hydrogen-free WS2/W-DLC composite solidlubrication coatings. The tribological property of the films before or after thetreatment was investigated by a MS-T3000friction and wear tester. SEM and three-dimensional light interfering profilometer were employed to observe themorphologies of surface of films, XRD was adopted to detect the surface phasestructure. Raman was adopted to characterize the structure of C atoms and XPS wasused to identify the valence state of different elements of the films. The influence ofW concentration on the micro-morphology, composition, microstructure, mechanicaland tribological property of the coatings were investigated. The results were shown asfollowed:
(1) The hydrogenated WS2/W-DLC composite solid lubrication films werefabricated by ion beam deposition+magnetron sputtering techniques in combinationwith low temperature ion sulfurization. The surfaces were smooth, only with somenanoscale particles. With the increasing of W concentration, the content of sp2increased, however the formation of hard nanoparticles WXC in carbon matrix to forma nanocomposite structure led to an enhancement in hardness. Graphitization and WS2was formed on the surface of W-DLC film after ion sulfuration, which made thehardness of W-DLC film decreases. The optimum wear performance with frictioncoefficient of0.19and wear rate of1.65×10-7mm3/Nm was achieved for27.7%WS2/W-DLC film.
(2) The hydrogen-free WS2/W-DLC composite solid lubrication film wasprepared by ion beam assistant deposition technique in combination with lowtemperature ion sulfurization. All the surfaces were nanoscale and without defect. Theroughness was lower than30nm after ion sulfurization. The hardness and elastic modulus of the films were increased gradually, as the W target current increased.After ion sulfurization the hardness decreased, due to the formation of metal sulfidesand graphite-rich composite solid lubrication layer on the top surface. The lowestfriction coefficient0.107and wear rate2.37×10-7mm3/Nm were achieved from thesample at W target beam current of75mA.
(3) The metal sulfides and graphite-rich composite solid lubrication layer on thetop surface contributed to the friction-reducing and wear-resistence. After ionsulfuizeation, the harder sublayer can provide a strong support for the softer WS2andgraphite-rich toplayer. Under dry friction condition, high W content WS2/W-DLCcomposite solid lubrication film decreased the contact area and plastic deformation,which led to reduce the friction and wear rate efficiently.
（1）利用阴极电弧+直流磁控溅射技术结合离子渗硫技术制备了含氢的WS2/W-DLC复合固体润滑薄膜。薄膜表面光滑，仅存在少量纳米级颗粒。薄膜的微观形貌、成分、力学及摩擦学性能均受到W含量的影响。随着W含量增加，薄膜中sp2含量增多，并促使WXC纳米晶生成，薄膜硬度之增大。渗硫处理后，由于石墨化和表层生成软质相WS2，造成薄膜硬度下降。其中渗硫处理W含量为27.7%的薄膜具有最优的摩擦学性能，摩擦系数为0.19，磨损率为1.65×10-7mm3/Nm。
（2）利用离子束辅助沉积技术结合离子渗硫制备了无氢的WS2/W-DLC复合固体润滑薄膜。薄膜具有纳米尺度光滑表面，无任何缺陷，渗硫处理后表面粗糙度小于30nm。随着W靶束流增大，薄膜硬度和弹性模量增大。渗硫处理后，由于表面生成金属硫化物和富石墨的复合固体润滑层，导致薄膜硬度值下降。渗硫处理W靶束流为75mA的薄膜具有最优的性能，摩擦系数为0.107，磨损率为2.37×10-7mm3/Nm。
（3）离子渗硫处理后的W-DLC膜，薄膜表层软质金属硫化物和富石墨层，是减摩抗磨主要原因。渗硫处理后，高钨含量的薄膜，为软质表层提高了良好的支撑。在干摩擦条件下，减小了摩擦接触面积和塑性变形，有效地改善了摩擦学性能。
With the purpose of improving the tribological property of W doped diamondlike carbon (W-DLC) film, on the basis of the coating concept of multilayer, twoseries of WS2/W-DLC composite solid lubrication films were prepared using hybriddeposition techniques in combination with low temperature ion sulfurizationtechnique, including hydrogenated and hydrogen-free WS2/W-DLC composite solidlubrication coatings. The tribological property of the films before or after thetreatment was investigated by a MS-T3000friction and wear tester. SEM and three-dimensional light interfering profilometer were employed to observe themorphologies of surface of films, XRD was adopted to detect the surface phasestructure. Raman was adopted to characterize the structure of C atoms and XPS wasused to identify the valence state of different elements of the films. The influence ofW concentration on the micro-morphology, composition, microstructure, mechanicaland tribological property of the coatings were investigated. The results were shown asfollowed:
(1) The hydrogenated WS2/W-DLC composite solid lubrication films werefabricated by ion beam deposition+magnetron sputtering techniques in combinationwith low temperature ion sulfurization. The surfaces were smooth, only with somenanoscale particles. With the increasing of W concentration, the content of sp2increased, however the formation of hard nanoparticles WXC in carbon matrix to forma nanocomposite structure led to an enhancement in hardness. Graphitization and WS2was formed on the surface of W-DLC film after ion sulfuration, which made thehardness of W-DLC film decreases. The optimum wear performance with frictioncoefficient of0.19and wear rate of1.65×10-7mm3/Nm was achieved for27.7%WS2/W-DLC film.
(2) The hydrogen-free WS2/W-DLC composite solid lubrication film wasprepared by ion beam assistant deposition technique in combination with lowtemperature ion sulfurization. All the surfaces were nanoscale and without defect. Theroughness was lower than30nm after ion sulfurization. The hardness and elastic modulus of the films were increased gradually, as the W target current increased.After ion sulfurization the hardness decreased, due to the formation of metal sulfidesand graphite-rich composite solid lubrication layer on the top surface. The lowestfriction coefficient0.107and wear rate2.37×10-7mm3/Nm were achieved from thesample at W target beam current of75mA.
(3) The metal sulfides and graphite-rich composite solid lubrication layer on thetop surface contributed to the friction-reducing and wear-resistence. After ionsulfuizeation, the harder sublayer can provide a strong support for the softer WS2andgraphite-rich toplayer. Under dry friction condition, high W content WS2/W-DLCcomposite solid lubrication film decreased the contact area and plastic deformation,which led to reduce the friction and wear rate efficiently.
引文
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