类金刚石薄膜的性能及结构的研究
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摘要
本文使用非平衡磁控溅射和等离子体增强化学气相沉积复合系统在国产W6Mo5Cr4V2高速钢上制备了掺杂类金刚石薄膜。采用金相显微镜、显微硬度计、旋转摩擦试验仪、X射线衍射(XRD)、电子探针(EPMA)、透射电子显微镜(TEM)等检测方法研究了薄膜的机械性能、表面形貌、微观结构等,讨论了薄膜的生长机理,并利用热分析方法研究了DLC薄膜的热稳定性。
结果表明,DLC薄膜中掺Mo促进了sp~3键向sp~2键的转化,降低了薄膜的硬度,为1888HV。在磨损过程中薄膜表面产生石墨结构转移膜,具有自润滑性能,降低摩擦系数,使薄膜具有良好的耐磨性。并且有金属韧性相的存在,提高了薄膜的韧性。掺Mo的DLC薄膜热稳定性不高,在空气中114℃发生H的析出及石墨化,在262℃发生C的氧化。
掺Si的DLC薄膜,Si与C形成sp~3键,提高了薄膜的sp~3含量,提高了薄膜的硬度,达3538HV。但在磨损过程中,因掺入Si阻碍了石墨转移膜的形成,摩擦系数提高,耐磨性降低。Si进入C的结构中,大大提高了薄膜的热稳定性,在495℃才发生石墨化,在温度升高过程中只发生了微量的H的析出及碳的氧化,薄膜的抗氧化性能提高。
同时掺Si和Mo的DLC薄膜,具有单独掺Mo和Si两者的特点,硬度较单独掺Si稍低,为3024HV,高于单独掺Mo的1888HV,Mo的掺入提高了韧性。在磨损过程中仍能形成转移膜,但因少量Si的掺入,推迟了转移膜的形成时间。其热稳定性也得到提高,石墨化温度提高至519℃,分别比单独掺Mo、Si的提高257℃、24℃,并且转变量也大幅减少。抗氧化性能也很好。
DLC薄膜主要为非晶结构,掺入Mo后形成了Mo、MoC、Mo_2C的纳米级晶粒,其颗粒尺寸约为20～30nm,这些颗粒均匀镶嵌在非晶碳的无序网络结构中。而掺Si的DLC薄膜中,由于Si在薄膜中不形成碳化物,同时薄膜是使用UBMS和RF-PECVD方法制备的,抑制了柱状晶的生长,因此掺Si后薄膜呈现层状生长,层与层之间的界面明显,层的厚度大约为5nm。同时掺Si和Mo的薄膜则同时存在纳米级的晶粒及层状非晶,但因Si含量的降低,层间界面模糊,并且因Mo掺入形成的纳米级颗粒阻碍了薄膜的大面积层状生长,层数变多且紊乱。这些纳米级的层状结构,可阻碍位错的产生与扩展,可显著提高薄膜的强度、硬度和耐磨性。
薄膜使用了过渡层,提高了薄膜和基体的结合力。在薄膜中引入成分梯度,可以消除在不同固体之间界面的热、弹性和塑性错配的突然转变,降低薄膜中应力集中,由成分梯度引起的界面不清晰性可以减轻拐角处的应力集中,防止裂纹产生,及薄膜破裂、剥落。
This letter studied the doped diamond like carbon(DLC) films prepared on the substrate of domestic high-speed steel W6Mo5Cr4V2 by a Teer hybrid unbalanced magenetron sputter ion-plating and PECVD deposition system. The mechanical property, surface topography and microstructure were observed by metallographic microscope, microhardness instrument, rotating friction tester, X-ray diffraction (XRD), electron probe microanalysis (EPMA) and transmission electron microscope (TEM). The thermal stability of DLC films was investigated by thermal analysis and the growth mechanism of films was discussed.
The results showed that: the hardness of Mo doped DLC films decreased to 1888 HV because the doped Mo lead to the promotion of sp~3 to sp~2. A transfer layer which had the same structure with graphitic was formed during wear testing. This transfer layer had the function of self-lubricating and decreasing the friction coefficient. As a result, the DLC films had good wear resistance. Toughness of the DLC films was improved because of the existence of ductile metal phase. The thermal stability of Mo doped DLC films was not good. Hydrogen could evolve from DLC films in air at 114℃when graphitization began to appear. The carbon was oxygenized at 262℃.
In the DLC films doped with Si, Si could form sp~3 bond with C. It advanced the content of sp~3 and improved the hardness up to 3538HV. Due to the doping of Si, the formation of graphite transfer layer was hindered; the fiction coefficient increased; the wear resistance decreased. Because Si has the same structure with diamond, it increased the thermal stability of DLC films greatly. Consequently, graphitization of Si doped films occured at 495℃. With the increase of temperature, only a trace amount of of hydrogen precipitated, and also little carbon was oxidized. The antioxidant properties of DLC films was improved.
The DLC films doped with Mo and Si simultaneously had the characteristics of the films doped with Mo and Si separately. The hardness was 3024HV which was slightly lower than the Si doped DLC films but higher than the Mo doped ones. And Mo could improve the toughness. Although graphitic transfer film still formed during wear testing, their formation time was delayed because of the doping of a small amount of Si. These film had better thermal stability and higher graphitization temperature of 519℃, which was 257℃or 24℃higher than the Mo or Si doped DLC films. The volume of transformation was significantly reduced. The films had good oxidation resistance.
While DLC films were mainly amorphous structure, nanocrystals of Mo, Mo_2C, Mo_2C were formed because of the doped Mo. These particles, which size was about 20～30nm, distributed uniformly in the disordered amorphous carbon network structure. In the Si doped DLC films, owing to the fact that Si didn't form carbide and the films were prepared by UBMS and RF-PECVD system, the growth of columnar crystal was inhibited. Therefore, the films grew as layers with clear interfaces and the thickness of the layers was about 5nm. The DLC films doped with Si and Mo simultaneously had nanocrystals and layered amorphous carbon. And the interfaces between layers were fuzzy because of the lower Si content. Due to the nano-particles formed by the doping of Mo, the growth of layers in large areas was hindered, and the layers had an increase in number but become disordered. These nano-layered structure could inhibit the formation and expansion of dislocations, and significantly improve the strength hardness and wear resistance of the films.
Buffer layers used in DLC films enhanced the adhesion between DLC film and the substrate. The compositional gradient in DLC films could eliminate the sudden change of thermal, elastic and plastic mismatch in the interface between different solids, and also could decrease the stress concentration in the films. As a result of the compositional gradient, the interfaces were not clear, which could decrease the stress concentration in the corner, and prevent the generation of cracks, abruption and peeling off of the films.
结果表明,DLC薄膜中掺Mo促进了sp~3键向sp~2键的转化,降低了薄膜的硬度,为1888HV。在磨损过程中薄膜表面产生石墨结构转移膜,具有自润滑性能,降低摩擦系数,使薄膜具有良好的耐磨性。并且有金属韧性相的存在,提高了薄膜的韧性。掺Mo的DLC薄膜热稳定性不高,在空气中114℃发生H的析出及石墨化,在262℃发生C的氧化。
掺Si的DLC薄膜,Si与C形成sp~3键,提高了薄膜的sp~3含量,提高了薄膜的硬度,达3538HV。但在磨损过程中,因掺入Si阻碍了石墨转移膜的形成,摩擦系数提高,耐磨性降低。Si进入C的结构中,大大提高了薄膜的热稳定性,在495℃才发生石墨化,在温度升高过程中只发生了微量的H的析出及碳的氧化,薄膜的抗氧化性能提高。
同时掺Si和Mo的DLC薄膜,具有单独掺Mo和Si两者的特点,硬度较单独掺Si稍低,为3024HV,高于单独掺Mo的1888HV,Mo的掺入提高了韧性。在磨损过程中仍能形成转移膜,但因少量Si的掺入,推迟了转移膜的形成时间。其热稳定性也得到提高,石墨化温度提高至519℃,分别比单独掺Mo、Si的提高257℃、24℃,并且转变量也大幅减少。抗氧化性能也很好。
DLC薄膜主要为非晶结构,掺入Mo后形成了Mo、MoC、Mo_2C的纳米级晶粒,其颗粒尺寸约为20～30nm,这些颗粒均匀镶嵌在非晶碳的无序网络结构中。而掺Si的DLC薄膜中,由于Si在薄膜中不形成碳化物,同时薄膜是使用UBMS和RF-PECVD方法制备的,抑制了柱状晶的生长,因此掺Si后薄膜呈现层状生长,层与层之间的界面明显,层的厚度大约为5nm。同时掺Si和Mo的薄膜则同时存在纳米级的晶粒及层状非晶,但因Si含量的降低,层间界面模糊,并且因Mo掺入形成的纳米级颗粒阻碍了薄膜的大面积层状生长,层数变多且紊乱。这些纳米级的层状结构,可阻碍位错的产生与扩展,可显著提高薄膜的强度、硬度和耐磨性。
薄膜使用了过渡层,提高了薄膜和基体的结合力。在薄膜中引入成分梯度,可以消除在不同固体之间界面的热、弹性和塑性错配的突然转变,降低薄膜中应力集中,由成分梯度引起的界面不清晰性可以减轻拐角处的应力集中,防止裂纹产生,及薄膜破裂、剥落。
This letter studied the doped diamond like carbon(DLC) films prepared on the substrate of domestic high-speed steel W6Mo5Cr4V2 by a Teer hybrid unbalanced magenetron sputter ion-plating and PECVD deposition system. The mechanical property, surface topography and microstructure were observed by metallographic microscope, microhardness instrument, rotating friction tester, X-ray diffraction (XRD), electron probe microanalysis (EPMA) and transmission electron microscope (TEM). The thermal stability of DLC films was investigated by thermal analysis and the growth mechanism of films was discussed.
The results showed that: the hardness of Mo doped DLC films decreased to 1888 HV because the doped Mo lead to the promotion of sp~3 to sp~2. A transfer layer which had the same structure with graphitic was formed during wear testing. This transfer layer had the function of self-lubricating and decreasing the friction coefficient. As a result, the DLC films had good wear resistance. Toughness of the DLC films was improved because of the existence of ductile metal phase. The thermal stability of Mo doped DLC films was not good. Hydrogen could evolve from DLC films in air at 114℃when graphitization began to appear. The carbon was oxygenized at 262℃.
In the DLC films doped with Si, Si could form sp~3 bond with C. It advanced the content of sp~3 and improved the hardness up to 3538HV. Due to the doping of Si, the formation of graphite transfer layer was hindered; the fiction coefficient increased; the wear resistance decreased. Because Si has the same structure with diamond, it increased the thermal stability of DLC films greatly. Consequently, graphitization of Si doped films occured at 495℃. With the increase of temperature, only a trace amount of of hydrogen precipitated, and also little carbon was oxidized. The antioxidant properties of DLC films was improved.
The DLC films doped with Mo and Si simultaneously had the characteristics of the films doped with Mo and Si separately. The hardness was 3024HV which was slightly lower than the Si doped DLC films but higher than the Mo doped ones. And Mo could improve the toughness. Although graphitic transfer film still formed during wear testing, their formation time was delayed because of the doping of a small amount of Si. These film had better thermal stability and higher graphitization temperature of 519℃, which was 257℃or 24℃higher than the Mo or Si doped DLC films. The volume of transformation was significantly reduced. The films had good oxidation resistance.
While DLC films were mainly amorphous structure, nanocrystals of Mo, Mo_2C, Mo_2C were formed because of the doped Mo. These particles, which size was about 20～30nm, distributed uniformly in the disordered amorphous carbon network structure. In the Si doped DLC films, owing to the fact that Si didn't form carbide and the films were prepared by UBMS and RF-PECVD system, the growth of columnar crystal was inhibited. Therefore, the films grew as layers with clear interfaces and the thickness of the layers was about 5nm. The DLC films doped with Si and Mo simultaneously had nanocrystals and layered amorphous carbon. And the interfaces between layers were fuzzy because of the lower Si content. Due to the nano-particles formed by the doping of Mo, the growth of layers in large areas was hindered, and the layers had an increase in number but become disordered. These nano-layered structure could inhibit the formation and expansion of dislocations, and significantly improve the strength hardness and wear resistance of the films.
Buffer layers used in DLC films enhanced the adhesion between DLC film and the substrate. The compositional gradient in DLC films could eliminate the sudden change of thermal, elastic and plastic mismatch in the interface between different solids, and also could decrease the stress concentration in the films. As a result of the compositional gradient, the interfaces were not clear, which could decrease the stress concentration in the corner, and prevent the generation of cracks, abruption and peeling off of the films.
引文
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