PVD制备超硬多层复合薄膜材料工艺与性能研究
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摘要
硬质薄膜材料可以广泛应用于机械制造、汽车工业、纺织工业、地质钻探、模具工业、航空航天等领域。在实际的工业应用中,硬度是诸多技术要求中的一个重要指标,除此之外,还有高温硬度和韧性、抗氧化性、化学稳定性等。人们对硬质材料的摩擦系数和磨损率、涂层的附着强度、导热系数等也都有一定的要求,不同的使用环境下对薄膜材料的技术要求也各有侧重。自1985年Knotek等首次发表了关于涂层的研究成果后,TiAlN薄膜以其优异的性能,引起了世界各国的关注,并逐渐成为TiN的更新换代涂层。人们对其良好的使用性能表示了极大的关注,已经用多种PVD方法成功制备了TiAlN薄膜。
为更好的利用PVD方法制备TiAlN薄膜及TiN/TiAlN复合薄膜,并研究其性能,本文利用多弧离子镀、空心阴极离子镀及空心阴极辅助多弧离子镀等镀膜技术分别对TiN薄膜、TiAlN薄膜、TiN/TiAlN复合薄膜的镀制工艺参数进行了大量实验研究,特别是对TiN/TiAlN复合薄膜的靶材成分、镀制方式、镀制循环时间及清洗与镀制工艺参数进行了较深入的研究。使用微纳米压(划)痕及表面轮廓测试系统对薄膜的表面压痕(硬度)、划痕、弹性模量以及薄膜在基体上的附着力等机械性能进行了测试分析研究,还通过X射线衍射(XRD)、扫描电镜(SEM)、场发射扫描电镜(FE—SEM)、激光共聚焦显微镜(CLSM)等实验分析手段研究了薄膜的形貌、结构及性能特征。
重点分析讨论了多层膜体系的结构和性能以及工艺参数之间的相互关系,特别是研究了不同调制周期和不同靶材镀制对薄膜结构和性能的影响。通过观察TiN/TiAlN多层膜的表面与截面形貌,表明在同等沉积条件下,“55”靶在基体上的沉积速率要高于用“37”靶在基体上的沉积速率,并且用“55”靶沉积的样品表面大颗粒较少,表面较为平整,凹坑少且较浅,其力学性能要好于“37”靶沉积的样品。多层薄膜XRD中显示薄膜中有TiN、AlFe3、AlN、Ti2AlN等相存在,说明多层膜形成了良好的相结构。通过微纳米压(划)痕仪测出的样品压痕(硬度)表明：本实验的TiN/TiAlN多层膜的硬度最高达到了40.12GPa,远高于本试验与文献中给出的TiN薄膜及TiAlN薄膜的硬度。在同等条件下用“55”靶镀制的样品的硬度要高于“37”靶镀制的样品硬度。划痕实验表明,“55”靶镀制的TiN/TiAlN多层膜样品的临界载荷要高于“37”靶镀制的TiN/TiAlN多层膜样品的临界载荷,“37”靶镀制TiN/TiAlN多层膜样品的临界载荷要高于TiAIN单层膜样品的临界载荷。“55”靶镀制的样品的弹性恢复能力和硬度都优于“37”靶镀制的样品的弹性恢复能力和硬度；“55”靶及“37”靶镀制的TiN/TiAlN多层膜样品的弹性恢复能力和硬度都要高于TiAlN单层膜弹性恢复能力和硬度。
通过实验研究,获得了镀制多层膜的最佳工艺参数,确定了镀制TiAlN薄膜与TiN/TiAlN复合薄膜的最佳镀制方法,并在W6Mo5Cr4V2高速钢基体上镀制了性能较好的TiAlN薄膜及TiN/TiAlN多层复合薄膜。研究结果表明,用空心阴极辅助多弧离子镀工艺可以良好的进行TiN/TiAlN复合薄膜的镀制工作。在空心阴极辅助多弧离子镀工艺下对“55”靶的应用具有良好的应用前景。
The horniness films can be used at the making machine, automobile industry, spinning industry, geological drilling, dieing industry and aerospace engineering very comprehensive. In the actual industry, hardness is the most important technical requirement at the lots of datas. Besides this, the hardness at the high temperature, toughness, non-oxidizability and chemical stability are also very important. Peplo also have some requirements to hard material, such as friction factor, wear rate, adhesive strength and coefficient of heat conductivity. The different environment has the different emphases to the technical requirement of the thin-film material. Since 1985 Knotek published the research production about the coating, because of the good performance of TiAIN films that it has makes attention all the world. It is replacing TiN films. Peplo has paied for attentions to its service performance and has use some of PVD methods to make the TiAlN films.
For use the PVD method to make the TiAIN and TiN/TiAlN films better and research its performance. In this paper, we use the AIP, HCD and AIP+HCD methods to make the TiN film, TiAIN film and TiN/TiAlN films. For researching the films we have found the processing parameter, specially to the component of the targets, making methods, cycle time and cleaning processing parameter. Use the multi-specimen test system to make the analytical study about the hardness, scratch marks, elastic ratio and adhesive power. Also use XRD, SEM, FE-SEM and CLSM to reaserch the pattern, structure and performance of the films.
The focal point is to discuss and analysis the relationship between the structure, performance and processing parameter, especially the influence that be made by the different periods and targets. From observing the surface and sectional pattern about TiN/TiAlN films, it can be seen that at the same condition of the aggradation, the rate of the aggradation on the base stock, "55" target is better than "37" target. The samples are made by "55" target is very well. Its bulky grains are less, the surface is smooth, the pits are less and shallow and its mechanical property is better than "37" target. From XRD, the multi-films can be seen have the structure of TiN、AlFe3、AlN、Ti2AlN, explained the multilayer films formed the modulate sturcture favorable, crystal intergrality preferably. The multi-specimen test system test show that:the hardness of TiN/TiAlN multilayer films is tiptop to 40.12GPa, outclass the TiN films and TiAIN films. The hardness of films by 55 target is excel the 37 target in same condition. Scratch test show that:The critical load of the TiN/TiAlN multilayer films made by 55 target is excelled the films made by 37 target.The critical load of the TiN/TiAIN multilayer films made by 37 target is excelled the TiAIN monolayer films. The flexibility resume ability and hardness of the TiN/TiAIN multilayer films made by 55 target is excelled the films made by 37 target, and there are all excelled the TiAIN monolayer films.
In this research, obtained the best parameter of how to made the multilayer films, confirm the best plating method of TiAIN and TiN/TiAlN films, and plating the TiAlN and TiN/TiAIN films in W6Mo5Cr4V2 surface successful. From the result, it can be seen that: use the AIP+HCD can made the favorable TiN/TiAIN films. The applycation of 55 target have a better foreground by AIP+HCD.
为更好的利用PVD方法制备TiAlN薄膜及TiN/TiAlN复合薄膜,并研究其性能,本文利用多弧离子镀、空心阴极离子镀及空心阴极辅助多弧离子镀等镀膜技术分别对TiN薄膜、TiAlN薄膜、TiN/TiAlN复合薄膜的镀制工艺参数进行了大量实验研究,特别是对TiN/TiAlN复合薄膜的靶材成分、镀制方式、镀制循环时间及清洗与镀制工艺参数进行了较深入的研究。使用微纳米压(划)痕及表面轮廓测试系统对薄膜的表面压痕(硬度)、划痕、弹性模量以及薄膜在基体上的附着力等机械性能进行了测试分析研究,还通过X射线衍射(XRD)、扫描电镜(SEM)、场发射扫描电镜(FE—SEM)、激光共聚焦显微镜(CLSM)等实验分析手段研究了薄膜的形貌、结构及性能特征。
重点分析讨论了多层膜体系的结构和性能以及工艺参数之间的相互关系,特别是研究了不同调制周期和不同靶材镀制对薄膜结构和性能的影响。通过观察TiN/TiAlN多层膜的表面与截面形貌,表明在同等沉积条件下,“55”靶在基体上的沉积速率要高于用“37”靶在基体上的沉积速率,并且用“55”靶沉积的样品表面大颗粒较少,表面较为平整,凹坑少且较浅,其力学性能要好于“37”靶沉积的样品。多层薄膜XRD中显示薄膜中有TiN、AlFe3、AlN、Ti2AlN等相存在,说明多层膜形成了良好的相结构。通过微纳米压(划)痕仪测出的样品压痕(硬度)表明：本实验的TiN/TiAlN多层膜的硬度最高达到了40.12GPa,远高于本试验与文献中给出的TiN薄膜及TiAlN薄膜的硬度。在同等条件下用“55”靶镀制的样品的硬度要高于“37”靶镀制的样品硬度。划痕实验表明,“55”靶镀制的TiN/TiAlN多层膜样品的临界载荷要高于“37”靶镀制的TiN/TiAlN多层膜样品的临界载荷,“37”靶镀制TiN/TiAlN多层膜样品的临界载荷要高于TiAIN单层膜样品的临界载荷。“55”靶镀制的样品的弹性恢复能力和硬度都优于“37”靶镀制的样品的弹性恢复能力和硬度；“55”靶及“37”靶镀制的TiN/TiAlN多层膜样品的弹性恢复能力和硬度都要高于TiAlN单层膜弹性恢复能力和硬度。
通过实验研究,获得了镀制多层膜的最佳工艺参数,确定了镀制TiAlN薄膜与TiN/TiAlN复合薄膜的最佳镀制方法,并在W6Mo5Cr4V2高速钢基体上镀制了性能较好的TiAlN薄膜及TiN/TiAlN多层复合薄膜。研究结果表明,用空心阴极辅助多弧离子镀工艺可以良好的进行TiN/TiAlN复合薄膜的镀制工作。在空心阴极辅助多弧离子镀工艺下对“55”靶的应用具有良好的应用前景。
The horniness films can be used at the making machine, automobile industry, spinning industry, geological drilling, dieing industry and aerospace engineering very comprehensive. In the actual industry, hardness is the most important technical requirement at the lots of datas. Besides this, the hardness at the high temperature, toughness, non-oxidizability and chemical stability are also very important. Peplo also have some requirements to hard material, such as friction factor, wear rate, adhesive strength and coefficient of heat conductivity. The different environment has the different emphases to the technical requirement of the thin-film material. Since 1985 Knotek published the research production about the coating, because of the good performance of TiAIN films that it has makes attention all the world. It is replacing TiN films. Peplo has paied for attentions to its service performance and has use some of PVD methods to make the TiAlN films.
For use the PVD method to make the TiAIN and TiN/TiAlN films better and research its performance. In this paper, we use the AIP, HCD and AIP+HCD methods to make the TiN film, TiAIN film and TiN/TiAlN films. For researching the films we have found the processing parameter, specially to the component of the targets, making methods, cycle time and cleaning processing parameter. Use the multi-specimen test system to make the analytical study about the hardness, scratch marks, elastic ratio and adhesive power. Also use XRD, SEM, FE-SEM and CLSM to reaserch the pattern, structure and performance of the films.
The focal point is to discuss and analysis the relationship between the structure, performance and processing parameter, especially the influence that be made by the different periods and targets. From observing the surface and sectional pattern about TiN/TiAlN films, it can be seen that at the same condition of the aggradation, the rate of the aggradation on the base stock, "55" target is better than "37" target. The samples are made by "55" target is very well. Its bulky grains are less, the surface is smooth, the pits are less and shallow and its mechanical property is better than "37" target. From XRD, the multi-films can be seen have the structure of TiN、AlFe3、AlN、Ti2AlN, explained the multilayer films formed the modulate sturcture favorable, crystal intergrality preferably. The multi-specimen test system test show that:the hardness of TiN/TiAlN multilayer films is tiptop to 40.12GPa, outclass the TiN films and TiAIN films. The hardness of films by 55 target is excel the 37 target in same condition. Scratch test show that:The critical load of the TiN/TiAlN multilayer films made by 55 target is excelled the films made by 37 target.The critical load of the TiN/TiAIN multilayer films made by 37 target is excelled the TiAIN monolayer films. The flexibility resume ability and hardness of the TiN/TiAIN multilayer films made by 55 target is excelled the films made by 37 target, and there are all excelled the TiAIN monolayer films.
In this research, obtained the best parameter of how to made the multilayer films, confirm the best plating method of TiAIN and TiN/TiAlN films, and plating the TiAlN and TiN/TiAIN films in W6Mo5Cr4V2 surface successful. From the result, it can be seen that: use the AIP+HCD can made the favorable TiN/TiAIN films. The applycation of 55 target have a better foreground by AIP+HCD.
引文
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