摘   要：现代机械工业和干式切削的快发展对刀具刃具涂层材料提出了越来越高的要求，硬质多层结构涂层作为提高刀具寿命的手段而被广泛研究。如何在保证涂层硬度的同时，提高其高温抗氧化性成为目前的研究热点。金属氧化物因具有较高的硬度同时具有较好的稳定性而被提出应用在涂层中。本文从制备含有金属氧化物的多层结构涂层和单层氧化物层两方面进行研究，对于单层膜，我们使用纯铝和纯锆靶制备了ZrxOy单层膜和AlxOy单层膜，考察靶材功率、通入氧气和氩气气体流量对膜层结构和成分的影响，为后期制备多层结构膜提供实验参数。同时我们还使用了ZrO2靶材和纯铝靶尝试制备了周期结构多层膜，并对制备的膜层进行了厚度和硬度测试。实验中我们采用了扫描电镜和能谱仪对膜层的形貌和成分进行测试，薄膜的厚度和硬度分别使用了台阶仪和纳米压痕测试系统进行了表征。SEM的结果表明薄膜表面致密均匀。固定氧气和氩气比例，不同功率下制备的氧化锆薄膜，其氧和锆的原子百分比随着功率增加变化不大；固定靶材功率和气体比例，不同氧气和氩气气体流量比例的制备薄膜，对于氧化锆薄膜，随氧气的加入，氧和锆的原子百分比变化很小的；对于氧化铝膜，随氧气的加入，氧和铝的原子百分比是增加的。对比氧化锆和氧化铝膜发现，同样的气体比例，氧化锆膜中的氧锆原子比例远远大于氧化铝中的氧铝原子比例。我们对厚度约为700nm的ZrO2/AlxOy周期结构薄膜进行了硬度测试，得到了硬度约为13.0GPa。

关键词：硬质涂层；金属氧化物；多层结构薄膜；磁控溅射

Abstract：The rapid development of modern machinery industry and dry cutting has put forward higher and higher requirements for cutting tool coating materials, and the hard multilayer structure coating has been widely studied as a means to improve tool life. How to improve the hardness of the coating at the same time, to improve its high temperature oxidation resistance has become the current research focus. The metal oxide is used in the coating because of its high hardness and good stability. In this paper, we study the multilayer structure coating and monolayer oxide layer containing metal oxide. We fabricated ZrxOy monolayer and AlxOy monolayer by using pure aluminum and pure zirconium target. The influence of target power, inlet oxygen and argon gas flow on the structure and composition of the film was studied, and the experimental parameters were provided for the later preparation of multilayer structural films. At the same time, we also used ZrO2 target and pure aluminum target to prepare the periodic structure multilayer, and the thickness and hardness of the prepared film were tested. During the experiment, we used scanning electron microscopy and energy dispersive spectrometer to test the morphology and composition of the film. The thickness and hardness of the film were characterized by step meter and nanoindentation test system respectively. SEM results show that the film surface is dense and uniform. The atomic ratio of oxygen and zirconium to zirconium oxide prepared at different power ratios varies with the increase of power. The fixed target power and gas ratio, the preparation ratio of different oxygen and argon gas flow rate , For the addition of oxygen, the atomic percentage of oxygen and zirconium slightly varies with respect to the zirconia film; for the alumina film, the atomic percentage of oxygen and aluminum increased with the increasing of oxygen. Compared with the zirconia and alumina films, it was found that the proportion of zirconium oxide in the zirconia film was much larger than that in the alumina. We measured the hardness of ZrO2/AlxOy periodic films with a thickness of about 700 nm, resulting in a hardness of about 13.0 GPa.

Keywords: Hard coating；Metal oxide; multilayer structure film; magnetron sputtering