引用本文:高海洋,张斌,魏殿忠,但敏,金凡亚.脉冲频率对HiPIMS制备TiN薄膜组织和力学性能的影响[J].中国表面工程,2022,35(5):192~199
GAO Haiyang,ZHANG Bin,WEI Dianzhong,DAN Min,JIN Fanya.Effects of Pulse Frequency on the Microstructure and Mechanical Property of TiN Films Prepared by HiPIMS[J].China Surface Engineering,2022,35(5):192~199
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脉冲频率对HiPIMS制备TiN薄膜组织和力学性能的影响
高海洋1,2, 张斌2, 魏殿忠3, 但敏4, 金凡亚4
1.中国科学院兰州化学物理研究所材料磨损与防护重点实验室 兰州 730000;2.中国科学院大学材料与光电技术学院 北京 101408;3.兰州精新电源设备有限公司 兰州 730000;4.核工业西南物理研究院等离子体工程研究中心 成都 610041
摘要:
为探究脉冲频率对通过高功率脉冲磁控溅射制备 TiN 薄膜组织力学性能的影响，选用 Ti 靶和 N2气体，采用反应磁控溅射技术通过改变高功率脉冲磁控溅射(HiPIMS)电源脉冲频率在 Si(100)晶片上制备不同种 TiN 薄膜。利用 X 射线衍射仪(XRD)、X 射线光电子能谱仪和扫描电子显微镜(SEM)对所制薄膜晶体结构和成分、表面和断面形貌进行分析，利用纳米压痕仪对薄膜的硬度和弹性模量进行表征，并计算 H / E 和 H3 / E2 。结果表明，高离化率 Ti 离子轰击促使薄膜以低应变能的晶面优先生长，所制 TiN 薄膜具有(111)晶面择优取向。薄膜平均晶粒尺寸均在 10.3 nm 以下，随着脉冲频率增大晶粒尺寸增大，结晶度和沉积速率降低，柱状生长明显，致密度下降，影响薄膜力学性能。在 9 kHz 时，TiN 薄膜的晶粒尺寸可达 8.9 nm，薄膜组织致密具有最高硬度为 30 GPa，弹性模量 374 GPa，弹性恢复为 62.9 %，具有最优的力学性能。
关键词:  高功率脉冲磁控溅射(HiPIMS)  脉冲频率  TiN 薄膜  微观组织  力学性能
DOI：10.11933/j.issn.1007?9289.20220103002
分类号:TB383;TG174
基金项目:甘肃省科技支撑(20YF8WA006)和中国科学院青年创新促进会(2017489)资助项目
Effects of Pulse Frequency on the Microstructure and Mechanical Property of TiN Films Prepared by HiPIMS
GAO Haiyang1,2, ZHANG Bin2, WEI Dianzhong3, DAN Min4, JIN Fanya4
1.Key Laboratory of Wear and Protection of Materials, Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences, Lanzhou 730000 , China;2.College of Materials and Opto-Electronic Technology, University of Chinese Academy of Sciences,Beijing 101408 , China;3.Lanzhou Jingxin Power Equipment Co., LTD, Lanzhou 730000 , China;4.The Research Center for Plasma Engineering, Southwestern Institute of Physics, Chengdu 610041 , China
Abstract:
In order to explore the effect of pulse frequency on the mechanical properties of TiN films prepared by high-power pulsed magnetron sputtering, different kinds of TiN films are prepared on Si(100) wafers by changing the pulse frequency of High-power impulse magnetron sputtering(HiPIMS) power supply through reactive magnetron sputtering technology. The crystal structure and composition, surface and cross-sectional morphology of the films are characterized by XRD, XPS and SEM. The hardness and elastic modulus of the films are characterized by nanoindenter, and H / E and H3 / E2 are calculated. The results show that the high ionization rate Ti ion bombardment promotes the preferential growth of the film with low strain energy crystal planes, and the prepared TiN film has a (111) preferred orientation. The average grain size of the films is below 10.3 nm, but as the pulse frequency increases, grain size increases, crystallinity and the deposition rate decrease, columnar growth is obvious, and the density decreases, which affects the mechanical properties of the film. At 9 kHz, the grain size of the TiN film is 8.9 nm, and the film has the densest structure with the highest hardness of 30 GPa, an elastic modulus of 374 GPa, and elastic recovery is 62.9%, meaning that the film has the best mechanical properties.
Key words:  high-power impulse magnetron sputtering(HiPIMS)  pulse frequency  TiN films  microstructure  mechanical property
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