| 摘要: |
| 晶态氧化铝薄膜与非晶态相比，具有更加优良的力学性能和宽波段光学透过性能。基于等离子体发射光谱(OES)反馈控制方法(PEM)，引入高能脉冲磁控溅射(HiPIMS)技术，实现了室温条件下晶态 γ-Al2O3薄膜的快速制备。采用高压探针、电流探针传感器和数字示波器监测 HiPIMS 的放电特性，采用等离子体发射监测器进行时间平均的 OES 研究，采用 X 射线衍射仪和扫描电镜分析薄膜的晶相结构、晶粒尺寸及断面形貌，采用纳米压痕仪测试薄膜的纳米硬度和模量。结果表明， HiPIMS 条件下的成膜环境出现大量的离子态，主要包括 AlⅡ、ArⅡ甚至高价态粒子 OⅣ参与反应。随着溅射电压由 650 V 增加至 800 V，晶粒逐渐细化，由 18 nm 减小到 8 nm，同时沉积速率从 27 nm / min 增加到 55 nm / min。基体偏压对薄膜的沉积速率，微结构以及力学性能等方面均有显著的影响。随着基体偏压的增加，γ-Al2O3 的择优取向由(422)转变为(311)， 薄膜在偏压 Us= ?100 V 条件下获得了最高硬度 19.3 GPa。通过对成膜粒子能量的设计与调控，进一步优化了薄膜的结构和性能，为功能薄膜氧化铝的大规模产业化奠定良好的应用基础。 |
| 关键词: HiPIMS 氧化铝薄膜 室温 晶化诱导 能量调控 |
| DOI：10.11933/j.issn.1007?9289.20211230004 |
| 分类号:TG174 |
| 基金项目:国家自然科学基金资助项目(51701229、51871230) |
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| Particle Energy Regulation of Crystalline Alumina Films Sputtered at Room Temperature by HiPIMS |
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GAO Fangyuan1,2, XU Yi1,2, Li Guodong1,2, LI Guang1,2, XIA Yuan1,2
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1.Institute of mechanics, Chinese Academy of Sciences, Beijing 100190 , China;2.School of Engineering Science, University of Chinese Academy of Science, Beijing 100049 , China
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| Abstract: |
| Compared with amorphous alumina film, crystalline alumina film has better mechanical properties and wide band optical transmittance. Based on the PEM feedback control method, the HiPIMS technology is introduced to realize the rapid preparation of crystalline γ-Al2O3 films at room temperature. The discharge characteristics of HiPIMS are monitored by high voltage probe, current probe sensor and digital oscilloscope. The time-averaged OES study is carried out by plasma emission monitor. The crystal structure, grain size and cross-sectional morphology of the film are analyzed by X-ray diffractometer and scanning electron microscope. The nanohardness and modulus of the film are measured by nanoindentation instrument. The results show that a large number of ionic states appeared in the film-forming environment under HiPIMS conditions, mainly including AlII, ArII and even high-valent particle OIV participating in the reaction. With the increase of sputtering voltage from 650 V to 800 V, the grain size gradually decreases from 18 nm to 8 nm, and the deposition rate increases from 27 nm / min to 55 nm / min. The substrate bias has a significant effect on the deposition rate, microstructure and mechanical properties of the films. With the increase of substrate bias, the preferred orientation of γ-Al2O3 changes from (422) to (311), and the highest hardness of 19.3 GPa is obtained under bias Us = ?100 V. Through the design and regulation of film-forming particle energy, the structure and properties of the film are further optimized, which laid a good foundation for the large-scale industrialization of functional film alumina. |
| Key words: HiPIMS alumina film room temperature crystallization induction energy regulation |
