大尺寸自支撑金刚石膜制备工艺及其红外透过性能研究  

Study of Large-area Free-standing Diamond Films and its Property of Infrared Transmittance

作　　者：杨国永 熊绍阳 鲁云祥 王博[1] 易剑 江南[1] Yang Guoyong;Xiong Shaoyang;Lu Yunxiang;Wang Bo;Yi Jian;Jiang Nan(Ningbo Material Technology and Engineering Research Institute,Chinese Academy of Sciences)

机构地区：[1]中国科学院宁波材料技术与工程研究所,浙江宁波315201

出　　处：《硬质合金》2020年第5期350-356,共7页Cemented Carbides

基　　金：中国科学院科研仪器设备研制项目《2英寸以上金刚石单晶合成用大功率微波等离子体CVD装备研制》(ZDKYYQ20200001)。

摘　　要：金刚石膜具有能够媲美单晶金刚石的优异物理化学性能,同时能够满足大尺寸的制备要求,是理想的红外窗口和芯片散热材料。本文采用微波等离子体化学气相沉积(MPCVD)设备,研究了不同沉积温度和甲烷浓度对金刚石膜沉积的影响,并通过SEM和Raman对其进行了表征分析。结果表明,当沉积温度过高时,会导致等离子体中的活性粒子能量增大,从而使金刚石晶粒变大;当沉积温度过低时,会造成金刚石膜中的石墨相含量增加。甲烷浓度的变化会引起环境中含碳基团浓度的变化,影响原子氢对石墨相的刻蚀作用,进而导致金刚石膜内石墨相含量的明显变化,影响金刚石膜质量。本文最终选用850℃的沉积温度和5.0%的甲烷浓度作为金刚石膜生长的沉积参数,通过长时间生长成功制备了直径76.2 mm的金刚石自支撑膜,并对其进行了XRD和红外透过性能测试。红外透过测试结果表明制备的自支撑金刚石膜在8~12μm波段透过率良好,平均透过率达到了56.8%。In virtue of its excellent physical and chemical properties rivaling single crystalline diamond as well as the ability of the preparation with large area,diamond film is a perfect material in the fields of infrared window and chip heat dissipation.In this study,diamond films were prepared using microwave plasma chemical vapor deposition.The effects of deposition temperature and methane concentration on diamond films were studied by SEM and Raman characterizations.The results show that there is a critical temperature for the deposition of diamond films.When the deposition temperature is higher than the critical value,energy of reactive particle in atmosphere is enhanced and the grain size of diamond becomes much larger.Otherwise,the content of graphite in the diamond film increases.Besides,the methane concentration also has an important influence on graphite content,because its variation will change concentration of carbon-containing particle in atmosphere and influence etching of graphite by hydrogen.Consequently,large-area diamond film with 76.2 mm in diameter was prepared by increasing growth duration at the 850℃and the methane concentration of 5.0%.Infrared transmission spectrum shows thatits average transmittance is about 56.8%for the infrared wave of 8~12μm.

关 键 词：MPCVD 金刚石膜 大尺寸 自支撑 散热材料 红外窗口材料 

分 类 号：TQ163[化学工程—高温制品工业]