915 MHz高功率MPCVD设备生长8-inch金刚石外延膜  

Eight-Inch Diamond Epitaxial Films Grown by High-Power MPCVD Reactor of 915 MHz

作　　者：杨国永 杨明阳 王博 王跃忠 鲁云祥 宋惠 易剑 西村一仁 江南 Yang Guoyong;Yang Mingyang;Wang Bo;Wang Yuezhong;Lu Yunxiang;Song Hui;Yi Jian;Kazuhito Nishimura;Jiang Nan(Key Laboratory of Marine Materials and Related Technologies,Zhejiang Key Laboratory of Marine Materials and Protective Technologies,Ningbo Institute of Materials Technology and Engineering(NIMTE),Chinese Academy of Sciences,Ningbo Zhejiang 315201,China)

机构地区：[1]中国科学院宁波材料技术与工程研究所,海洋材料及相关技术重点实验室,浙江省海洋材料与防护技术重点实验室,浙江宁波315201

出　　处：《硬质合金》2023年第2期98-104,共7页Cemented Carbides

基　　金：宁波市科技攻关重大专项《高功率芯片封装用大尺寸金刚石散热基底关键制造与加工技术》(20211ZDYF020198);宁波市甬江引才工程青年创新人才项目《红外光学材料技术》(2021A-108-G)。

摘　　要：金刚石外延膜具有良好的热学、光学和化学稳定性,同时能够满足大尺寸的制备需求,是红外窗口和散热应用中理想的材料。受限于目前金刚石应用中尺寸较小等问题,制备大尺寸高质量的金刚石一直是人们追求的目标。本文采用自行研制的915 MHz/75 kW的微波等离子体化学气相沉积(MPCVD)设备,研究了不同沉积温度对直径8 inch(1 inch=25.4 mm)的金刚石膜沉积的影响,并通过SEM和Raman对其进行表征分析。结果表明,沉积温度会影响金刚石膜的晶体取向和结晶质量,过低的温度不利于金刚石膜规则地取向生长;而过高的温度会产生sp2石墨相,降低金刚石膜的结晶质量和取向生长。本文最终在1000°C的沉积温度和1.0%的甲烷浓度(甲烷与氢气流量之比为0.01)下成功制备了具有良好的结晶质量和厚度均匀的8 inch(111)取向的金刚石外延膜,该外延膜具有较低的氮杂质含量,生长表面均匀,无生长裂纹产生,晶粒尺寸在3~5 mm。红外透过测试结果表明12μm处的透过率达到了67.8%,8~12μm之间的平均透过率为67.3%。Due to its excellent thermal,optical,and chemical stability,as well as its ability to meet the requirements of large-size preparation,diamond epitaxial film has become an ideal material applied in infrared windows and heat dissipation.As the currently used diamond has a small size,people have been trying to prepare diamonds with large sizes and high quality.In this paper,a self-developed microwave plasma chemical vapor deposition(MPCVD)equipment of 915 MHz/75 kW was used to study the effect of different deposition temperatures on the deposition of an 8-inch(1 inch=25.4 mm)diamond epitaxial film,and its characterization was analyzed by SEM and Raman.The results show that deposition temperature affects the crystalline orientation and quality of diamond films.When the deposition temperature is too low,the regular orientation growth of diamond films will be affected;when the temperature is too high,sp2 graphite phase will be produced,which will reduce the quality and orientation growth of the films.In this paper,an 8-inch(111)diamond epitaxial film with great crystalline quality and thickness uniformity was successfully prepared at a deposition temperature of 1000℃and a methane concentration of 1.0%(The ratio of methane to hydrogen flow rate is 0.01).The epitaxial film shows low nitrogen impurity content,uniform growth surface,and zero growth cracks,and its grain size is in the range of 3-5 mm.The result of the infrared transmission test shows that the transmittance of the film reaches about 67.8%at 12μm,and the average transmittance is about 67.3%in the range of 8-12μm.

关 键 词：金刚石外延膜 大尺寸 MPCVD 红外窗口材料 915 MHz 

分 类 号：TQ163[化学工程—高温制品工业] TB383.2[一般工业技术—材料科学与工程]