Advances in studies and applications of thick diamond films prepared by microwave plasma chemical vapor deposition
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摘要: 近年来，随着化学气相沉积（CVD）制备金刚石技术的发展，关于金刚石的研究与应用受到越来越多的关注。目前，主要的CVD技术有微波等离子体化学气相沉积（MPCVD）、热丝化学气相沉积、直流电弧等离子体喷射化学气相沉积和热阴极等离子体化学气相沉积等。MPCVD技术因其生长的金刚石品质高，被认为是制备大面积、高质量金刚石厚膜的最佳方法。首先介绍MPCVD的基本原理和设备，比较几种主要MPCVD技术的优缺点，并对国内外的研究进展进行总结，包括金刚石生长工艺的研究，特别是国内外单晶/多晶金刚石厚膜的制备研究，然后总结近年来金刚石厚膜在电子、光学、热沉等高新技术领域的应用，最后对金刚石厚膜的发展前景进行展望。
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关键词:
- 金刚石厚膜 /
- 微波等离子体化学气相沉积（MPCVD） /
- CVD设备
Abstract:Significance With the wide range of important applications of diamond, the demand for large-area diamond has been increasing in recent years. Compared to other chemical vapor deposition (CVD) methods, the microwave plasma chemical vapor deposition (MPCVD) method is recognized as the best technology for depositing high-quality diamond films. To realize CVD diamond thick films for optical, electrical, and thermal applications, it is necessary to meet the requirements in terms of crystalline quality, optical transmittance, thermal conductivity, size, thickness, and strength. Therefore, obtaining diamond materials with sufficient size and quality is the foundation of their applications. Especially since this century, MPCVD equipment and processes have made breakthroughs, and the preparations of single crystal diamond and high-quality polycrystalline diamond thick films have been successfully realized. This paper introduces the principles and process of preparing diamond thick films by MPCVD, and summarizes the research and application progress of MPCVD-prepared diamond films at home and abroad in recent years. Our views on the future development of MPCVD-prepared diamond films are also proposed in this paper. Progress The MPCVD equipment originated overseas, initially developed by Japanese scientist Yoshihiko Kuriyama and researchers from Nippon Electric Company around the 1980s. Subsequently, countries such as Germany, Britain, the United States, and Russia also engaged in research and development efforts. The evolution of MPCVD chambers has seen a transition from quartz tubes and quartz bell jars to cylindrical resonance chambers, loop antennas, and ellipsoidal resonance chambers. Concurrently, power output has escalated from hundreds of watts to thousands and tens of kilowatts. The advancement of MPCVD technology was spearheaded by foreign entities like E6 (UK), Michigan State University (USA), and the Institute of Applied Physics (Russia), which gradually increased power levels and evolved cavity designs. With progress in diamond film deposition technology and ongoing exploration of microwave sources, higher-power 915 MHz MPCVD systems have been developed. The longer wavelength of 915 MHz microwaves enables these devices to achieve higher power levels, which facilitates an increase in the deposition rate and quality of diamond films, as well as the capability to produce larger-sized diamond films. Domestic development of MPCVD technology began relatively late, with institutions such as the University of Science and Technology Beijing, Hebei Province Laser Research Institute, and Xi'an University of Electronic Science and Technology developing 2.45 GHz and 915 MHz MPCVD equipment after the year 2000. Diamonds possess a high refractive index and significant dispersion, exhibiting superior thermal, mechanical, and optical properties. High-quality polycrystalline diamond films synthesized via the MPCVD method closely resemble natural type IIa diamonds in many aspects. Consequently, MPCVD-prepared diamond films have found extensive applications in optical window materials, thermal management, semiconductor devices, quantum technology, and optoelectronic devices. The third section of the paper provides a detailed account of the progress in applied research within these areas. Conclusions and Prospects Diamond is a material of significant interest and extensive research in the contemporary world. Over the decades, CVD diamond technology has matured, with preparation processes becoming well-established and the equipment continuously evolving and refining. Among the various CVD techniques, MPCVD equipment has seen particularly rapid development. Through persistent exploration, research, and development, the performance gap between domestically produced 2.45 GHz and 915 MHz MPCVD equipment in China and their foreign counterparts is narrowing, although there is still room for improvement in terms of power enhancement, equipment stability, and cavity design. MPCVD-method-prepared diamond thick films hold great promise for a variety of high-tech applications, including optics, thermal management, and electronics. However, their growth rate, size, and uniformity remain areas that require further attention. Looking ahead, ongoing research is essential in several key areas: optimizing and enhancing equipment, refining the growth process, and innovating process parameters (such as atmosphere, power, and substrate) to achieve higher growth rates, superior quality, and reduced costs. These efforts aim to meet the demands of commercialization, thereby facilitating the widespread adoption of diamond thick films in thermal deposition and optical applications. -
图 9 (a)基于多晶金刚石光电探测器线性阵列的成像系统示意图(b)~(e)显示从具有不同光学图案的光电探测器线性阵列获得的相应成像结果[95]
Figure 9. (a) Schematic of imaging system based on polycrystalline diamond photodetector linear array (b)~(e) Bottom figures show corresponding imaging results acquired from photodetector linear array with different optical patterns[95]
腔室类型 开始时间 最初研究单位 微波功率 P / kW 缺点 石英管式 20世纪80年代初 日本无机材料研究所 膜质量低、速率慢，石英管污染导致微波功率受限 石英钟罩式 20世纪80年代末 德国philips、美国ASTeX（现Seki） 1～3 石英钟罩污染导致微波功率受限 圆柱谐振腔式 1992年前后 美国ASTeX（现Seki） 1～5 石英窗易受等离子影响而损毁 环形天线式 1993年 美国ASTeX（现Seki） 6～8 沉积条件、谐振状态无法调整和优化 椭球谐振腔式 1997年前后 德国Fraunhofer研究所 6 
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腔室类型 研究单位 微波功率 P / kW 沉积速率 V / (μm·h−1) 沉积直径 D 石英管式 日本近畿大学 1和7 1和50 10 mm 石英钟罩式 美国密歇根州立大学 30 0.03～0.46 10～20 cm 环形天线式 美国ASTeX（现Seki） 60～100 10 8 in 椭球谐振腔式 德国Fraunhofer研究所 60 1～15 150 mm
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表 3 沉积气体对MPCVD金刚石膜的影响
Table 3. Effect of deposition gas on MPCVD diamond film
气体 对沉积速率的影响 主要作用 CH4 提高 随着CH4浓度的增加，碳氢基团比例增加，沉积速率增加，但过量的CH4会形成非金刚石石墨相，使质量下降 H2 降低 刻蚀生长过程中产生的非金刚石相，对金刚石也有微弱的刻蚀作用 CO2 提高 刻蚀非金刚石相，促进CH4解离，提升金刚石质量 O2 提高 提高金刚石纯度，过量O2不利于金刚石生长 N2 提高 较大程度地提升金刚石沉积速率和质量，但会引入氮缺陷 Ar 提高 提高金刚石生长的均匀性
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