2英寸MPCVD光学级均匀金刚石膜的制备研究

doi:10.15541/jim20230202

无机材料学报 ›› 2023, Vol. 38 ›› Issue (12): 1413-1419.DOI: 10.15541/jim20230202

所属专题：【信息功能】透明陶瓷与闪烁晶体（202312）

2英寸MPCVD光学级均匀金刚石膜的制备研究

产思义¹(), 屠菊萍¹, 黄珂¹, 邵思武¹, 杨志亮¹, 刘鹏¹, 刘金龙¹(), 陈良贤¹, 魏俊俊¹^,², 安康³, 郑宇亭¹^,², 李成明¹()

1.北京科技大学新材料技术研究院, 北京 100083
2.北京科技大学顺德创新学院, 佛山 528399
3.北方工业大学机械与材料工程学院, 北京 100144

收稿日期:2023-04-24 修回日期:2023-05-25 出版日期:2023-09-12 网络出版日期:2023-09-12
通讯作者: 刘金龙, 研究员. E-mail: liujinlong@ustb.edu.cn;
李成明, 教授. E-mail: chengmli@mater.ustb.edu.cn
作者简介:产思义(1998-), 男, 硕士研究生. E-mail: g20209343@xs.ustb.edu.cn
基金资助:
国家磁约束核聚变发展研究专项基金(2019YFE03100200)

Uniform Growth of Two-inch MPCVD Optical Grade Diamond Film

CHAN Siyi¹(), TU Juping¹, HUANG Ke¹, SHAO Siwu¹, YANG Zhiliang¹, LIU Peng¹, LIU Jinlong¹(), CHEN Liangxian¹, WEI Junjun¹^,², AN Kang³, ZHENG Yuting¹^,², LI Chengming¹()

1. Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083, China
2. Shunde Innovation School, University of Science and Technology Beijing, Foshan 528399, China
3. School of Mechanical and Materials Engineering, North China University of Technology, Beijing 100144, China

Received:2023-04-24 Revised:2023-05-25 Published:2023-09-12 Online:2023-09-12
Contact: LIU Jinlong, professor. E-mail: liujinlong@ustb.edu.cn;
LI Chengming, professor. E-mail: chengmli@master.ustb.edu.cn
About author:CHAN Siyi (1998-), male, Master candidate. E-mail: g20209343@xs.ustb.edu.cn
Supported by:
National MCF Energy R&D Program of China(2019YFE03100200)

摘要/Abstract

摘要：

均匀生长大尺寸光学级金刚石膜一直是微波化学气相沉积(Microwave plasma chemical vapor deposition, MPCVD)金刚石研究领域的热点和难点, 沉积台的结构与位置对于金刚石膜均匀性以及厚膜生长的长期稳定性至关重要。本研究通过COMSOL模拟结合实验研究了沉积台高度对衬底表面电场均匀性、等离子体状态和温度均匀性的影响规律, 优化了光学级金刚石膜均匀生长的工艺参数, 在最佳沉积台高度(2 mm)下沉积得到的2英寸金刚石膜(最大厚度337 μm), 厚度不均匀性<11%, 从膜中心到边缘的拉曼半峰全宽为3~4 cm^-1, 可见光波段内最高透过率为69%~70%, 10.6 μm处红外透过率为70%。结果表明: 金刚石膜的厚度和品质较为均匀, 实现了两英寸光学级金刚石膜的均匀沉积。沉积台高度对衬底表面的电场分布、等离子体形状和温度分布都有一定影响, 随着沉积台高度增加, 衬底表面电场分布均匀性和温度均匀性得到明显改善, 且衬底表面的等离子体分布更均匀, H原子和含碳基团的浓度增加。

关键词: 光学级金刚石膜, 温度均匀性, 红外透过率, 沉积台高度, COMSOL模拟

Abstract:

The uniform growth of large-size optical grade diamond films has been one of the hot spots and difficulties in the field of microwave plasma chemical vapor deposition (MPCVD) diamond research, in which the structure and position of the deposition platform are crucial to the uniformity of diamond films and the long-term stability of thick film growth. Here, the effect of deposition platform height on the electric field uniformity, plasma state and temperature uniformity on the substrate surface was investigated by COMSOL simulation combined with experiments to optimize the process parameters for the uniform growth of optical grade diamond films. The 2-inch diamond film with thickness of 337 μm and inhomogeneity <11% was obtained at the optimal deposition platform height of 2 mm. The full width of the Raman half-peak from the center to the edge of the film is in the range of 3-4 cm^-1, and the maximum transmittance is 69%-70% in the visible light band and 70% in the infrared light at 10.6 μm. This indicates that thickness and quality of the diamond film are relatively uniform, thus the uniform deposition of 2-inch optical grade diamond film is achieved. Above results show that the deposition platform height has a great influence on the electric field distribution and plasma state on the substrate surface, and the electric field uniformity on the substrate surface is significantly improved with the increase of the deposition height, but the influence on the temperature uniformity is smaller.

Key words: optical grade diamond film, temperature uniformity, infrared transmittance, deposition platform height, COMSOL simulation

中图分类号:

O484

产思义, 屠菊萍, 黄珂, 邵思武, 杨志亮, 刘鹏, 刘金龙, 陈良贤, 魏俊俊, 安康, 郑宇亭, 李成明. 2英寸MPCVD光学级均匀金刚石膜的制备研究[J]. 无机材料学报, 2023, 38(12): 1413-1419.

CHAN Siyi, TU Juping, HUANG Ke, SHAO Siwu, YANG Zhiliang, LIU Peng, LIU Jinlong, CHEN Liangxian, WEI Junjun, AN Kang, ZHENG Yuting, LI Chengming. Uniform Growth of Two-inch MPCVD Optical Grade Diamond Film[J]. Journal of Inorganic Materials, 2023, 38(12): 1413-1419.

图/表 10

图1 不同沉积台高度的衬底放置示意图

Fig. 1 Schematic diagram of substrate placement for different deposition platform heights (a) 2 mm; (b) 0 mm; (c) -2 mm

表1 实验参数

Table 1 Experimental parameters

Nucleation					Growth
Power/ kW	Pressure/ kPa	Gas: CH₄/H₂	Time/ min	Temperature/ ℃	Power/ kW	Pressure/ kPa	Gas: CH₄/O₂/H₂	Temperature/ ℃	Height/ mm
4.7	21	35/500	40	880	4.7-4.9	21-22	25/5/500	870-880	2

图2 不同沉积台高度下的衬底上方电场模拟

Fig. 2 Electric field simulations above the substrate for different deposition platform heights (a) 2 mm; (b) 1 mm; (c) 0 mm; (d) -1 mm; (e) -2 mm

图3 不同沉积台高度下衬底上方电场不均匀性(a)和电场强度分布(b)

Fig. 3 Electric field inhomogeneity (a) and electric field intensity distributions (b) above the substrate at different deposition platform heights 1 inch=25.4 mm

图4 不同沉积台高度下的等离子体球的形状图

Fig. 4 Shape diagrams of the plasma spheres at different deposition platform heights (a) 2 mm; (b) 1 mm; (c) 0 mm; (d) -1 mm; (e) -2 mm

图5 不同沉积台高度下光发射光谱(a), C2、Hα、Hβ、CH峰强度和IC2/IHα、ICH/IHα、IHβ/IHα变化趋势(b)

Fig. 5 Optical emission spectra (a), relative C2, Hα, Hβ, CH emission intensities and variations in IC2/IHα, ICH/IHα, IHβ/IHα ratio (b) at different deposition platform heights

图6 不同沉积台高度下的温度分布均匀性

Fig. 6 Uniformity of temperature distributions at different deposition platform heights (a) 2 mm; (b) 0 mm; (c) -2 mm

图7 金刚石膜沉积态(a)和抛光态(b)的照片及沉积态的厚度分布图(c)

Fig. 7 Photographs of deposited state of the sample (a), polished state on both sides (b), and thickness distribution of the deposited state (c)

图8 金刚石膜的(a)XRD谱图和(b)拉曼光谱图

Fig. 8 XRD pattern (a) and Raman spectra (b) of the diamond films

图9 金刚石膜的(a)紫外-可见透过光谱图和(b)红外透过光谱图

Fig. 9 UV-Vis transmission spectra (a) and IR transmission spectra (b) of the diamond film Colorful figures are available on website

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2英寸MPCVD光学级均匀金刚石膜的制备研究

Uniform Growth of Two-inch MPCVD Optical Grade Diamond Film

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