基于托卡马克装置内壁硼膜材料的制备及其性能研究

doi:10.11949/0438-1157.20200025

化工学报 ›› 2020, Vol. 71 ›› Issue (5): 2413-2422.DOI: 10.11949/0438-1157.20200025

• 材料化学工程与纳米技术 • 上一篇下一篇

基于托卡马克装置内壁硼膜材料的制备及其性能研究

田小让^1,^2,³(),赵鑫³,赵冠超³,高志开³,韩培德^1,²

^1.中国科学院半导体研究所，集成光电子学国家重点实验室，北京 100083
^2.中国科学院大学电子电气与通信工程学院，北京 100049
^3.新奥科技发展有限公司，河北廊坊 065001

收稿日期:2020-01-07 修回日期:2020-02-22 出版日期:2020-05-05 发布日期:2020-05-05
通讯作者: 田小让
作者简介:田小让（1980—），男，博士，高级工程师，tianxiaorang@semi.ac.cn
基金资助:
国家重点研发计划项目(2018YFB1500500);中科院联合基金项目(Y072051002)

Systematic study on preparation and properties of boron film materials based on inner wall of Tokamak device

Xiaorang TIAN^1,^2,³(),Xin ZHAO³,Guanchao ZHAO³,Zhikai GAO³,Peide HAN^1,²

^1.State Key Laboratory on Integrated Optoelectronics, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China
^2.School of Electronic, Electrical and Communication Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
^3.ENN Science & Development Co. , Ltd. , Langfang 065001, Hebei, China

Received:2020-01-07 Revised:2020-02-22 Online:2020-05-05 Published:2020-05-05
Contact: Xiaorang TIAN

摘要/Abstract

摘要：

在真空腔室内壁生长硼膜是托卡马克装置至关重要的壁处理技术。自主搭建了球形辉光放电真空室，选用乙硼烷为硼源，采用等离子体化学气相沉积(PECVD)法在真空室内壁成功制备出硼膜。扫描电镜和结合力测试表明：制备出的硼膜结构致密，覆盖完整，结合力良好，膜层的结合力>240 N/m。同时系统研究了乙硼烷浓度、气压、电流密度和温度对硼膜生长的影响规律，并得出了室温条件下，乙硼烷浓度1%~2%，气压在5~10 Pa，电流密度4.7~6.2 μA/cm²的最佳制备工艺。通过残余气体分析仪(RGA)检测腔室内残余气体压力，进而研究硼膜对杂质的抑制性能。结果表明：硼化后腔室内残余气体H₂O、CO₂、CO和O₂的分压明显降低，比硼化前分别降低了200%，400%，200%和10%。结合腔室残余气体的分压结果和硼膜成分的X射线光电子能谱分析(XPS)，推测出硼膜对杂质的抑制机理。

关键词: 硼膜, 生长规律, 制备工艺, 抑制性能

Abstract:

Growing a boron film on the inner wall of a vacuum chamber is a critical wall treatment technology for a Tokamak device. In this paper, the spherical glow discharge vacuum chamber was built by ourselves. The boron film was successfully prepared on the wall of the vacuum chamber by plasma chemical vapor deposition with diborane as boron source. The results of SEM and adhesion test show that the boron film has compact structure, complete coverage and good adhesion, and the adhesion of the film is more than 240 N/m. The effects of the concentration of diborane, pressure, current density and temperature on the growth of boron films were systematically studied. The optimum preparation conditions of room temperature, 1%—2% ethoborane, 5—10 Pa pressure and 4.7—6.2 μA/cm² current density are obtained. The suppression effect of boron film on impurities in the vacuum chamber was explored via a residual gas analyzer (RGA). The results show that the partial pressures of the residual gases H₂O, CO₂, CO and O₂ after boronization are lower 200%, 400%, 200% and 10% than that before boronization, respectively. The suppression mechanism was deduced by analyzing the partial pressure of residual gases and the composition of boron film obtained by X-ray photoelectron spectroscopy (XPS).

Key words: boron film, growth law, preparation process, suppression performance

中图分类号:

TQ 013

田小让, 赵鑫, 赵冠超, 高志开, 韩培德. 基于托卡马克装置内壁硼膜材料的制备及其性能研究[J]. 化工学报, 2020, 71(5): 2413-2422.

Xiaorang TIAN, Xin ZHAO, Guanchao ZHAO, Zhikai GAO, Peide HAN. Systematic study on preparation and properties of boron film materials based on inner wall of Tokamak device[J]. CIESC Journal, 2020, 71(5): 2413-2422.

图/表 18

图1 硼膜生长实验装置平面示意图

Fig.1 Simplified schematic of boronization system

图2 氢气辉光清洗和硼化过程监控照片

Fig.2 Photos of hydrogen glow cleaning and boronization process

图3 硼化膜层SEM图

Fig.3 SEM images of boron films

图4 硼膜在真空腔室内的覆盖情况图

Fig.4 Coverage of boron film on vacuum chamber wall

图5 XPS表征分析数据

Fig.5 XPS analysis of boron film

图6 膜层和基底间结合力测试结果

Fig.6 Results from the test of adhesion between film and substrate

图7 乙硼烷浓度与硼膜沉积速率的关系

Fig.7 Relationship of B2H6 concentration and deposition rate of boron films

图8 不同硼烷浓度条件下，硼膜表面形貌图

Fig.8 Surface morphology of boron films prepared at different B2H6 concentrations

图9 腔室内的样品放置

Fig.9 Placement of samples inside cavity

表1 不同位置硼膜厚度

Table 1 Thickness of boron film at different positions

Positions	Thickness/nm
0°	150
90°	83
180°	170
270°	90

图10 不同放置位置硼膜生长情况图片

Fig.10 Pictures of growth of boron film at different locations

图11 气压和硼膜沉积速率的关系

Fig.11 Relationship between pressure and deposition rate of boron film

图12 不同压力沉积硼膜的典型形貌

Fig.12 Typical morphologies of boron films deposited under different pressures

图13 电流和硼膜沉积速率的关系

Fig.13 Relationship between current and deposition rate of boron film

图14 电流和硼膜结合力的关系

Fig.14 Relationship between current and adhesion of boron film

图15 腔室温度对硼膜制备的影响

Fig.15 Effect of chamber temperature on preparation of boron film

图16 不同厚度硼膜对杂质气体H2O和CO2的抑制效果

Fig.16 Inhibition effect of boron film with different thickness on impurity gas H2O and CO2

图17 硼化前后残余气体分析结果

Fig.17 Analysis results of residual gases before and after boronization

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基于托卡马克装置内壁硼膜材料的制备及其性能研究

Systematic study on preparation and properties of boron film materials based on inner wall of Tokamak device

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