PECVD沉积和原位退火时间对h-BN薄膜组成及光学带隙的影响

doi:10.3724/SP.J.1077.2014.13549

无机材料学报 ›› 2014, Vol. 29 ›› Issue (7): 729-734.DOI: 10.3724/SP.J.1077.2014.13549 CSTR: 32189.14.SP.J.1077.2014.13549

PECVD沉积和原位退火时间对h-BN薄膜组成及光学带隙的影响

秦毅, 赵婷, 王波, 杨建锋

(西安交通大学金属材料强度国家重点实验室, 西安710049)

收稿日期:2013-10-25 修回日期:2014-01-26 出版日期:2014-07-20 网络出版日期:2014-06-20
作者简介:秦毅(1983-), 男, 博士研究生. E-mail:qinyi.andy@gmail.com
基金资助:
国家自然科学基金(51272205);中国科学院上海硅酸盐研究所高性能陶瓷和超微结构国家重点实验室开放课题基金(SKL200904SIC)

Influence of Deposition and in situ Annealing Time on Composition and Optical Band Gap of h-BN Films Deposited by PECVD

QIN Yi, ZHAO Ting, WANG Bo, YANG Jian-Feng

(State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049, China)

Received:2013-10-25 Revised:2014-01-26 Published:2014-07-20 Online:2014-06-20
About author:QIN Yi. E-mail:qinyi.andy@gmail.com
Supported by:
National Natural Science Foundation of China(51272205);Open Project Foundation of State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences (SKL200904SIC)

摘要/Abstract

摘要：

采用射频等离子增强化学气相沉积设备, 以高纯N₂和B₂H₆为气源, 制备了系列h-BN薄膜, 得到适合生长h-BN薄膜的最佳工艺条件。在此条件下, 研究了不同沉积时间和退火时间对薄膜组成和光学带隙的影响。采用傅立叶变换红外光谱仪、紫外可见光分光光度计和场发射扫描电子显微镜对样品进行了表征。实验结果表明: 在衬底温度、射频功率和气源流量比率一定的条件下, 沉积时间对h-BN薄膜成膜质量和光学带隙都有较大影响, 且光学带隙与膜厚呈指数关系变化。700℃原位退火不同时间对h-BN薄膜的结晶质量有所影响, 而物相和光学带隙基本没有改变。

关键词: h-BN薄膜, 沉积时间, 退火时间, 光学带隙

Abstract:

Series of h-BN films were grown by RF plasma enhanced chemical vapor deposition (PECVD) technique using high purity nitrogen and diborane as the precursor gases. The optimized experimental conditions for preparing h-BN films were explored. Based on these explorations, influences of deposition time and in situ annealing time on the composition and optical band gap of the films were investigated. All specimens were characterized by Fourier transform infrared spectroscope, utraviolet-visible spectrophotometer and field emission scanning electron microscope. The results show that the deposition time has a significant impact on the quality and optical band gap of the samples, and the optical band gap exhibits an exponential relation with the varied thickness of the films. Moreover, in situ annealing at 700℃ can affect the crystal quality, but almost not the phase and optical band gap of the h-BN films.

Key words: h-BN films, deposition time, annealing time, optical band gap

中图分类号:

TB34

秦毅, 赵婷, 王波, 杨建锋. PECVD沉积和原位退火时间对h-BN薄膜组成及光学带隙的影响[J]. 无机材料学报, 2014, 29(7): 729-734.

QIN Yi, ZHAO Ting, WANG Bo, YANG Jian-Feng. Influence of Deposition and in situ Annealing Time on Composition and Optical Band Gap of h-BN Films Deposited by PECVD[J]. Journal of Inorganic Materials, 2014, 29(7): 729-734.

图/表 5

表1 BN薄膜前期沉积条件

Table1 Preliminary deposition conditions for the BN films

No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

图1 在前期实验条件下沉积薄膜样品的FTIR光谱图

Fig.1 FTIR spectra of samples deposited at preliminary conditions

图2 h-BN薄膜样品横截面SEM照片

Fig. 2 Cross-section SEM image of the h-BN films The inset shows the results of line scanning by EDX in the film near the BN/Si interface

图3 (a)不同Dt样品的FTIR光谱, (b)层内(I1380)和层间(I780)成键的振动峰强度随Dt的变化规律; (c)沉积70 min并进行不同At处理样品的FTIR光谱

Fig. 3 FTIR spectra of the samples prepared with different Dt (a), I1380, I780 and I1380/ I780 as a function of Dt (b), FTIR spectra of the samples prepared with different At ( Dt=70 min) (c) depos-ited under conditions of sample 7#

图4 不同退火时间样品的表面形貌(a、b、c)和经过腐蚀后露出晶粒的样品表面(d)( Dt=70 min)

Fig. 4 Surface morphologies of the samples treated at different At(a, b, c) and surface morphology of the sample etched by 5vol% HF (d) ( Dt=70 min) Inset in (d) is morphology of the particle near the BN/Si interface

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PECVD沉积和原位退火时间对h-BN薄膜组成及光学带隙的影响

Influence of Deposition and in situ Annealing Time on Composition and Optical Band Gap of h-BN Films Deposited by PECVD

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No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

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No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30

No	T_s/℃	P/W	R	D_t/min
1^#	300	20	2	30
2^#	300	60	4	30
3^#	300	100	8	30
4^#	500	20	4	30
5^#	500	60	8	30
6^#	500	100	2	30
7^#	700	20	8	30
8^#	700	60	2	30
9^#	700	100	4	30