溅射功率对磁控溅射法制备MgF2薄膜组织和性能的影响

doi:10.15541/jim200190565

无机材料学报 ›› 2020, Vol. 35 ›› Issue (9): 1064-1070.DOI: 10.15541/jim200190565

所属专题：功能材料论文精选(一)：光学材料(2020)

• 研究快报 • 上一篇

溅射功率对磁控溅射法制备MgF₂薄膜组织和性能的影响

赵长江^1,^2,³(),马超^1,²,刘俊成^1,²(),刘治钢³,陈燕³

1.天津工业大学材料科学与工程学院, 天津 300387
2.天津工业大学分离膜材料与膜过程国家重点实验室, 天津 300387
3.北京空间飞行器总体设计部, 北京 100086

收稿日期:2019-11-06 修回日期:2019-12-10 出版日期:2020-09-20 网络出版日期:2020-08-26
作者简介:赵长江(1978–), 男, 博士研究生. E-mail: ZCJ780525@163.com
ZHAO Changjiang(1978–), male, PhD candidate. E-mail: ZCJ780525@163.com

Sputtering Power on the Microstructure and Properties of MgF₂ Thin Films Prepared with Magnetron Sputtering

ZHAO Changjiang^1,^2,³(),MA Chao^1,²,LIU Juncheng^1,²(),LIU Zhigang³,CHEN Yan³

1. School of Materials Science and Engineering, TIANGONG University, Tianjin 300387, China
2. State Key Laboratory of Membrane Separation and Membrane Process, Tianjin 300387, China
3. Beijing Institute of Spacecraft System Engineering, Beijing 100086, China

Received:2019-11-06 Revised:2019-12-10 Published:2020-09-20 Online:2020-08-26
Supported by:
National Natural Science Foundation of China(51352002)

摘要/Abstract

摘要：

为了减少磁控溅射法沉积MgF₂薄膜的F贫乏缺陷, 在工作气体Ar₂中加入SF₆作为反应气体, 在石英玻璃衬底上用射频磁控溅射法制备了MgF₂薄膜, 研究了溅射功率对MgF₂薄膜化学成分、微观结构和光学性能的影响。结果表明, 随着溅射功率从115 W增加到220 W, F: Mg的原子比不断增加, 185 W时达到2.02, 最接近理想化学计量比2 : 1;薄膜的结晶度先提高后降低, 最后转变为非晶态; MgF₂薄膜的颗粒尺寸先是有所增加, 轮廓也变得更加清晰, 最后又变得模糊。MgF₂薄膜的折射率先减小后增大, 在185 W时获得最低值, 550 nm波长的折射率1.384非常接近MgF₂块体晶体;镀膜玻璃在300~1100 nm范围内的透光率(以下简称薄膜透光率)先增大后减小, 185 W时达到94.99%, 比玻璃基底的透光率高出1.79%。

关键词: MgF₂薄膜, F贫乏, 透光率, 减反射, 溅射功率, 磁控溅射

Abstract:

To reduce the F deficiency defect in MgF₂ thin films deposited with magnetron sputtering, SF₆ was added to the working gas Ar₂ as the reactive gas, and MgF₂ thin films were prepared on quartz glass substrates with radio frequency (RF) magnetron sputtering. The effects of sputtering power on the chemical compositions, microstructure and optical properties of MgF₂ thin film were investigated. The results show that with sputtering power increase from 115 to 220 W, the atomic ratio of F to Mg increased continuously, and reached 2.02 at 185 W, close to ideal stoichiometric ratio of 2: 1. The crystallinity of MgF₂ film improved first, then decreased, and finally changed into amorphous state. Profile of particles composing MgF₂ film became clearer at first, and finally became blurred. Refractive index of MgF₂ film decreased firstly and then increased, and got the lowest value at 185 W, 1.384 at 550 nm wavelength which is very close to that of MgF₂ bulk crystal. The integral transmittance of the coated glass within 300-1100 nm (hereinafter referred to as the transmittance of the thin film) increased first and then decreased, and reached 94.99% at 185 W, higher than that of the bare glass substrate by 1.79%.

Key words: MgF₂ thin film, F deficiency, transmittance, antireflection, sputtering power, magnetron sputtering

中图分类号:

赵长江,马超,刘俊成,刘治钢,陈燕. 溅射功率对磁控溅射法制备MgF₂薄膜组织和性能的影响[J]. 无机材料学报, 2020, 35(9): 1064-1070.

ZHAO Changjiang,MA Chao,LIU Juncheng,LIU Zhigang,CHEN Yan. Sputtering Power on the Microstructure and Properties of MgF₂ Thin Films Prepared with Magnetron Sputtering[J]. Journal of Inorganic Materials, 2020, 35(9): 1064-1070.

图/表 8

Fig. 1 Effect of sputtering power on XPS spectrum of MgF2 film

Fig. 2 Effect of sputtering power on XRD pattern of MgF2 thin film

Table 1 Molar ratio of F to Mg and XRD analysis results of MgF2 films

Sample	n(F) : n(Mg)	2θ/(°)	Intensity/(a.u.)	FWHM	Interplanar spacing/nm	Grain size/nm
115 W	1.65	57.832	127	0.95	0.1593	9.6
150 W	1.88	56.447	36086	0.534	0.1629	17.2
185 W	2.02	56.968	158	0.874	0.1615	10.4
220 W	2.44	Amorphous	-	-	-	-

Fig. 3 Effect of sputtering power on the surface micro morphology of MgF2 film

Fig. 4 Effect of sputtering power on refractive index spectra of MgF2 thin film

Table 2 Thickness, refractive index and integral transmittance of MgF2 film

Sputtering power/ W	Thickness/ nm	Refractive index within 300-1100 nm	Refractive index at 550 nm	Integral transmittance within 300-1100 nm/%
115	65	1.525-1.494	1.501	92.489
150	63	1.483-1.452	1.459	93.433
185	67	1.408-1.377	1.384	94.990
220	76	1.508-1.477	1.484	92.925
Glass	0		1.46	93.20

Fig. 5 Effect of sputtering power on transmission spectra of MgF2 thin film

Fig. 6 Relation between integrated transmittance within 300-1100 nm and refractive index of thin film at 550 nm

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溅射功率对磁控溅射法制备MgF₂薄膜组织和性能的影响

Sputtering Power on the Microstructure and Properties of MgF₂ Thin Films Prepared with Magnetron Sputtering

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