溶胶-凝胶SiO2减反膜的制备与光学性能研究

doi:10.15541/jim20230567

无机材料学报 ›› 2024, Vol. 39 ›› Issue (5): 525-530.DOI: 10.15541/jim20230567

溶胶-凝胶SiO₂减反膜的制备与光学性能研究

沈斌¹^,²(), 张旭¹, 熊怀¹, 李海元¹, 谢兴龙¹^,²()

1.中国科学院上海光学精密机械研究所, 高功率激光物理重点实验室, 上海201800
2.中国科学院大学材料与光电研究中心, 北京 100049

收稿日期:2023-12-08 修回日期:2024-01-09 出版日期:2024-05-20 网络出版日期:2024-01-22
通讯作者: 谢兴龙, 研究员. E-mail: xiexl329@mail.shcnc.ac.cn
作者简介:沈斌(1987-), 男, 博士研究生, 高级工程师. E-mail: bingo2011@siom.ac.cn
基金资助:
国家自然科学基金(12074399);中国科学院战略性先导科技专项A类(XDA25020305)

Preparation and Optical Properties of Sol-Gel SiO₂ Antireflective Films

SHEN Bin¹^,²(), ZHANG Xu¹, XIONG Huai¹, LI Haiyuan¹, XIE Xinglong¹^,²()

1. Key Laboratory of High Power Laser and Physics, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China
2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2023-12-08 Revised:2024-01-09 Published:2024-05-20 Online:2024-01-22
Contact: XIE Xinglong, professor. E-mail: xiexl329@mail.shcnc.ac.cn
About author:SHEN Bin (1987-), male, PhD candidate, senior engineer. E-mail: bingo2011@siom.ac.cn
Supported by:
National Natural Science Foundation of China(12074399);Strategic Priority Research Program of Chinese Academy of Sciences(XDA25020305)

摘要/Abstract

摘要：

碱催化溶胶-凝胶多孔SiO₂减反膜具有优异的光学性能及抗激光损伤性能, 是高功率激光装置中的重要组成部分, 但其与光学元件之间的结合强度低, 使得膜层易发生接触破坏。本研究以“神光 II”高功率激光装置溶胶-凝胶多孔SiO₂减反膜为基础, 通过提拉法在其表层涂覆致密的SiO₂薄层后得到机械强度提升的双层SiO₂减反膜(SiO₂-MTES), 并与常用的单层氨固化SiO₂减反膜(SiO₂-HMDS)进行相关应用性能的综合比较。结果表明, 涂覆SiO₂-MTES的熔石英在约800 nm处的峰值透过率大于99.6%, 运用1-on-1激光损伤阈值测试方法测得该双层SiO₂减反膜的零几率激光损伤阈值为51.9 J/cm²(1064 nm, 9.1 ns), 与涂覆SiO₂-HMDS的性能相当。同时, SiO₂-MTES膜层与水的接触角达到117.3°, 且在相对湿度大于90%的高湿环境中膜层的透过率较稳定。多次擦拭实验结果表明SiO₂-MTES的耐摩擦机械强度明显优于SiO₂-HMDS, 有效提升了膜层与光学元件之间的结合强度。

关键词: 溶胶-凝胶, 减反膜, SiO₂, 机械强度

Abstract:

Base-catalyzed sol-gel porous SiO₂ antireflective film, an important part of high power laser (such as "Shenguang II" high power laser) facilities, has excellent optical properties and laser damage resistance. However, its low binding strength with optical components can lead to the film frustrated with contact destruction. Based on this antireflective film, a double-layer SiO₂ antireflective film (SiO₂-MTES) was prepared with improved mechanical strength by coating a thin dense SiO₂ film on its surface using dip coating method. Then the SiO₂-MTES was compared with a commonly used single-layer ammonia cured SiO₂ antireflective film (SiO₂-HMDS). Results indicate that the peak transmittance of the fused quartz substrate coated with SiO₂-MTES reaches greater than 99.6% at about 800 nm and the zero probability laser damage threshold is measured to be 51.9 J/cm² (1064 nm, 9.1 ns) by 1-on-1 laser induced damage threshold testing method, equivalent to the performances of the fused quartz substrate with SiO₂-HMDS. Meanwhile, the contact angle between SiO₂-MTES and water reaches 117.3°, and the transmittance stability of the SiO₂-MTES is good in the high humidity environment with relative humidity greater than 90%. Results of multi-wiping experiments show that the friction-resistant mechanical strength of SiO₂-MTES is significantly better than that of SiO₂-HMDS, which effectively improves the binding strength between the film and the optical components.

Key words: Sol-Gel, antireflective film, SiO₂, mechanical strength

中图分类号:

O484

沈斌, 张旭, 熊怀, 李海元, 谢兴龙. 溶胶-凝胶SiO₂减反膜的制备与光学性能研究[J]. 无机材料学报, 2024, 39(5): 525-530.

SHEN Bin, ZHANG Xu, XIONG Huai, LI Haiyuan, XIE Xinglong. Preparation and Optical Properties of Sol-Gel SiO₂ Antireflective Films[J]. Journal of Inorganic Materials, 2024, 39(5): 525-530.

图/表 10

图1 溶胶2的制备流程图

Fig. 1 Preparation process of sol 2

图2 SiO2-MR膜层的折射率

Fig. 2 Refractive index of SiO2-MR film

图3 不同膜层的透过率

Fig. 3 Transmittances of different films

图4 膜层与水的接触角

Fig. 4 Water contact angles of films (a) SiO2-AR; (b) SiO2-HMDS; (c) SiO2-MTES; (d) SiO2-HMDS (90% RH); (e) SiO2-MTES (90% RH)

图5 SiO2溶胶粉末的水吸附性能

Fig. 5 Water adsorption performance of SiO2 sol powders (a) SiO2-AR; (b) SiO2-MR

图6 膜层表面AFM形貌

Fig. 6 AFM morphologies of films (a) SiO2-HMDS; (b) SiO2-MTES

表1 绸布擦拭后膜层的光学性能

Table 1 Optical properties of the films after rubbing with silk fabric

Coating category	Peak transmittance	Peak transmittance after rubbing
Coating category	Peak transmittance	10 times	100 times
SiO₂-HMDS	99.84%@760 nm	92.90%@760 nm	—
SiO₂-MTES	99.75%@830 nm	99.44%@830 nm	93.04%@830 nm

图7 经10次擦试后膜层表面状况

Fig. 7 Surface conditions of the films after 10 rubs (a) Blank substrate; (b) SiO2-HMDS; (c) SiO2-MTES

图8 膜层的激光损伤阈值

Fig. 8 Laser induced damage threshold of films (a) SiO2-HMDS; (b) SiO2-MTES

图9 膜层的透过率变化情况

Fig. 9 Changes in transmittance of films

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溶胶-凝胶SiO₂减反膜的制备与光学性能研究

Preparation and Optical Properties of Sol-Gel SiO₂ Antireflective Films

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