辛基三甲氧基硅烷改性SiO2疏水减反膜的制备

doi:10.15541/jim20150490

无机材料学报 ›› 2016, Vol. 31 ›› Issue (5): 499-504.DOI: 10.15541/jim20150490

辛基三甲氧基硅烷改性SiO₂疏水减反膜的制备

牛彦彦¹, 王晓栋², 姚兰芳¹, 田冰涛², 冯建斌¹, 曹媛媛², 张清华³, 沈军²

(1. 上海理工大学理学院, 上海200093; 2. 同济大学物理科学与工程学院, 上海市特殊人工微结构材料与技术重点实验室, 上海200092; 3. 成都精密光学工程研究中心, 成都610041)

收稿日期:2015-10-12 修回日期:2015-12-22 出版日期:2016-05-20 网络出版日期:2016-04-25
作者简介:牛彦彦(1990–), 女, 硕士研究生. E-mail: niuyanyan7365@163.com
基金资助:
国家自然科学基金青年基金(11304228).国家自然科学基金NSAF 联合基金(U1230113).2013 年度上海航天科技创新基金(SAST201370).上海市教育发展基金会和上海市教育委员会“晨光计划”(14CG19)中央高校基本科.

Preparation of Octyltrimethoxysilane Modified SiO₂ Hydrophobic Antireflective Coating

NIU Yan-Yan¹, WANG Xiao-Dong², YAO Lan-Fang¹, TIAN Bing-Tao², FENG Jian-Bin¹, CAO Yuan-Yuan², ZHANG Qing-Hua³, SHEN Jun²

(1. College of Science, University of Shanghai for Science and Technology, Shanghai 200093, China; 2. Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology, School of Physics Science and Engineering, Tongji University, Shanghai 200092, China; 3. Chengdu Fine Optical Engineering Research Centre, Chengdu 610041, China)

Received:2015-10-12 Revised:2015-12-22 Published:2016-05-20 Online:2016-04-25
About author:NIU Yan-Yan. E-mail: niuyanyan7365@163.com
Supported by:
Young Scientists Fund of the National Natural Science Foundation of China (11304228).National Natural Science Foundation of China (U1230113).Innovation Foundation of Shanghai Academy of Spaceflight Technology Development Foundation (14CG19).Fundamental Research Funds for the Central Universities

摘要/Abstract

摘要：

以正硅酸乙酯为前驱体, 氨水为催化剂制备标准SiO₂溶胶, 然后在回流前后分别对普通SiO₂溶胶添加适量的辛基三甲氧基硅烷(OTMS)进行修饰, 得到OTMS改性SiO₂溶胶。用未进行OTMS修饰、回流前修饰和回流后修饰的溶胶分别制备减反膜, 并使用傅里叶变换红外光谱仪、核磁共振波谱仪、紫外-可见-近红外分光光度计、原子力显微镜和接触角测试仪对薄膜的结构和性能进行表征。结果表明: 回流前添加OTMS修饰剂制备的改性SiO₂减反膜具有最优异的耐潮湿环境稳定性能, 最高透过率可达99.7%以上; 与水的接触角达到120°, 在潮湿环境中放置4 w后, 透过率只下降0.23%。

关键词: 溶胶-凝胶, 减反膜, 辛基三甲氧基硅烷

Abstract:

The standard SiO₂ sol was prepared by sol-gel process using tetraethylorthosilicate (TEOS) as precursor and ammonia as catalyst. Octyltrimethoxysilane (OTMS) was added into the standard SiO₂ sols before and after refluxing to obtain different organosilane modified silica sols, respectively. Silica antireflective (AR) coatings were then prepared from different SiO₂ sols by dip-coating method. The optical and structural properties of the AR coatings were characterized by Fourier transform infrared spectroscopy, liquid-state ²⁹Si NMR, UV-Vis-NIR spectrometer, atomic force microscope and water contact angle measurement. The results show that the AR coating prepared from OTMS modified before refluxing has the best moisture-resistant performance. The coated glass substrate obtains a high peak transmittance of 99.7%, with water contact angle of 120°. After been placed in a humid environment for 4 w, the transmittance of SiO₂ coatings modified before refluxing is decreased only by 0.23%.

Key words: Sol-Gel, antireflective coating, octyltrimethoxysilane

中图分类号:

O484

牛彦彦, 王晓栋, 姚兰芳, 田冰涛, 冯建斌, 曹媛媛, 张清华, 沈军. 辛基三甲氧基硅烷改性SiO₂疏水减反膜的制备[J]. 无机材料学报, 2016, 31(5): 499-504.

NIU Yan-Yan, WANG Xiao-Dong, YAO Lan-Fang, TIAN Bing-Tao, FENG Jian-Bin, CAO Yuan-Yuan, ZHANG Qing-Hua, SHEN Jun. Preparation of Octyltrimethoxysilane Modified SiO₂ Hydrophobic Antireflective Coating[J]. Journal of Inorganic Materials, 2016, 31(5): 499-504.

图/表 6

图1 OTMS改性溶胶制备流程图

Fig. 1 Flow chart of OTMS modified silica sols synthesis process

图2 未改性SiO2减反膜(a)与回流后(b)、回流前(c)添加OTMS改性SiO2减反膜的AFM形貌

Fig. 2 Surface morphologies of SiO2 coating prepared from unmodified (a), OTMS modification after refluxing (b) and before refluxing (c) sols

图3 未改性SiO2薄膜(a)和回流后(b)、回流前(c)添加OTMS改性SiO2薄膜样品的FTIR图谱

Fig. 3 FTIR spectra of SiO2 coatings prepared from unmodified (a), OTMS modification after refluxing (b) and before refluxing (c) sols

图4 回流前添加OTMS改性溶胶的29Si NMR图谱

Fig. 4 29Si NMR spectra of sols prepared from OTMS modification before refluxing

图5 镀制SiO2减反膜基底的透过率光谱(a)及在潮湿环境中镀膜基底的透过率峰值变化(b)

Fig. 5 Transmittance spectra for the substrate coated with silica antireflective coatings (a) and evolution of peak transmittance for the coated substrate in humid enviroment (b)

图6 薄膜样品的水接触角

Fig. 6 Water contact angles of silica coatings (a) F0; (b) AF-0.5-1; (c) AF-1-1; (d) BF-0.5-1; (e) BF-1-1

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辛基三甲氧基硅烷改性SiO₂疏水减反膜的制备

Preparation of Octyltrimethoxysilane Modified SiO₂ Hydrophobic Antireflective Coating

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