Preparation of transparent, thick films with high refractive index by the sol-gel method and application to the fine patterning process

溶胶-凝胶法制备透明高折射率厚膜及其在精细图形加工中的应用

• 批准号: 13555242
• 负责人: MINAMI Tsutomu
• 金额: $ 8.45万
• 依托单位: Osaka Prefecture University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 2001
• 资助国家: 日本
• 起止时间: 2001 至 2002
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-13555242/
• 关键词: Sol-Gel method; Thick film; refractive index; Micropatterning; Silsesquioxane; Organic-inorganic hybrid; Transparent; UV-irradiation; ゾルーゲル法

1. Transparent, thick films with high refractive index have been successfully prepared using silsesquioxanes from such as phenyltriethoxysilane and benzyltriethoxysilane and metal oxides. Titania-silsesquioxane films showed the highest refractive index. Thick films from diphenyldimethoxysilane and titania showed higher refractive index than the films from phenyltrietoxysilane and titania. Thick films from diphenylmethoxysilane showed fluidity with less than 30 mol % of titania.2. Changes of structure, morphology, and optical properties of silsesquioxane-titania thick films by UV-irradiation have been investigated. Irradiation of UV-light led to depletion of Si-C bonds in the thick films, and hardness and refractive index of the films were increased. It was found that hardness of the vinylsilsesquioxane-titania films mostly increased.3. Micropatterns of phenylsisisesquioxane-titana thick films were successfully prepared by the embossing process. Convexly shaped micropatterns have been formed on hydrophobic-hydrophilic patterned substrate with titania and fluoroalkylsilanes thin layer, based on the difference in the surface free energy and fluidity of the phenylsilsesquioxane-titana at temperatures higher than then-glass transition temperatures.

1.利用苯基三乙氧基硅烷、苄基三乙氧基硅烷和金属氧化物制备了高折射率的透明厚膜。二氧化钛-倍半硅氧烷薄膜的折射率最高。厚膜从二苯基二甲氧基硅烷和二氧化钛表现出较高的折射率比从苯基三乙氧基硅烷和二氧化钛的膜。厚膜从二苯基甲氧基硅烷显示流动性与小于30摩尔%的二氧化钛。研究了倍半硅氧烷-二氧化钛厚膜在紫外光照射下的结构、形貌和光学性质的变化。紫外光照射导致厚膜中Si-C键的耗尽，薄膜的硬度和折射率增加。结果表明，乙烯基倍半硅氧烷-二氧化钛薄膜的硬度有较大幅度的提高.采用模压工艺成功地制备了苯基硅倍半氧烷-二氧化钛厚膜微图案。基于苯基倍半硅氧烷-二氧化钛在高于玻璃化转变温度的温度下的表面自由能和流动性的差异，在具有二氧化钛和氟烷基硅烷薄层的疏水-亲水图案化基底上形成了凸形微图案。

项目成果

A. Matsuda: "Photocatalytic Micropatterning of Transparent Ethylsesesqiuoxane-Titania Hybrid Films"Chem. Mater.. 14[6]. 2693-2700 (2002)

A. Matsuda：“透明乙基倍半氧烷-二氧化钛混合薄膜的光催化微图案化”Chem。

K. Tadanaga: "Micropatterning of Inorganic-Organic Hybrid Coaling Films from Various Tri-Functional Silicon Alkoxides with a Double Bond in Their Organic Components"J. Sol-Gel Sci. Tech.. 26[1]. 431-434 (2003)

K. Tadanaga：“有机成分中带有双键的各种三官能硅醇盐的无机-有机杂化涂层薄膜的微图案化”J。

K. Tadanaga: "Formation of Superhydrophobic and Superhydrophlic Surfaces by the Sol-Gel Method (review)(in Japanese)"Material Stage. 1[1]. 34-38 (2001)

K. Tadanaga：“通过溶胶-凝胶法形成超疏水和超疏水表面（评论）（日语）”材料阶段。

A.Matsuda: "Preparation of Copolymerized Phenylsilsesquioxane-Benzylsilsesquioxane Particles"J. Sol-Gel Sci. Tech.. 23. 247-252 (2002)

A.Matsuda：“共聚苯基倍半硅氧烷-苄基倍半硅氧烷颗粒的制备”J。

A.Matsuda: "Preparation and Characterization of Copolymerized Methylsilsesquioxane-Benzylsilsesquioxane Microparticles for Electrophoretic Sol-Gel Deposition"J. Mater. Sci.. (accepted for publication).

A.Matsuda：“用于电泳溶胶-凝胶沉积的共聚甲基倍半硅氧烷-苄基倍半硅氧烷微粒的制备和表征”J。