溶膠凝膠法製備紫外光硬化型抗反射鍍膜

Preparation of UV-curable antireflective coatings by sol-gel process

黃逢璽(Feng-His Huang)

指導教授 ： 陳慶鐘

共同指導教授 ： 鄭廖平

淡江大學/工學院/化學工程與材料工程學系碩士班/碩士(2005年)

https://doi.org/10.6846/TKU.2005.00698

摘要

在本研究中的無機單體為四丁氧基鈦TBOT、四乙氧基矽TEOS，有機偶合劑為MSMA、GPTMS，透過溶膠凝膠製程，將TBOT與GPTMS合成高折射率薄膜， TEOS與MSMA合成低折射率薄膜，探討不同無機含量對折射率的影響。並研究旋轉塗佈的轉速及無機物濃度對於膜厚的影響，最後經由電腦輔助模擬來設計出抗反射效果最佳之薄膜厚度與折射率等操作參數。
本研究針對其中無機成分的添加比例，探討其對混成材料之光學性質、熱性質及形態學之影響；並以光干涉原理設計抗反射膜，模擬膜厚及折射率對光干涉現象的影響，進而將模擬結果用於實際鍍膜，比較理論鍍膜與實際鍍膜之光學性質差異，藉以改善鍍膜製程。
結果部分，提高SiO2的添加量，混成薄膜的折射率也隨之降低，由1.53降至1.49。而提高TiO2的添加量，混成薄膜的折射率也隨之升高，由1.6提升至1.75。不同厚度的折射率差異很小，故薄膜在可見光範圍內吸收度很小。探討固成份及轉速與厚度的關係，發現膜厚與固成分成正比而與轉速成反比，且固成分對膜厚影響較大而轉速影響較小，以此控制模厚。接著，將光的干涉效應向量化，即可以數值方法模擬反射率，得到有效的塗佈厚度與折射率，再配合厚度及折射率的控制技術進行鍍膜。利用預烤及後烤改善紫外光硬化薄膜的熱性質，SiO2溶膠及TiO2溶膠分別以80 ℃及90 ℃預烤1分鐘可改善紫外光硬化效率，硬化後之薄膜以200 ℃後烤15分鐘可大幅改善材料熱性質。經過上述製程探討，成功製備雙層抗反射薄膜，光波長550nm左右之折射率約為1%，已達到可見光抗反射效果。

關鍵字

溶膠凝膠法 ； 混成材料 ； 旋轉塗佈 ； 紫外光硬化 ； 抗反射鍍膜

並列摘要

Antireflective coatings produced from sol-gel techniques have received extensive interest recently. Such hybrid materials are used to synthesize new electronic and optical materials.
In this investigation, we prepare organic-inorganic hybrid sol by sol-gel process and synthesize the Poly(MSMA-SiO2) and Poly(GPTMS-TiO2) using UV-curing. The organic monomers were γ-Glycidoxy propyl trimethoxysilane (GPTMS), and 3-(trimethoxysilyl) propyl methacrylate (MSMA); inorganic monomers for the preparation were Tetrabutoxyltitanium (TBOT), and tetraethoxysilane (TEOS). The effects of the ratio of inorganic material on the morphology and optical properties of the composites were investigated. We added the photosensitive monomers, photoinitiator, and other additives to the composites to prepare antireflective coatings. Furthermore, FTIR was employed to investigated the evolution of chemical bonds between component molecules at polymerization and sol-gel process. TEM, and FESEM were used to find out the effects of the size and distribution of inorganic particles of the composite on the physical properties of the sols, and thin film. TGA was used to measure the degradation temperature respectively, and find out the effects of post bake. The optical properties were measured by n&k.
The experimental results showed that refractive index decreasing with increasing weight ratio of SiO2 and increasing with increasing weight ratio of TiO2. The thickness of hybrid films was varied from 100nm to 70nm by the solid content of hybrid sols and frequency of spin coating. Therefore, we can control the reflection by controlling the refractive index and thickness of thin film. The thermal stability of the prepared hybrid films increased with post bake for 15 mins at 200oC. Finally we obtained the antireflective coatings which had low reflection (1% at wavelength 550nm) at visible range.

並列關鍵字

sol-gel process ； organic-inorganic hybrid ； spin coating ； UV-curing ； antireflective coatings

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