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    题名: 感光性有機-無機奈米複合材料的製備與其於光學鍍膜之應用
    其它题名: Preparation of photo-sensitive organic-inorganic nanocomposites for application in optical coatings
    作者: 黃逢璽;Huang, Feng-hsi
    贡献者: 淡江大學化學工程與材料工程學系博士班
    鄭廖平;Cheng, Liao-ping
    关键词: 感光性塗料;有機-無機 奈米複合材料;光學鍍膜;photo-sensitive;organic-inorganic nanocomposites;optical coatings
    日期: 2010
    上传时间: 2010-09-23 17:31:53 (UTC+8)
    摘要: 本研究以溶膠凝膠法搭配紫外光硬化製程,製備感光性有機-無機奈米複合材料並應用於光學鍍膜上。論文首先建立了一個有機-無機奈米複合材料的設計概念,並用於設計四種光學鍍膜,所得重要結論如下。
    高硬度-抗霧光學鍍膜:吾人已成功合成含雙鍵的介面活性劑(親水劑),可以直接添加到塗料中參與聚合反應。透過雙層塗佈的設計也製備出高硬度且耐水浸泡之親水型抗物鍍膜。利用AFM檢測可以預先觀察鍍膜表面的親水劑分佈狀況,提供塗料配置的參考。改質之Tween20介面活性劑,在10 wt%的添加量,可以使鍍膜有高透明度,高硬度5H,耐水浸泡及很好的抗霧效果。
    光致變色光學鍍膜:利用溶膠凝膠法吾人成功的製備二氧化矽/磷鎢酸複合材料。經由製程的調整再進一步控制粒子的尺寸,PS1製程可得到1.2 nm的二氧化矽/磷鎢酸混成粒子,而PS2製程可得到10 nm的混成粒子。FTIR、 XRD和HRTEM 都指出相同重量比下,較小的混成粒子能提供較多的Si-OH基團,能連結較多的磷鎢酸單元,抑制磷鎢酸的結晶,也有較好的光致變色及退色效率。合成的二氧化矽/磷鎢酸混成粒子分別以兩種偶合劑進行表面改質,並加入有機感光性單體及光啟始劑成為感光塗料,隨後製備光致變色鍍膜。鍍膜程序會降低光致變色及退色效率。特別的是TMES改質的鍍膜硬度中等,但是給予二氧化矽/磷鎢酸混成粒子很好的保護,使其不受交聯反應影響維持在粉體時的狀況,讓光學鍍膜達到3-5分鐘的退色速率。
    彩色光學鍍膜:吾人成功合成出偶合劑ICPTES改質紅色染料,並將改質染料接枝於二氧化矽表面。DSC及TGA熱性質分析可以發現,越小的二氧化矽粒子對熱性質影響越大;而直接將染料接枝於二氧化矽表面對熱性質的影響又要比混摻來的好。將改質染料-g-二氧化矽混成材料導入光學鍍膜中,在250 oC的熱處理下可以防止染料裂解,而280 oC時也只有眼睛無法辨識的退色發生。利用三成份物性圖我們可以有效的圈選符合應用條件的彩色鍍膜。
    高折射率光學鍍膜:吾人藉由溶膠凝膠法成功的製備出可以長時間保持穩定的二氧化鈦溶膠與二氧化鈦複合溶膠。這些溶膠藉由多官能基的壓克力單體在PMMA基板上形成透明且具高折射率的塗層。FTIR與UV-vis說明了二氧化鈦與偶合劑之間的相互作用。所合成的二氧化鈦粒子大小約為3.7 nm。添加偶合劑可以避免聚集的大粒子生成。所有的複合薄膜在PMMA基材上呈現一個良好的附著度表現。薄膜的折射率隨的二氧化鈦含量的增加從1.64增加到1.77。薄膜的表面平坦度良好且透過偶合劑可以進一步改善平坦度。這些實驗結果顯現製備的二氧化鈦複合薄膜在光學元件上如抗反射塗層有應用的潛力。
    期盼藉由此研究能突破一般商用光學鍍膜物化性質的門檻,進而開發出具商業價值的產品。
    In this study, photosensitive organic - inorganic nanocomposites are prepared by sol-gel method and UV curing process then applied on optical coating. The design concept of organic - inorganic nanocomposites is established, and use for designing four optical coatings, the main conclusions are as follows.
    High hardness anti-fog optical coating: We have been synthesized surfactants containing double bonds successfully. These modified surfactants can be added into the coatings directly involved in polymerization. Through the design of double-layer coating, high hardness and water resistant material coating is prepared. AFM detection can observe the distribution of hydrophilic agent on the surface to provide a reference on coating composition. As coatings containing modified Tween20 surfactant 10 wt%, bring the high transparency, high hardness (5H), water resistance and good anti-fog effect.
    Photochromic PWA/SiO2 hybrid coatings: Photochromic PWA/SiO2 hybrid powder is prepared by the sol-gel process. The size of the primary particles was controlled by feeding PWA either initially or in the middle of the sol-gel reaction. For the former case (PS2 series), the average particle size is 1.2 nm, whereas for the latter (PS1 series), 10 nm. Photochromic coating is carried out by modified PWA/SiO2 hybrid sol, photo-sensitive monomer and photoinitiator. UV irradiation of the photochromic induces a coloration response (deep blue), for which the deepness of color increases with increasing exposure time. Also, the coloration/bleaching rate for the PS2 series coatings, in particular TMES medium modification, is found to be higher than those in the PS1 series due to more PWA-SiOH interactions in the former case.
    Color Optical Coating: We successfully synthesized coupling agent (ICPTES) modified red dye, then grafted onto the silica surface. Thermal properties can be found by DSC and TGA analysis, the smaller silica particles size has greater thermal impact; and thermal properties of direct dye grafted onto the silica surface is better than blend. The modified dye-g-silica hybrid materials are added into optical coating to prevent the dye cracking in the heat treatment of 250 oC, even at 280 oC only has little dye cracking that eyes do not recognize.
    High reflection index coating: In this work, long-term stable TiO2 sol and TiO2 hybrid sols with different surface coupling agents were successfully prepared by the sol-gel process, and high RI transparent optical thin films were prepared by these sols with a acrylic monomer DPHA using spin-coating followed by UV curing on PMMA substrates. FT-IR and UV-visible spectra suggested the existence of interaction between TiO2 sol and the coupling agent by coordination. Analysis of particle size indicated that the synthesized TiO2 sol was close to or less than 3.8 nm and larger particles (< 10 nm) may result from aggregation and can be separated by the coupling agent. All hybrid thin films prepared by TiO2 sol or TiO2 hybrid sol with DPHA show a good adhesion to the PMMA substrate. The refractive indices increased from 1.64 to 1.77 with the increasing TiO2 content for the hybrid thin films. Surface planarity of the prepared hybrid thin films was good and improved by the coupling agent. The results suggested the potential application of the prepared TiO2 hybrid films in optical devices, such as anti-reflective coatings.
    Through this research, we hope to overcome the physical and chemical properties of commercial optical coating, and develop economic products.
    显示于类别:[化學工程與材料工程學系暨研究所] 學位論文

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