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系統識別號 U0002-2508201108311100
中文論文名稱 應用於紫外光交聯高折射率有機-無機混成薄膜之二氧化鈦溶膠的製備與分析
英文論文名稱 Preparation and characterization of TiO2 sol for UV-cured high-refractive-index organic-inorganic hybrid thin films
校院名稱 淡江大學
系所名稱(中) 化學工程與材料工程學系碩士班
系所名稱(英) Department of Chemical and Materials Engineering
學年度 99
學期 2
出版年 100
研究生中文姓名 林佳穎
研究生英文姓名 Chia-Ying Lin
學號 698400198
學位類別 碩士
語文別 中文
口試日期 2011-07-21
論文頁數 70頁
口試委員 指導教授-張朝欽
委員-陳慶鐘
委員-鄭廖平
委員-游洋雁
委員-張朝欽
中文關鍵字 光學塗膜  二氧化鈦  高折射率  紫外光交聯  有機-無機混成 
英文關鍵字 optical coatings  organic-inorganic nanocomposites  UV-curable  high refractive index  titanium dioxide 
學科別分類
中文摘要 本研究利用紫外光交聯二氧化鈦溶膠混和壓克力單體在PMMA基材上成功製備出混成薄膜。使用溶膠-凝膠法在室溫且無添加表面活性劑下,合成二氧化鈦奈米粒子。藉由加熱回流程序,二氧化鈦奈米粒子轉變為部分結晶型態。所製備的二氧化鈦溶膠可提供旋轉塗佈製備混成薄膜時操作的控制。高折射率複合薄膜含有高比例的二氧化鈦奈米粒子和良好的透明性。在T1-sol中的二氧化鈦粒子雖然已有產生部分結晶但光催化能力並不好。這可能是由於有限程度的結晶二氧化鈦僅能降解部分有機分子。所有複合薄膜表現出良好的附著力,折射率隨二氧化鈦比例增加分佈在1.66-1.82範圍之間。這些結果證明所製備的二氧化鈦複合薄膜在光學元件上有應用的潛力,如防反射塗層。二氧化鈦溶膠的特性將藉由DLS、TEM、XRD和UV-Vis吸收來鑑定,而二氧化鈦複合薄膜則進行UV-Vis吸收、FTIR、N&K、TGA、SEM、AFM和接觸角的分析。
英文摘要 In this study, UV-cured hybrid optical thin films were successfully prepared on PMMA substrates using TiO2 sols and acrylic monomers. TiO2 nanoparticles were synthesized via a sol-gel route at room temperature. Through the heat reflux process, the TiO2 nanoparticles became partial crystalline. The prepared TiO2 sols can provide operating control for the preparation of hybrid thin films by spin coating. Transparent high-refractive-index thin films were obtained with high TiO2 content. Photocatalytic ability of synthesized TiO2 nanoparticles was poor while some crystal structure existed. This may resulted from limited crystallinity of TiO2, and avoided a distinct degradation of organic moieties in the hybrids. TiO2 sols were characterized by DLS, TEM, XRD, and UV-Vis absorption, while TiO2 hybrid thin films were analyzed by UV-Vis absorption, FTIR, N&K, TGA, SEM, AFM, and contact angle. All hybrid thin films showed good adhesion to the PMMA substrate with refractive index falling over the range 1.66-1.82. These results suggested the potential application of present TiO2 hybrid films in optical devices, such as anti-reflective coatings.
論文目次 本文目錄
本文目錄 III
圖目錄 V
表目錄 VIII
第一章 緒論 1
1-1 前言 1
1-2 研究動機與方法 2
第二章 文獻回顧 4
第三章 實驗部分 9
3-1 實驗藥品 9
3-2 實驗步驟 10
3-2-1 二氧化鈦溶膠的合成 10
3-2-2 製備高折射率光學塗膜 10
3-2-3 光催化實驗 11
3-3 實驗儀器 13
第四章 結果與討論 18
4-1 溶膠性質分析 18
4-1-1 溶膠粒子DLS分析 18
4-1-2 溶膠粒子TEM觀測 21
4-1-3 溶膠粒子XRD光譜分析 22
4-1-4 紫外光-可見光光譜分析 26
4-2 塗膜性質分析 29
4-2-1紫外光-可見光光譜分析 29
4-2-2 紅外線光譜分析(FTIR) 31
4-2-3 塗膜與光學性質 35
4-2-4 塗膜表面形態鑑定 39
4-2-5 塗膜熱性質分析 46
4-2-6 塗膜接觸角分析 49
第五章 結論 51
參考文獻 52
附錄 56

圖目錄

圖3-1 製備二氧化鈦混成塗膜及檢測流程圖 12
圖4-1 T-sol在不同溫度加熱1小時後的粒徑變化 19
圖4-2 T-sol在70 o C下隨加熱時間的粒徑分佈 19
圖4-3 T-sol在不同溫度下隨加熱時間的粒徑變化 20
圖4-4 T-sol溶膠粒子TEM及SAD影像 21
圖4-5 T-sol在70 o C加熱3 h的TEM及SAD影像 22
圖4-6 T-sol在70 o C加熱6 h的TEM及SAD影像 22
圖4-7 T-sol溶膠在70 o C不同加熱時間下的XRD光譜 24
圖4-8 T-sol溶膠在80 o C不同加熱時間下的XRD光譜 25
圖4-9 T-sol溶膠在70 o C不同加熱時間下的UV-Vis光譜 26
圖4-10 T-sol溶膠在80 o C不同加熱時間下的UV-Vis光譜 27
圖4-11 二氧化鈦粒子光催化表現圖 28
圖4-12 T1-sol (3h)溶膠塗膜的UV-VIS吸收光譜圖 29
圖4-13 T1D80與T1-100厚膜的UV-VIS穿透光譜圖 30
圖4-14 不同二氧化鈦含量T1-sol製備塗膜FTIR圖譜 33
圖4-15不同二氧化鈦含量T-sol塗膜FTIR圖譜 34
圖4-16 塗膜折射率隨二氧化鈦含量變化圖 38
圖4-17 純DPHA塗膜表面SEM圖 40
圖4-18 純DPHA塗膜截面SEM圖 40
圖4-19 TD80塗膜表面SEM圖 41
圖4-20 TD80塗膜截面SEM圖 41
圖4-21 T1D60塗膜表面SEM圖 42
圖4-22 T1D60塗膜截面SEM圖 42
圖4-23 T1D80塗膜表面SEM圖 43
圖4-24 T1D80塗膜截面SEM圖 43
圖4-25 T1R80塗膜表面SEM圖 44
圖4-26 T1R80塗膜截面SEM圖 44
圖4-27 T1D80塗膜表面AFM圖 45
圖4-28 T1DR80塗膜表面AFM圖 45
圖4-29 T1R80塗膜表面AFM圖 45
圖4-30 T1-sol塗膜TGA分析圖 47
圖4-31 T-sol塗膜TGA分析圖 48
圖4-32 T-sol經70 oC加熱後塗佈的薄膜及80 wt.%混成薄膜接觸角變化圖 49
圖4-33 T1-sol塗佈的薄膜接觸角隨二氧化鈦含量變化圖 50
圖A-1 T-sol在70 o C下不同加熱時間的粒徑分佈(intensity) 56
圖B-1 T-sol光學能階圖 57
圖B-2 T-sol在70 o C加熱1小時光學能階圖 57
圖B-3 T-sol在70 o C加熱2小時光學能階圖 58
圖B-4 T-sol在70 o C加熱3小時光學能階圖 58
圖B-5 T-sol在70 o C加熱6小時光學能階圖 59
圖C-1 T1R80塗膜的UV-VIS吸收光譜圖 60
圖C-2 T1DR80塗膜的UV-VIS吸收光譜圖 60
圖C-3 T1-sol (3h)溶膠塗膜的UV-VIS穿透光譜圖 61
圖C-4 T-sol溶膠塗膜的UV-VIS吸收光譜圖 61
圖C-5 T-sol溶膠塗膜的UV-VIS穿透光譜圖 62
圖C-6 T1R80塗膜的UV-VIS穿透光譜圖(厚膜) 62
圖C-7 T1DR80塗膜的UV-VIS穿透光譜圖(厚膜) 63
圖C-8 DPHA、TMPTA厚膜的UV-VIS穿透光譜圖 63
圖D-1有機單體DPHA、TMPTA塗膜FTIR圖譜 64
圖E-1 純DPHA塗膜表面AFM圖 65
圖F-1 T1-100塗膜TGA分析圖 66
圖F-2 T1D80塗膜TGA分析圖 66
圖F-3 T1D60塗膜TGA分析圖 67
圖F-4 T1D40塗膜TGA分析圖 67
圖F-5 T1D20塗膜TGA分析圖 68
圖F-6 T-100塗膜TGA分析圖 68
圖F-7 TD80塗膜TGA分析圖 69
圖F-8 TD60塗膜TGA分析圖 69

表目錄

表3-1 二氧化鈦混成感光性塗料配方 11
表4-1 T-sol溶膠在70 o C的UV-Vis光譜結果整理 27
表4-2 T-sol溶膠在80 o C的UV-Vis光譜結果整理 27
表4-3 二氧化鈦、壓克力酯類主要特性吸收峰表 32
表4-4 T-sol塗膜物性量測表 36
表4-5 T-sol不同加熱時間與塗膜不同硬烤時間物性量測表 36
表4-6 T1-sol塗膜物性量測表 37
表4-7 塗膜光澤度量測結果表 37
表4-8 T1-sol塗膜TGA分析整理表 47
表4-9 T-sol塗膜TGA分析整理表 48
表4-10 塗膜接觸角測試結果整理表 50
表G-1 T1D60塗膜元素分析表 70

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