本研究研發奈米粒子改質型彩色光阻，以改良傳統彩色濾光片中彩色光阻之性質。首先是以自由基聚合法合成Poly(BZMA-MAA-2HEMA)共聚合壓克力樹脂作為光阻的結合劑，並以三成分組成座標圖來決定其最佳之單體比例。再以溶膠－凝膠法製備表面富含反應性雙鍵之SiO2奈米粒子，由於此無機奈米粒子之平均粒徑可小於10 nm，於導入光阻系統中可與光阻中的感光性多官能基單體反應而製備出有機無－機奈米混成光阻。此奈米粒子改質型光阻可以提升光阻的硬度至5H，且熱穩定性(Td、Tg)也相對提高，而熱膨脹係數(αI、αII)則隨奈米粒子的導入量增加而下降。最後結合了顏料分散液後，則製備出奈米粒子改質型彩色光阻。此彩色光阻除了量測其光穿透率及CIE色度座標值外，由解析度測試結果亦可觀察到，彩色光阻的解析度可達小於10µm之水平。

In this research, a novel type of nano-silica modified color resist were developed for improving the properties of the conventional color resist applied in color filter. First, free radical polymerization was employed to synthesize the binder of the photoresist, the acrylate resin, i.e., poly(BZMA-MAA-2HEMA). The optimal composition of the prepared binder could be identified using ternary composition diagram. Then, surface modified SiO2 nanoparticles, mean particle size smaller than 10 nm, prepared by the formulation sol-gel method were introduced to the photoresist. Because the SiO2 particles contain considerable amount of reactive double bonds (C=C) on their surface, they would react with the photosensitive polyfunctional monomers in the photoresist to form an organic-inorganic nanohybrid. Incorporation of nanoparticles enhance the hardness (5H) and thermal stability of the prepared photoresist: Td and Tg were found to increase, whereas αI and αII decrease with increasing nanoparticles content. After the desired pigment dispersant was introduced into the photoresist, the nano-silica modified color resist were prepared. Light transmittance and CIE chromaticity coordinates of the developed color resist were studied, and the resolution of the circuit could reach the level of＜10µm.

中文摘要………………………………………………………………………..Ι
英文摘要……………………………………………………………………….II
誌    謝...........................................................................................................Ⅲ
目    錄……………………………………………………………………...Ⅳ
圖表索引...........................................................................................................Ⅸ

第一章  緒論 
1.1  前言………………………………………………………………............1
1.2  研究動機…………………………………….........……………………...2
1.3  研究架構及目標…………………………………….....................……...2

第二章  結合劑的合成及選擇性 
2.1  前言………………………………………….........……………………...5
2.2  理論及文獻回顧.........…………………………………………………...5
2.2.1  彩色光阻之簡介.....................................................................................5
2.2.1.1  光阻劑之種類及應用..........................................................................6
2.2.1.2  彩色光阻之組成..................................................................................7
2.2.2  結合劑之特性及其合成.........................................................................9
2.2.2.1  結合劑之特性......................................................................................9
2.2.2.2  結合劑之合成....................................................................................11
2.3  實驗方法及步驟......................................................................................13
2.3.1  藥品.......................................................................................................13
2.3.2  實驗步驟...............................................................................................14
2.3.2.1  結合劑之代號....................................................................................14
2.3.2.2  合成不同比例之結合劑....................................................................14
2.3.3  實驗儀器...............................................................................................16
2.4  結果與討論..............................................................................................18
2.4.1  二成份結合劑.......................................................................................18
2.4.1.1  不同MAA含量對結合劑之影響.......................................................19
2.4.1.2  固定MAA含量並改變合成溶劑之影響...........................................25
2.4.1.3  起始劑添加量對結合劑之影響........................................................26
2.4.1.4  固定MAA添加量下所合成結合劑之分子量與其溶液黏度...........29
2.4.1.5  FTIR結構鑑定....................................................................................30
2.4.2  三成份結合劑.......................................................................................32
2.4.2.1  三成份結合劑之合理添加量............................................................33
2.4.2.2  三成份結合劑之黏度測試................................................................34
2.4.2.3  三成份結合劑之分子量量測............................................................36
2.4.2.4  三成份結合劑之熱性質....................................................................37
2.4.2.5  三成份結合劑之化學結構鑑定........................................................44
2.4.2.6  三成份結合劑之酸價量測................................................................49
2.4.2.7  最佳化之三成份結合劑....................................................................52
2.5  結論..........................................................................................................53
2.6  參考文獻..................................................................................................54

第三章  含奈米粒子光阻之製備及性質測試
3.1  前言..........................................................................................................57
3.2  理論及文獻回顧......................................................................................57
3.2.1  有機－無機奈米複合材料...................................................................57
3.2.2  溶膠－凝膠法.......................................................................................58
3.3  實驗方法及步驟......................................................................................62
3.3.1  藥品.......................................................................................................62
3.3.2  實驗步驟...............................................................................................63
3.3.2.1  溶膠－凝膠法製備無機奈米粒子....................................................63
3.3.2.2  奈米粒子懸浮液之製備....................................................................64
3.3.2.3  製備奈米粒子改質型光阻................................................................65
3.3.3  實驗儀器...............................................................................................68
3.4  結果與討論..............................................................................................72
3.4.1  奈米粒子之鑑定...................................................................................72
3.4.1.1  FTIR結構鑑定....................................................................................72
3.4.1.2  MSiO2之TEM形態.............................................................................74
3.4.1.3  MSiO2之光散射粒徑分析.................................................................76
3.4.1.4  奈米粒子懸浮液之製備及鑑定........................................................79
3.4.2  奈米粒子改質型光阻...........................................................................84
3.4.2.1  熱性質分析........................................................................................84
3.4.2.2  光穿透率............................................................................................94
3.4.2.3  硬度及密著度....................................................................................97
3.4.2.4  光阻解析度測試................................................................................99
3.5  結論........................................................................................................108
3.6  參考文獻................................................................................................109

第四章  奈米粒子改質型彩色光阻之製備
4.1  前言........................................................................................................112
4.2  理論及文獻回顧....................................................................................112
4.2.1  顏料之種類及分散.............................................................................112
4.2.1.1  顏料簡介..........................................................................................112
4.2.1.2  有機顏料之特性..............................................................................113
4.2.1.3  有機顏料之種類..............................................................................117
4.2.2  顏料分散法製備彩色濾光片.............................................................119
4.2.3  顏色量測之簡介.................................................................................122
4.2.3.1  視覺系統的感知..............................................................................122
4.2.3.2  光譜光視效率..................................................................................123
4.2.3.3  等色函數..........................................................................................125
4.2.3.4  CIE 1931色度座標圖.......................................................................126
4.2.4  顏料分散型彩色濾光片之製程.........................................................129
4.2.5  顏料分散型彩色光阻之條件限制.....................................................130
4.3  實驗方法及步驟....................................................................................135
4.3.1  藥品.....................................................................................................135
4.3.2.1  顏料分散液之製備..........................................................................136
4.3.2.2  奈米粒子改質型彩色光阻..............................................................136
4.3.3  實驗儀器.............................................................................................138
4.4  結果與討論............................................................................................140
4.4.1  奈米粒子改質型紅色光阻.................................................................140
4.4.1.1  顏料之分散性..................................................................................140
4.4.1.2  顏料添加量......................................................................................142
4.4.1.3  硬度及密著度..................................................................................145
4.4.1.4  CIE色度座標...................................................................................147
4.4.1.5  光穿透率..........................................................................................148
4.4.1.6  解析度測試......................................................................................151
4.4.2  奈米粒子改質型綠色光阻.................................................................154
4.4.2.1  顏料之分散性..................................................................................154
4.4.2.2  顏料添加量......................................................................................156
4.4.2.3  硬度及密著度..................................................................................158
4.4.2.4  CIE色度座標...................................................................................159
4.4.2.5  光穿透率..........................................................................................160
4.4.2.6  解析度測試......................................................................................162
4.4.3  奈米粒子改質型藍色光阻.................................................................166
4.4.3.1  顏料之分散性..................................................................................166
4.4.3.2  顏料添加量......................................................................................168
4.4.3.3  硬度及密著度..................................................................................170
4.4.3.4  CIE色度座標...................................................................................171
4.4.3.5  光穿透率..........................................................................................173
4.4.3.6  解析度測試......................................................................................175
4.4.4  抗溶劑測試.........................................................................................179
4.5  結論........................................................................................................181
4.6  參考文獻................................................................................................182

第五章  結論與未來展望
5.1  結論........................................................................................................184
5.2  未來展望................................................................................................186

附 錄
附錄Ι  結合劑的合成與選擇.......................................................................188
附錄II  含奈米粒子光阻之製備及性質測試..............................................193
附錄Ⅲ  奈米粒子改質型彩色光阻之製備.................................................199
作者簡歷.........................................................................................................209
圖 表 索 引

表2.1 顏料分散型彩色光阻之主要組成..........................................................8
表2.2 二成份結合劑之玻璃轉移溫度表........................................................21
表2.3 二成份結合劑之熱裂解溫度總表........................................................23
表2.4 二成份結合劑之重量平均分子量及黏度............................................24
表2.5 相同二成份結合劑於不同合成溶劑下之一般性質............................26
表2.6 改變起始劑及鏈轉移劑添加量時結合劑之基本性質........................27
表2.7 固定起始劑及MAA添加量之黏度及分子量變化...............................30
表2.8 三成份結合劑之黏度總表....................................................................35
表2.9 三成份結合劑之重量平均分子量........................................................36
表2.10 三成份結合劑之玻璃轉移溫度..........................................................39
表2.11 三成份結合劑之熱裂解溫度..............................................................43
表2.12 三成份結合劑之FTIR特性吸收峰位置..............................................44
表2.13 結合劑之酸價總表..............................................................................50
表3.1 奈米粒子改質型光阻液之組成............................................................66
表3.2 奈米粒子改質型光阻之玻璃轉移溫度總表........................................87
表3.3 奈米粒子改質型光阻之熱裂解溫度總表............................................90
表3.4  TMA所量測之熱膨脹係數及玻璃轉移溫度總表.............................93
表3.5 三特定波長下之光穿透率總表............................................................96
表3.6 奈米粒子改質型光阻之硬度及密著度................................................98
表3.7 奈米粒子改質型光阻之解析度測試..................................................100
表4.1 常見之發色團及助色團結構..............................................................115
表4.2 有機顏料之種類..................................................................................118
表4.3 各製程之彩色濾光片特性之比較......................................................120
表4.4 彩色光阻中所需顏料之種類及結構..................................................121
表4.5 彩色濾光片對光阻層之規格限制......................................................133
表4.6 彩色光阻於特定波長下之光穿透率規範..........................................133
表4.7 彩色光阻之CIE色度座標限制............................................................134
表4.8 紅色及黃色顏料分散液之粒徑分析表..............................................141
表4.9 紅色顏料添加量之光阻總組成表......................................................143
表4.10 改變紅色顏料添加比例之CIE色度座標..........................................145
表4.11 奈米粒子改質型紅色光阻之硬度及密著度....................................146
表4.12 奈米粒子改質型紅色光阻之色度座標............................................147
表4.13 紅色光阻於特定波長下之光穿透率................................................151
表4.14 綠色顏料分散液之粒徑分析表........................................................155
表4.15 綠色光阻之總組成配方表................................................................156
表4.16 改變綠色顏料添加比例之CIE色度座標..........................................157
表4.17 奈米粒子改質型綠色光阻之硬度及密著度....................................158
表4.18 奈米粒子改質型綠色光阻之CIE色度座標......................................159
表4.19 藍色及紫色顏料分散液之粒徑分析表............................................166
表4.20 藍色光阻之總組成配方表................................................................168
表4.21 改變藍色顏料添加比例之CIE色度座標..........................................169
表4.22 奈米粒子改質型藍色光阻之硬度及密著度....................................171
表4.23 奈米粒子改質型藍色光阻之色度座標............................................172
表4.24 奈米粒子改質型彩色光阻之抗溶劑性測試....................................180


圖1.1  TFT-LCD顯示器之結構圖....................................................................1
圖1.2 研究架構流程圖......................................................................................3
圖2.1二成份結合劑poly(BZMA-MAA)之合成示意圖..................................10
圖2.2 三成份結合劑poly(BZMA-MAA-2HEMA)之合成示意圖.................10
圖2.3 三成份壓克力單體之三角座標圖........................................................12
圖2.4 結合劑之合成及結果分析流程圗........................................................15
圖2.5 二成份結合劑之三角座標圖................................................................19
圖2.6 二成份結合劑之DSC二次升溫曲線圖.................................................20
圖2.7 二成份結合劑B80M20H0之TGA及DTG圖.........................................22
圖2.8 二成份結合劑之TGA曲線圖................................................................22
圖2.9 MAA含量對二成份結合劑黏度之影響................................................24
圖2.10 不同起始劑及鏈轉移劑下結合劑之重量平均分子量變化..............28
圖2.11 不同起始劑及鏈轉移劑下結合劑黏度之變化..................................29
圖2.12 二成份(a)與三成份(b)結合劑之FTIR結構鑑定.................................31
圖2.13 三成份結合劑之四個族群..................................................................32
圖2.14 三成份結合劑之三成分組成座標圖..................................................33
圖2.15 三成份結合劑之DSC二次升溫曲線圖...............................................38
圖2.16 結合劑之TGA熱重損失曲線；(a) 2-HEMA 的添加比例固定為10 mol%，(b)BZMA：MAA＝8：2............................................................42
圖2.17 三成份結合劑B54M36H10之FTIR光譜，(a)尚未烘烤前；(b)以220℃烘烤1hr................................................................................................45
圖2.18 三成份結合劑B63M27H10之FTIR光譜，(a)尚未烘烤前；(b)以220℃烘烤1hr................................................................................................46
圖2.19 三成份結合劑B48M32H20之FTIR光譜，(a)尚未烘烤前；(b)以220℃烘烤1hr................................................................................................46
圖2.20 二成份結合劑“B80M20H0”之1H NMR圖.........................................48
圖2.21 二成份結合劑“B60M40H0”之1H NMR圖.........................................48
圖2.22 三成份結合劑“B54M36H10”之1H NMR圖.......................................49
圖2.23 符合酸價要求的三成份結合劑..........................................................51
圖2.24 最佳化三成份結合劑之比例區塊......................................................52
圖3.1 溶膠－凝膠法製備奈米懸浮液之示意圖............................................61
圖3.2 奈米粒子之製備流程圖........................................................................64
圖3.3 具反應性奈米粒子懸浮液之製備流程圖............................................65
圖3.4 奈米粒子改質型光阻之製備流程圖....................................................67
圖3.5 silica sol(a)及MSiO2 sol(b)之FTIR光譜圖.............................................73
圖3.6 MSiO2 sol烘乾後之TEM影像................................................................74
圖3.7 MSiO2 sol存放於4℃環境下之粒徑分析圖；(a)存放一天，(b)存放三天.........................................................................................................77
圖3.8 不同存放時間下，MSiO2奈米粒子之動態平均粒徑變化圖...............78
圖3.9 純的(a)H2O及(b)IPA之原始GC曲線圖................................................80
圖3.10 純的(a)乙醇及(b)甲醇之原始GC曲線圖............................................81
圖3.11 操作溫度於40℃下抽出物之原始GC曲線圖.....................................82
圖3.12 操作溫度於35℃下抽出物之原始GC曲線圖.....................................82
圖3.13 操作溫度於30℃下抽出物之原始GC曲線圖.....................................83
圖3.14 不同操作溫度下抽出物之原始GC曲線疊圖.....................................83
圖3.15 PR63-MSix系列之DSC疊圖................................................................85
圖3.16 PR54-MSix系列之DSC疊圖................................................................86
圖3.17 PR48-MSix系列之DSC疊圖................................................................86
圖3.18 PR63-MSix系列之TGA圖....................................................................88
圖3.19 PR54-MSix系列之TGA圖....................................................................89
圖3.20 PR48-MSix系列之TGA圖....................................................................89
圖3.21 傳統高分子光阻PR54之TMA圖.........................................................92
圖3.22 奈米粒子改質型光阻PR54-MSi20之TMA圖....................................92
圖3.23 PR63-MSix系列之光穿透率圖............................................................95
圖3.24 PR54-MSix系列之光穿透率圖............................................................95
圖3.25 PR48-MSix系列之光穿透率圖............................................................96
圖3.26 光阻PR63之光學顯微鏡圖：(a)線路圖；(b)解析度測試..................101
圖3.27 光阻PR54之光學顯微鏡圖：(a)線路圖；(b)解析度測試..................102
圖3.28 光阻PR48之光學顯微鏡圖：(a)線路圖；(b)解析度測試..................103
圖3.29 奈米粒子改質型光阻之解析度圖：(a)PR63-MSi10；(b) PR54-MSi10；(c) PR48-MSi10..........................................................104
圖3.30 光阻PR63-MSi20之光學顯微鏡圖：(a)馬賽克圖；(b)解析度測試..105
圖3.31 光阻PR48-MSi20之光學顯微鏡圖：(a)線路圖；(b)解析度測試......106
圖3.32 光阻PR54-MSi20之光學顯微鏡圖：(a)馬賽克圖；(b)放大倍率之解析度測試...........................................................................................107
圖4.1 色素分類示意圖..................................................................................113
圖4.2 光譜顏色及波長範圍對應圖..............................................................114
圖4.3 有機顏料之聚集方式..........................................................................116
圖4.4 眼睛細胞光譜相對敏感圖(虛線：柱狀細胞；實線：錐狀細胞)..........122
圖4.5 光譜光視效應曲線圖(虛線為暗視覺；實線為明視覺)......................123
圖4.6 RGB表色體系之等色函數(三刺激值)................................................125
圖4.7 XYZ表色體系之CIE等色函數(三刺激值)..........................................127
圖4.8 標準CIE 1931色度座標圖...................................................................128
圖4.9 顏料分散型彩色濾光片之側面構造圖..............................................129
圖4.10 顏料分散型彩色光阻之塗佈製程....................................................130
圖4.11 標準RGB彩色濾光片之分光圖........................................................132
圖4.12 標準RGB彩色濾光片之CIE色度座標圖..........................................134
圖4.13 奈米粒子改質型彩色光阻之製備流程圖........................................137
圖4.14 三種溶媒對紅色顏料PR177之粒徑分佈圖.....................................141
圖4.15 三種溶媒對黃色顏料PY139之粒徑分佈圖.....................................142
圖4.16 改變紅色顏料添加比例之CIE色度座標圖......................................144
圖4.17 奈米粒子改質型紅色光阻之CIE色度座標圖..................................148
圖4.18 紅色光阻改變顏料添加量之光穿透率圖........................................149
圖4.19 奈米粒子改質型紅色光阻之光穿透率圖........................................150
圖4.20 奈米粒子改質型紅色光阻之解析度測試圖，(a) PR48-R8Y1；(b) PR48-R8Y1-MSi5.............................................................................152
圖4.21 奈米粒子改質型紅色光阻之解析度測試圖，(a) PR48-R8Y1-MSi10；(b) PR48-R8Y1-MSi15....................................153
圖4.22 奈米粒子改質型紅色光阻PR48-R8Y1-MSi20之解析度測試圖.......................................................................................................154
圖4.23 不同溶媒下綠色顏料PG36之平均粒徑圖.......................................155
圖4.24 改變綠色顏料添加比例之CIE色度座標圖......................................157
圖4.25 奈米粒子改質型綠色光阻之CIE色度座標圖..................................160
圖4.26 綠色光阻之光穿透率圖，(a)改變顏料添加量；(b)導入不同比例奈米粒子...............................................................................................161
圖4.27 奈米粒子改質型綠色光阻之解析度測試圖，(a) PR48-G9Y1；(b) PR48-G9Y1-MSi5.............................................................................163
圖4.28 奈米粒子改質型綠色光阻之解析度測試圖，(a) PR48-G9Y1-MSi10；(b) PR48-G9Y1-MSi15...................................164
圖4.29 奈米粒子改質型綠色光阻PR48-G9Y1-MSi20之解析度測試圖，(a) 馬賽克圖；(b)解析度測試.................................................................165
圖4.30 三種溶媒下藍色顏料PB15:3之平均粒徑圖....................................167
圖4.31 三種溶媒下紫色顏料PV23之平均粒徑圖.......................................167
圖4.32 改變藍色顏料添加比例之CIE色度座標圖......................................170
圖4.33 奈米粒子改質型藍色光阻之CIE色度座標圖..................................172
圖4.34 藍色光阻之光穿透率圖，(a)改變顏料添加量；(b)導入不同比例奈米粒子...............................................................................................174
圖4.35 奈米粒子改質型藍色光阻之解析度測試圖，(a) PR48-B7V05；(b) PR48-B7V05-MSi5...........................................................................176
圖4.36 奈米粒子改質型藍色光阻之解析度測試圖，(a) PR48-B7V05-MSi10；(b) PR48-B7V05-MSi15................................177
圖4.37 奈米粒子改質型藍色光阻PR48-B7V05-MSi20之解析度測試圖，(a)馬賽克圖；(b)解析度測試.................................................................178

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