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研究生: 李東霖
Li, Tung-Lin
論文名稱: 耐高溫ITO/聚亞醯胺透明塑膠基板的製備
Preparation of High Temperature Transparent ITO/Polyimide Plastic Substrates
指導教授: 許聯崇
Hsu, Lien-Chung
學位類別: 碩士
Master
系所名稱: 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年: 2005
畢業學年度: 93
語文別: 中文
論文頁數: 105
中文關鍵詞: 聚亞醯胺透明基板
外文關鍵詞: transparent substrates, polyimide
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  •   利用6FDA(4,4’- Hexafluoroisopropylidene diphthalic anhydride)、3,3’DDS(3,3’-Diaminodi-phenyl sulfone)、4,4’MBCA(4,4’-Diaminodi-cyclohexylmethane)等單體在無水極性溶劑DMAc(Dimethylacetamide)中進行縮聚合反應,成功合成出2種不同結構之聚亞醯胺(Polyimide)前驅物PAA(Poly(amic acid))。將其於300℃高溫環化後得到2組不同結構之透明無色聚亞醯胺。此2種不同結構PAA之固有黏度(inherent viscosity)為0.58~0.71 (dL/g),其結構由FTIR及元素分析中得到鑑定。

      此2種聚亞醯胺皆具有高的玻璃轉移溫度(Tg)且在可見光範圍內的穿透率達86%。以磁控濺鍍法將ITO膜沈積於無色聚亞醯胺基板上。將ITO/PI在氮氣下進行退火熱處理。由XRD繞射分析顯示,隨著退火溫度提升ITO膜由非晶相轉為結晶相。製程條件最佳電阻率約為4 x 10-4Ω-cm,電子遷移率及載子濃度分別為21.8 cm2/V和1.3x1025cm-3。其可見光範圍內的穿透度為82.1%。

     Two kinds of transparent polyimide precurors , poly(amic acid), were prepared from 4,4’-Hexafluoroisopropylidene diphthalic anhydride
    (6FDA), 3,3’-Diaminodiphenyl sulfone (3,3’DDS) and 4,4’-Diaminodi-cyclohexylmethane (4,4’MBCA). Subsequently, thermal cyclization of the poly(amic acid) precursors at 300℃ produced the corresponding polyimides. The inherent viscosities of the precursor polymers were 0.58~0.71 dL/g. The fluorinated polyimides had high glass transition temperatures. The structures of the precursor polymers and the fully cyclized polymers were characterized by FTIR and elemental analysis. The optical transmittance of these polyimide films were up to 86%.

     Transparent and conductive ITO were coated on the colorless polyimide films by RF magnetron sputtering. The ITO/PI films were annealed at nitrogen atmosphere. The XRD diffraction showed that the amorphous ITO phase transferred into crystalline phase as the annealing temperature increased. After heat treatment, the best resistivity was 4×10-4Ω-cm. The electron mobility and the carrier concentration were 21.8 cm2/V and 1.3x1025cm-3 respectively. The optical transmittance was over 82%.

    總目錄 中文摘要..............................................................Ⅰ Abstract................................................... Ⅱ 誌謝..................................................................Ⅲ 總目錄...............................................................Ⅳ 表目錄.................................................................Ⅸ Scheme目錄..........................................................Ⅹ 圖目錄............................................................XI 第一章 緒論..........................................................1 1-1 前言............................................................1 1-2 研究動機與目的.............................................1 1-3 研究架構......................................................2 第二章 文獻回顧及原理............................................3 2-1 聚亞醯胺之介紹.............................................3 2-1-1 加成型聚亞醯胺..........................................6  2-1-2 縮合型聚亞醯胺..............................................8 2-1-3 改質型聚亞醯胺..........................................13 2-1-4 透明聚亞醯胺..........................................13 2-2濺鍍原理...............................................................15 2-2-1 電漿原理..................................................15 2-2-2 射頻放電..........................................................17 2-2-3 磁控濺鍍法.....................................................19 2-3 薄膜成長理論..............................................................21 2-3-1 薄膜成核與成長............................................21 2-4 銦錫氧化物(ITO)透明導電膜之特性.......................................23 2-4-1 基本性質......................................................23 2-4-2 電性......................................................24 2-4-3 光學性質.....................................................27 2-5銦錫氧化物(ITO)之應用與製造......................................32 2-5-1 ITO膜的研發近況................................................32 2-5-2 ITO膜的應用....................................................34 第三章 實驗方法與步驟......................................................35 3-1 實驗藥品與儀器..........................................................35 3-1-1 藥品........................................................35 3-1-2 實驗儀器....................................................36 3-2 二酸酐的純化.....................................................37 3-3 實驗步驟.........................................................37 3-3-1 PI-1前驅物PAA-1之合成......................................37 3-3-2 PI-2前驅物PAA-2之合成...............................................40 3-3-3 聚亞醯胺薄膜之製備..............................................42 3-4 結構鑑定與分析........................................................44 3-4-1 聚亞醯胺固有黏度測定................................................44 3-4-2 傅立葉紅外線光譜儀分析(FT-IR)....................................44 3-4-3 元素分析(EA) .....................................................44 3-4-4 熱性質分析........................................................45 3-4-4-1 微差掃瞄卡計分析(DSC)..............................45 3-4-4-2 熱重損失分析(TGA)..............................................45 3-4-5 薄膜機械性質分析..................................................45 3-4-6 薄膜吸濕性分析..................................................46 3-4-7 穿透度測試.....................................................46 3-5 鍍膜實驗流程........................................................47 3-5-1 實驗系統說明.......................................................48 3-5-2 實驗鍍膜參數.......................................................51 3-5-3 鍍膜步驟..........................................................51 3-5-4 鍍膜熱處理..........................................................51 3-6 鍍膜性質分析.......................................................52 3-6-1 膜厚及成長速率之量測.........................................52 3-6-2 表面型態及粗糙度分析.. ..............................................52 3-6-3 X-ray 繞射分析.. ...............................................52 3-6-4 電性量測.. ........................................................53 3-6-5 光學量測............................................................56 第四章 結果與討論.......................................................57 4-1聚醯胺酸及聚亞醯胺之合成與分析...................................58 4-1-1 6FDA+3,3’DDS系統..............................................58 4-1-2 6FDA+4,4’MBCA系統............................60 4-2 聚亞醯胺熱性質分析...................................................62 4-2-1 微差掃描熱分析(DSC).......................................62 4-2-2 熱重損失分析(TGA).........................................62 4-3 聚亞醯胺機械性質分析...............................................63 4-4 聚亞醯胺吸濕性分析................................................64 4-5 穿透度測試(UV-Vis)..............................................65 4-6 ITO 薄膜之分析.......................................................66 4-6-1 ITO 薄膜成長條件的探討.......................................66 4-7熱處理對ITO薄膜性質之研究............................................69 4-7-1 XRD 繞射分析.................................................69 4-7-2 SEM表面型態觀察................................................69 4-7-3 AFM 表面粗糙度探討...........................................70 4-8 ITO薄膜光電性質分析.......................................................71 4-8-1薄膜電性分析....................................................71 4-8-2薄膜光學性質分析...................................................73 4-8-3 ITO/polyimide薄膜外觀 .............................................74 第五章 結論.......................................................98 參考文獻...........................................................99 自述.............................................................................................................105

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