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研究生:江政慶
研究生(外文):Jeng-Chin Jiang
論文名稱:利用溶-凝膠法製備二氧化矽/環氧樹脂/酸酐奈米複合材料
論文名稱(外文):Preparation of Silica /Epoxy/Anhydride Nanocomposite by Sol-Gel Process
指導教授:黃永慈
指導教授(外文):Yeong-Tsyr Hwang
學位類別:碩士
校院名稱:南台科技大學
系所名稱:化學工程與材枓工程系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2006
畢業學年度:94
語文別:中文
論文頁數:87
中文關鍵詞:二氧化矽環氧樹脂複合材料
外文關鍵詞:SilicaEpoxyNanocomposite
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中文摘要
本研究在製備出高透明性的環氧樹脂(DGEBA)/硬化劑(MHHPA)與二氧化矽(silica)之奈米有機無機複合材料。其中利用sol-gel的製程,將TEOS經水解、縮合反應製備出奈米級的二氧化矽來導入無色的透明有機系統環氧樹脂中。其在無機水解過程中我們將利用HCl、TSA、MHHPA、CH3COOH等不同觸媒且改變不同製程如溫度、時間、水的含量,來製備出奈米級不同粒徑之silica無機顆粒。
在研究過程中將利用29Si NMR監控無機結構的交聯與SiO2成長,並以FTIR、TEM、SEM 觀測有機/無機複合材料的型態(morphology),以TGA量測此複合材料的耐熱性與所含的silica含量,並研究有機、無機二相反應製程,來尋求控制最後生成物的透
明度、耐濕性、CTE等性能的方法。
結果顯示本研究所製備出之奈米級silica大小約在5~50nm。當以HCl為無機系統中水解的觸媒,其silica容易聚集使複合材料失去透明性,但添加入THF、IPA等溶劑可消除聚集現象,所得之silica粒徑成為奈米級,而使有機無機複合材料仍保持透明性。其silica產量也比以弱酸MHHPA為觸媒來的高。
Abstract
In this study, a highly transparent epoxy, DGEBA (diglycidyl ether of bisphenol-A) and a clear anhydride, 4-methyl hexahydrophthalic anhydride (MHHPA), was cured by a tertiary amine catalyst (C11Z-CN). A sol-gel process was employed to convert tetraethoxysilane into a SiO2 inorganic network, which was interpenetrating with the epoxy organic network. Thermogravimetric analysis (TGA) was used to determine the extent of SiO2 formation, while optical microscope or TEM were used to observe the development of the morphology for this organic-inorganic hybrid. After carefully studied the effect of reaction conditions, several interesting reaction formulations and processes were identified to prepare a transparent epoxy-based organic-inorganic interpenetrating network.
Furthermore, strong acids, HCl, TSA and weak acids, MHHPA, CH3COOH were used separately to catalyze the sol-gel reaction of TEOS. The sol-gel reaction was carefully studied by changing the reaction temperature and the content of H2O.The results showed that the formation of inorganic particle size were in the range of 5~50nm. TEM were used to observe the development of the morphology of silica particles both in the inorganic phase and in the organic-inorganic hybrid. While HCl could produce silica particle quite rapidly, the particle were easily aggregated and resulted in an organic-inorganic hybrid with opaque appearance. By introducing solvent, such as THF or IPA, the particle size was then reduced to nano-scale with very homogeneous dispersion. As for MHHPA, the organic-inorganic hybrid thus prepared is transparent. However, the yield of silica was not as high as that obtained by HCl system.
目錄
致謝…………………………………………………………I
中文摘要……………………………………………………I
英文摘要……………………………………………………III
目錄…………………………………………………………IV
表目錄………………………………………………………IX
圖目錄………………………………………………………X

第一章:緒論………………………………………………1
1.1前言…………………………………………………………1
1.2環氧樹脂簡介………………………………………………3
1.2.1環氧樹脂之硬化(curing)……………………………3
1.2.2環氧樹脂官能基數的表示………………………………7
1.2.3環氧樹脂具有下列特性…………………………………8
1.2.4環氧樹脂之應用…………………………………………9
1.2.5 環氧樹脂相關文獻……………………………………9
1.3 奈米級二氧化矽簡介……………………………………11
1.3.1 奈米粒子簡介…………………………………………11
1.3.2二氧化矽簡介…………………………………………13
1.4溶膠-凝膠法(sol-gel method)簡介……………………14
1.4.1 溶凝膠反應機制…………………………………………15
1.4.2 製程對奈米二氧化矽之影響……………………………16
1.4.3溶凝膠法(sol-gel process)之優缺點………………16
1.4.4溶凝膠技術之應用…………………………………………17
1.4.5溶膠-凝膠法之相關文獻…………………………………17
1.5奈米有機/無機複合材料介紹…………………………………19
1.5.1奈米有機/無機複合材料之優點…………………………20
1.5.2 製備奈米有機/無機複合材料的方法……………………20
1.5.3 有機/無機複合材料相關文獻……………………………22
1.6研究目的…………………………………………………………24

第二章、研究用藥品與儀器…………………………………………26
2.1實驗藥品…………………………………………………………26
2.1.1有機高分子部份……………………………………………26
2.1.2無機部份……………………………………………………27
2.2實驗儀器…………………………………………………………29
2.3分析儀器…………………………………………………………29

第三章:利用sol-gel法製備奈米silica無機物…………………32
3.1探討不同觸媒對Silica之影響………………………………32
3.1.1 目的…………………………………………………………32
3.1.2實驗步驟……………………………………………………32
3.1.3 結果與討論………………………………………………33
3.2探討水含量對Silica生成之影響…………………………43
3.2.1 目的………………………………………………………43
3.2.2實驗步驟……………………………………………………43
3.2.3 結果與討論………………………………………………43
3.3探討溶劑對Silica生成之影響………………………………45
3.3.1目的…………………………………………………………45
3.3.2實驗步驟……………………………………………………45
3.3.3 結果與討論………………………………………………45

第四章:以sol-gel法製備奈米silica/epoxy有機無機複合材料…………51
4.1 探討有機高分子聚合/無機sol-gel反應同時進行製備之複合材料…51
4.1.1研究目的………………………………………………………………51
4.1.2實驗步驟………………………………………………………………51
4.1.3 結果與討論……………………………………………………………52
4.2探討不同酸觸媒影響silica/epoxy 複合材料之Tg之透明度………54
4.2.1研究目的…………………………………………………………………54
4.2.2實驗步驟…………………………………………………………………54
4.2.3 結果與討論………………………………………………………………55
4.3以MHHPA為觸媒探討不同水解系統對複合材料之影響……………………60
4.3.1研究目的…………………………………………………………………60
4.3.2實驗步驟…………………………………………………………………60
4.3.3 結果與討論………………………………………………………61
4.4以MHHPA為觸媒探討水解時間與溫度對複合材料之影響………65
………………………………………………………………………………65
4.4.1研究目的…………………………………………………………65
4.4.2實驗步驟…………………………………………………………65
4.4.3 結果與討論………………………………………………………66
4.5 以MHHPA為觸媒探討水含量不同對複合材料之影響………………68
.
4.5.1研究目的……………………………………………………………68
4.5.2實驗步驟……………………………………………………………68
4.5.3 結果與討論…………………………………………………………69


4.6 以HCl為觸媒探討silica/epoxy複合材料…………………………75
4.6.1研究目的………………………………………………………………75
4.6.2實驗步驟………………………………………………………………75
4.6.3 結果與討論……………………………………………………………76

第五章 總結論…………………………………………………………………81
參考文獻………………………………………………………………………84
自述………………………………………………………………………………87
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