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研究生： 詹佳樺
Chia-Hua Chan
論文名稱： 溶膠-凝膠法製備聚甲基丙烯酸甲酯 / 二氧化矽混成體之研究
指導教授： 陳暉
Hui Chen
口試委員:
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程與材料工程學系
Department of Chemical & Materials Engineering
畢業學年度： 89
語文別： 中文
論文頁數： 100
中文關鍵詞： 四乙氧基矽烷 、混成體 、甲基丙烯酸甲酯 、溶膠-凝膠法 、同時聚合 、前置物
外文關鍵詞： in-situ, TEOS, hybrid, MMA, sol-gel, precurso
相關次數： 點閱：5  下載：0 
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    • 本研究分別利用同時聚合（in-situ）以及前置物（precursor）兩種不同的反應系統，藉由溶膠-凝膠法(sol-gel process)來製備透明之聚甲基丙烯酸甲酯( PMMA)與二氧化矽( SiO2)混成材料。
    在同時聚合法的系統，有機-無機混成材料的製備方法是在酸性環境下，於四乙氧基矽烷（TEOS）與甲基丙烯酸甲酯單體（MMA）、水以及乙醇所組成的反應液中導入偶氮異二丁月青（AIBN）作為起始劑，使得在二氧化矽網狀結構生成的同時也產生聚甲基丙烯酸甲酯高分子。研究結果顯示反應系統中添加適量的酸觸媒以及水有助於透明混成體的生成。實驗所得的產物經由氮氣吸附孔隙儀（ASAP）、凝膠滲透層析儀（GPC）、微差掃描熱分析儀（DSC）和熱重分析儀（TGA）以及掃描式電子顯微鏡（SEM）等儀器分析證實所得的透明聚甲基丙烯酸甲酯與二氧化矽高分子混成材料為奈米程度混成且其熱性質亦有改變。
    在前置物法的系統，先將無機系統中的四乙氧基矽烷、水以及乙醇在酸性環境下進行水解-縮合反應後，再與甲基丙烯酸甲酯單體及偶氮異二丁月青的有機系統進行溶膠-凝膠聚合反應。研究結果顯示，利用前置物法有助於改善同時聚合系統中因為水含量與有機單體之間相溶性不佳而造成產物不透明的相分離情形。實驗所得的產物經由核磁共振儀（NMR）、霍氏轉換紅外光譜儀（FTIR）、微差掃描熱分析儀（DSC）和熱重分析儀（TGA）、凝膠滲透層析儀（GPC）以及掃描式電子顯微鏡（SEM）等儀器分析結果顯示利用此法可得到高有機比例之透明混成體高分子，同時其玻璃轉移溫度隨著產物中矽含量的增加而明顯提升。

    目錄…………………………………………………………………….Ⅰ 表索引………………………………………………………………….Ⅲ 圖索引………………………………………………………………….Ⅴ 第一章 前言……………………………………………………………..1 第二章 實驗…………………………..………………………………..18 2-1 實驗藥品………………………………………………………...…19 2-2 實驗儀器…………………………………………………………...20 2-3 有機-無機混成體之製備………………………………………….21 2-3-1同時聚合法製備有機-無機混成體………………………………21 2-3-2前置物法製備有機-無機混成體…………………………………23 2-4 有機-無機混成體物性測試……………………………………….25 2-4-1 玻璃轉移溫度測試…………………………………………… ..25 2-4-2 熱重量損失測試………………………………………………...25 2-4-3 孔洞體積、表面積與孔徑大小之分析…………………………25 2-4-4 聚甲基丙烯酸甲酯高分子之分子量測定……………………...26 2-4-5 核磁共振光譜測定………………………………………………26 2-4-6 紅外線光譜分析………………………………………………...26 2-4-7 聚甲基丙烯酸甲酯 / 二氧化矽混成體微結構觀察…………..27 第三章 同時聚合法製備聚甲基丙烯酸甲酯/二氧化矽混成體……..28 3-1 有機-無機混成材料之製備實驗參數探討……………………….29 3-1-1 起始劑濃度對有機-無機混成材料的影響……………………..29 3-1-2 系統中溶劑用量對有機-無機混成材料的影響………………..31 3-1-3 pH值對反應系統的影響………………………………………...37 3-1-4 水含量對有機-無機混成材料的影響…………………………..37 3-2 甲基丙烯酸甲酯/二氧化矽混成體熱重損失分析……………..48 3-3 甲基丙烯酸甲酯/二氧化矽混成體玻璃轉移溫度探討………..53 3-4 甲基丙烯酸甲酯/二氧化矽混成體之表面積、孔洞體積及孔徑 大小………………………………………………………………56 3-5甲基丙烯酸甲酯/二氧化矽混成體表面結構分析……………….61 3-6 結論………………………………………………………………..65 第四章 前置物法製備聚甲基丙烯酸甲酯/二氧化矽混成體………..66 4-1 有機-無機混成材料之製備參數探討…………………………….67 4-1-1起始劑濃度對有機-無機混成材料的影響………………………67 4-1-2 pH值對反應系統的影響………………………………………...69 4-1-3水含量對有機-無機混成材料的影響……………………………69 4-2前置物法對四乙氧基矽烷水解的影響……………………………77 4-3 聚甲基丙烯酸甲酯/二氧化矽混成體定性分析…………………..79 4-4有機-無機混成體之聚甲基丙烯酸甲酯分子量探討……………..81 4-5 聚甲基丙烯酸甲酯/二氧化矽混成體熱性質分析………………..85 4-6甲基丙烯酸甲酯/二氧化矽混成體表面結構分析………………...88 4-7 結論………………………………………………………………...91 第五章 總結……………………………………………………………92 參考文獻………………………………………………………………..94

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