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研究生:張料峰
研究生(外文):Chang Liao Feng
論文名稱:不飽和聚醯胺酯/聚矽酸混成材料
論文名稱(外文):On the Synthesis of Unsaturated Polyamide-ester/ Polysilisic Acid Hybird Materials and their Properties
指導教授:許應舉
指導教授(外文):Ying Gev Hsu
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:纖維及高分子工程系
學門:工程學門
學類:紡織工程學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:84
中文關鍵詞:有機-無機混成材料
外文關鍵詞:organic-inorganic hybrid
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本論文旨在合成一不飽合聚醯胺酯(unsaturated polyamide-ester, UPAE),並加入具奈米尺寸之聚矽酸(nano polysilicic acid,nPSA) 顆粒,以製備有機-無機混成材料(organic-inorganic hybrid materials)。論文中先將偏矽酸鈉(sodium metasilicate Na3SiO3)在HCl的存在下先反應形成nPSA,同時亦將nPSA顆粒與3-glycidylpropyl trimethoxylsilane(GPTS)反應成表面含有環氧基之改質nPSA(簡稱M-nPSA)。UPAE與N-N-dimethyl acrylamide(NDMA)混合溶液分別與nPSA及M-nPSA之THF溶液混合均勻後,減壓除去THF,並加入起始劑,使之進行自由基聚合反應,形成兩種結構不同之低收縮性有機-無機混成材料UPAE/NDMA/nPSA及UPAE/NDMA/M-nPSA。此兩種材料分別以FT-IR 、SEM、DSC、DMA等分析混成材料之微細結構、有機-無機成分間之相行為(phase behavior)及其他機械性質,進而瞭解nPSA及M-nPSA對混成材料各性質之影響;另外,混成材料在nPSA及M-nPSA的存在下,硬化時收縮率有下降的趨勢。

The transparent organic-inorganic hybrid materials, UPAE/NDMA/nPSA and UPAE/NDMA/M-nPSA were prepared through free radical polymerization of polysilicic acid (nPSA) and M-nPSA, modified nPSA through the reation of nPSA with 3-glycidylpropyl trimethoxylsilane(GPTS), respectively. The hydroxyl containing UPAE was obtained by the ring-opening reaction of diglycidyl ether of bisphenol (DGEBA) with 1.6-uexamethylene diamine:bissemimaleamide(HBSM) under the catalization of tetrethylammoniumbromide, while nPSA was prepared through hydrolysis and condensation of metasilicate salt. The interfacial behavior, microstructure, thermal, and dynamic properties of UPAE/NDMA/nPSA and UPAE/NDMA/M-nPSA hybrids were compared with each other before and after heat treatment.

中文摘要…………………………………………………..….Ⅰ
英文摘要…………………………………………………..….Ⅱ
誌 謝…………………………………………………..…Ⅲ
目 錄…………………………………………………..…Ⅳ
附圖索引…………………………………………………..….Ⅶ
附表索引…………………………………………………..….Ⅷ
1. 前 言…………………………………………………..…1
2. 文獻回顧………………………………………………..5
2.1 溶膠-凝膠法的研究背景與發展歷史.……………..5
2.2 溶膠-凝膠法在有機-無機混成材料上的應用.……7
2.3 PSA法的研究背景與發展歷史……………..……..12
2.4 PSA法在有機-無機混成材料上的應用…..………13
2.5 低收縮性有機-無機混成材料之製備……..……….14
3. 基本原理..………………………………………………..15
3.1 溶膠-凝膠法的製程及其步驟…………………..…..15
3.2 nPSA法的製程及其步驟…………………………….20
4. 實驗部份……..………………………………………………….22
4.1 實驗藥品………………………………………………………22
4.2 實驗方法………………………………………………….24
4.2.1 奈米nPSA顆粒之合成及粒徑測試………………..24
4.2.2 單體HBSM之合成………………….……………………..27
4.2.3 聚醯胺酯(UPAE)之合成…………………………………...30
4.2.4 混成材料之製備……………………………………………33
4.3 材料之分析與性質測試……………………………………….36
5. 結果與討論………………………….………………...…..40
5.1 有機高分子合成及結構分析………………….……………..40
5.2 奈米nPSA顆粒之粒徑………………………………………41
5.3 混成材料之外觀形態與微細構造…………………….…43
5.3.1 外觀形態….……………..………….……………………..43
5.3.2 微細構造………....……………..………….…………44
5.4 混成材料之相間作用力………………………………..46
5.4.1 相間作用力之測試與分析………………………………46
5.4.2 熱效應研究…...……………………………………………..50
5.4.3 有機-無機相間共價鍵(Si-O-C)的形成……….….54
5.5 混成材料之熱性質試驗…..……………………………………58
5.6 混成材料之物性測試…………..………………………68
5.6.1 混成材料之溶解性測試….….……………………..68
5.6.2 混成材料之動態機械性質分析….………………………71
5.7 混成材料之收縮效應…………..…….…………………….…75
6. 結 論………………………………….…………………….78
7. 參考文獻……………………….…….……………………..80

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