矽偶合劑存在下環氧樹脂/二氧化矽混成體之研究

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研究生：	林汝潔 Ru-Jei Lin
論文名稱：	矽偶合劑存在下環氧樹脂/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：	94
語文別：	中文
論文頁數：	85
中文關鍵詞：	環氧樹脂、二氧化矽
外文關鍵詞：	Silica, epoxy
相關次數：	點閱：13 下載：0
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本研究利用溶膠-凝膠法（sol-gel process）製備環氧樹脂（Epoxy）與二氧化矽（SiO2）有機無機混成體。首先，將無機系統中的四乙氧基矽烷、矽偶合劑、水、乙醇先進行初步水解反應生成前置物，再將此前置物與有機系統環氧樹脂均勻混合，加熱硬化即可製得環氧樹脂/二氧化矽有機無機混成體，並將所製備的有機無機混成體利用微差掃瞄熱分析儀（DSC）、熱重分析儀（TGA）、掃描式電子顯微鏡（SEM）以及霍氏轉換紅外線光譜儀（FTIR）等儀器進行分析。結果顯示，在無機系統中添加適量矽偶合劑（KBM403）可以有效地提高混成體的耐熱性質，因為矽偶合劑KBM403一端帶有環氧官能基可與有機環氧樹脂進行開環反應產生架橋，另一端矽氧烷官能基同時可與四乙氧基矽烷、水進行水解縮合反應產生-O-Si-O-共價鍵結，能有效地在有機無機相間提供部分的共價鍵結，但是添加過量時會降低架橋密度反而會使耐熱性質下降，由TGA與DSC的結果可以發現添加5mole%的KBM403之混成體耐熱性質最佳。除此之外，由TGA與DSC的結果可以得知，混成體隨著無機物添加量的增加，其IPDT值（Integral procedure decomposition temperature）、Tg（玻璃轉化溫度）、Tdmax（最大熱裂解速率之溫度）都有提升的趨勢，也就表示無機物的添加有效地提高混成體的耐熱性質與熱穩定性。

目錄......................................................................................................I
表目錄.................................................................................................III
圖目錄..................................................................................................IV
第一章 緒論..........................................................................................1
第二章 實驗........................................................................................13
2-1 實驗藥品...............................................................................14
2-2 實驗儀器...............................................................................15
2-3 環氧樹脂/二氧化矽混成材料之製備..................................15
2-4環氧樹脂/二氧化矽混成材料之測試...................................16
2-4-1 熱重損失測試................................................................16
2-4-2恆溫式DSC測試...........................................................17
2-4-3 玻璃轉移溫度測試.......................................................17
2-4-4 紅外線光譜分析...........................................................17
2-4-5 SEM測試.......................................................................17
第三章 結果與討論............................................................................18
3-1 環氧樹脂與有機無機混成材料的反應溫度分析.................19
3-2環氧樹脂/二氧化矽混成材料的製備條件....................... .....23
3-2-1 無機前置物製備條件對混成材料的影響............... ....23
I
3-2-2 反應時間對混成材料的影響........................................28
3-2-3矽偶合劑種類對混成材料的影響.................................32
3-3 環氧樹脂/二氧化矽混成材料的性質分析............................38
3-3-1 矽偶合劑添加量對混成材料性質的影響....................38
3-3-2 無機添加量對混成材料性質的影響............................53
3-4環氧樹脂/二氧化矽混成材料定性分析.................................66
3-4-1 FTIR分析.......................................................................66
3-4-2 SEM分析.......................................................................68
第四章 結論........................................................................................71
參考文獻..............................................................................................73 II
表目錄
Table 3-1 Preparation conditions of epoxy and epoxy/SiO2 hybrid materials……………………………………………………….…..20
Table 3-2 preparation conditions and appearance of epoxy and epoxy/SiO2 hybrid materials…………………………………….…26
Table 3-3 preparation conditions and appearance of epoxy/SiO2 hybrid materials………………………………...…………………………30
Table 3-4 preparation conditions and appearance of epoxy and epoxy/SiO2 hybrid materials……………………………………….35
Table 3-5 preparation conditions and appearance of epoxy/SiO2 hybrid materials…………………………………………………………...42
Table 3-6 The thermal characteristics of various Epoxy/SiO2 hybrid materials…………………………………………………….……..45
Table 3-7 preparation conditions and glass transition temperatute of epoxy/SiO2 hybrid materials……………………………………....50
Table 3-8 preparation conditions and appearance of epoxy and epoxy/SiO2 hybrid materials……………………………………......56
Table 3-9 The thermal characteristics of Epoxy and Epoxy/SiO2 hybrid materials……………………………………………………….…..59
III
圖目錄
Fig 1-1 The structure of DGEBA…………….…………………....…...3
Fig 1-2 Effects of PH in aqueous silica sol-gel system............................10
Fig 3-1 DSC curves of epoxy and epoxy/SiO2 hybrid material at 800C...21
Fig 3-2 DSC curves of epoxy and epoxy/SiO2 hybrid material at 1700C.22
Fig 3-3 the TGA curves of epoxy(A0) and epoxy/ SiO2 hybrids materials (P1T60、P2T60、P1T30、P2T30)…………………………………..27
Fig 3-4 The TGA curves of epoxy/ SiO2 hybrids materials (m15、m30、h1、h2、h3)………………………………………………………….31
Fig 3-5 The structure of coupling agents………………………………..36
Fig 3-6 TGA curves of epoxy(E0) and different epoxy/SiO2 hybrids (M403、E402、M603、M13、M22)………………………………..37
Fig 3-7 TGA curves of different epoxy/SiO2 hybrid materials(M5、M10、M20、M40、M80、M100) under N2………………………………..43
Fig 3-8 TGA curves of different epoxy/SiO2 hybrid materials(M5、M10、M20、M40、M80、M100) under air………………………….….44
Fig 3-9 Effect of KBM403 content in Epoxy/SiO2 hybrid materials on IPDT under nitrogen and air conditions…………………………...46
Fig 3-10 DTG curves of different epoxy/SiO2 hybrid（M5、M10、M20、M40、M80、M100）under N2……………………………………..47
Fig 3-11 DTG curves of different epoxy/SiO2 hybrid（M5、M10、M20、
IV
M40、M80、M100）under air………………………….……..48
Fig 3-12 Effect of KBM403 content in Epoxy/SiO2 hybrid materials On Tdmax……………………………….…………………….……...49
Fig 3-13 DSC curves of different epoxy/SiO2 hybrids （M5、M10、M20、M40、M80、M100）.............51
Fig 3-14 Effect of KBM403 content of Epoxy/SiO2 hybrid materials on Tg………………………….……………………………………52
Fig 3-15 TGA curves of epoxy(S0) and different epoxy/SiO2 hybrids (S2、S5、S10) under air……………….………………………57
Fig 3-16 TGA curves of epoxy(S0) and different epoxy/SiO2 hybrid (S2、S5、S10) under N2…………………………….……………….58
Fig 3-17 Effect of Silica content of Epoxy and Epoxy/SiO2 hybrid materials on IPDT under nitrogen and air conditions……….….60
Fig 3-18 DTG curves of epoxy(S0) and different epoxy/SiO2 hybrid (S2、S5、S10) under air…………………………….…………61
Fig 3-19 DTG curves of epoxy(S0) and different epoxy/SiO2 hybrid (S2、S5、S10) under N2………………………………….……62
Fig 3-20 Effect of Silica content of Epoxy and Epoxy/SiO2 hybrid materials on Tdmax ………………….…………………………..63
Fig 3-21 DSC curves of epoxy(S0) and different epoxy/SiO2 hybrids (S2、S5、S10)…………………………………………………64
Fig 3-22 Effect of Silica content of Epoxy and Epoxy/SiO2 hybrid materials on Tg…………………………………………………65
V
Fig 3-23 FTIR spectra of （a）pure Epoxy （b）Epoxy/SiO2 （10%）（c）SiO2.........................................................................................67
Fig 3-24 SEM of epoxy/SiO2 hybrid materials without KBM403….......69 Fig 3-25 SEM of epoxy/SiO2 hybrid materials with 5mole％KBM403..70
VI

                                

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