矽烷偶合劑接枝之氧化石墨烯及熱脫層氧化石墨烯之合成及探討其對環氧樹脂之聚合固化反應動力、玻璃轉移溫度、X光散射特性、聚合固化樣品微觀型態結構、體積收縮、機械性質、熱傳導及導電性質的影響

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研究生：	林楷洋 Kai-Yang Lin
論文名稱：	矽烷偶合劑接枝之氧化石墨烯及熱脫層氧化石墨烯之合成及探討其對環氧樹脂之聚合固化反應動力、玻璃轉移溫度、X光散射特性、聚合固化樣品微觀型態結構、體積收縮、機械性質、熱傳導及導電性質的影響 Synthesis of silane-grafted graphene oxide (sg-GO) and silane-grafted thermally reduced graphene oxide (sg-TRGO), and their effects on the cure kinetics, glass transition temperatures, X-ray scattering characteristics, cured sample morphologies, volume shrinkage, mechanical properties, and thermal and electrical conductivities for epoxy resins
指導教授：	黃延吉 Yan-Jyi Huang
口試委員:	黃延吉 Yan-Jyi Huang 陳崇賢 Chorng-Shyan Chern 邱文英 Wen-Yen Chiu
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	中文
論文頁數：	145
中文關鍵詞：	氧化石墨烯、熱脫層氧化石墨烯、矽烷接枝之氧化石墨烯、矽烷接枝之熱脫層氧化石墨烯、抗收縮劑、環氧樹脂、聚合固化、聚合固化反應動力、微分掃描熱分析儀、玻璃轉移溫度、動態機械分析儀、X光散射特性、微觀型態結構、掃描式電子顯微鏡、體積收縮、機械性質、熱傳導性質、導電性質
外文關鍵詞：	graphene oxide, silane-grafted graphene oxide, thermally reduced graphene oxide, low-profile additive, epoxy resins, curing, curing kinetics, DSC, glass transition temperature, DMA, X-ray scattering characteristics, SAXS, mechanical properties, SEM, volume shrinkage, thermal conductivity, electrical property
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本研究探討添加氧化石墨烯 (GO)、矽烷接枝氧化石墨 (GPS-GO) 和熱脫層氧化石墨 (TRGO) 對環氧樹脂(epoxy)/4, 4'-二胺基二苯甲烷(DDM)系統的體積收縮、固化反應動力、X光散射特性、機械性質、玻璃轉移溫度、熱傳導性質及導電性質的影響。GO是使用改良的Hummers法合成出，TRGO則是GO在1050℃ 高溫還原，矽烷接枝氧化石墨是用 (3-縮水甘油氧基丙基) 三甲氧基矽烷作改質，並使用廣角度散射儀 (WAXS) 和熱重分析 (TGA) 鑑定，鑑定結果確實成功合成出；加入所合成的特殊添加劑進環氧樹脂/4, 4'-二胺基二苯甲烷系統探討其對體積收縮、機械性質、玻璃轉移溫度、熱傳導性質及導電性質的影響，並用掃描電子顯微鏡(SEM)和穿透式電子顯微鏡 (TEM) 觀測其微觀型態結構並解釋前述所得之結果，最後使用差示掃描量熱儀 (DSC) 和傅立葉遠紅外光譜儀(FTIR)研究其固化反應動力。

The effects of graphene oxide (GO), silane-grafted graphene oxide (sg-GO) , thermally reduced graphene oxide (TRGO) as special additives on the cured sample on the cure kinetics, glass transition temperature, X-ray scattering characteristics, morphology, volume shrinkage characteristics, thermal conductivity and electrical properties of the Epoxy/DDM/Additive ternary system cured after a stepwise isthermal process of 100℃/180℃ were investigated. The thermally reduced graphene oxide (TRGO) was produced by placing graphene oxide (GO) in a high-temperature furnace kept at 1050℃, which was synthesized from natural graphites with average particle size of 75μm by a modified Hummers method. The silane-grafted GO (sg-GO) was synthesized by using the silane coupling agent bearing epoxy functional group, namely, γ-glycidyloxy propyl trimethoxy silane (GPS), as a surface modifier for the surface treatment of GO. Moreover, the reaction kinetics for the Epoxy/DDM/Additive ternary system during the cure was measured by differential scanning calorimetry (DSC) and Fourier Transform Infrared Spectroscopy(FTIR). Finally, based on the Takayanagi mechanical models, the glass transition temperature in each region of the cured samples for Epoxy/DDM/special additive ternary system has been measured by dynamic mechanical analysis (DMA). Finally, the effects of additives synthesized, such as, GO, sg-GO, and TRGO, on the volume shrinkage, mechanical properties, thermal and electrical conductivities for the Epoxy/DDM/Additive ternary systems after the cure have also been investigated.

第一章 緒論.......................................................................... 1
第二章  文獻回顧................................................................ 3
2-1 二氧化矽......................................................................... 3
2-2 石墨烯、氧化石墨與熱脫層氧化石墨................................ 4
2-3 矽烷偶合劑.................................................................. 7
2-4 自由基聚合反應.............................................................. 9
2-5 乙烯基樹脂............................................................... 11
2-6 環氧樹脂....................................................................... 11
第三章 實驗方法與設備..................................................... 13
3-1 實驗原料.................................................................... 13
3-2 實驗藥品................................................................... 14
3-3 實驗耗材和儀器設備.................................................... 18
3-4 實驗步驟...................................................................... 26
3-5 性質測定與分析方法............................................. 36
第四章 結果與討論.................................................................. 41
4-1 二氧化矽合成及鑑定........................................................... 41
4-2 熱重分析鑑定...................................................... 46
4-2-1  SiO2熱重分析鑑定................................................ 46
4-2-2  氧化石墨、熱還原氧化石墨熱重分析鑑定.................................... 48
4-3 小角度X光散射儀鑑定樣品...................................... 49
4-3-1  鑑定石墨、氧化石墨和熱還原氧化石墨........................................ 49
4-3-2  鑑定EPR (n=0.15)/DDM/GO複合材料.......................................... 52
4-3-3  鑑定EPR (n=0.15)/DDM/TRGO-90複合材料............................... 54
4-4 拉曼光譜鑑定石墨、GO、TRGO-30和TRGO-90................................... 55
4-5 體積收縮量測........................................... 56
4-5-1  St/VER (n=2)雙成分系統................................ 56
4-5-2  EPR (n=0.15)/DDM雙成分系統................................... 58
4-5-3  EPR (n=0.15)/DDM/GO三成分系統.............................................. 59
4-5-4  EPR (n=0.15)/DDM/GPS-GO三成分系統..................................... 62
4-5-5  EPR (n=0.15)/DDM/TRGO-90三成分系統.................................... 63
4-6 DSC 量測反應動力........................................... 65
4-6-1  St/VER (n=2) 雙成分系統............................................. 65
4-6-2  不同當量比(ER)之EPR/DDM雙成份系統................................... 66
4-6-3  EPR/DDM/TRGO-90三成份系統.................................................. 71
4-7  AFM量測GO懸浮於DMF後之厚度..................................................... 75
4-8  SEM微觀型態分析.................................... 79
4-8-1  GO和TRGO微觀型態結構........................................................ 79
4-8-2  EPR (n = 0.15)/DDM 雙成份系統............................................... 82
4-8-3  EPR (n = 0.15)/DDM/GO三成份系統.......................................... 83
4-8-4  EPR (n = 0.15)/DDM/GPS-GO...................................... 87
4-8-5  EPR (n = 0.15)/DDM/TRGO-90三成份系統................................ 90
4- 9  TEM微觀型態分析.................................................... 94
4-9-1  EPR/DDM雙成份系統..................................... 94
4-9-2  EPR/DDM/TRGO90三成份系統.................................................. 94
4-10  以DMA量測玻璃轉移溫度........................................... 97
4-10-1  EPR/DDM雙成份系統........................................... 97
4-10-2  EPR/DDM/TRGO-90三成份系統............................................. 101
4-11 熱傳導係數的測定.................................................... 105
4-11-1  EPR/DDM雙成份的熱傳導係數.............................................. 105
4-11-2  EPR/DDM/GO三成份的熱傳導係數....................................... 106
4-11-3  EPR/DDM/GPS-GO三成份的熱傳導係數............................... 109
4-11-4  EPR/DDM/TRGO-90三成份的熱傳導係數............................. 111
4-12 導電係數的測定...................................................... 113
4-12-1  EPR/DDM/TRGO-90三成份系統............................................. 113
4-13  FTIR校正曲線測定.............................................. 115
4-13-1  環氧樹脂.............................................. 116
4-13-2  4, 4'-二胺基二苯甲烷(DDM)................................... 119
4-14 FTIR測定反應動力.............................................. 122
4-14-1  EPR/DDM雙成份系統.......................................... 122
4-14-2  EPR/DDM/TRGGO-90三成份系統.......................................... 130
第五章結論........................................................ 133
第六章未來工作................................................. 136
第七章附錄............................................................. 137
7-1 EPR/DDM雙成份系統機械試片................................ 137
7-2 EPR/DDM/GPS-GO三成份系統機械試片......................................... 137
7-3 EPR/DDM雙成份系統機械試片拉伸量測............................................. 138
7-4 EPR/DDM雙成份系統機械試片耐衝擊量測............................................ 141
第八章 參考文獻............................................................... 142
                                

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