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研究生: 郭忠倫
Kuo, Chung-lun
論文名稱: 氧化鋁粒徑尺寸與晶型對表面反應性的影響
Particle size and morphology effects on surface reactivity of alumina
指導教授: 王紀
Wang, Chi
學位類別: 碩士
Master
系所名稱: 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年: 2008
畢業學年度: 96
語文別: 中文
論文頁數: 92
中文關鍵詞: 氧化鋁晶型矽烷耦合劑
外文關鍵詞: alumina, morphology, silane coupling agent
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  • 本研究將各種不同晶型與直徑的氧化鋁粒子(Alumina, Al2O3)和Methacryloxypropyltrimethoxysilane (MPS)進行反應,研究氧化鋁不同晶型(alpha與gamma氧化鋁)和直徑(0.08~25um)對矽烷耦合劑的反應性。
    FTIR結果顯示酸洗或鹼洗均無法在一定時間(16小時)內,增加微米級alpha-Al2O3表面OH基披覆量。奈米等級的alpha-Al2O3,由於表面積增加,與MPS間有較佳的反應性。而gamma-Al2O3表面有明顯較多的OH基批覆量,對矽烷耦合劑間的反應性最好。
    固態NMR結果顯示gamma-Al2O3與MPS間可產生Si-O-Al鍵結。利用TGA分析可知當反應系統中的MPS/gamma-Al2O3重量比超過0.86時,反應於gamma-Al2O3上的MPS比例便不會隨著MPS添加量的增加而增加,而最高反應量約為0.12 g MPS/g gamma-Al2O3。FT-IR結果顯示MPS在230oC恆溫5分鐘後,已產生明顯的裂解。

    In this research, we used several kinds of Al2O3 particles with different particle sizes or crystalline morphology to react with methacryloxypropyltrimethoxysilane (MPS). In an tempt to understand the reactivity of Al2O3 particles with MPS.

    FT-IR results showed that neither acid nor base treatment did not produce OH group on the surface of micrometer-sized alpha-Al2O3 particles. The nanometer-sized alpha-Al2O3 particles had a slightly better reactivity with MPS due to the possession of a larger surface area. The gamma-Al2O3 particles had much more OH groups on surface than alpha-Al2O3 (or theta-Al2O3), and thus resulted in a better reactivity with MPS.

    Solid-state NMR results showed the presence of Si-O-Al bonds between MPS and the gamma-Al2O3 particles after reaction. TGA results showed that the amount of grafted MPS did not increase when the weight ratio of MPS to gamma-Al2O3 in reaction system is over 0.86. The maximum amount of grafted MPS is about 0.12 g MPS/g gamma-Al2O3. MPS was apparently degraded after being held at 230oC for 5 min.

    中文摘要………………………………………………………………… i Abstract…………………………………………………………………… ii 目錄……………………………………………………………………… iii 表目錄…………………………………………………………………… v 圖目錄…………………………………………………………………… vi 符號……………………………………………………………………… ix 一、前言……………………………………………………………….... 1 二、簡介……………..………………………………………………….. 2 三、文獻回顧…………………………………………………………… 3 3-1 氧化鋁簡介……………………………………………… 3 3-2 活性氧化鋁簡介……………………………………….... 3 3-3 alpha-Al2O3的表面性質……………………………………... 4 3-4 gamma-Al2O3的表面性質……………………………………... 5 3-5 矽烷耦合劑和氧化鋁反應原理………………………… 5 3-6 MPS的水解及縮合特性………………………………… 6 3-7 以矽烷耦合劑將Al2O3表面改質之應用……………... 7 四、實驗………………………………………………………………… 20 4-1 實驗藥品………………………………………………… 20 4-2 實驗儀器………………………………………………… 21 4-3 實驗步驟………………………………………………… 23 4-3-1 氧化鋁酸洗或鹼洗…………….………………. 23 4-3-2 以MPS將氧化鋁進行表面改質..…………….. 23 4-3-3 廣角X光繞射儀 (WAXD)……………………. 24 4-3-4 掃描式電子顯微鏡 (SEM)……………………. 24 4-3-5 穿透式電子顯微鏡 (TEM)……………………. 24 4-3-6 傅立葉轉換紅外線光譜儀 (FT-IR)…………… 24 4-3-7 固態核磁共振光譜儀 (solid-state NMR)……... 25 4-3-8 熱重分析儀 (TGA)……………………………. 25 4-3-9 MPS耐熱度的測試……………………………. 25 4-3-10 gamma-Al2O3/聚碳酸酯複材的混鍊…………………. 25 4-3-11 聚碳酸酯的流變性質量測…………………….. 26 4-3-12 gamma-Al2O3/聚碳酸酯複材的機械性質量測 26 五、結果與討論………………………………………………………… 28 5-1 氧化鋁特徵鑑定………………………………………… 28 5-1-1 Al2O3晶型的鑑定……………………………… 28 5-1-2 Al2O3粒徑大小與表面形態的觀測…………… 28 5-1-3 表面官能基鑑定……………………………….. 29 5-2 以酸洗或鹼洗方式對氧化鋁進行表面處理…………… 29 5-3 各種氧化鋁與MPS的反應性…………………………... 30 5-3-1 MPS的水解……………………………………. 30 5-3-2 不同尺寸的alpha-Al2O3與MPS的反應…………... 30 5-3-3 不同晶型Al2O3與MPS反應性的差異………. 31 5-4 矽烷耦合劑與氧化鋁的鍵結鑑定……………………… 32 5-5 矽烷耦合劑於氧化鋁表面披覆量……………………… 32 5-6 矽烷耦合劑的耐熱性…………………………………… 33 5-7 聚碳酸酯的流變性質…………………………………… 34 5-8 gamma-Al2O3/聚碳酸酯複材性質……………………………... 36 六、結論………………………………………………………………… 88 七、參考文獻…………………………………………………………… 89 八、自述………………………………………………………………… 92

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