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研究生: 張詠勛
Yung-Hsun Chang
論文名稱: 孔洞碳材與碳包覆磁性奈米粒子的製備與鑑定
Preparation and Characterization of Porous Carbon Materials and Carbon-Coated Magnetic Nanoparticles
指導教授: 楊家銘
Chia-Ming Yang
口試委員:
學位類別: 碩士
Master
系所名稱: 理學院 - 化學系
Department of Chemistry
論文出版年: 2007
畢業學年度: 95
語文別: 中文
論文頁數: 109
中文關鍵詞: 中孔洞碳材磁性奈米粒子
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  • 本論文主要分為三大部分:第一部分為利用中孔洞SBA-15二氧化矽當作模板,以蔗糖或夫喃醇為前驅物合成出具棒狀實心的中孔洞CMK-3碳材以及具中空管狀的中孔洞CMK-5碳材,我們對這些材料的成分與結構均以X光粉末繞射儀、氮氣物理吸脫附儀、熱分析儀與穿透式電子顯微鏡作鑑定與分析,並對其製備條件進行探討並找到最佳合成條件。第二部分是利用階層性孔洞二氧化矽塊材當作模板,以酚醛樹酯為碳前驅物製備同時具有微米尺度巨孔與奈米中孔結構的孔洞碳塊材,我們對其階層性孔洞形貌與性質以氮氣物理吸脫附儀與掃描式電子顯微鏡進行分析與鑑定。第三部分是利用具羧基之功能化中孔洞SBA-15二氧化矽當作模板,合成出具有碳包覆之磁性奈米金屬粒子,其磁性經超導量子干涉儀進行分析,我們更進一步用硝酸將包覆於奈米金屬外的碳層表面氧化成羧基,並以傅氏轉換紅外光譜儀作成分鑑定。這些碳包覆磁性奈米金屬粒子可用來嫁接不同的官能基或其他物質於碳表面,未來將研究其在生化醫療方面的應用。


    The thesis is divided into three parts. In the first part, mesoporous carbon materials with rod-like morphology, CMK-3, and those with tube-like morphology, CMK-5, have been synthesized by template synthesis using mesoporous SBA-15 silica as a hard template and sucrose or furfuryl alcohol as carbon precursors. The composition and the structure of these carbon materials were characterized by X-ray diffraction, nitrogen physisorption analysis, thermal analysis and transmission electron microscopy. Based on the data, the synthesis conditions have also been optimized. In the second part, monolithic carbon materials with hierarchically bimodal meso- and macroporosity have been prepared by using a hierarchically meso/macroporous silica monolith as a hard template and phenolic resin as the carbon source. The pore structure of the carbon monoliths were investigated by nitrogen physisorption analysis and scanning electron microsopy. In the third part, carbon-coated magnetic metal nanoparticles have been synthesized by using the carboxylate-functionalized mesoporous SBA-15 silica as a hard template. The magnetic properties of these nanoparticles were studied by Superconducting Quantum Interference Device. In addition, the outer carbon layers on these nanoparticles were oxidized to bear carboxylate groups by the treatment with nitric acid, and Fourier-transformed infrared spectroscopy was applied for characterizations. With these carboxylate groups, the carbon-coated magnetic nanoparticles can be further grafted with a variety of functional groups and other molecules for biomedical applications in the future.

    中文摘要Ⅰ 英文摘要Ⅱ 目錄Ⅲ 圖目錄Ⅵ 表目錄ⅩⅠ 第一章 緒論 1 1-1 孔洞材料簡介 1 1-2 界面活性劑的膠體化學 2 1-3 中孔洞二氧化矽MCM-41的形成機制 5 1-4 中孔洞二氧化矽SBA-15 8 1-5 具階層孔洞的二氧化矽塊材 10 1-6 孔洞碳材的合成 12 1-6-1 中孔洞碳材 13 1-6-2 階層性孔洞碳塊材 16 1-7 磁性奈米粒子簡介與應用 18 1-7-1 磁性的分類 18 1-7-2 磁性奈米粒子的保護與穩定化 19 1-7-3 碳包覆之磁性奈米粒子 20 1-7-4 磁性奈米粒子的應用 20 1-8 研究動機與目的 21 第二章 實驗部分 22 2-1 實驗藥品 22 2-2 模板孔洞材料合成 23 2-2-1 SBA-15的合成 23 2-2-2 階層性孔洞二氧化矽塊材的合成 24 2-3 模板法合成孔洞碳 26 2-3-1 CMK-3之合成方法 26 2-3-1-1 以蔗糖為碳之前驅物 26 2-3-1-2 以夫喃醇為碳之前驅物 26 2-3-2 CMK-5之合成方法 27 2-3-2-1 以氯化鋁當催化劑合成CMK-5 27 2-3-2-2 以草酸當催化劑合成CMK-5 28 2-3-3 階層性孔洞碳塊材的合成 28 2-4 磁性奈米粒子之合成 29 2-4-1 合成具有羧基SBA-15的模板 29 2-4-2 磁性金屬/碳核殼奈米粒子的合成 30 2-4-3 奈米粒子外層碳的氧化 30 2-5 實驗鑑定儀器 31 2-5-1 X光粉末繞射儀 31 2-5-2 氮氣等溫吸脫附分析儀 33 2-5-3 穿透式電子顯微鏡 39 2-5-4 掃描式電子顯微鏡 41 2-5-5 熱重量分析 42 2-5-6 拉曼光譜儀 43 2-5-7 傅立葉轉換紅外光譜儀 44 2-5-8 超導量子干涉儀 45 第三章 結果與討論 47 3-1 中孔洞碳材CMK-3的合成與鑑定 47 3-2 中孔洞碳材CMK-5的合成與鑑定 57 3-3 階層性孔洞碳塊材 79 3-4 具羧基功能化SBA-15模板合成磁性奈米粒子 91 第四章 結論 102 第五章 參考文獻 104

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