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研究生： 吳宗哲
Tsung-che Wu
論文名稱： 透明的中孔二氧化矽塊材
Transparent Mesoporous Silica Monoliths
指導教授： 蔣孝澈
Anthony S.T. Chiang
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： 95
語文別： 中文
論文頁數： 67
中文關鍵詞： 中孔塊材 、共熔物 、離子液體 、中孔 、透明的 、二氧化矽 、塊材
外文關鍵詞： ionic liquid, silica, Mesoporous Monoliths, Monoliths, eutectic, Mesopore, Transparent
相關次數： 點閱：12  下載：0 
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    • 我們使用TEOS當我們溶膠的前趨物，共熔物（1choline chloride：2尿素）或乙二醇則當模板，在酸性條件下用溶-凝膠法在常壓下合成透明的二氧化矽乾膠。在適當的老化反應、常壓乾燥、煅燒程序後，我們可合成出即使在550oC移除有機物後，還不會發生破裂，而且保持透明性的二氧化矽塊材。所得之產物經過熱重損失和紅外線光譜、氮氣恆溫吸附、掃瞄式電子顯微鏡等分析。而煅燒過的塊材以紫外－可見光光譜測量穿透度。合成出來的透明多孔二氧化矽塊材，具有450~700 m2/g的表面積，有2~14 nm的孔隙分佈，和0.2~1.4 cm3/g的孔體積，而3.9 mm厚的二氧化矽塊材，在600 nm波長的穿透度有達80%。

    Transparent silica xerogels were synthesized by the sol-gel process under atmospheric conditions, using tetraethoxysilane(TEOS) as the alkoxide precursor and eutectic (1Choline Chloride : 2Urea) or EG as a template, under acid conditions. With proper aging, atmospheric drying and calcination procedures, we had successfully synthesized silica monoliths that remain transparent and crack free after calcination at 550oC. The resulting gels were characterized by thermogravimetric analysis, infrared spectroscopy and scanning electron microscopy. The transmittance of calcined monoliths were analyzed using ultraviolet-visible spectroscopy. Nitrogen adsorption isotherms was used for surface area and pore volume determination. The synthesized transparent mesoporous silica monoliths exhibit BET surface areas of 450-700 m2/g, a BJH pore diameter of 2-14 nm, and a pore volume of 0.2-1.4 cm3/g. The transmittance of an 3.9 mm thick silica monoliths can be as high as 80% @600 nm.

    摘 要 i Abstract ii 誌 謝 iii 目 錄 v 圖目錄 vii 表目錄 ix 第一部份：透明的二氧化矽導電塊材 第一章：緒論 1 1.1 前言 1 1.2 離子液體的簡介 1 1.3 文獻回顧 3 1.4 研究方向與動機 3 第二章：實驗部份 5 2.1 實驗藥品 5 2.2 實驗儀器 5 2.3 實驗流程 6 2.3.1 合成低溫共熔物（eutectic mixture[1]） 6 2.3.2 合成透明溶膠 6 2.3.3 膠的老化與乾燥 6 第三章：結果與討論 8 3.1 形成均相透明溶膠的條件 8 3.2 形成透明溼膠的條件 8 3.2.1 醇矽比對膠透明程度的影響 8 3.2.2 水矽比對膠透明程度的影響 9 3.2.3 離矽比對膠透明程度的影響 11 3.3 含有eutectic的溶膠，鍍膜的測試 12 3.4 膠浸泡在eutectic中，在高溫中反應． 12 3.5 膠的導電度測試 13 第四章：結論與建議 16 參考文獻 17 第二部份：透明的中孔二氧化矽塊材 第一章：緒論 18 1.1 中孔材料的簡介 18 1.2 中孔材料的應用 19 1.3 中孔塊材的文獻回顧 20 1.4 溶凝膠（sol-gel）法合成塊材 23 1.5研究動機與方向 25 1.5.1均一的孔徑分佈 25 1.5.2移除有機物後塊材不會破裂 25 1.5.3透明塊材 26 第二章：實驗部份 27 2.1 實驗藥品 27 2.2 實驗儀器 28 第三章：使用eutectic合成透明的中孔二氧化矽塊材 29 3.1 前言 29 3.2 合成透明塊材的實驗流程 29 3.3 特微化包覆eutectic的膠 30 3.3.1 TGA分析 30 3.3.2 FT-IR分析 31 3.3.3 X-ray繞射分析 32 3.3.4 UV-visible分析 34 3.3.5孔隙分析 36 3.3.5.1 eutectic的量對孔隙分佈的影響 36 3.3.5.2膠浸泡在eutectic中，對孔隙分佈造成的影響 38 3.3.5.3不同溫度下老化反應，對孔隙分佈的影響 40 3.4 移除有機物後，塊材不會破裂的方法與條件 42 3.4.1 使用不同溶劑替換，減少揮發時產生界面張力 42 3.4.2 使用矽烷將塊材表面改成疏水性 45 3.4.3 塊材浸泡在乙二醇中，減少老化反應時的破裂 47 3.4.4 移除有機物升溫條件的實驗 48 3.5 其它實驗的測試 52 3.5.1摻雜金屬到二氧化矽溶膠中 52 第四章：使用乙二醇合成透明的中孔二氧化矽塊材 54 4.1 前言 54 4.2 合成透明塊材的實驗流程 54 4.3 特微化在550oC移走有機物後不會破裂的塊材 55 4.3.1 UV-visible分析 56 4.3.2 孔隙分析 57 4.3.3 SEM分析 59 4.4 拉長塊材的反應時間 59 第五章：結論與建議 62 參考文獻 65

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