無機多孔質材料因其高強度與耐熱性廣為各領域所應用，而近年發展迅速的溶膠凝膠法由於能以化學法製作出擁有奈米等級微孔的無機多孔質材料而深受各界重視，其可利用作生物、觸媒、過濾及吸附的載體或母材等等應用。本研究的目的便是要建立利用溶膠凝膠法製作二氧化矽多孔質塊材的製程技術基礎與找出各項製程參數的影響趨勢，然後再加入乾燥控制化學添加劑(DCCA)以測試其效果。最後藉由孔隙分析瞭解實驗獲得的樣本之孔隙大小、孔徑分佈與表面積的資料，藉以找出可以製作具有奈米級孔徑、集中的孔徑分佈與大表面積之載體的加工條件，以作為未來開發功能性材料的參考。研究結果顯示，莫耳水量多、酸催化、低溫反應、低轉速及較短攪拌時間有獲得較小粒徑的趨勢，而DCCA的添加明顯地縮短結膠時間、減少裂痕與增加成形性。本研究獲得的樣本平均孔隙大小約6nm、孔徑分佈集中於4.5nm且表面積為308.6185m2/g。

The sol-gel processing route to advanced glasses and ceramics is a way of manipulating molecular precursors to form bulk oxide materials. The nanoporous bulk oxide materials can be used as filters, catalytic matrices, and sensors.
The purpose of this thesis is using sol-gel method to synthesize silica bulk and to compare the influence of the parameters in this process consist of solvents, catalysis, reaction temperature, stirring speed, and reaction times. Then, the use of drying control chemical additives to avoid fracture and crack formation in the conversion of the wet gel to dry gel is favorable. The pore’s structure changes were studied by BET analysis, which were prepared to be the reference of the future further research.
A sample study is presented here: from the composition chosen, the pore distribution is very well monodispersed and centred on 4.5nm. The average pore diameter is 58.9497 Å and the surface area is 308.6185m2/g.

中文摘要………………………………………………………Ⅰ
英文摘要………………………………………………………Ⅱ
致謝……………………………………………………………Ⅲ
目錄……………………………………………………………Ⅳ
表目錄…………………………………………………………Ⅵ
圖目錄…………………………………………………………Ⅶ
第一章 緒論…………………………………………………1
1.1 研究背景…………………………………………………1
1.2 文獻回顧…………………………………………………2
1.3 研究動機與目的…………………………………………3
1.4 研究方法…………………………………………………4
第二章 溶凝膠法……………………………………………5
2.1 溶凝膠製程………………………………………………5
2.2 溶膠與凝膠………………………………………………6
2.3 水解與縮合………………………………………………7
2.4 以溶凝膠法製作功能性材料之優點……………………8
第三章 溶凝膠法製作塊材實驗……………………………10
3.1 實驗目的…………………………………………………10
3.2 實驗材料與設備…………………………………………10
3.2.1 實驗材料……………………………………………10
3.2.2 實驗藥品……………………………………………12
3.2.3 實驗儀器……………………………………………12
3.3 實驗方法……………………………………………… 13
3.3.1實驗流程….…………………………………………13
3.3.2實驗參數設定…………………………………………13
3.3.3溶膠的配製……………………………………………13
3.3.4樣本製作……………….….…………………………14
3.3.5凝膠之乾燥處理………………………………………14
3.3.6乾膠之高溫熱處理……………………………………14
3.4 實驗過程控制與結果之檢測分析………………………15
3.4.1 熱重量分析…………………………………………15
3.4.2 雷射粒徑分析………………………………………15
3.4.3 收縮分析……………………………………………15
3.4.4 破裂觀察……………………………………………15
3.4.5 孔徑分佈測定………………………………………16
3.4.6 掃瞄式電子顯微鏡觀察……………………………16
第四章 實驗結果與討論…………………………………17
4.1 實驗控制與操作………………………………………17
4.2 熱重量分析……………………………………………18
4.3 溶膠之粒徑分析……………………………………18
4.4 凝膠之乾燥處理………………………………………20
4.5 乾膠燒結………………………………………………22
4.6 孔隙分佈與表面積分析………………………………23
第五章 結論………………………………………………26
參考文獻……………………………………………………28
附表…………………………………………………………35
附圖…………………………………………………………46
附錄…………………………………………………………115

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