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研究生:徐文傑
研究生(外文):WEN-CHIEH HSU
論文名稱:以溶膠–凝膠法製備介孔氧化鋁
論文名稱(外文):Synthesis of Mesoporous Al2O3 by Sol-Gel Method
指導教授:張莉毓
指導教授(外文):Lay Gaik Teoh
學位類別:碩士
校院名稱:國立屏東科技大學
系所名稱:機械工程系所
學門:工程學門
學類:機械工程學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:58
中文關鍵詞:溶膠–凝膠法介孔材料界面活性劑模板劑
外文關鍵詞:sol-gel methodmesoporous materialssurfactantstemplate
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氧化鋁在工業化學上是相當重要的,主要應用作為陶瓷、研磨劑、吸附、催化劑和催化劑載體等。而自組織介孔氧化鋁在商業應用上尤其是催化劑有極高的潛力。介孔氧化鋁相較於一般奈米材料,具有孔洞尺寸大小均勻、比表面積大的特性,可使得材料的性質大為提升,因此近年來已成為重要的研究課題。
在此篇論文中,以三嵌段兩性共聚物F68為界面活性劑模板,硝酸鋁為鋁源,以溶膠-凝膠法合成介孔氧化鋁。以煆燒溫度和二氧化鈰含量的改變探討對合成介孔氧化鋁結構所造成之影響。並以XRD,SAXS,TEM和氮氣吸附/脫附曲線分析其微結構與比表面積。
實驗結果顯示經煆燒溫度800 ℃時由XRD分析得知晶體結構為立方晶體,為γ- Al2O3。觀察煆燒溫度500 ℃的TEM繞射圖,由圖中發現,應為蟲狀孔洞結構,且介孔形態明顯。另外觀察其氮氣吸附/脫附曲線圖與孔徑分佈圖,由圖中可明顯觀察到type Ⅳ 之遲滯曲線,表示產物中具有介孔結構。於實驗中加入硝酸亞鈰,以BET分析,發現其500~800 ℃之吸附/脫附曲線近乎重疊,可維持一較穩定之吸附/脫附曲線,亦即增加其熱穩定性。當煆燒溫度500 °C,硝酸鈰添加量為1.5 g時,其比表面積為87.69 m2/g,平均孔徑147.7 Å。當煆燒溫度升至800 °C時,而其比表面積為71.12 m2/g,則平均孔徑為140.01 Å。
關鍵字:溶膠–凝膠法、介孔材料、界面活性劑、模板劑

Al2O3 is an important element industrial chemistry that has applied widely as adsorbents, ceramics ,abrasives, catalysts and catalyst supports, ext. Especially organized mesoporous alumina has a high potential on commercial applications in catalysis. Mesostructured alumina compares with general nanometer materials which has the character of tailor pore structures and high surface areas .Thus ,it has become an important research study in recent years.
First, in this study,organized mesoporous alumina is synthesized by the sol-gel process method with nitrate alumina as source of alumina, organic surfactant triblock copolymer F68 as template. Second, the influence of various conditions on the structure of organized mesoporous alumina was discussed. Finally, by XRD, BET, SAXS, SEM, TEM and N2 adsorption-desorption isotherms, we analyzed the microstructure and specific surface area.
The results showed that using triblock copolymer as the template and calcined above 800 ℃, mesoporous γ-Al2O3 with the cubic structure was obtained by XRD analysis. Observing the TEM pattern of the mesoporous Al2O3 calcined at 500 ℃, we found it should be the structure of wormhole-like mesoporous Al2O3,and the mesoporous structure was decidedly. According to the nitrogen adsorption/desorption isotherms of the mesoporous Al2O3 ,the shape of type Ⅳ lagged curve was observed. It also represented the adduct having mesoporous structure. Analyzing from BET and BJH, we found the temperature at 500~800 ℃ was closely overlap when adding Ce(NO3)3 • 6H2O in the experiment. It can keep the N2 adsorption-desorption isotherms curves stability. That is to say adding its heat temperature stability. When adding Ce(NO3)3 to 1.5 g and calcined at 500 ℃, the mesoporous Al2O3 had a specific surface area of 87.69 m2/g and the average pore size of 147.7 Å. However, as the calcining temperature increasing to 800 ℃, the specific surface area of mesoporous Al2O3 became to 71.1 m2/g and the pore volume was 140.01 Å.




Keywords : sol-gel method, mesoporous materials, surfactants,template

目錄
摘要 I
ABSTRACT II
謝誌 IV
目錄 V
表目錄 VI
圖目錄 VII
第1章 緒論 1
1.1前言 1
1.2介孔材料 1
1.3研究動機與目的 7
第2章 理論基礎 9
2.1 界面活性劑簡介 9
2.2 微胞的形成 14
2.3 界面活性劑分子聚集體之結構 17
2.4 介孔材料之合成與分析 20
2.5氧化鋁基本物理性質 24
2.6 氧化鋁之製備方法 25
2.7 溶膠-凝膠法 (SOL-GEL) 25
第3章 實驗方法與步驟 31
3.1 化學藥品 31
3.2 介孔氧化鋁之合成步驟: 31
3.3 製程參數 33
3.4 材料分析 33
第4章 結果與討論 37
4.1三嵌段兩性共聚物F68添加量和煆燒溫度對合成介孔氧化鋁之影響 37
XRD分析 37
小角度X-ray 散射分析 38
TEM分析 41
氮氣吸附/脫附曲線分析 41
4.2添加硝酸亞鈰對合成介孔氧化鋁之影響 46
XRD 分析 46
TEM 分析 48
氮氣吸附/脫附曲線分析 48
第5章 結論 51
參考文獻 53
作者簡介 59


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