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研究生：	廖美儀 Liao, Mei-Yi
論文名稱：	介尺度奈米金屬氧化物之合成與性質研究 Synthesis and Characterization of metal-based nanomaterials
指導教授：	林弘萍 Lin, Hong-Ping
學位類別：	碩士 Master
系所名稱：	理學院 - 化學系碩士在職專班 Department of Chemistry (on the job class)
論文出版年：	2006
畢業學年度：	94
語文別：	中文
論文頁數：	127
中文關鍵詞：	中孔洞材料、氧化鋁、揮發誘導自組裝、光激發放光、氧化鋅、修飾、有機矽烷、鎳-碳複合材料
外文關鍵詞：	silane, evaporation-induced self-assemble, photoluminescence, ZnO, modification, aluminum oxide, Ni-C hybrid materials, mesoporous
相關次數：	點閱：111 下載：9
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本論文主要分為三大研究主題，第一個主題為製備中孔洞氧化矽材料，並經過表面修飾過程以達到應用的效能。第二個主題是以揮發誘導自組裝程序製備中孔洞金屬氧化物材料。第三個主題是以水熱法彽溫成長六角對稱氧化鋅奈米花(six-fold flower-like ZnO)，此材料能產生綠光之陰極射線發光效應。

第一部分：直接表面修飾有機矽烷於中孔洞氧化矽材料
本研究的目標是發展簡便的反應流程，將各種有機矽烷直接表面修飾於初合成中孔洞氧化矽材料上，此方法有別於一般傳統表面修飾方式，在不需經過高溫煅燒移除界面活性劑，並免除繁瑣的真空除水流程，即可達到高效率表面修飾效果。我們將針對研究結果探討silica-surfactant間作用力對表面修飾的影響。
因為silica-surfactant彼此間作用力，主要取決於初合成中孔洞氧化矽材料的合成條件，中孔洞氧化矽材料合成環境於中性( )以及酸性( )底下，彼此間是以較弱的氫鍵鍵結，所以界面活性劑經silane表面修飾後被移除率幾乎高達100 %，反之當中孔洞氧化矽合成環境於鹼性條件下，silica與界面活性劑彼此間是採較強的靜電吸引力，直接進行表面修飾時，所需跨越的活化能較高，對於界面活性劑拔除能力相對的較差，即使是界面活性劑拔除能力較差，但有機矽烷表面修飾效果仍高達80 %以上。此外，利用改變作用力的想法，於鹼性條件下( )合成的中孔洞氧化矽材料，可先利用酸處理步驟將silica-surfactant間強靜電吸引力轉換成較弱的氫鍵作用形式，或者直接利用反應中會分解HCl的silane進行表面修飾，這些方式都可促使silane表面修飾效果幾乎高達100 %。

第二部分：ㄧ步合成金屬氧化物中孔洞材料
本研究重大突破是在大氣環境下利用揮發誘導自組裝方式，一步驟合成(one-step synthesis)具有高表面積介孔尺度的氧化鋁材料，利用揮發誘導自組裝概念(evaporation-induced self-assembly；EISA)，將溶劑慢慢揮發誘導引發有機高分子-無機硝酸鋁鹽自組裝形成超分子結構，於400℃底下促使金屬氧化物結晶化並移除界面活性劑產生孔洞特性。經穿透式電子顯微鏡(TEM)觀察可看到明顯中孔洞結構，並且由氮氣吸附脫附等溫曲線分析結果得知，中孔洞氧化鋁材料具有高表面積約250-300 m2g-1以及均勻的孔洞大小，實驗結果除了展現高度再現性，也成功利用相似的方式(揮發誘導自組裝)製備出氧化鋯、氧化鈰中孔洞材料和多孔性之磁性碳材(鎳-碳複合材料)。

第三部分：綠光發光體之六角對稱氧化鋅奈米花
本研究利用水熱法合成六角對稱氧化鋅奈米花(six-fold flower-like ZnO)，合成的方式是將硫酸鋅(Zn(SO¬4)•9H2O)與中性界面活性劑P123於1.0 M氨水溶液反應後得到白色沉澱物，經由SEM觀察為平板狀物質，收集沉澱物後在100℃氨水溶液中水熱處理，經水熱反應後得到具有結晶性的氧化鋅材料，由掃描式電子顯微鏡觀察下可發現氧化鋅晶體具有六角對稱，產物的純度經由XRD的判定高達100 %，此外，針對產物的光學特性我們使用光激發光光譜與陰極激發光光譜進行研究，雖然藉由調控加入界面活性劑的種類可改變產物的外型(陽離子型界面活性劑CTAB：放射狀；不加界面活性劑：柱狀)，但其發光特性均是展現高的綠光/紫外光比值強度。

In this thesis, there are three major researching parts: 1. Synthesis and surface modification of the mesoporous silicas. 2. Preparation of mesoporous metal oxides by using evaporation-induced self-assemble (EISA) method. 3. Fabrication of six-fold flower-like ZnO nanoparticles via a simple sol-gel reaction.

Part I: Direct silane-modification of the mesoporous silicas:
A simple surface modification of the mesoporous silicas can be achieved by refluxing the as-synthesized mesoporous silicas in a silane ethanolic solution. Different form the typical silane-grafting methods; the time- and energy-consuming procedures including calcination and water-preventing can be avoided and hence the surface of the mesopores was efficiently modified with different silanes.
The extent of silane-modification is dependent on the interaction strength between silica and surfactant. Due to the relatively weak hydrogen-bonding interaction in the acid-made mesoporous silicas (S+X-I0, S0I0), the surfactant was almost competently replaced by the chemical-bonding silanes. In contrast, the extent of surface modification for the base-made mesoporous silica with strong electrostatic interaction of the surfactant and silica (S+I-) is reduced to 80 %. Accordingly, stronger silica-surfactant interactions lead to higher activation energy for the silane modification. In order to achieve a entire surface-modification for the based-made mesoporous silica, a treatment in the highly acidic solution or using a silane with the release of HCl was performed.

Part II. Preparation of mesoporous metal oxides by using one-step EISA method:
Under ambient condition, the mesoporous aluminum oxide can be prepared via a simple EISA method. In the EISA synthetic method, the solvent of the solution of copolymer surfactant and aluminum nitrate salt was spontaneously evaporated to the environment, and the surfactant and aluminum salts was self-assembly into the mesostructures. After calcination at 400 oC, the mesoporous aluminum oxide was obtained. The mesostructures and porosity of the mesoporous aluminum oxide was characterized by TEM observation, N2 adsorption-desorption isotherm. The EISA method can be applied to prepare other mesoporous metal oxides such as ZrO2, CeO2 and Ni-C hybrid materials.

Part III. Fabrication of six-fold flower-like ZnO nanoparticles as green-light photoluminescence emitter:
In this study, a hydrothermal reaction was used to fabricate the symmetric six-fold flower-like ZnO nanoparticles. The typical synthetic procedure is described as followed: Add the solution of ZnSO4 and P123 dropwise to an ammonia solution to form a white gel solution. After centrifugation, white precipitate was obtained. This Zn complex precursor is palate-like. Combining with a proper amount of ammonia solution, the palate-like Zn complex was gradually transformed to ZnO nanoparticles during the hydrothermal treatment at 100 oC. The morphology of ZnO nanoparticles is dependent on the added surfactant and surfactant concentration. With a well control on the P123 surfactant content, the symmetric six-fold flower-like ZnO nanoparticles with crystalline purity close to 100 % were generated. In the presence of the cationic surfactant, ZnO particle is radio-like. The prism-like ZnO particles were formed in the absence of surfactant. These ZnO particles possess high photoluminescence especially in the green-yellow region. The photoluminescence spectra of these ZnO particles are independent on the morphology.

第一章 緒論................................................................1
1. 中孔洞材料介紹..........................................................1
2. 界面活性劑性質簡介......................................................3
2.1. 界面活性劑的分類....................................................3
3. 中孔洞材料之合成........................................................4
3.1. 以超分子模板建構之氧化矽中孔洞結構..................................4
3.2. 以超分子模板建構之金屬氧化物中孔結構................................6
4. 中孔洞材料近年來應用....................................................7
4.1. 表面修飾有機官能基..................................................7
4.2. 表面修飾有機官能基之應用............................................8
4.3. 材料應用............................................................9

第二章  實驗部份............................................................17
1. 化學藥品...............................................................17
1.1. 直接表面修飾有機矽烷於中孔洞氧化矽.................................17
1.2. ㄧ步合成金屬氧化物中孔洞材料.......................................18
1.3. 綠光發光體之六角對稱氧化鋅奈米花材料...............................18
2. 產物之分析與鑑定.......................................................19
2.1. X光粉末繞射儀光譜..................................................19
2.2. 氮氣等溫吸附/脫附量測..............................................19
2.3. 場發射掃描式電子顯微鏡.............................................20
2.4. 場發射穿透式電子顯微鏡.............................................20
2.5. 穿透式電子顯微鏡...................................................20
2.6. 熱重分析...........................................................20
2.7. 霍氏紅外線光譜儀...................................................21
2.8. 元素分析...........................................................21
2.9. 固態魔角旋轉核磁共振...............................................21
2.10. 拉曼光譜	..........................................................21
2.11. 陰極光偵測系統....................................................22

第三章  直接表面修飾有機矽烷於中孔洞氧化矽..................................23
1. 研究動機及目的.........................................................23
2. 中孔洞氧化矽材料的合成與鑑定...........................................24
2.1. 中孔洞氧化矽材料的合成.............................................24
2.1.1. 初合成中孔洞氧化矽材料.........................................24
2.1.2. 直接表面修飾初合成中孔洞氧化矽材料.............................25
2.2. 中孔洞碳材的合成...................................................25
2.2.1. 以酚醛樹脂作為碳源製備中孔洞碳材的合成法.......................25
2.2.2. 以呋喃醇作為碳源製備中孔洞碳材的合成法.........................26
2.3. 中孔洞氧化矽材料的鑑定.............................................27
3. 實驗結果與討論.........................................................28
3.1. 初合成(as-synthesis)中孔洞氧化矽...................................28
3.2. 鹽類效應對不同pH值合成中孔洞材料結構的影響.........................29
3.3. 不同修飾環境對初合成氧化矽材修飾能力的影響.........................30
4. 改善鹼性合成中孔洞氧化矽材料的新修飾系統...............................31
4.1. 修飾前初合成的中孔洞氧化矽材料先經酸處理...........................31
4.2. 選用會釋放出酸離子的silane 3.......................................32
5. 機制探討...............................................................32
6. 應用此作用力合成中孔洞碳材.............................................33
6.1. 以酚醛樹脂製備中孔洞碳材之研究.....................................33
6.2. 以呋喃醇製備中孔洞碳材之研究.......................................35
7. 結論...................................................................36

第四章 ㄧ步合成金屬氧化物中孔洞材料.......................................53
1. 研究動機與目的.........................................................53
2. 金屬氧化物中孔洞材料的合成與鑑定.......................................54
2.1. 中孔洞氧化矽材料的合...............................................54
2.2. 鎳-碳複合材料的合成................................................55
2.3. 氧化鋁中孔洞材料的鑑定.............................................57
3. 實驗結果與討論.........................................................58
3.1. 金屬鹽類含量對氧化鋁中孔洞材料結構的影響...........................58
3.2. 煅燒溫度對氧化鋁中孔洞材料結構的影響...............................58
3.3. 煅燒時持溫時間對氧化鋁中孔洞材料結構的影響.........................59
3.4. 氧化鋁相轉變溫度及形態.............................................59
3.5. 合成氧化鋁中孔洞材料結論...........................................60
3.6. 材料開發Ⅰ.........................................................60
3.6.1. 氧化鋯 (Zirconium Oxide；ZrO2).................................60
3.6.2. 氧化鈰 (cerium dioxide；CeO2)..................................61
3.6.3. 氧化鈷(Cobalt oxide；Co3O4)....................................62
3.6.3. 氧化鎳(Nickel Oxide；NiO)......................................62
3.6.4. 不同金屬材料開發結論...........................................63
3.7. 材料開發Ⅱ.........................................................63
4. 結論	...................................................................65

第五章  綠光發光體之六角對稱氧化鋅奈米花....................................84
1. 研究動機與目的.........................................................84
2. 六角對稱氧化鋅奈米花的合成與鑑定.......................................86
2.1. 六角對稱氧化鋅奈米花合成步驟.......................................86
2.2. 六角對稱氧化鋅奈米花的鑑定.........................................87
3. 實驗結果與討論.........................................................87
3.1. 前驅物鑑定.........................................................87
3.1.1. 以P123合成的前驅物.............................................87
3.1.2. 以CTAB合成的前驅物.............................................89
3.2. 終產物的鑑定.......................................................89
3.3. 反應時間對結構的影響...............................................90
3.4. 不同硫酸鋅含量對產物造成的影響.....................................91
3.5. 不同水熱環境對產物造成的影響.......................................91
3.5.1. 改變水熱環境P123的濃度.........................................91
3.5.2. 水熱環境改變界面活性劑種類.....................................91
3.5.3. 反應濃度效應(氨水濃度).........................................92
3.6. 改變反應溫度對結構的影響...........................................93
3.7. 水熱中外加流場對結構的影響.........................................93
3.8. 分析光譜...........................................................93
4. 結論	...................................................................95

第六章 結論..............................................................116
參考文獻...................................................................120

                                    

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