臺灣博碩士論文加值系統

本研究分別利用硬模版與軟模版法製備奈米級矽中空球。在硬模版的研究中是以聚丙烯酸/幾丁聚醣 (PAA-CS) 的奈米顆粒為模版，在室溫下添加矽酸膠使其包覆於PAA-CS的顆粒中而形成核殼結構，最後再利用鹽酸 (HCl) 調整pH值至1可將PAA-CS 溶解，使其形成奈米級矽中空球。由研究結果發現，利用2種不同分子量的幾丁聚醣可以改變模版大小，即可以控制中空粒子的尺寸。且由BET儀得知中空粒徑較小的，表面積愈大。
軟模版的研究是以Al(OH)3所既有的孔洞經 pH 調整後成為泡泡, 將此泡泡作為模版加入矽酸膠，矽酸膠顆粒會吸附在泡泡的表面，再添加硝酸將溶液調至 pH=1 ，將殘餘的Al(OH)3膠溶解掉，可獲得中空SiO2。在研究中，分別探討Al（OH）3 pH = 5、pH = 4為模版，皆可得到中空粒子，其中以pH = 5所得中空SiO2最佳，因為量多、粒徑小，且表面積最大。由EDS的實驗結果可證實利用VTMO矽烷可以有效地分離出矽與鋁成分而得到純二氧化矽的中空粒子。本研究經過連續性的探討，發現只要提高矽酸膠加入的量，並加入VTMO進行表面改質，亦可獲得微米級中空SiO2。

Nano-grade silica hollow sphere were synthesized by the hard template method and the soft template method, respectively. Nano-grade polycyclic acid - chitosan (PAA-CS) particles were used as the hard template in this study. Colloidal silica was added for shell which was absorbed on the surface of PAA-CS particle to form the core-shell structure at room temperature. The core material PAA-CS particle was removed by only adjusting pH to ＜ 1 to form the hollow silica sphere. The PAA-CS powder and hollow silica sphere were changed by the change of the molecular weight of chitosan. The formed hollow silica sphere had a small particles size with a large specific area.
In another part of this study, the soft template, the porous Al (OH)3 was adopted to synthesize the nano grade hollow silica sphere. Colloidal silica was mixed with the aged precipitate of Al(OH)3. During adjusting the solution to pH=1 with 1 M HNO3 , the precipitate of Al(OH)3 was dissolved and the colloidal silica would trap the nano bubble to form the hollow silica sphere.The pH value of solution were the important parameter for controlling the particle size of hollow silica sphere. According to the experimental results, the aged at pH=5 of Al(OH)3 precipitate was the best condition to synthesize the small and uniform hollow silica sphere. In addition, the product of hollow silica sphere could be separated from the aluminum ion solution by using vinyltrimethoxysilane (VTMO) to modify the particle surface and gel the precipitate in the mixing solvent of ethanol and butanol thereafter. The composition of the precipitate was only silica was detected by EDS analysis.

目錄
中文摘要............................................................i
英文摘要 ..........................................................ii
致謝..............................................................iii
目錄...............................................................iv
表目錄............................................................vii
圖目錄...........................................................viii
第一章 緒論.........................................................1
1.1 前言...........................................................1
1.2 前人文獻........................................................2
1.3 研究目的........................................................4
第二章 理論部分.....................................................5
2.1矽酸膠..........................................................5
2.1.1矽酸膠之特性...................................................5
2.1.2探討酸鹼值對矽膠體的影響.........................................7
2.2幾丁聚醣........................................................10
2.2.1幾丁質與幾丁聚醣之介紹..........................................10
2.2.2幾丁聚醣之特性.................................................11
2.2.3 幾丁聚醣之應用................................................11
2.3鋁化合物之介紹...................................................13
2.3.1氧化鋁........................................................13
2.3.2鋁氫氧化物....................................................13
2.4模版法..........................................................15
2.5膠體粒子吸附理論.................................................17
2.6中空SiO2........................................................20
2.6.1中空SiO2主要特性...............................................20
2.6.2中空SiO2之應用................................................21
2.7中空SiO2之孔隙度測定.............................................23
第三章 實驗部分.....................................................28
3.1藥品............................................................28
3.2實驗分析儀器.....................................................30
3.3實驗方法與實驗步驟................................................31
3.3.1矽酸膠合成.....................................................31
3.3.2以PAA-C.S為模版合成之中空二氧化矽................................33
3.3.3以Al（OH）3為模版合成之中空二氧化矽..............................35
第四章 結果與討論 ..................................................37
4.1矽酸膠性質......................................................37
4.2以PAA-C.S為模版合成之中空二氧化矽.................................38
4.2.1不同分子量CS對PAA-CS複合材的影響................................38
4.2.2不同尺寸的模版對核殼結構粒子的影響...............................38
4.2.3不同尺寸的模版對中空粒子的影響...................................38
4.2.4不同尺寸中空SiO2表面積及孔隙度之探討.............................43
4.2.5合成中空SiO2特性分析...........................................47
4.2.6中空SiO2反應機制...............................................49
4.3以Al（OH）3其氣泡為模版合成之中空二氧化矽...........................51
4.3.1 Al（OH）3模版之性質...........................................51
4.3.2以Al（OH）3為模版之核殼結構探討..................................54
4.3.3不同pH值Al(OH)3對中空SiO2之影響................................54
4.3.4不同尺寸中空SiO2表面積及孔隙度之探討.............................57
4.3.5中空SiO2反應機制..............................................61
4.3.6 SiO2表面改質................................................62
第五章 結論........................................................66
參考文獻...........................................................68

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