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研究生：	陳鐸文 Chen, Duo-Wen
論文名稱：	合成各種型態、尺度、及含有金奈米粒子之中孔洞材料在液晶顯示器應用、SERS之應用 Synthesis of mesoporous silica in various form and AuNP@mesoporous silica for the applications in liquid crystal displayer and SERS
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 Department of Chemistry
論文出版年：	2012
畢業學年度：	100
語文別：	中文
論文頁數：	119
中文關鍵詞：	金奈米粒子、生物成礦、酸水熱處理法
外文關鍵詞：	AuNPs@MS, biomineralization, hydrothermal in acid
相關次數：	點閱：73 下載：0
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本論文之研究主題是以氧化矽為主軸，可將之分為三大部分：第一部分為合成AuNPs@MS材料及其在拉曼增顯之應用，以不同的合成方式得到AuNPs@MS材料，其合成方法有：一般合成、加酸(或鹽類、或鹼)的合成條件、使用硼氫化鈉或檸檬酸鈉的還原、異相合成法。探討其對AuNPs的粒徑大小與在MS中的分散度、及其對金奈米粒子(AuNPs@MS)做拉曼增顯效果之影響，找出最適當的合成方法得到可應用於拉曼增顯的AuNPs@MS材料。第二部分為探討酸水熱處理法對中孔洞氧化矽(MS)的模板移除及擴孔作用，以明膠做為有機模板而得到的MS材料，通常於移除有機模板的方法為煅燒或有機萃取法，在本實驗發現另一種移除明膠方法─酸水熱處理法。在此章節會探討：酸溶液之濃度、於不同pH值之水熱效果、改變水熱天數、改變合成MS之熟化時間，對合成MS之比表面積與孔徑分佈的影響，因此可藉由實驗參數去調控合成MS的孔徑分佈及比表面積。第三部分為使用陰─陽離子混合界面活性劑合成各種形態之氧化矽材料，依據生物成礦的概念，使用C16TMAB與SA，硬脂酸(或LA，月桂酸)的界面活性劑，做為有機模板，製做出各種形態之氧化矽材料。在合成系統中，調控合成pH值、陰/陽離子界面活性劑之比例、溫度、總水量、及加鹽類之劑量，探討實驗變因對氧化矽之形貌及其粒徑的影響。

According to the mesoporous silica we synthesize in this thesis, the experiment can be divided into three main part:
1. Synthesis of Au nanoparticles@mesoporous silica (AuNPs@MS) for the application in SERS. By tuning the pH value, adding acid (or salt, or base), and using different kind of reductants, we can control the size of AuNPs and the dispersity of AuNPs in MS. We discussed about finding the best synthesis way to get the material for the good application in SERS.
2. We use the gelatin as the organic template to synthesize the MS. In this thesis, we find the way by hydrothermal in acid solution can easily remove the gelatin from the MS. We can control the surface area and the pore size of MS by adjusting the concentration of acid solution, the days and the pH value of hydrothermal treatment, the aging time of sodium silicate.
3. According to the concept of biomineralization, we synthesize the various form of MS by turning the ratio of the anionic surfactant (SA or LA) and the cationic surfactant (C16TMAB), the pH value, the concentration of surfactant, adding the salt and so on.

第一章	緒論...................................................................................................1
1.1	中孔洞氧化矽材料之發展..............................................................................1
1.1.1 中孔洞的定義......................................................................................1
1.1.2 中孔洞材料的主要研究範疇..............................................................2
1.2	奈米材料之介紹..............................................................................................4
1.2.1  奈米效應............................................................................................5
1.2.2  製備奈米粒子的方法........................................................................6
1.3	表面增強拉曼光譜之簡介..............................................................................8
1.4	生物成礦(Biomineralization)之發展與研究............................................9
1.5	界面活性劑之簡介........................................................................................10
1.5.1  界面活性劑的基本性質..................................................................10
1.5.2  界面活性劑的分類..........................................................................11
1.5.3  界面活性劑的行為..........................................................................12
1.5.4  陽性─陰性離子型界面活性劑所組成的系統..............................14
1.5.5  明膠的簡介......................................................................................15
1.6	氧化矽源之介紹............................................................................................16
1.6.1  矽酸鹽的性質..................................................................................16
1.6.2  TEOS 的性質....................................................................................17
1.7 氧化矽材料修飾用之矽烷...........................................................................19
1.8 液晶之基本簡介...........................................................................................20
    1.8.1  液晶的光電特性.............................................................................21
    1.8.2  液晶顯示器與電子窗簾的基本介紹.............................................23

第二章	實驗部分...........................................................................................26
2.1 實驗藥品.......................................................................................................26
2.2 實驗合成步驟...............................................................................................27
    2.2.1  合成金奈米粒子的中孔洞氧化矽材料..........................................27
          2.2.1.1  一般的合成方法..............................................................27
          2.2.1.2  加入強酸或鹽類的合成方法..........................................29
          2.2.1.3  異相的合成方法..............................................................31
    2.2.2  用酸水熱法移除界面活性劑..........................................................32
    2.2.3  製作液晶顯示器..............................................................................33
    2.2.4  以陰陽離子界面活性劑混合系統合成各種特殊形態的氧化矽材料......................................................................................................34
 2.3 儀器之鑑定..................................................................................................35
    2.3.1  穿透式電子顯微鏡(Transmission Electron Microscopy, 
           TEM)..................................................................................................35
    2.3.2  掃描式電子顯微鏡(Scanning Electron Microscopy, 
           SEM)..................................................................................................35
    2.3.3  X光能量散部光譜儀(Energy Dispersive Spectrometer, 
           EDS)..................................................................................................35
    2.3.4  熱重分析儀(Thermogravimetric Analysis, 
           TGA)...................................................................................................35
    2.3.5  氮氣等溫吸附─脫附測量(N2 adsorption/desorption 
           isotherm).........................................................................................36
    2.3.6  X─射線粉末繞射光譜(Powder X-ray 
           Diffraction)...................................................................................36
    2.3.7  顯微拉曼光譜(Microscope Raman 
           Spectrometer).................................................................................37

第三章	含奈米金粒子的中孔洞氧化矽材........................................................38
3.1 實驗動機與目的.............................................................................................38
3.2 改變煅燒溫度對AuNPs@MS的影響................................................................39
3.3 探討在合成AuNPs@MS步驟中加酸、加鹽類或加鹼的影響........................46
3.4 利用檸檬酸鈉還原合成AuNPs@MS於不同pH值的影響..............................57
3.5 利用異相合成法合成AuNPs@MS材料.............................................................63

第四章	探討酸處理對AuNPs@MS材料之影響機制............................................73
4.1 實驗動機與目的.............................................................................................73
4.2 探討移除有機模板所需無機酸溶液與反應的條件.....................................74
4.3 探討酸水熱法對改變MS合成參數之影響...................................................79
4.4 廢酸液回收再利用.........................................................................................82
4.5 將MS材料混合液晶製作液晶顯示器............................................................83

第五章	以C16TMAB - SA或LA - H2O系統合成各種特殊型態之中孔洞氧化矽材.........................................................................................................87
5.1 實驗動機與目的.............................................................................................87
5.2 於pH=3合成，探討改變SA(或LA)/C16TMAB莫耳比及合成溫度對氧化矽型
    態的影響.........................................................................................................88
5.3 於pH=5合成，探討改變SA(或LA)/C16TMAB莫耳比及合成溫度對氧化矽型 
    態的影響.........................................................................................................91
5.4 於pH=6合成，探討改變SA(或LA)/C16TMAB莫耳比及合成溫度對氧化矽型
    態的影響.........................................................................................................95
    5.4.1  於40℃，微調SA/C16TMAB莫耳比對披薩狀氧化矽材料的影
           響........................................................................................................98
    5.4.2  於40℃，微調合成pH值對披薩狀的氧化矽材料之影
           響.....................................................................................................100
    5.4.3  於40℃，改變合成總水量對披薩狀的氧化矽材料之影
           響.....................................................................................................103
    5.4.4  於40℃，在合成條件加入鹽類對披薩狀的氧化矽材料之影
           響.....................................................................................................104
5.5 於pH=7合成，探討改變SA(或LA)/C16TMAB莫耳比及合成溫度對氧化矽型
           態的影響.........................................................................................106
5.6 於pH=9合成，探討改變SA(或LA)/C16TMAB莫耳比及合成溫度對氧化矽型
           態的影響.........................................................................................110

第六章	總結論................................................................................................114

參考文獻.........................................................................................................116

                                    

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