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系統識別號 U0002-2508201012595900
中文論文名稱 利用毛細管電泳分析在不同界面活性劑中所合成的金奈米粒子
英文論文名稱 Analysis of Gold Nanoparticles Synthesized in Different Surfactants by Capillary Electrophoresis
校院名稱 淡江大學
系所名稱(中) 化學學系碩士班
系所名稱(英) Department of Chemistry
學年度 98
學期 2
出版年 99
研究生中文姓名 蔡鎮鴻
研究生英文姓名 Jhen-Hong Tsai
學號 697160249
學位類別 碩士
語文別 中文
口試日期 2010-07-19
論文頁數 187頁
口試委員 指導教授-吳俊弘
委員-鄭建中
委員-鄧金培
中文關鍵字 毛細管電泳  金奈米粒子  界面活性劑 
英文關鍵字 Capillary electrophoresis  Gold nanoparticles  Surfactant 
學科別分類 學科別自然科學化學
中文摘要 從不同帶電性穩定劑中所合成的金奈米粒子(AuNPs),經由中性界面活性劑(Hex-OPE-PEO)在其表面進行修飾反應後,可以利用微胞電動層析法(MEKC)加以分析。利用此方法,我們可以測定表面帶有不同穩定劑的AuNPs之大小和分布情形。在本論文中我們利用此電泳技術研究分別以陰離子型、陽離子型、中性以及兩性離子型界面活性劑為穩定劑所合成的AuNPs的性質。
我們發現,反應物混合方法會影響所合成AuNPs的性質。例如,在陰離子(SDS)系統中使用一次加入合成法可以得到粒徑分布較窄的結果;反之,在陽離子(CTAB)系統中使用分段逐次合成法所得產物之再現性與保存穩定性較佳。在陰、陽離子型界面活性劑中添加飽和芘,都可以在合成過程中有效抑制AuNPs成長反應,得到粒徑較小的產物。
在雙界面活性劑中(中性F127+陽離子或陰離子型界面活性劑)合成AuNPs,若添加還原劑(NaBH4),易形成粒徑分布廣的產物;若只由F127擔任還原劑,則所得粒徑大小可由F127濃度控制,且分布較小。在兩性離子型界面活性劑(TDAPS)系統中,除了在低濃度(0.1 mM)TDAPS中,否則改變NaBH4濃度、TDAPS濃度或合成方法,對於所合成粒徑並無顯著影響。我們發現在SDS中以一次添加合成法合成AuNPs時,當提高還原劑濃度或在低溫進行合成反應,會得到較小粒徑AuNPs。此外,在SDS系統中使用晶種促進成長法合成AuNPs時,似乎應在適當濃度晶種中以分次少量方式添加HAuCl4和NaBH4,降低新晶種的形成,而在原添加晶種上成長,如此才能合成粒徑分布較窄的AuNPs。
英文摘要 Gold nanoparticles (AuNPs) synthesized in surface stabilizers with different charge polarities can be analyzed by micellar electrokinetic chromatography (MEKC) after undergoing surface modification reaction with a neutral surfactant (Hex-OPE-PEO). By using this approach, the particle sizes and distributions of AuNPs capped with different stabilizers can thus be determined. In the thesis, we utilized this CE-based method to study the properties of AuNPs synthesized in anionic, cationic, neutral, and zwitterionic surfactants, respectively.
We found that mixing reactants in different ways would result in AuNPs with different properties. For example, in the anionic (SDS) system, one-pot synthetic method could produce AuNPs with narrower distribution. On the other hand, in the cationic (CTAB) system, stepwise addition method would generate AuNPs with better reproducibility and storage stability. With the addition of saturated pyrene in anionic and cationic surfactants, particle growth reaction could be suppressed and smaller size of AuNPs would be obtained.
In the binary surfactant system (i.e., neutral F127 + cationic or anionic surfactant), AuNPs with broad size distribution would be produced if another reductant (e.g., NaBH4) was added. Without adding additional reductant, F127 could serve as the only reductant in the system as well as the usual surface stabilizer. In so doing, the size of AuNPs could be regulated by F127 concentration and narrower size distribution would be obtained. In the zwitterionic surfactant (TDAPS), except at low TDAPS concentration (0.1 mM), particle size would not be affected by NaBH4 concentration, TDAPS concentration, and reactant mixing method. In the SDS system of one-pot synthetic method, increasing reductant concentration or lowering reaction temperature would reduce particle size. Furthermore, when the seed-mediated method was used in the SDS system, it seemed that multi-step additions of small amounts of HAuCl4 and NaBH4 into appropriate concentration of seeds would decrease the formation of new seeds and enable the particle growth on the added seeds, and therefore produce AuNPs with narrower distribution.
論文目次 中文摘要……………………………………………………………..I
英文摘要……………………………………………………………..II
目錄……………………………………………………………..IV
緒論……………………………………………………………..1
1.1 前言…...……………………………………………………………..1
1.2 金奈米粒子簡介………..…….……………………………………..2
1.3 毛細管電泳介紹………..……………………………………...……5
1.4 毛細管電泳對於金奈米粒子的分離機制..…………...…..………..9
1.5 本章參考資料..…………………………………………………….12
第二章 實驗部分………………………………………………………17
2.1 儀器………………………………………………………………...17
2.1.1 毛細管電泳儀……………………………………………………17
2.1.2 毛細管……………………………………………………………17
2.1.3 穿透式電子顯微鏡………………………………………………17
2.1.4 去離子水處理器…………………………………………………18
2.1.5 高速離心機………………………………………………………18
2.1.6 UV-vis光譜儀…………………………………………………….18
2.2 藥品部分…………………………………………………………...19
2.2.1 金奈米粒子樣品…………………………………………………19
2.2.2 毛細管電泳緩衝溶液……………………………………………19
2.2.3 合成金奈米試劑…………………………………………………19
2.2.4 金奈米粒子表面修飾劑…………………………………………20
2.3 實驗步驟…………………………………………………………...21
2.3.1 聚丙烯醯胺塗層步驟……………………………………………21
2.3.2 金奈米粒子合成步驟……………………………………………22
(1) 分段逐次合成法…..……………………………………………….22
(2) 一次加入合成法…..……………………………………………….22
(3) 在界面活性劑中添加飽和的芘(pyrene)來合成金奈米粒子.…...22
(4) 在陰離子界面活性劑系統中使用晶種成長合成方法(seed-mediated method)合成金奈米粒子.…………………………23
2.3.3 Hex-OPE-PEO的合成步驟………………………………………24
2.3.4 金奈米粒子修飾步驟……………………………………………25
2.3.5 毛細管電泳實驗步驟……………………………………………26
2.3.6 TEM樣品製備步驟………………………………………………26
2.4 本章參考資料……………………………………………………...27
第三章 結果與討論……………………………………………………30
3.1利用毛細管電泳結合表面修飾劑分析不同方式合成的金奈米粒子
............................................................................................................30
3.1.1前言..………………………………………………………………30
3.1.2利用中性界面活性劑作為金奈米粒子的表面修飾劑..................32
3.1.2.1 利用Hex-OPE-PEO作為表面修飾劑..............................32
3.1.2.2最佳電泳條件與電泳再現性.............................................33
3.1.3鑑定不同合成方式所得到的金奈米粒子………………………..36
3.1.4結論………………………………………………………………..41
3.2表面修飾劑濃度對於由陽離子界面活性劑中所合成金奈米粒子
的粒徑影響........................................................................................42
3.2.1前言………..……………………………………………………....42
3.2.2使用不同Hex-OPE-PEO濃度修飾金奈米粒子表面……....……43
3.2.3結論………………………………………………………………..48
3.3以毛細管電泳分析在陽離子界面活性劑中所合成的金奈米粒子
………………………………………………………………………51
3.3.1前言………………………………………………………………..51
3.3.2在陽離子界面活性劑中合成的金奈米粒子……………………..51
3.3.2.1利用hexadecyltrimethylammonium bromide (CTAB)
作為金奈米粒子穩定劑…………………………………51
3.3.2.2在CTAB系統下提高還原劑濃度對於合成金奈米粒子
的影響…..………………………………………………..55
3.3.2.3在hexadecyltrimethylammonium bromide系統下比較使
用分段逐次合成法和一次加入合成法的差別……..…..60
3.3.2.4觀察改變不同反離子對於合成金奈米粒子的影響…….62
3.3.2.5觀察改變不同碳鏈長度對合成金奈米粒子的影響…….66
3.3.2.6在陽離子界面活性劑系統中添加飽和芘(pyrene)對於合
成金奈米粒子之影響……………………………………74
3.3.3結論……………………………………………………………….81
3.4以毛細管電泳分析在混合系統(mix micelle system)中合成的金奈米粒子……………………………………………………………..83
3.4.1前言….……………………………………………………………83
3.4.2利用CTAB-F127混合之雙界面活性劑系統合成金奈米粒子.....84
3.4.3利用SDS-F127混合之雙界面活性劑系統合成金奈米粒子……94
3.4.4利用SDeS-F127混合之雙界面活性劑系統合成金奈米粒子…102
3.4.5 結論………...……...………………………………..…………..111
3.5以毛細管電泳分析在兩性離子界面活性劑中所合成的金奈米粒子
……………………………………………………………………..112
3.5.1 前言..............................................................................................112
3.5.2 在TDAPS界面活性劑中合成金奈米粒子................................112
3.5.3 結論………………………………………...…………………...118
3.6以毛細管電泳分析在陰離子界面活性劑中所合成的金奈米粒子
……………………………………………………………………..119
3.6.1 前言..............................................................................................119
3.6.2在陰離子型界面活性劑中改變不同濃度NaBH4以分段逐次合成法來合成金奈米粒子…………………………………………...120
3.6.3在陰離子型界面活性劑中改變不同合成溫度以分段逐次合成法來合成金奈米粒子……………………………………………...123
3.6.4在陰離子型界面活性劑中改變不同的合成方法來合成金奈米粒子………………………………………………………………...126
3.6.5 在SDS中以一次加入合成法合成金奈米粒子………………..127
3.6.6 在SDeS中以一次加入合成法來合成金奈米粒子…..………..133
3.6.7 結論……………………………………………………………..143
3.7以毛細管電泳分析在陰離子系統中,使用晶種促進成長法
(seed-mediated method)來合成金奈米粒子……………………...144
3.7.1前言................................................................................................144
3.7.2成長溶液中含有芘(pyrene)對合成金奈米粒子之影響….…….145
3.7.3 改變還原劑種類對合成金奈米粒子之影響…………..………166
3.7.4 改變合成方法對於金奈米粒子之影響…..……..…….……….174
3.7.5 結論……………………………………………………………..179
3.8 本章參考資料…………………………………………………….182
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第三章
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