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研究生：	阮玉勝 Thang, Nguyen Ngoc
論文名稱：	膠體原的合成、特性探討及其對奈米銀結構體之誘導研究 Synthesis and Characterization of Predesigned Gelators and Their Templated Fabrication of Silver Nanoconstructions
指導教授：	劉瑞祥 Liu, Jui-Hsiang
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	207
中文關鍵詞：	膠體、Cholesteryl pyridine carbamate 、聚乙烯醇、殼聚醣、丙烯酸、奈米銀結構體
外文關鍵詞：	Cholesteryl pyridine carbamate, Soft template, Nanotube, Silver nanowire, Poly(vinyl alcohol), Chitosan, UV irradiation, Hydrogel thin films, Silver nanoparticle, Biomedical applications
相關次數：	點閱：153 下載：4
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凝膠於材料科學、環境科學、奈米科技、再生醫學及藥物輸送等基礎領域的應用上均有重大的貢獻，在軟性材料領域中佔有一席之地。本研究設計、合成並鑑定兩種新穎的凝膠材料，分別為分子凝膠及聚合物凝膠，並進一步探討凝膠於製備銀奈米結構之軟性基板特性。
首先本研究設計並合成含膽固醇基團之凝膠分子cholesteryl-pyridine-carbamate (CPC)，並探討此具有光學活性之凝膠體於不同單一溶劑和混合溶劑下的自組裝行為，以得到特殊的自組裝型態。多種檢測證實CPC凝膠體可於17種溶劑下形成凝膠，並具有高度規則的奈米纖維結構，特別是在水-苯甲醚以及水-乙醇的混合溶劑中此光學活性凝膠體會自組裝形成奈米管狀結構。為了探討軟性材料於奈米加工製程的應用潛力，本研究進一步利用CPC於水-苯甲醚混合溶劑系統所形成奈米管，作為製備銀奈米結構，包含銀奈米鏈段及銀奈米線的軟性基板。藉由室溫下的銀鏡反應可得直徑於20~70奈米且長度達數百微米之極高長徑比銀奈米線。研究結果顯示該系統不僅提供另一種奈米元件製備的方式，亦能使奈米材料應用於不同領域之前瞻性研究。
第二類凝膠體為利用聚乙烯醇 (PVA)、殼聚醣 (CTS)與作為交聯劑的丙烯酸 (AA)經紫外光照射聚合而成的一系列生物相容性水凝膠薄膜，且聚合反應過程中無添加任何具生物毒性的光起始劑。研究中使用數種分析工具檢測PVA/CTS水凝膠薄膜特性如膨潤現象、分子間化學鍵結、分子結構、熱性質、結晶度、表面及內部結構形態，以及UV照射時間及AA濃度對上述性質之關係。SEM結果顯示水凝膠體薄膜內部呈現分布均勻的多孔性結構，其可逆的膨潤現象可藉由pH值調整。此外為了應用此水凝膠薄膜系統於前瞻性生物醫學領域，此研究葡萄糖作為還原劑，氫氧化鈉為催化劑進行硝酸銀的in-situ還原反應，成功以綠色方法合成出無毒性之負載銀奈米粒子之PVA/CTS水凝膠薄膜複合材料。此薄膜複合材料以數種分析儀器及機械性質量測儀器進行檢測，結果顯示高度交聯而緻密的多孔網狀基板可有效地防止銀奈米粒子的聚集，拉伸試驗顯示於水凝膠網狀結構中存在分散均勻之銀奈米粒子可有效提高複合膜之彈性係數。上述結果顯示PVA/CTS水凝膠薄膜及其奈米複合薄膜同時具備酸鹼性響應、抗菌性及高機械性質等優點，可預期其在生物醫學如傷口敷料有的應用價值。

Gels, one of the most important class of soft materials, have received a great interest in terms of both fundamental and practical application in a variety of fields such as material science, environmental science, nanotechnology, regenerative medicine and drug delivery. Herein, two attractive types of gels, molecular gels and polymeric gels, have been designed, synthesized, characterized, and further investigated as soft templates for fabrication of silver nanoconstructions.
For the first gel type, a molecular gelator based on cholesterol, cholesteryl-pyridine-carbamate (CPC), has been designed and synthesized. The self-assembly behaviors of this chiral gelator in various organic solvents and mixed solvents have been examined in order to obtain specific molecular aggregations. A number of testing means confirmed that the CPC gelator formed the gel in 17-solvent examinations with well-ordered nanofibrous structures. Especially, the chiral gelator promoted the formation of long nanotubes in the mixed solvents of water-anisole and water-ethanol. To realize the potential applications of soft materials in the bottom-up nanofabrication, the CPC nanotubes in the water-anisole system have been further developed as the soft templates for the fabrication of silver nanostructures, especially silver nanochains and silver nanowires. The ultra-high aspect ratio silver nanowires with diameters in the range of 20-70 nm and lengths up to hundreds of micrometers have been obtained via the classic silver mirror reaction at room temperature. Based on these results, the author anticipated that such system may not only advance the field of nanodevice fabrication, but also enable the development of various new nanomaterials for diverse promising applications.
For the second gel type, a series of hydrogel thin films based on biocompatible polymers of poly(vinyl alcohol) (PVA) and chitosan (CTS) has been synthesized via ultraviolet (UV) irradiation using acrylic acid (AA) monomer as a crosslinker, without the addition of any other photo-initiator. The characteristics of the PVA/CTS hydrogel thin films, such as swelling behaviors, intermolecular chemical bonds, molecular structures, thermal behaviors, degrees of crystallinity, morphologies of the surfaces and internal structure, and their relationship to the UV irradiation time and AA concentration, have been examined by several analysis tools. It confirmed that the hydrogel films encompassed a uniform inter-porous structure and exhibited reversible swelling in response to changes in the pH of the media. To further extend promising applications of the prepared hydrogels for biomedical field, a green synthesis of silver nanoparticle-loaded PVA/CTS hydrogel thin films has been performed through the in situ reduction of silver nitrate by using glucose as a non-toxic reducing agent and sodium hydroxide as an accelerator. The composite films were characterized using several analysis tools and mechanical test. The results showed that the nanoparticle agglomeration was prevented through the use of the high-crosslinking and dense inter-porous network as an effective nanoreactor template. The tensile test revealed that the effective incorporation of silver nanoparticles within the hydrogel networks rendered the composite films more elastic. From these results, the author expected that the PVA/CTS hydrogel thin films and their nanocomposite films could provide smart hydrogels with some advantages of pH-responsive, antibacterial and good mechanical properties for biomedical applications such as wound dressing.

Acknowledgement i
Abstract ii
中文摘要 v
Table of contents vii
List of tables xiii
List of figures and schemes xiv
Abbreviations and Symbols xxiii
Chapter 1. Introduction 1
1 Overview 1
2 Objectives and scopes of the study 7
3 References 9
PART I. MOLECULAR GEL AND ITS APPLICATIONS 13
Chapter 2. Literature review 14
1 Introduction 14
2 Classification of molecular gelators 15
2.1 Hydrogelators 15
2.1.1 Amino acid and dipeptide derivatives 15
2.1.2 Nucleoside derivatives 16
2.1.3 Carbohydrate-based derivatives 18
2.1.4 Gemini surfactants 18
2.2 Organogelators 20
2.2.1 ALS, A(LS)2 and A(LS)3 derivatives 20
2.2.2 Fatty acid derivatives 22
2.2.3 Sugar derivatives 23
2.2.4 Amino acid derivatives 24
2.2.5 Nucleoside derivatives 25
2.2.6 Urea derivatives 25
3 Templated techniques for synthesis of inorganic nanostructures 26
3.1 Molecular gels based templates 26
3.1.1 Simple gelators 26
3.1.2 Cholesterol-based gelators 28
3.1.3 Sugar-based gelators 29
3.1.4 Amide-, amino acid-, peptide-based gelators 31
3.2 Strategies for templated techniques based on LMWGs 32
4 Conclusions 34
5 References 34
Chapter 3. An Organogel of Cholesteryl Pyridine Carmbamate:
Water-induced Nanofiber-to-Nanotube Transformation 44
Abstract 44
1 Introduction 45
2 Experimental 46
2.1 Chemicals 46
2.2 Synthesis of CPC 46
2.3 Gelation behaviors 47
2.4 Preparation of self-assembled CPC nanotubes 49
2.5 Instrumental analyses 49
3 Results and discussion 50
3.1 Synthesis and characterization of CPC 50
3.2 Gelation behaviors 51
3.3 Thermotropic properties of organogels 52
3.4 Morphologies of organogels 54
3.5 Driving force analysis 55
3.6 Water-induced nanofiber-to-nanotube transformation 58
4 Conclusions 62
5 References 62
Chapter 4. Wet Chemical Synthesis of Ultralong Silver Nanowires Based on a Soft Template of Cholesteryl Pyridine Carbamate Organogel 66
Abstract 66
1 Introduction 67
2 Experimental 70
2.1 General methods 70
2.2 Preparation of silver nanostructures 71
3 Results and Discussion 72
3.1 Formation of the complex gel 72
3.2 Thermotropic properties of complex gel 74
3.3 Characterization of coordination and driving forces 75
3.4 Morphology of complex gel 81
3.5 Organogel template directed synthesis of silver nanostructures 83
4 Conclusions 91
5 References 92
PART II. POLYMERIC GEL AND ITS APPLICATIONS 96
Chapter 5. Literature review 97
1 Introduction 97
2 Polymer based hydrogel systems 99
2.1 Polysaccharide hydrogels 100
2.1.1 Chitosan-based hydrogels 100
2.1.1.1 Chitosan-based physical hydrogels 100
2.1.1.2 Chitosan-based chemical crosslinked hydrogels 103
2.1.2 Alginate-based hydrogels 107
2.1.3 Hyaluronic acid-based hydrogels 108
2.2 Synthetic polymer-based hydrogels 109
2.2.1 Poly(vinyl alcohol)-based hydrogels 109
2.2.1.1 PVA-based physical hydrogels 110
2.2.1.2 PVA-based chemical crosslinked hydrogels 110
2.2.2 Poly(acrylic acid)-based hydrogels 113
3 Hydrogel thin films 114
3.1 Crosslinking by high energy irradiation 115
3.2 Crosslinking with reactive groups 115
3.3 Crosslinking using the addition of multi-functional monomers 116
3.4 Physical crosslinked film by the layer-by-layer technique 118
4 Conclusions 119
5 References 120
Chapter 6. Fabrication and Characterization of Poly(vinyl
alcohol)/Chitosan Hydrogel Thin Films via UV Irradiation 137
Abstract 137
1 Introduction 138
2 Experimental 141
2.1 Materials 141
2.2 Preparation of the hydrogel thin films 141
2.3 Gel-fraction measurements 142
2.4 Swelling measurements 143
2.5 Instrumental analyses 144
3 Results and Discussion 145
3.1 Appearance of the hydrogel thin films 145
3.2 Fourier-transform infrared spectroscopy 147
3.3 X-ray diffraction 149
3.4 Differential scanning calorimetry 150
3.5 Thermogravimetric analysis 153
3.6 Gel fractions 155
3.7 Swelling behaviors 160
3.8 Morphological studies 167
4 Conclusions 170
5 References 171
Chapter 7. A Green Method for in Situ Synthesis of Poly(vinyl alcohol)/Chitosan Hydrogel Thin Films with Entrapped Silver Nanoparticles 176
Abstract 176
1 Introduction 177
2 Experimental 180
2.1 Materials 180
2.2 Fabrication of AgNPs in the hydrogel thin films 180
2.3 Instrumental analyses 181
3 Results and Discussion 183
3.1 Template-mediated in situ fabrication of AgNPs in the
hydrogel thin films 183
3.2 UV/Vis analyses 185
3.3 Morphological studies 186
3.4 XRD measurements 189
3.5 FTIR characterizations 190
3.6 Mechanical properties 192
4 Conclusions 194
5 References 195
Chapter 8. Conclusions 199
APPENDICES 202
                                    

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