定量分析金屬奈米晶體的成核、成長、熱穩定與光催化特性

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研究生：	楊東翰 Yang, Tung-Han
論文名稱：	定量分析金屬奈米晶體的成核、成長、熱穩定與光催化特性 Toward a Quantitative Understanding of the Nucleation, Growth, and Thermal Stability of Colloidal Metal Nanocrystals with the Photocatalytic Application
指導教授：	吳振名 Wu, Jenn-Ming 李奕賢 Lee, Yi-Hsien
口試委員:	果尚志 Gwo, Shangjr 陳力俊 Chen, Lih-Juaan 郭俊宏 Kuo, Chun-Hong 張嘉升 Chang, Chia-Seng
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2017
畢業學年度：	106
語文別：	英文
論文頁數：	185
中文關鍵詞：	金屬、奈米材料、還原反應、合成、動力學
外文關鍵詞：	metal, nanomaterials, reduction reaction, synthesis, kinetics
相關次數：	點閱：2 下載：0
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本論文致力發展一套定量的分析方法去深入了解金屬奈米晶體的成核、成長、熱穩
定性與光催化特性。本論文成功利用吸收光譜技術定量解析反應前驅物在晶體生長中的反
應還原動力特性，並建立動力學模型去解析反應前驅物的還原路徑。基於動力學的分析，
成功發現反應前驅物可能先在溶液中就被還原成原子(溶液還原路徑)或是在金屬奈米晶體
的表面被還原成原子(表面還原路徑)。再者，藉著使用不同晶體當作種子，我們進一步達
成定量了解不同晶面的成長速率與能障高度。了解金屬奈米晶體的生長機制後，我們緊接
著利用臨場電子顯微鏡分析技術成功了解金屬奈米晶體的熱穩定性。最後，我們展示如何
利用雙官能基的有機架橋分子成功整合金屬奈米晶體與一維半導體形成異質結構。此異質
結構擁有優異且穩定的光催化特性。

This dissertation is focused on the development of a quantitative analysis of the nucleation, growth, and thermal stability of metal nanocrystals with the photocatalytic application. In a first project, I quantitatively analyze the reaction kinetics involved in the seed-mediated growth of metal nanocrystals using a spectroscopy method and further had it correlated to the reduction pathway (solution reduction vs. autocatalytic surface reduction) of a salt precursor. Based on the quantitative data, I conclude that the pathway is mainly determined by the reduction kinetics involved in the synthesis. In a second project, I further demonstrate that autocatalytic surface reduction can be employed to enable the formation of metal nanocrystals with predictable and well-controlled shapes through seed-mediated growth. In a third project, with the concave, multiply-twinned icosahedral metal nanocrystals as an example, I develop a method for quantifying the thermal stability of metal nanocrystals by using in situ transmission electron microscopy, to identify the equilibration pathways of this far-from-equilibrium structure. In a fourth project, I demonstrate an approach to integrate the metal nanocrystals with nanostructured semiconductors for efficient conversion of solar to chemical energy application. The quantitative result suggests that the photocatalytic reaction rate increases non-linearly with the metal content due to the plasmonic coupling effects of the neighboring metal nanocrystals, which is consistent with the electromagnetic field simulations. The quantitative understanding achieved in this dissertation represents a major step forward toward the rational design and deterministic synthesis of colloidal metal nanocrystals with the photocatalytic application.

Table of Contents
中文摘要                                                                                                                                           IV
英文摘要                                                                                                                                           V
Chapter
   Introduction                                                                                                                   1
1    Shape-Controlled Synthesis of Colloidal Metal Nanocrystals                                      1
2 Quantitative Analysis of the Reduction kinetics of a Salt Precursor                            7
2.1 Reduction Reaction                                                                                                         7
2.2 Reduction Kinetics                                                                                                          9
2.3 Techniques for Quantifying the Reduction Kinetics                                          11
3 Scope of This Work                                                                                                          15
4 References                                                                                                                         17

   Toward a Quantitative Understanding of the Reduction Pathways of a Salt Precursor in the Synthesis of Metal Nanocrystals                                                        21
1    Introduction                                                                                                                      21
2 Results and Discussion                                                                                                     21
3 Summary                                                                                                                           34
4 Supporting Information                                                                                                  34
5 References                                                                                                                         68

   Autocatalytic Surface Reduction and Its Role in Controlling Seed-Mediated Growth of Metal Nanocrystals                                                                                                      71
1 Introduction                                                                                                                      71
2 Results and Discussion                                                                                                     72
3 Summary                                                                                                                           85
4 Supporting Information                                                                                                  86
5 References                                                                                                                       108

   Quantifying the Thermal Stability of Metal Nanocrystals: An Investigation on the Surface and Bulk Reconstructions of Concave, Multiply-Twinned Icosahedra      113
1 Introduction                                                                                                                    113
2 Results and Discussion                                                                                                   115
3 Summary                                                                                                                         123
4 Supporting Information                                                                                                123
5 References                                                                                                                       126

   Ultrahigh Density Unaggregated Metal Nanocrystals on Semiconductor Nanostructures Function as Photocatalysts for Efficient Conversion of Solar to Chemical Energy                                                                                                            129
1 Introduction                                                                                                                    129
2 Results and Discussion                                                                                                   131
3 Summary                                                                                                                         156
4 Supporting Information                                                                                                157
5 References                                                                                                                       177

   Conclusions and Future Directions                                                                              182
1 Conclusions                                                                                                                     182
2 Future Directions                                                                                                           184
3 References                                                                                                                       185

                                

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