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
1. Introduction 1
1.1 Shape-Controlled Synthesis of Colloidal Metal Nanocrystals 1
1.2 Quantitative Analysis of the Reduction kinetics of a Salt Precursor 7
1.2.1 Reduction Reaction 7
1.2.2 Reduction Kinetics 9
1.2.3 Techniques for Quantifying the Reduction Kinetics 11
1.3 Scope of This Work 15
1.4 References 17

2. Toward a Quantitative Understanding of the Reduction Pathways of a Salt Precursor in the Synthesis of Metal Nanocrystals 21
2.1 Introduction 21
2.2 Results and Discussion 21
2.3 Summary 34
2.4 Supporting Information 34
2.5 References 68

3. Autocatalytic Surface Reduction and Its Role in Controlling Seed-Mediated Growth of Metal Nanocrystals 71
3.1 Introduction 71
3.2 Results and Discussion 72
3.3 Summary 85
3.4 Supporting Information 86
3.5 References 108

4. Quantifying the Thermal Stability of Metal Nanocrystals: An Investigation on the Surface and Bulk Reconstructions of Concave, Multiply-Twinned Icosahedra 113
4.1 Introduction 113
4.2 Results and Discussion 115
4.3 Summary 123
4.4 Supporting Information 123
4.5 References 126

5. Ultrahigh Density Unaggregated Metal Nanocrystals on Semiconductor Nanostructures Function as Photocatalysts for Efficient Conversion of Solar to Chemical Energy 129
5.1 Introduction 129
5.2 Results and Discussion 131
5.3 Summary 156
5.4 Supporting Information 157
5.5 References 177

6. Conclusions and Future Directions 182
6.1 Conclusions 182
6.2 Future Directions 184
6.3 References 185

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