有效率的使用金屬氧化物異質結構作為光水解產氫反應之催化劑的研究近來日益增長，而文獻上氧缺陷在增強光電化學反應效率的上亦為一個關鍵因子。有關氧缺陷數量多寡與合成材料時真空條件之關聯性的研究甚少。本研究透過在不同真空條件之系統下合成二氧化錫/三氧化二銦異質結構作為光水解產氫之催化劑，探討不同真空條件合成出之異質結構對於產氫效率之影響。
二氧化錫/三氧化二銦之異質結構可藉由爐管系統(底壓:100 Pa)合成或透過超高真空臨場電子顯微鏡(底壓: 5 x 10-8 Pa)成長且異質結構合成時之微結構變化可藉由熱力學及清晰的直接觀察影像來解釋。在超高真空系統下所合成出之二氧化錫/三氧化二銦之異質結構利用X射線光電子光譜及螢光光譜分析後，可歸納出異質結構內部氧缺陷數量在超高真空製程下可被減少。進一步使用兩種不同真空製程條件之異質結構作為光催化劑進行光水解產氫實驗，產氫效能的結果顯示使用超高真空系統製程之異質結構有最佳表現，並將此結果歸納於異質結構內部有較多氧空缺所致。
這些結果顯示利用異質結構作為光催化劑有助於提升光水解產氫之效能。此外，在適當的條件下使用超高真空系統合成異質結構，可以增加異質結構內部氧缺陷的數目，亦有助於提升光水解產氫的效能。

Photocatalyic water splitting with metal oxide heterostructure as photocatalysts has been a valuable and efficient hydrogen production method in recent years. Previous studies have shown that oxygen vacancies formed in photoelectrochemical reactions play an important part in the efficiency enhancement. However, the relation between the oxygen vacancy formation and the vacuum level of synthesis system has not been investigated. In this work, SnO2-x/In2O3-y heterostructures, as water splitting photocatalysts, were prepared in the synthesis systems with different vacuum levels. A series of in situ transmission electron microscope (TEM) observation had been carried out, observing the detailed changes during SnO2-x/In2O3-y heterostructures formation, basically following the thermodynamic rules. X-ray photoelectron spectroscopy, photoluminescence measurements and in situ TEM observations indicate that the amount of oxygen vacancies increase in SnO2-x/In2O3-y heterostructures synthesized in ultra-high vacuum (UHV) system compared to SnO2-x/In2O3-y heterostructures formed in a low vacuum furnace. The observed 25~30% higher hydrogen production efficiency in SnO2-x/In2O3-y heterostructures formed in UHV comparing with SnO2-x/In2O3-y heterostructures formed in furnace ambient is attributed to presence of the more abundant oxygen vacancies. The results indicate that an optimized heterostructured photocatalyst can be designed by controlling the vacuum level in the synthesis process.

Contents
Abstract I
摘要 II
Contents III
Acknowledgments VII
Chapter 1 Introduction 1
1.1 Overview of Nanotechnology 1
1.2 Heterostructure 2
1.2.1 Overview of Heterostructure 2
1.2.2 Axial Heterostructure Nanowires 3
1.2.3 Radial Heterostructure Nanowires 4
1.3 In situ Transmission Electron Microscopy 6
1.3.1 Transmission Electron Microscopy (TEM) 6
1.3.2 In situ Transmission Electron Microscopy 8
1.4 The Gibbs Free Energy 9
1.5 Photocatalytic Water Splitting 10
1.6 Scope and Organization of the Thesis 12
Chapter 2 Experimental Section 13
2.1 Experimental Procedures 13
2.1.1 Synthesis of SnO2 Nanowires 14
2.1.2 Fabrication of SnO2-x/ In2O3-y Heterostructure in Furnace Ambient 16
2.1.3 Fabrication of SnO2-x/ In2O3-y Heterostructure under UHV condition 16
2.1.4 Measurement of Optical Properties with Different Defects Level SnO2-x/ In2O3-y Heterostructure Devices 18
2.1.5 Measurement of Hydrogen Production Efficiency in SnO2-x/ In2O3-y Heterostructure 18
2.2 Experimental Details 19
2.2.1 Furnace Setup 19
2.2.2 Three-axis Oil Hydraulic Micromanipulator 19
2.2.3 Electron Beam Evaporation System 20
2.2.4 X-ray Diffractometer 21
2.2.5 Scanning Electron Microscope (SEM) 21
2.2.6 Transmission Electron Microscope (TEM) 22
2.2.7 UHV in situ TEM System 22
2.2.8 Energy Dispersive X-ray Spectrometer (EDS) 23
2.2.9 X-ray Photoelectron Spectroscopy (XPS) 23
2.2.10 Photoluminescence System (PL) 24
2.2.11 Gas Chromatography (GC) 24
Chapter 3 Fabrication of SnO2-x/ In2O3-y Heterostructure under Different Vacuum Level Conditions 26
3.1 Introduction and Motivation 26
3.2 Results and Discussion 28
3.2.1 Analysis of SnO2 Nanowires 28
3.2.2 Synthesizing SnO2-x/In2O3-y Heterostructures in Furnace Ambient and under UHV in situ TEM 32
3.3 Summary and Conclusions 43
Chapter 4 Optical Properties of SnO2-x/ In2O3-y Heterostructure under Different Vacuum Level Conditions 44
4.1 Introduction and Motivation 44
4.2 Results and Discussion 45
4.2.1 The PL Measurements 45
4.2.2 The XPS analysis 48
4.3 Summary and Conclusions 50
Chapter 5 Water Splitting with SnO2-x/ In2O3-y Heterostructures 51
5.1 Introduction and Motivation 51
5.2 Results and Discussion 53
5.2.1 Hydrogen Production by SnO2-x/ In2O3-y Heterostructures with Different Amount of Oxygen Vacancy 53
5.2.2 Hydrogen Production with Large-Area Thin Film SnO2-x/ In2O3-y Heterostructures 58
5.3 Summary and Conclusions 64
Chapter 6 Summary and Conclusions 65
6.1 Fabrication of SnO2-x/ In2O3-y Heterostructure under Different Vacuum Level Conditions 65
6.2 Optical Properties of SnO2-x/ In2O3-y Heterostructure under Different Vacuum Level Conditions 67
6.3 Water Splitting with SnO2-x/ In2O3-y Heterostructures Synthesized under Different Vacuum Conditions 68
Chapter 7 Future Prospects 69
7.1 Observation of Phase Transformation in Real Time and Control the Phase Formation in SnO2-x/ In2O3-y Heterostructures 69
7.2 SnO2-x/ In2O3-y Heterostructures for Lithium Ion Battery Electrode 72
References 73

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