臺灣博碩士論文加值系統

本研究主要將銅鋅錫硫(CZTS)四元材料於能源元件上之應用，能源材料包括能源轉換與能源儲能材料。然而尋找製程便宜簡單，易調控四元比例及奈米結構的製程條件以及材料本身具有化學及物理的穩定性為主要的開發的目標。故本論文以溶劑熱合成法經由改變操作條件來使其製程參數最適化(e.g. 溫度, 硫之比例, 反應步驟及時間)。接著以鋰離子電池為主要研究系統，利用各種分析儀器(臨場及非臨場)之解析能力探討銅鋅錫硫(CZTS)材料於電解液系統中穩定性及高效能。
第一部份為銅鋅錫硫作為電極材料之鑑定及穩定性探討，研究主要是藉由溶劑熱合成法製備無機材料，其必需具有良好的結晶性、反應穩定性和表面親疏水性；在此我們藉由引進奈米環境網於我們材料中；此概念來自於生態工法的修護方法,製備其我們的銅鋅錫硫電極材料,而成長使用的溶劑為乙二醇。當基板經由的奈米環境網修飾可以使材料具有較佳的機械以及化學穩定性等特性。主要由於成長的奈米結構本身具有孔洞使其不論是液體的流動或者氣體的產生的應力，可經由孔洞分散其外在的影響，另外使用乙二醇為我們成長之溶劑可使表面具親水性，使得應用於電解液為極性溶劑有較佳的潤濕性。
第二部份為利用上述的優點，當此結構製備電極材料於鋰離子電池中，在長效的測試時結果可得到， 經過修飾後的基板經過100 cycles後結構幾乎無變化，證明了修飾後的電極材料具有較佳的化學穩定性，另外最適化鋰電池負極材料經由長效測試及倍率性測試都可獲得較佳的結果(Specific capacity of 1400 mAhg-1 with retention of about 100% after 450 cycles)。而這部分經由非臨場的XPS分析技術驗證可得到由於金屬(銅及鋅)的導入於二硫化錫的系統中，有效使得二價的銅離子易完全的氧化還原，並不會造成一價的銅離子溢於電解液中造成電池穩定度下降，另一方面由非臨場的XRD分析技術驗證銅鋅錫硫特殊結構以及觸媒特性使得當經過長時間的充放電，反應過後其負極材料還具有結晶性，此跟現今負極材料(矽或錫)相比有其優異性於鋰離子電池中。
最後由於使用此方法不僅可以長在不同的基板上使其應用面較廣，另外本身具有較佳的光觸媒特性，當我們將材料製備於可撓式的碳材或者金屬箔亦或者是透明導電玻璃上應用於水分解中以及還原二氧化碳的結果中可得到不錯的產氫電流及還原產物選擇率，在初試結果中可得到當Voc為-0.27時可得到產氫電流為-1.53 mAcm-2，在此論文不僅僅探討了奈米環境網對於結構以及元件穩定性的影響也希望透過此概念能夠在未來的能源相關產業都能夠有所發揮及斬獲。

Nowadays CZTS is widely used as absorber layer or electrode material for a variety of applications. Despite its popularity, there is still a need to look for a cheaper and easier way to obtain CZTS with its unique structures and better chemical and physical stability. In this study, the solvothermal process was used to synthesize the CZTS from a low-cost and abundant source viz. copper, zinc, tin and sulfur precursor. The reaction pathway was optimized by monitoring the process and observing the various effects of the variable parameters such as temperature, sulfur ratio, reaction time and step. Using various analytical tools, a better understanding of the reaction process is highlighted. The tuning of sulfur ratio i.e., from 2112 to 2116 in the solvothermal process allowed us to synthesize different CZTS nanostructures for energy applications. For higher sulfur ratio, CZTS could easily aggregate to form nanosphere cluster. Finally, we found that the optimized sulfur ratio was 2115 that could form the CZTS nanostructures.
Since most of the electrode materials including CZTS known to require better crystallinity, reaction stability and surface wettability for the electrolyte system. Ecological engineering methods (EEM) inspired nanostructures offers great promises in the fabrication of electrode materials that are difficult to engineer through the conventional approaches. Here, we utilize this concept for the synthesis of hierarchical porous single crystalline CZTS nanowall arrays (NWAs) on arbitrary substrates. The CZTS nanocrystals with hierarchical structured porous material showed the hydrophilic behavior that helps CZTS nanocrystals to be used in electrolyte system such as dye-sensitized solar cells with the prepared counter electrode, lithium-ion batteries with a high specific capacitance and outstanding cycling stability.
Further we investigating CZTS nanowalls, a cascade mechanism are highlighted in improving the lithium ion storage performance of transition metal sulfides anodes. An ultrahigh and stable capacity, 1400 mAh g-1 at a current density of 1000 mA g-1, was achieved over 400 cycles; besides, the rate capability of CZTS nanowalls is also remarkable, which can be charged within 1 min and deliver a capacity of 495 mAg g-1. The special lithium ion storage mechanism in mixed metal chalchogenide is proposed in this dissertation. In short, a combinational redox reaction from metal sulfides to lithium sulfides, highly porous nanosturctures and proper composition of transition metals lead to excellent and stable lithium ion storage performance. Our results and proposed strategies provide useful guidance and open an opportunity to the design of anode materials for next generation lithium ion batteries
Finally, the CZTS nanostructures could be extended its application to the photocatalytic activity system due to the superior light harvesting behavior. Initial photoelectrochemical water splitting data have shown that a photocurrent density of -1.53 mAcm-1 at -0.27 V versus RHE under illumination of AM 1.5 and catalytic reduction of carbon dioxide (CO2) for the sunlight-driven conversion of CO2 into alcohol under irradiation by AM 1.5 simulated sunlight. Such a highly integrated template and ligand free electrodes made by directly growing photoactive CZTS porous nanowalls on arbitrary substrates. The CZTS NW would be expected to give a great impetus to applicable to any kind of electrodes and will open the door to the new possibility that make commercially viable attractive energy technologies.

Chinese Abstract (中文摘要) III
Abstract V
Acknowledgement VII
Table of Contents IX
List of Abbreviations XIII
List of Figures XIV
List of Tables XIX
Chapter 1 Introduction and Motivation 1
1.1 Preface 1
1.1.1 Global Energy Challenge 1
1.1.2 The Need of Electrochemical Energy Storage (EES) System 2
1.1.3 The Choices of Batteries 4
1.2 General Introduction of Lithium Ion Battery (LIB) 5
1.2.1 Basic Principle of Lithium Ion Battery 5
1.2.2 Major Configuration of Lithium Ion Battery 6
1.3 Cathode Material (Positive electrode) in Lithium Ion Battery 8
1.4 Anode Material (Negative electrode) in Lithium Ion Battery 9
1.4.1 Intercalation/de-intercalation materials 11
1.4.2 Alloy/de-alloy materials 11
1.4.3 Conversion materials 12
1.5 Electrolyte in Lithium Ion Battery 14
1.6 Copper Zinc Tin Sulfide (CZTS) as an Anode Material 15
1.6.1 Properties of CZTS 15
1.6.2 Crystal Structure of CZTS 16
1.7 Overview Dissertation 18
1.7.1 The Reason Why CZTS 18
1.7.2 Issues with CZTS 18
1.7.3 Aim and Objective of the Study 19
1.7.4 Dissertation Structure . 20
Chapter 2 Background, Concepts and Literature Review 22
2.1 Development of Synthetic Transition Metal Chalcogenides Methods 22
2.1.1 Crucial parameters governing solvo-thermal reactions 24
2.1.1.1 Chemical parameters 24
2.1.1.2 Physical parameters 25
2.2 Degradation Study and Mechanism of TMCs in Lithium Ion Battery 26
2.2.1 Lithiation Mechanism 26
2.2.2 Electrolyte compatibility (Effect of polysulfides shuttling) 27
2.2.3 Voltage hysteresis 29
2.2.4 Unambiguous excess capacity 30
2.3 Engineering TMCs for Lithium Ion Battery 31
2.3.1 Systematic evolution in structure and morphology 32
2.3.2 Carbon-Materials-Supported Electrode Materials 33
2.3.3 Depositing Passivation Layers 34
2.4 Geogrid-Inspired Technique 36
Chapter 3 Methodology 39
3.1 Experimental Section 39
3.1.1 Materials 39
3.1.2 Fabrication of CZTS Nanogeogrid 39
3.1.3 Fabrication of the CZTS nanowall with and without nanogeogrid 40
3.2 Instrumentation for Characterization 41
3.2.1 X-ray Diffraction analysis (XRD) 41
3.2.1.1 Experimenatal Considerations 42
3.2.2 Confocal Micro-Raman Spectroscopy 43
3.2.2.1 Metal Sulfide Material 44
3.2.2.2 Experimenatal considerations 44
3.2.3 Scanning Electron Microscope with EDS analysis 45
3.2.4 Transmission Electron Microscope with SAED and EDS analysis 46
3.2.4.1 Experimenatal considerations 47
3.2.5 X-ray Photoelectron Spectrometer (XPS) 47
3.2.5.1 Experimenatal considerations 48
3.2.6 Brunauer–Emmett–Teller (BET) 48
3.2.7 Nanoindenter setup 49
3.3 Battery Test and Electrochemical Setup . 50
3.3.1 Battery Test 50
3.3.2 Cyclic Voltammetry (CV) 52
3.3.3 Electrocheical Impedance Spectroscopy (EIS) 53
Chapter 4 Results and Discussion 55
4.1 Synthesis and Optimization of CZTS Nanostructures for understanding its growth mechanism and Suitable application in Lithium ion Battery 55
4.1.1 Fabrication of CZTS NWD and NOD 55
4.1.2 Growth Mechanism study 60
4.1.2.1 The rationality of choosing precursor ratio of C:Z:T:S for the growth of nanogeogrid and nanowall 60
4.1.2.2 Formation mechanism of CZTS NWD and NOD 62
4.1.3 Mechanical and Electrochemical Study 66
4.1.4 BET Study (Nitrogen adsorption–desorption isotherms) 71
4.1.5 Summary 72
4.2 CZTS NWD as Anode Material for Lithium-Ion Batteries 72
4.2.1 Introduction 72
4.2.2 Lithium-Ion Batteries Behavior 75
4.2.3 Structure and Properties of Electrode Materials after Cycling 81
4.2.3.1 Structure Evolution of CZTS nanowalls 82
4.2.3.2 Ex situ XPS analyses 85
4.2.4 Mechanistic Insights of CZTS Nanowall in LIBs 88
4.2.5 Summarys 91
Chapter 5 Conclusion and Perspectives 94
5.1 Conclusion 94
5.2 Perspectives 96
5.2.1 Low-temperature electrochemical performance in LIBs 96
5.2.2 Wearable photoelectric devices 97
5.2.3 Counter electrode material in DSSCs 98
5.2.4 Photocathode material in HER (Hydrogen evolotion reaction) 100
5.2.5 Photocatalyst for CO2 reduction 102
Reference 104
Appendix 123
Curriculum Vitae 125

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