此篇論文主要探討以不同方法開發快速充放電鋰離子電池和電化學電容器。第一章與第二章分別為鋰離子電池、電化學電容器的發展背景以及實驗的步驟與方法。
第三章中討論鋰離子電池具奈米結構的陰極，藉由加入石墨烯或鹼改質之氧化石墨烯作為提升導電性的添加劑。現今的鋰離子電池主要是添加碳黑作為幫助導電的添加劑，但是碳黑顆粒很難均勻分散在材料中形成良好的導電網絡，因此只能添加大量的碳黑來改善導電網絡的問題，然而增加碳黑的用量，同時導致電池的比容量下降。本章詳細說明電極成分最佳化的條件，包含調整嵌入材料的比例與粒徑大小以及導電助劑的添加(例：石墨烯與碳黑) ，得以改善材料間的連通與導電性問題，使鋰離子陰極材料 Li(Ni1/3Mn1/3Co1/3)O2 能在高速率充放電下仍有優越的表現。
第二部分主要是以過渡金屬氧化物作為電化學電容器的開發，本篇選擇二氧化錳作為研究材料。二氧化錳是目前受大家關注且具有發展潛力的擬電容材料，由於其離子與電子導電性不佳的限制因素，在實際應用上會受到影響。於第四章探討藉由一個簡單且可被量化的製程，以合成大量具有隨機錯層的二氧化錳。此合成條件促使材料形成無序結構，因而可讓離子在材料中自由移動，不被固相態的擴散所限制，利用相對低溫與鈉離子添加成功抑制了大顆粒且高結晶材料形成，此無序的奈米片狀 Na0.35MnO2 在極高掃速與大電流密度 (1000 mV s-1與200 A g-1) 下具備相當優異的電容維持率。
第五章延續第四章 Na0.35MnO2 的實驗成果，進一步探討不同鹼金屬離子嵌入二氧化錳。結果顯示，在相控制合成上，其關鍵在於較大的非水合鉀離子 (離子半徑：1.52 Å) 等鹼金屬離子，可在形成二氧化錳的層狀結構時作為模板，因而抑制有序層狀結構的形成。而較小的非水合鋰離子(離子半徑：0.9Å) 無法抑制此現象，故形成電化學表現相對較差的相二氧化錳。
在第六章中於水相系統，以 Na0.35MnO2 作為擬電容的正極電極材料，活性碳 (AC) 當作負極，組裝出一非對稱式電化學電容器。藉由調整正負兩極的電荷平衡與添加少量的碳酸氫鈉於0.5 M 硫酸鈉電解液，可以有效抑制二氧化錳的溶解與氫氣的產生，因而能提高至 2.4 V 的電壓同時電容能維持長時間的效能。

This thesis focuses on several approaches for the development of high charge/discharge rate lithium-ion batteries and electrochemical capacitors. The general background of lithium-ion batteries and electrochemical capacitors, and experimental techniques and methods are presented in the Chapter 1 and Chapter 2.
The Chapter 3 in this thesis discusses the development of nanostructured cathodes for lithium-ion battery by introducing graphene or base washed graphene oxide as conductive additive. The carbon black is the most used conductivity enhancing additive in today’s lithium-ion batteries, nevertheless, makes it difficult for carbon black particles to form a wide-ranging “point-to-point” conductive network. Essentially, higher amounts of carbon black should be added in the electrodes to achieve percolation, leading to a lowering of the gravimetric capacity of the battery. Chapter 3 will detail the conditions used to investigate the optimal electrode composition containing different ratios and particle sizes of intercalation material and conductive additives (graphene and carbon black) in order to improve connectivity and conductivity leading to superior performance of a lithium-ion cathode material, Li(Ni1/3Mn1/3Co1/3)O2 at high charge/discharge rates.
The second part of this work is focuses on electrochemical capacitors based on transition metal oxide. Manganese oxide (MnO2) is recognised as promising pseudocapacitive material, however poor ionic and electronic conductivity is the major limiting factor for its practical application. Chapter 4 discuss that through a straightforward and scalable synthesis it is possible to develop a bulk MnO2 material with randomly isolated layers. The synthesis conditions promote the formation of disordered material that allow ion transfer throughout the material that is not limited by solid state diffusion. Relatively low temperatures and inclusion of Na+ disrupt the formation of a highly crystalline material with a large domains size leading to a capacitance of ~200 F g-1 which was maintained at extremely high rates (1000 mV s-1 and 200 A g-1) for disordered Na0.35MnO2 nanosheets.
In Chapter 5, an aqueous asymmetric electrochemical capacitor was assembled with Na0.35MnO2 pseudocapacitive electrode material as the positive electrode and activated carbon (AC) as the negative electrode. The optimisation charge balance between positive and negative electrodes, and modification of 0.5 M Na2SO4 aqueous electrolyte with addition of small amount of NaHCO3, is possible to suppress manganese oxide dissolution and hydrogen evolution, leading to long-term cycling at extended cell voltage of 2.4 V.
In Chapter 6 following the promising results with Na0.35MnO2 within Chapter 4, other alkali metal intercalated MnO2 were investigated. Results show that the inclusion of the larger non-hydrated K+ (ionic radius = 1.52 Å) is key in the phase-controlled synthesis, where alkaline ion can serve as a template in the formation of layered structures of MnO2. Moreover, inclusion of small non-hydrated Li+ (ionic radius = 0.9 Å) was unable to prevent from forming α-MnO2 phase leading to relatively poor electrochemical performance.

Abstract i
中文摘要 iii
Acknowledgements v
List of Figures xii
List of Tables xx
List of Abbreviations xxii
Chapter 1 1
Introduction 1
Brief History of Electricity 3
1.1 Introduction and objectives 6
1.2 Basics of rechargeable lithium-ion battery 13
1.3 Lithium intercalation materials 17
1.3.1 Cathode materials 19
1.3.1.1 Layered lithium metal oxides 20
1.3.1.2 Manganese spinel cathodes 22
1.3.1.3 Phospho-olivine cathodes 24
1.4 Improvement of cathode material performance 26
1.4.1 Lithium mixed transition metal oxides – graphene composites as cathode materials 29
1.5 Fundamentals and applications of electrochemical capacitors 33
1.5.1 Charge storage mechanism of electrical double layer capacitor 34
1.6 Redox based electrochemical capacitors 38
1.6.1 Mechanism of pseudo-capacitive charge storage 38
1.6.2 Asymmetric and hybrid electrochemical capacitors 40
1.6.3 Electrode Materials for electrochemical capacitor 45
1.6.3.1 Carbon Based Material for Electrochemical Supercapacitors 45
1.7 Pseudocapacitive material for electrochemical capacitors 49
1.7.1 Conducting polymers (CPs). 49
1.7.2 Transition metal oxides 50
1.7.2.1 Ruthenium oxide (RuO2) 51
1.7.2.2 Manganese Oxide (MnO2) 53
1.7.2.2.1 Factors affecting the pseudocapacitance of MnO2 54
1.7.2.2.2 Challenges and opportunities for MnOx for electrochemical capacitors. 61
1.8 References 64
Chapter 2 80
Experimental Techniques 80
2.1 Synthetic methods 82
2.1.1 Hydrothermal synthesis 82
2.1.2 Co-precipitation synthesis 83
2.1.3 Resorcinol-formaldehyde gel synthesis 84
2.1.4 Base washed graphene oxide synthesis 85
2.2 Structural characterisation techniques 86
2.2.1 Powder X-ray diffraction 86
2.2.2 Inductively couple plasma optical emission spectroscopy 87
2.2.3 Scanning electron microscopy 88
2.2.4 Transmission electron microscopy 90
2.2.5 Nitrogen adsorption/desorption isotherms 91
2.2.6 Raman spectroscopy 94
2.2.6.1 Experimental procedures of ex situ and in situ Raman spectroscopy 96
2.3 Electrochemical studies set up 99
2.3.1 Fabrication of electrodes for lithium-ion battery cell 99
2.3.2 Fabrication of electrodes for symmetric and asymmetric (full cell) electrochemical capacitor 101
2.4 Basic principles of electrochemical energy storage/conversion 103
2.4.1 Faraday’s Law 104
2.4.2 Cell potential 105
2.4.3 Theoretical cell capacity and capacitance 106
2.4.4 Specific energy and power density 108
2.5 Electrochemical methods 111
2.5.1 Cyclic voltammetry 111
2.5.2 Galvanostatic cycling 113
2.5.3 Rate of charge-discharge and kinetics 114
2.5.3.1 Cyclability 115
2.5.4 Differential capacity plots 116
2.5.5 Electrochemical impedance spectroscopy 118
2.6 Practical electrochemical procedures 121
2.6.1 Potentionstats and battery cycler 121
2.6.2 Electrochemical cells for aqueous electrochemical capacitors 121
2.7 References 123
Chapter 3 126
Electrode Nanostructures of 126
Graphene – Metal Oxide Composites for Lithium-ion Batteries 126
Abstract 129
3.1 Introduction 130
3.2 Experimental methods 133
3.3 Results 136
3.3.1 Structural characterisation of the synthesised Li(Ni1/3Mn1/3Co1/3)O2 136
3.3.2 Structural characterisation of carbon materials 140
3.4 Electrochemical characterisation of the H-CP derived metal oxide Li(Ni1/3Mn1/3Co1/3)O2 and carbon materials 143
3.5 Electrochemical characterisation of the R-F gel derived Li(Ni1/3Mn1/3Co1/3)O2 and carbon materials 152
3.5.1 Electrochemical investigation of R-F derived Li(Ni1/3Mn1/3Co1/3)O2 with 10 μm in lateral dimension of graphenic materials 154
3.5.2 Electrochemical investigation of R-F derived Li(Ni1/3Mn1/3Co1/3)O2 with 5 μm in lateral dimension of graphenic materials 156
3.5.3 Electrochemical investigation of R-F derived 88 wt% Li(Ni1/3Mn1/3Co1/3)O2 with graphenic materials 157
3.6 Discussion and concluding remarks 159
3.7 Further work 166
3.8 References 167
Chapter 4 171
Manganese Dioxide Compounds as a Pseudocapacitance Material for Energy Storage 171
Abstract 173
4.1 Introduction 174
4.2 Experimental details 177
4.3 Structural characterisation of α-MnO2 179
4.4 Electrochemical characterisation of α-MnO2 184
4.5 Structural characterisation of Na0.15MnO2 189
4.6 Electrochemical characterisation of Na0.15MnO2 195
4.7 In situ Raman Spectroscopy of Na0.15MnO2 material 198
4.8 Structural characterisation of Na0.35MnO2 203
4.9 Electrochemical characterisation of Na0.35MnO2 213
4.10 Performance of Na0.35MnO2 with different mass loadings 217
4.11 In situ Raman spectroscopy of Na0.35MnO2 material 225
4.12 Discussion 229
4.13 Conclusions 232
4.14 Future work 234
4.15 References 235
Chapter 5 241
Asymmetric Electrochemical Capacitor 241
Abstract 243
5.1 Introduction 244
5.2 Experimental methods 246
5.3 Results and discussion 248
5.3.1 Charge balance calculation for asymmetric type electrochemical capacitor 248
5.3.2 Electrochemical characterisation of asymmetric capacitor in 0.5 M Na2SO4 electrolyte 252
5.3.3 Electrochemical characterisation of asymmetric capacitor in 0.5 M Na2SO4 with additive of 2mM NaHCO3 electrolyte 256
5.4 Concluding remarks and future work 265
5.5 References 267
Chapter 6 269
Future work 269
Optimising Alkali Metal Enriched MnO2 as a Pseudocapacitive Material 269
Abstract 271
6.1 Introduction 272
6.2 Experimental details 273
6.3 Structural characterisation of LixMnO2 275
6.4 Electrochemical characterisation of Li0.01MnO2 278
6.5 Structural characterisation of KxMnO2 280
6.6 Electrochemical characterisations of K0.11MnO2 and K0.35MnO2 288
6.7 Discussion 292
6.8 Future work 295
6.9 References 297
Chapter 7 299
Summary and Further Work 299
7.1 Summary 301
7.2 Further work 302
Appendix 305
Summary of the Research Papers and Conference Presentations 310

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