本研究利用金屬氫氧化物和農業廢棄物衍生的生物炭進行了三種不同複合材料的製備與鑑定，同時作為高性能超級電容器的新穎電極材料。此三種材料包括花瓣狀 Ni(OH)2/茶葉衍生生物炭 (NiNF@TBC)、Co(OH)2/柑橘皮衍生生物炭 (CoNF@OBC) 和海膽狀 Ni-Co 氫氧化物/羅望種子衍生的生物炭 (U-NiCo-OH@TTBC)。研究結果發現複合材料的高度孔洞結構和層化結構有利於電解質離子和電子的擴散和傳輸，從而減少擴散路徑並提高儲能應用的電導率。複合材料中使用的生物炭載體的比表面積在 610 – 1340 m2 g-1 間，相當適合作為能源儲存的基材，同時也可作為綠色碳源。當使用三電極系統和對稱超級電容器裝置評估複合材料的電化學性能時， NiNF@TBC 電極表現出優異的電化學性能，在三電極電池中 1 A g-1 下的比電容為 945 F g-1，10,000 次循環後穩定性高達 95%；而利用 NiNF@TBC 製造的對稱超級電容器在 1 M Na2SO4 溶液中則具有 163 F g-1 的比電容值，且Ragone 圖譜顯示能量密度及功率密度可分別在 19 – 58 Wh kg-1 及 826 – 6321 W kg-1 範圍內。 CoNF@OBC 複合材料在 1 A g-1 下表現出 563 F g-1 的超高儲存能力，並在 10,000 次循環後保持 96% 的電容保持率。而利用CoNF@OBC製作的對稱超級比電容為102 F g-1，其能量密度在10 – 41 Wh kg-1，功率密度則在811~5143 W kg-1間。 U-NiCo-OH@TTBC 複合材料在 1 A g-1 時具有 759 F g-1 的比電容量。對稱性超級電容的功率密度為787~7183 W kg-1，能量密度為16~54 Wh kg-1。此外，此三種不同超級電容器在 10,000 次充放電循環後都顯示出 92 – 94% 的長期循環穩定性。此些結果證明了利用農業廢棄物作為綠色碳源並將其與各種金屬氫氧化物結合，可製備出具有高性能和高穩定性超級電容器應用的奈米材料。而研究也顯示所開發材料與技術具有高成本效益和環境友善的潛能，同時提供更穩定及潔淨的綠色能源。

This study presents a detailed investigation of three different composite materials based on metal hydroxides and agricultural waste-derived biochar as promising electrode materials for high-performance supercapacitors. Specifically, flower-like Ni(OH)2/spent tea leaf-derived biochar (NiNF@TBC), Co(OH)2/orange peel-derived biochar (CoNF@OBC), and urchin-shaped Ni-Co hydroxide/tamarind seed-derived biochar (U-NiCo-OH@TTBC) composites are synthesized and characterized for their electrochemical properties. The highly porous and hierarchical structure of the composites facilitates electrolyte ion and electron diffusion and transport, resulting in a decrease in diffusion path and an increase in conductivity for energy storage applications. The specific surface areas of the biochar supports used in the composites range from 610 m2 g-1 to 1340 m2 g-1, indicating their high potential as green carbon sources for sustainable energy storage. The electrochemical properties of the composites are evaluated using a three-electrode system and symmetric supercapacitor devices. The NiNF@TBC electrode shows excellent electrochemical properties with a specific capacitance of 945 F g-1 at 1 A g-1 in a three-electrode cell and high stability of 95% after 10,000 cycles. The symmetric supercapacitor fabricated with NiNF@TBC delivers a specific capacitance of 163 F g-1 in 1 M Na2SO4 solution. The Ragone plot of the symmetric device exhibits energy density in the range of 19 – 58 Wh kg-1 with power density in the scale of 826 – 6321 W kg-1. The CoNF@OBC composite exhibits an ultra-high remarkable storage capability of 563 F g-1 at 1 A g-1 and maintains 96% capacitance retention after 10,000 cycles. The symmetric device made with CoNF@OBC has a specific capacitance of 102 F g-1, and its Ragone plot shows that its energy density is between 10 and 41 Wh kg-1, and its power density is between 811 and 5143 W kg-1. The U-NiCo-OH@TTBC composite has an outstanding storage capacity of 759 F g-1 at 1 A g-1, with a specific capacitance of 158 F g-1 for the device. The power density of the symmetric device is between 787 and 7183 W kg-1, and its energy density is 16 to 54 Wh kg-1. Furthermore, all three devices show long-term cyclic stability of 92-94% after 10,000 charge-discharge cycles. Overall, these results demonstrate the feasibility of utilizing agricultural waste as a green carbon source and combining it with various metal hydroxides to produce hybrid nanomaterials for high-performance and sustainable supercapacitor applications. The study highlights the potential for cost-effective and eco-friendly energy storage solutions that can contribute to a more sustainable and cleaner future.

Abstract…………………………………………………………………………………………………...I
Acknowledgement……………………………………………………………………………………….V
Abbreviations…………………………………………………………………………………………...VI
Chapter 1. Introduction 1
1.1. Motivation 1
1.2. Overviews of supercapacitor 2
1.2.1. Supercapacitor as one promising energy storage device 2
1.2.2. Evolution of supercapacitor 8
1.2.3. Supercapacitor: Applications 10
1.2.4. Types of supercapacitors 11
1.2.5. Comparison of supercapacitors with other energy storage devices 21
1.2.6. Fundamental requirement of supercapacitor 24
1.3. Limitations of Supercapacitors 26
1.3.1. Low Energy Density: A Major Hurdle for Supercapacitors 26
1.3.2. Impact of low energy density on the storage capacity 28
1.3.3. Strategies to improve the energy density of supercapacitors 29
1.3.4. Metal Oxide-Biochar Composites as a Sustainable Approach 32
1.3.5. Metal Oxide Nanoparticles: Redox Properties and High Specific Capacitance 33
1.3.6. Biochar: Sustainable Carbon-based Material for Electrochemical Applications 35
Chapter 2. Literature Review 38
2.1. Metal oxide 38
2.1.1. Preparation Methods of Metal oxide 39
2.1.2. Electrochemical properties of Metal oxide 41
2.1.3. Metal oxide for supercapacitor production 42
2.2. Biochar 44
2.2.1. Biochar-derived carbon materials 45
2.3. Preparation Methods of Biochar-Derived Carbon Materials 48
2.3.1. Pyrolysis 48
2.3.2. Gasification 50
2.3.3. Hydrothermal carbonization (HTC) 51
2.3.4. Torrefaction 53
2.3.5. Isothermal carbonization 55
2.4. Post-treatment for biochar produced from agricultural waste 57
2.4.1. Activation process 57
2.5. Suitability of agricultural waste biochar in supercapacitor applications 62
2.6. Previous Research on Metal Oxide-Biochar Composites for Supercapacitors. 64
2.7. Aim and objectives 67
2.8. Thesis outline 70
Chapter 3. Material and Methodology 71
3.1. Reagents and chemical 71
3.2. Experimental 71
3.2.1. Preparation of hierarchical TBC 71
3.2.2. Synthesis of NiNF@TBC 72
3.2.3. Synthesis of hierarchical OBC 72
3.2.4. Synthesis of CoNF@OBC 73
3.2.5. Synthesis of hierarchical TTBC 74
3.2.6. Synthesis of U-NiCo-OH@TTBC 74
3.3. Characterization 75
3.3.1. X-ray diffraction………………………………………………………………………………75
3.3.2. Electron microcopy……………………………………………………………………………75
3.3.3. Nitrogen adsorption analysis………………………………………………………………….76
3.3.4. X-ray photoelectron spectroscopy……………………………………………………………76
3.3.5. Raman spectroscopy…………………………………………………………………………..77
3.3.6. Fourier transform infrared…………………………………………………………………...77
3.3.7. Thermal gravimetric analysis…………………………………...............................................77
3.4. Electrochemical analysis 78
Chapter 4. Flower-like nickel hydroxide@tea leaf-derived biochar composite for high-performance supercapacitor application………………………………………………………………………………80
4.1. Characterization of TBC and NiNF@TBC.............................................................................80
4.2. Electrochemical properties of electrodes…………………………………………………….87
4.3. Electrochemical properties of symmetric supercapacitor 96
Chapter 5. Cobalt-Doped orange peel-derived biochar for high-performance supercapacitor application 100
5.1. Characterization of OBC and CoNF@OBC 100
5.2. Electrochemical properties of electrodes 105
5.3. Electrochemical properties of symmetric supercapacitor .113
Chapter 6. Urchin-like binary nickel-cobalt hydroxide @tamarind seed-derived biochar composite for high-performance supercapacitor application 117
6.1. Characterization of TBC and U-NiCo-OH@TTBC 117
6.2. Electrochemical properties of electrode 124
6.3. Electrochemical properties of symmetric supercapacitor 131
Chapter 7: Conclusions and future scope of the work 134
7.1. Conclusion 134
7.2. Future scope of the work 138
References 141

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