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Title Page 2

Abstract 5

Contents 9

Chapter Ⅰ. Lithium-ion Battery 17

Chapter Ⅱ. A study on the High Capacity Si-C Anode Materials Prepared from anthracite for Lithium Dual-ion batteries 27

1. Introduction 27

2. Experiment 32

2.1. Material synthesis 32

2.2. Material characterization 42

2.3. Electrochemical measurements 43

3. Results and discussion 47

3.1. PAG characterization 47

3.2. Materials characterization 56

4. Conclusion 128

Conclusion 131

Reference 133

List of Tables 15

Table 1. ICP component measurement of Refined anthracite 49

Table 2. ID, IG, ID/IG value from Raman spectra[이미지참조] 64

Table 3. Micro, meso, total pore volume and area of PAG-Si, PAG-Si-ABC,... 68

Table 4. Cycle performance of all samples 79

Table 5. Rate performance of pure Si 84

Table 6. Rate performance of PAG 85

Table 7. Rate performance of PAG-Si 86

Table 8. Rate performance of PAG-Si-ABC 87

Table 9. Rate performance of PAG-Si-ABC-CB 88

Table 10. Long-term cycle performance of all samples at 1A g⁻¹ after rate... 89

Table 11. Rₛ, RSEI, Rcₜ parameter from EIS[이미지참조] 93

Table 12. Cycle performance of 12 mm Full cell at 1 A g⁻¹ and 0.1 A g⁻¹ 111

Table 13. Comparison of cycle results of 12, 14 mm Full cell 112

Table 14. Comparison of Capacity and Energy Density of Previous Lithium-... 116

Table 15. Rate performance of 14 mm Full cell 117

Table 16. The elements spectrum and % ratio of Pristine Full cell in LDIB 125

Table 17. The elements spectrum and % ratio of Full Charge state Full cell... 126

Table 18. The elements spectrum and % ratio of Full Discharge state Full... 127

List of Figures 10

Fig. 1-1. (a) Schematic diagram of a model for inserting anions into graphite... 23

Fig. 2-1. Pulverization process of anthracite powder 34

Fig. 2-2. (a) Froth Flotation for high purity of anthracite powder (Denver... 36

Fig. 2-3. (a) Equipment for Artificial Graphite Manufacturing and (b)... 38

Fig. 2-4. Illustration of the synthesis process for PAG-Si composites via a... 40

Fig. 2-5. (a) SEM image (b) XRD (c) TGA analysis results of anthracite raw... 50

Fig. 2-6. (a) SEM (b) EDS mapping of powder after Froth Flotation 53

Fig. 2-7. (a) SEM images (b) XRD (c) TEM results of Artificial Graphite 54

Fig. 2-8. (a) XRD patterns of PAG-Si, (b) XRD patterns of PAG-Si-ABC-... 55

Fig. 2-9. XPS spectra of PAG-Si-ABC-CB showing (a) survey scan, (b) Si... 60

Fig. 2-10. (a) Raman spectra of 100 nm Si, PAG, PAG-Si, PAG-Si-ABC, and... 63

Fig. 2-11. (a) Nitrogen adsorption-desorption isotherm (linear plot) for all... 67

Fig. 2-12. SEM, TEM, HRTEM, and EDS mapping analyses of (a) PAG, (b)... 72

Fig. 2-13. Cycle voltammetry at 0.2mV s⁻¹ scan rate (a) PAG, (b), PAG-Si,... 75

Fig. 2-14. Voltage profile of (a) Si, (b) PAG, (c), PAG-Si, (d) PAG-Si-ABC,... 78

Fig. 2-15. (a) cycling performance at 0.1 A g⁻¹, (b) rate capability, (c) long-... 81

Fig. 2-16. (a) electrochemical impedance spectroscopy (EIS), (b) charge... 92

Fig. 2-17. (a) Galvanostatic Intermittent Titration Technique (GITT) curves,... 96

Fig. 2-18. (a) Various scan rate cycle voltammetry(VSCAN) from 0.1 to 2.2... 100

Fig. 2-19. Radar plots of properties (a) PAG-Si, (b) PAG-Si-CB-ABC 104

Fig. 2-20. Charge/Discharge mechanism of Lithium Dual Ion Battery... 106

Fig. 2-21. (a) Differential capacity plot of half cell (14mm EG), (b) Voltage... 108

Fig. 2-22. (a) Differential capacity plot of full cell (using 14mm EG) (b)... 110

Fig. 2-23. Ex-situ Raman spectra of (a) PAG-Si-ABC-CB anode, (b) EG... 119

Fig. 2-24. SEM&EDS mapping analysis of (a) Pristine, (b) Full Charge at... 123

초록보기

 Lithium-ion batteries have deeply penetrated our lives, from small batteries to electric vehicles and ESS [1-5]. As people have become accustomed to this lifestyle, they have gradually begun to demand higher capacity, lower prices, and environmental friendliness [6, 7]. In particular, people's awareness of safety has greatly increased due to the recent frequent electric vehicle fires. To satisfy this, research is being conducted to develop materials for lithium-ion batteries. However, since the cathode inevitably contains expensive transition metals [8, 9], there are limits to satisfying the conditions of reducing material costs and being environmentally friendly. Therefore, in this study, research was conducted to improve the performance of lithium dual-ion batteries using carbon-based materials as the cathode and anode. In particular, the anode was made by adding silicon to artificial graphite manufactured by processing anthracite, and the cathode was made by expanding existing graphite. Lithium dual-ion batteries require more research as a next-generation battery because they can satisfy not only environmental friendliness, which is currently the focus of the world, but also high safety, low price, and high energy density [10-13].

Chapter 1 covered the charging and discharging principles, components, characteristics, and previous studies of lithium dual-ion batteries. Chapter 2 reported the manufacturing of anthracite-based artificial graphite, the process of synthesizing active materials by adding silicon, half-cell tests using lithium metal, and lithium dual-ion battery tests using graphite cathode. It is difficult to expect the demand for Korean anthracite to increase due to environmental regulations and changes in heating methods [14-16]. On the other hand, the size of the global anthracite market is expected to grow [17, 18]. Therefore, this study optimized anthracite as an anode material for batteries, which is increasingly being applied, and discovered the possibility of industrialization.

This study synthesized artificial graphite-silicon composites using a simple two-step process of ball milling and annealing. Previous studies on silicon generally adopted a porous structure to alleviate volume expansion [19-22], and the process included complex Mg thermal reduction [19, 22, 23], use of hazardous HF [19, 24], expensive CVD [21,25], and laser methods [26,27]. However, this study secured structural stability by using a material called ammonium bicarbonate (ABC), which theoretically converts to a gaseous form at about 60 degrees, so it does not require a high temperature in the process [28, 29]. In addition, the stability for a low-cost and wide voltage window was secured by using an electrolyte containing LiNO₃ salt [30-32]. A small amount of SiC and SiO₂ present in the active material PAG-Si-ABC-CB was confirmed through XRD and XPS, and a significant change in the specific surface area was observed through BET measurement. The half-cell test results showed the best electrochemical and mechanical performance from GITT with an average capacity of 579.3 mAh g-¹ and a Li+ diffusion coefficient of 6.2 x 10-9 cm² s-¹. Subsequently, in a lithium dual-ion battery test, it showed an initial capacity of 248.1 mAh g-¹ at 0.5 Ag-¹, and an average energy density of 509.9 Wh kg-¹, which is higher than that of previous studies [33-44]. In addition, the changes in the bonding strength and distance between carbon layers due to the insertion/deintercalation of Li+ and PF6- were confirmed through ex-situ analysis. In other words, an anode material with high added value of loaded anthracite coal, thermal stability, light weight, and high recyclability was developed.

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