用於鋰離子無負極電池之高濃電解液｜國立臺灣科技大學博碩士論文系統

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研究生：	舒嘉應 RIF ATUSSAUFIYAH
論文名稱：	用於鋰離子無負極電池之高濃電解液 Highly Concentrated Electrolyte for Lithium Ion Anode Free Battery
指導教授：	黃炳照 Bing-Joe Hwang
口試委員:	蘇威年 Wei-Nien Su 程敬義 Jim Cherng
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	160
中文關鍵詞：	無負極電池、高濃度電解液、含氟溶劑、LiNO3 、KNO3
外文關鍵詞：	Anode Free, Highly Concentrated Electrolyte, Fluorinated Solvent, LiNO3, KNO3
相關次數：	點閱：273 下載：0
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近年，發展了一種新型態可充放鋰離子電池，稱為無負極電池。其最大優勢在於電池負極端僅有電流收集器的存在，能量密度非常高。但目前仍有許多問題需要克服，尤以鋰枝晶的形成與電解液的分解最迫切需要被克服，此會顯著影響電池性能，循環壽命大幅降低。在眾多研究中，其中一種策略是使用高濃度電解液 (High concentrated Electrolyte, HCE) ，即相比一般電解液加入更多鹽類以提升電解液濃度。
這項研究中主要目的是提升商業化LiTFSI DME/DOL(1:1)電解液在無負極電池之效能，藉由提升LiTFSI鹽類濃度,來克服前述問題。鹽類濃度由原本的1.3m提升至2.6m、3.9m與5.2m。為了再進一步改善HCE系統效能，嘗試添加10%(v/v)含氟溶劑1,1,2,2-Tetrafluoroethyl 2,2,3,3-tetrafluoropropyl ether (TTE)及Fluoroethylene carbonate (FEC),不僅如此,還另外添加少量(0.025、0.05、0.1% (w/w) ) LiNO3與(0.05%(w/w)) KNO3等固體添加劑。上述所有電解液組成會藉由充放電測試、SEM、Raman光譜檢測所有電解液組合,並利用XPS吸收光譜分析SEI組成分。
在上述電解液組成中顯現出效率最高為5.2m LiTFSI DME/DOL 添加10%(v/v) FEC與0.05%(w/w) LiNO3，第一圈之庫倫效率達到94.1%。這種改進是來自於高HCE溶液中陽離子與陰離子強力配位,像是Contact-Ion-Pair(CIP)與Aggregated-Ion-Pair(AIP)。除此之外,與一般稀釋電解液相比,高濃度電解液形成之SEI含有FEC和鹽類與陰離子分解後的產物,更加有助於保護電池並提升循環壽命。

A type of rechargeable lithium ion battery called anode-free battery was recently developed. The cathode-to-anode ratio of this battery is one, making it a quite phenomenal energy storage. Several important challenges that need to be addressed in the Cu|LFP anode free cell are the formation of lithium dendrite and the electrolyte decomposition. Both challenges can substantially affect the cycling performance of the cell. One strategy to mitigate these challenges is by utilizing a Highly Concentrated Electrolyte (HCE). HCE has an increased salt-to-solvent ratio compared to a dilute electrolyte.
This study aims to improve the performance of commercial 1.3m LiTFSI in DME/DOL (1:1) electrolyte in the Cu|LFP anode free cell. This was done by increasing the salt-to-solvent ration of LiTFSI in the DME/DOL (1:1) solution. The concentrations of HCE that were used are 2.6m, 3.9m, and 5.2m. To further improve the performance, a 10% (v/v) fluorinated solvents (TTE and FEC) and a small amount of salt additives (0.025, 0.05, 0.1 % (w/w) LiNO3 and 0.05% (w/w) KNO3) were added. Each electrolyte combination was tested using a charge-discharge test, SEM, Raman Spectroscopy, and the SEI layer components were checked using the XPS analysis.
The best cycling performance was shown by a combination of 5.2m LiTFSI/DME/DOL with 10% (v/v) FEC, and 0.05% (w/w) LiNO3 in which the initial coulombic efficiency was 94.10%. Such improvement came from the strong cation-anion coordination within the solution structure of HCE such as the Contact-Ion-Pair (CIP) and Aggregated-Ion-Pair (AIP). In addition to that, the formed SEI layer in HCE cell is more effective compared to the dilute electrolyte. The SEI layer components contain the FEC and salt-anion decomposition products.

Table of Contents

Abstract        i
摘要        ii
Acknowledgements    iii
Table of Contents    iv
List of Figures        vii
List of Tables        xii
List of Abbreviations    xv
Chapter 1 Introduction    1
1.1    Background    1
1.1.1    Objectives of Study    2
1.2    Rechargeable Battery    3
1.3    Battery Components    5
1.3.1    Electrode Materials    7
1.3.2    Separator    10
1.3.3    Electrolyte    11
1.4    Analysis Technique of the Electrochemical Performance    21
1.4.1    Charge-Discharge Test    21
1.4.2    Impedance Measurement    22
1.4.3    Scanning Electron Microscope (SEM)    23
1.4.4    Raman Spectroscopy    24
1.4.5    X-ray absorption spectroscopy (XPS)    25
Chapter 2 Experimental Method    27
2.1    Samples Preparation    27
2.1.1    Salt and Additive Drying    27
2.1.2    Molecular Sieve Drying    28
2.1.3    Solvents Drying    28
2.1.4    Electrolyte Fabrication    29
2.1.5    Copper Foil Preparation    35
2.1.6    LFP Cathode Preparation    36
2.1.7    Coin Cell Preparation    37
2.1.8    Coin Cell Assembly    38
2.1.9    SEM (Scanning Electron Microscope) Sample Preparation    41
2.1.10    Raman Electrolyte Scan Sample Preparation    41
2.1.11    XPS Scan Sample Preparation    42
2.2    Tests and Analysis    43
2.2.1    Charge-Discharge Tests    43
2.2.2    Impedance Test    47
2.2.3    SEM (Scanning Microscopy Electron) Scan    47
2.2.4    Raman Electrolyte Scan    48
2.2.5    XPS (X-Ray Photoelectron Spectroscopy) Scan    48
Chapter 3 Result and Discussion    49
3.1    Highly Concentrated Electrolyte (HCE) in Anode Free Battery    49
3.1.1    Electrochemical Performance    49
3.1.2    SEM (Scanning Electron Microscope) Surface Morphology Result    61
3.1.3    Raman Spectroscopy Result    65
3.1.4    XPS (X-ray Photoelectron Spectroscopy) Result    73
3.1.5    Summary of the HCE Study    78
3.2    Highly Concentrated Electrolyte (HCE) with Fluorinated Solvent (FS) as Diluent in Anode Free Battery    80
3.2.1    Electrochemical Performance    80
3.2.2    SEM (Scanning Electron Microscope) Surface Morphology Result    89
3.2.3    Ionic Conductivity Result    91
3.2.4    Raman Spectroscopy Result    92
3.2.5    XPS (X-ray Photoelectron Spectroscopy)    95
3.2.6    Summary of the HCE and Fluorinated Solvent Study    100
3.3    Highly Concentrated Electrolyte (HCE) with Fluorinated Solvents (FS) and Salt Additive (SA) in Anode Free Battery    103
3.3.1    Electrochemical Performance    103
3.3.2    SEM (Scanning Electron Microscope) Morphology Result    116
3.3.3    XPS (X-ray Photoelectron Spectroscopy) Result    119
3.3.4    Summary of the HCE combined with FS and Salt Additive Study    121
Chapter 4 General Conclusions and Recommendations    123
References        125
Appendices        130
Appendix A    Methodology Flow Diagrams    131
Appendix A.1    Salt and Additive Drying Flow Diagram    131
Appendix A.2    Molecular Sieve Drying Flow Diagram    132
Appendix A.3    Solvents Drying Flow Diagram    133
Appendix A.4    Electrolyte Fabrication Flow Diagram    134
Appendix A.5    Copper Foil Preparation Flow Diagram    135
Appendix A.6    Coin Cell Preparation: LFP Cathode Preparation Flow Diagram    136
Appendix A.7    Coin Cell Preparation: Separator Preparation Flow Diagram    137
Appendix A.8    Coin Cell Preparation: Cu-Foil Preparation Flow Diagram    138
Appendix A.9    Coin Cell Components Washing Flow Diagram    139
Appendix A.10    Coin Cell Preparation: Coin Cell Assembly    140
Appendix A.11    SEM Sample Preparation Flow Diagram    141
Appendix A.12    Raman Electrolyte Scan Sample Preparation Flow Diagram    142
Appendix A.13    Impedance Sample Preparation Flow Diagram    143
Appendix A.14    XPS Scan Sample Preparation Flow Diagram    144
Appendix B    Arbin Schedules    145
Appendix B.1    Arbin Schedule for Li|Cu Charge Discharge Schedule    145
Appendix B.2    Arbin Schedule for Li|LFP and Cu|LFP Charge Discharge Schedule    146
Appendix B.3    Arbin Schedule for Cu|LFP with Rested Step Charge Discharge Schedule    147
Appendix B.4    Arbin Schedule for SEM Cu|LFP Charge Discharge Schedule    149
Appendix B.5    Arbin Schedule for SEM Li|Cu Charge Discharge Schedule    150
Appendix B.6    Arbin Schedule for XPS Cu|LFP Charge Discharge Schedule    151
Appendix C    Calculations    152
Appendix C.1    Calculation of Electrolyte Concentrations    152
Appendix C.2    Calculation of LiTFSI Mass Added to Make Different Electrolyte Concentrations    153
Appendix C.3    Calculation of FEC and TTE Volume    155
Appendix C.4    Calculation of the Impedance Measurement    156
Appendix C.5    Calculation of LiNO3 Mass Additive with Different Concentrations    158
Appendix C.6    Calculation of KNO3 Mass Additive with Different Concentrations    160

                                

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