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研究生： Atetegeb Meazah Haregewoin
Atetegeb - Meazah Haregewoin
論文名稱： Investigation of Surface Reactions on Negative Electrodes of Lithium Ion Batteries Using Infrared Spectroscopy
Investigation of Surface Reactions on Negative Electrodes of Lithium Ion Batteries Using Infrared Spectroscopy
指導教授： 林昇佃
Shawn D. Lin
口試委員: 黃炳照
Bing-Joe Hwang
江志強
Jyh-Chiang Jiang
王復民
Wang, Fu-Ming
吳乃立
Nae-Lih Wu
潘金平
Jing-Pin Pan
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2013
畢業學年度： 101
語文別： 英文
論文頁數： 172
中文關鍵詞： SEI 、spectroelectrochemical cell 、in situ DRIFTS 、ATR 、maleimide 、additives 、impedance 、FTIR 、superoxide radical 、oxygen imputity 、EC 、PC 、DEC 、electrolyte composition 、lithium ion battery
外文關鍵詞： SEI, spectroelectrochemical cell, in situ DRIFTS, ATR, maleimide, additives, impedance, FTIR, superoxide radical, oxygen imputity, EC, PC, DEC, electrolyte composition, lithium ion battery
相關次數： 點閱：370  下載：2 
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    • The solid electrolyte interface formation process during the first charging/discharging of lithium ion battery consumes lithium ions permanently and results in an irreversible capacity. In this work, analysis of the SEI composition and formation mechanism in different electrolytes and electrolyte additive is performed using infrared spectroscopic and characterization techniques including microscopic and electrochemical techniques. The effect of trace amount of oxygen in the reduction of propylene carbonate (PC) is shown by combining CV, FTIR and XPS analysis. ATR-FTIR analysis, performed inside a glove box, confirms the formation of solvated Li2CO3 and (R-OCO2-Li(PC)2)2 due to propylene carbonate (PC) reduction in the potential range from OCV to -0.1 V. Our experimental results suggest that in the potential range from OCV to 1.6 V, PC, in the presence of O2, can be easily decomposed by the superoxide ion through a nucleophilic attack at the ethereal carbon atom and form (PC)2LiOC(O)OCH(CH3)CH2OLi(PC).
    A direct comparison of the reduction of PC, EC and DEC as single, binary and ternary solvent systems is studied. ATR-FTIR performed in a glove box after LSV indicates that the reduction behavior of an alkyl carbonate is not significantly influenced by the presence of other alkyl carbonate. (CH(CH3)CH2OCO2Li)2 and Li2CO3 are formed due to PC reduction, EC is reduced to (CH2OCO2Li)2 and Li2CO3, and DEC reduction leads to the formation of (CH2=CH-OCO2CH2CH3)Li. The reduction product of EC is responsible for the formation of a passivating surface film which prevents exfoliation caused by PC. We have designed a spectroelectrochemical cell which is compatible with our DRIFTS spectrometer and can work effectively for in-situ analysis of the SEI layer in a half cell mode of lithium ion battery. The electrochemical performance of the cell is tested with both aqueous and non-aqueous systems and the results confirm the good applicability of the cell for electrochemical reactions. The effectiveness of the specroelectrochemical cell for FTIR analysis of SEI layer is confirmed by comparing the results with ATR-FTIR experiments performed in a glove box. The reduction products and SEI formation mechanism of N,N’-1,4-phenylenedimaleimide (MI-2) is examined with 0.1% MI-2 in 1 M LiPF6/PC, 1 M LiPF6/ EC:PC (3:2) and 1 M LiPF6 in EC:PC:DEC (3:2:5) systems. The CV results reveal that MI-2 reduction occurs prior to the solvents whose reduction in the binary and ternary solvent systems is suppressed by MI-2. However, in the single solvent system, PC co-intercalation and reduction could not be inhibited even in the presence of MI-2. FTIR confirms that ring opening of maleimide group occurs in the binary and ternary solvent system but not in the single solvent system.
    In this work, we used both ex-situ ATR and in-situ DRIFTS mode FTIR analysis of surface films. Compared to the ATR mode, DRIFTS mode is good for the analysis of rough surfaces and coatings. This makes it more suitable to study electrode surface in lithium ion battery since they have rough surfaces and their roughness can increase by the SEI formation process. Furthermore, DRIFTS is an ideal technique for in-situ spectroelectrochemical analysis since it needs no IRE. In this work, we designed in-situ DRIFTS cell and carefully examined the analysis technique to study the SEI layer in lithium ion battery. The methodology that we have developed can eliminate the influence of electrolyte absorption which is a common problem when using in situ FTIR to study SEI layer. The electrochemical and spectroscopic measurements show the effectiveness of the technique and the methodology developed for the analysis of SEI in lithium ion battery.

    The solid electrolyte interface formation process during the first charging/discharging of lithium ion battery consumes lithium ions permanently and results in an irreversible capacity. In this work, analysis of the SEI composition and formation mechanism in different electrolytes and electrolyte additive is performed using infrared spectroscopic and characterization techniques including microscopic and electrochemical techniques. The effect of trace amount of oxygen in the reduction of propylene carbonate (PC) is shown by combining CV, FTIR and XPS analysis. ATR-FTIR analysis, performed inside a glove box, confirms the formation of solvated Li2CO3 and (R-OCO2-Li(PC)2)2 due to propylene carbonate (PC) reduction in the potential range from OCV to -0.1 V. Our experimental results suggest that in the potential range from OCV to 1.6 V, PC, in the presence of O2, can be easily decomposed by the superoxide ion through a nucleophilic attack at the ethereal carbon atom and form (PC)2LiOC(O)OCH(CH3)CH2OLi(PC).
    A direct comparison of the reduction of PC, EC and DEC as single, binary and ternary solvent systems is studied. ATR-FTIR performed in a glove box after LSV indicates that the reduction behavior of an alkyl carbonate is not significantly influenced by the presence of other alkyl carbonate. (CH(CH3)CH2OCO2Li)2 and Li2CO3 are formed due to PC reduction, EC is reduced to (CH2OCO2Li)2 and Li2CO3, and DEC reduction leads to the formation of (CH2=CH-OCO2CH2CH3)Li. The reduction product of EC is responsible for the formation of a passivating surface film which prevents exfoliation caused by PC. We have designed a spectroelectrochemical cell which is compatible with our DRIFTS spectrometer and can work effectively for in-situ analysis of the SEI layer in a half cell mode of lithium ion battery. The electrochemical performance of the cell is tested with both aqueous and non-aqueous systems and the results confirm the good applicability of the cell for electrochemical reactions. The effectiveness of the specroelectrochemical cell for FTIR analysis of SEI layer is confirmed by comparing the results with ATR-FTIR experiments performed in a glove box. The reduction products and SEI formation mechanism of N,N’-1,4-phenylenedimaleimide (MI-2) is examined with 0.1% MI-2 in 1 M LiPF6/PC, 1 M LiPF6/ EC:PC (3:2) and 1 M LiPF6 in EC:PC:DEC (3:2:5) systems. The CV results reveal that MI-2 reduction occurs prior to the solvents whose reduction in the binary and ternary solvent systems is suppressed by MI-2. However, in the single solvent system, PC co-intercalation and reduction could not be inhibited even in the presence of MI-2. FTIR confirms that ring opening of maleimide group occurs in the binary and ternary solvent system but not in the single solvent system.
    In this work, we used both ex-situ ATR and in-situ DRIFTS mode FTIR analysis of surface films. Compared to the ATR mode, DRIFTS mode is good for the analysis of rough surfaces and coatings. This makes it more suitable to study electrode surface in lithium ion battery since they have rough surfaces and their roughness can increase by the SEI formation process. Furthermore, DRIFTS is an ideal technique for in-situ spectroelectrochemical analysis since it needs no IRE. In this work, we designed in-situ DRIFTS cell and carefully examined the analysis technique to study the SEI layer in lithium ion battery. The methodology that we have developed can eliminate the influence of electrolyte absorption which is a common problem when using in situ FTIR to study SEI layer. The electrochemical and spectroscopic measurements show the effectiveness of the technique and the methodology developed for the analysis of SEI in lithium ion battery.

    Abstract i Acknowledgments iii Table of Contents vi List of Figures ix List of Tables xiv List of Scheme xvi List of Abbreviations xvii Chapter 1 Introduction 1 1.1. Lithium Ion Battery 1 1.2. Components of Lithium Ion Battery 4 1.2.1. Anode Materials 5 1.2.2. Cathode Materials 10 1.2.3. Electrolytes 13 1.3. Solid Electrolyte Interface (SEI) 21 1.4. Techniques for the analysis of SEI layer 28 Chapter 2 Experimental Methods 31 2.1. Cyclic Voltammetry (CV) 31 2.2. Battery Test 34 2.3. Electrochemical Impedance Spectroscopy (EIS) 35 2.4. Fourier Transform Infrared Spectroscopy (FTIR) 37 2.5. X-ray Photoelectron Spectroscopy (XPS) 42 2.6. The scanning electron microscope (SEM) 43 Chapter 3 Study of Surface Film Formation: Effect of Oxygen on the Reduction Mechanism of Propylene Carbonate 45 3.1. Introduction 45 3.2. Experimental Methods 46 3.3. Result and Discussion 47 3.3.1. Cyclic Voltammetry Measurements 47 3.3.2. FTIR Measurements 50 3.3.3. XPS Analysis 61 3.4. Summary 64 Chapter 4 Comparative Study on the Reduction of Various Alkyl Carbonates and SEI Formation in Lithium Ion Battery 65 4.1. Introduction 65 4.2. Experimental Methods 67 4.3. Results 69 4.3.1. Electrochemical cycling 69 4.3.2. Electrochemical Impedance Spectroscopy Analysis 70 4.3.3. Morphology analysis with SEM 73 4.3.4. Cyclic voltammetry 75 4.3.5. FTIR Measurement 77 4.4. Discussion 88 4.5. Summary 90 Chapter 5 In-situ DRIFTS Cell Design and Analysis of the Solid Electrolyte Interface in Lithium Ion Battery 92 5.1. Introduction 92 5.2. Experimental Method 95 5.3. Result and Discussion 96 5.3.1. Cell Design 96 5.3.2. Electrochemical Performance test: 99 5.3.3. In situ FTIR measurement 100 5.4. Summary 110 Chapter 6 The Reduction of N,N’-1,4-phenylenedimaleimide electrolyte additive and its SEI formation process 111 6.1. Introduction 111 6.2. Experimental 112 6.3. Result and Discussion 113 6.3.1. Cyclic Voltammetry measurement 113 6.3.2. FTIR Measurement 115 6.3.3. Electrochemical Impedance spectroscopy Analysis 128 6.4. Summary 134 Chapter 7 General Conclusions and Recommendations 135 References 140 Appendices 164 I. Specification of in situ DRIFTS cell 165 II. Battery performance test using 1 M LiPF6/ PC and 1 M LiPF6/ EC/PC(3:2) with and without 0.1% MI-2 172

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