臨場氣相分析探討無陽極鋰金屬電池之介面反應與其副反應之抑制方法開發

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研究生：	Kassie Nigus Shitaw Kassie Nigus Shitaw
論文名稱：	臨場氣相分析探討無陽極鋰金屬電池之介面反應與其副反應之抑制方法開發 Interfacial Chemistries by In Situ Gas Analysis and Mitigating Side Reactions in Anode-free Lithium Metal Battery
指導教授：	黃炳照 Bing-Joe Hwang 蘇威年 Wei-Nien Su
口試委員:	Bing-Joe Hwang Bing-Joe Hwang Wei-Nien Su Wei-Nien Su She-Huang Wu She-Huang Wu Chun-Chen Yang Chun-Chen Yang Nae-Lih Wu Nae-Lih Wu Hsisheng Teng Hsisheng Teng
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	210
中文關鍵詞：	無陽極鋰金屬電池、界面效應、氣體逸出、in-situ電化學質譜；成核屏障、成核屏障、死鋰、電解液配方、熱循環、雙鹽電解液
外文關鍵詞：	anode-free battery, interfacial phenomena, gas evolution, in-situ electrochemical mass spectroscopy, nucleation barrier, dead Li, SEI vs. electrolyte formulation, hot cycling, dual-salt electrolyte
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摘要

由於鋰金屬負極的高能量密度和較低的氧化還原電位(-3.04 V vs. SHE)，鋰金屬電池（LMB）是一種很有前途的下一代電池。其與有機液體電解質具有高度反應性，同時也導致安全問題、鋰枝晶沉積、死鋰形成、體積膨脹和循環穩定性差。所有這些問題都限制了鋰金屬電池的實際應用。因此，由於鋰金屬負極的反應性，使用鋰金屬電池製程來研究可充電電池正極和正極表面的界面反應是相當具有挑戰性的。發展一適當方法，了解鋰金屬電池中的界面現象為先決條件，以增強界面穩定性和提高可充電鋰金屬電池循環壽命的。
首先，我們通過將無陽極鋰金屬電池裝置與原位氣相色譜質譜相結合，成功地解耦並揭開了兩個電極的界面反應的神秘面紗。電解質1 M LiPF6 EC/DEC和 1 M LiPF6 EC/EMC (1:1 v/v)用於比較 Li/NMC111 和 Cu/NMC111 電池中的界面反應。由於SEI形成過程中銅表面的界面反應，得以了解Cu/NMC111電池初始狀態下氣體CO2、CO和C2H4的變化，而整個循環中高電壓下的CO2和CO氣體與在陰極進行化學或電解液氧化的電化學有關。然而，Li/NMC111電池陽極或陰極側的 CO2、CO、O2、C2H4、C2H6 和 POF3 副產物混合在一起，表明界面反應的解耦很困難。已經可以確定電解質對無陽極鋰金屬電池界面處的鋰金屬的穩定性明顯地影響了氣體的逸出。
在第二項工作中，使用亞磷酸三(三甲基甲矽烷基)( tris(trimethylsilyl) phosphite) (TMSP)添加劑的熱循環方案和電解質配方對沉積的鋰、非活性鋰（死鋰和用於SEI形成的鋰），且透過聚焦離子束掃描電子顯微鏡 (FIB-SEM)、滴定氣相色譜 (TGC)、原位氣相色譜質譜(原位 GC-MS) 和X 射線光電子能譜 (XPS) 分別有系統地研究了SEI的形成。電解液1 M LiPF6 EC/DEC (1:1) 在熱循環及TMSP 添加劑的輔助下的將成核的阻礙從76.2 mV降低到 21.7 mV，將沉積鋰的緻密性從31.5%提高到41.3%，並減少了非活性鋰的量，從45.18%到10.86% 和SEI中的鋰分別從31.04%至12.49%。由於協同效應，Cu/NMC111 電池在0.2 mA cm-2 下循環 60次後可實現 98.4%的平均庫侖效率和 51.2% 的容量保持率，而在 25°C 下使用 EC/DEC 的電池在15 次循環後仍提供 92.8% 的平均庫倫效率和40.4%的容量保持率。因此，碳酸鋰電解質中 LiPF6 鹽的濕度和溫度敏感性，以及不良鈍化層的形成會成為影響提高無陽極鋰金屬電池循環穩定性的問題。
最後，由LiDFOB和 LiPO2F2在EC/DEC (1:1 v/v) 中混合物組成的功能性雙鹽電解質的開發，已解決鋰金屬電池和無陽極鋰金屬電池的界面不穩定性。在此，設計了 EC/DEC中的雙鹽 (0.8LDF/0.2LPOF)，並使用約1%的TMSP 添加劑來形成電解質的離子電導率並在循環的過程中穩定這些鹽類。值得注意的是，由於在形成循環期間 LDF 和 LPOF 鹽的氧化還原分解，所開發的電解質可以在陰極和銅電流收集體界面形成堅固的CEI和SEI層。含0.8LDF/0.2LPOF 或 0.8LDF/0.2LPOF + 1% TMSP的Cu/NMC111 電池中沉積的Li較顯著緻密且均勻。因此，在 25°C和0.2 mA cm-2電流密度下循環 60次後，含0.8LDF /0.2LPOF電解質的電池的平均庫倫效率為97.97%，容量保持率為 49.57%，而含 0.8LDF /0.2LPOF +在相同的循環次數和循環條件下，1% TMSP 實現了 98.09% 的平均庫倫效率和61.55%的容量保持率。
總而來說，我們使用無陽極的Cu/NMC111裝置作為工具來深入研究無陽極鋰金屬電池中的界面反應和整體界面現象，這有助於設計合適的電解質以提高鋰金屬電池的循環穩定性。

Abstract

The lithium (Li)-metal battery (LMB) is a promising next generation battery due to the high energy density and lower redox potential (-3.04 V vs. SHE) of the Li-metal anode. However, the Li-metal anode is highly reactive with organic liquid electrolytes, and causes safety concerns, dendritic Li deposition, dead Li formation, volume expansion, and poor cycling stability. All these issues limit the practical applications of the LMBs. Therefore, due to the reactive nature of Li-metal anode, it is challenging to use Li-metal batteries (LMBs) protocol to investigate the interfacial reactions at the anode and cathode surfaces of rechargeable batteries. Understanding of the interfacial phenomena in the LMBs is a prerequisite to develop an appropriate strategy for the enhancement of interface stability and boosting cycling life of the rechargeable LMBs.
In the first work, we has been successfully decoupled and demystified the interfacial reactions at the two electrodes by combining the anode-free Li-metal battery (AFLMBs) configuration with gas chromatography mass spectroscopy (in situ GC-MS).1 The 1 M LiPF6 in EC/DEC and 1 M LiPF6 EC/EMC (1:1 v/v) electrolytes were used to compare the interfacial reactions in the Li/NMC111 and Cu/NMC111 cells. It is demystified that the evolution of CO2, CO and C2H4 gases at the initial staging state of Cu/NMC111 cell is due to interfacial reactions at Cu surface during SEI formation, while the CO2 and CO gases at high voltage in the entire cycle is associated with chemical and/or electrochemical electrolyte oxidation at the cathode. However, the CO2, CO, O2, C2H4, C2H6 and POF3 by-products from anode or cathode sides in the Li/NMC111 cell are mixed up, indicating decoupling of interfacial reactions is difficult. It has been identified that the stability of electrolyte against the Li metal at the interface of AFLMBs greatly influence the evolution of gases.
In the second work, hot cycling protocol and electrolyte formulation using tris(trimethylsilyl) phosphite (TMSP) additive effects on the interfacial phenomena of compactness of deposited Li, inactive Li (dead Li and Li for SEI formation “SEI-Li”), electrolyte decomposition, and SEI formation are systematically investigated by focused ion beam scanning electron microscope (FIB-SEM), titration gas chromatography (TGC), in-situ gas chromatography mass spectroscopy (in-situ GC-MS), and X-ray photoelectron spectroscopy (XPS), respectively. The synergy of hot cycling and TMSP additive in 1 M LiPF6 EC/DEC (1:1) electrolyte lowers the nucleation barrier from 76.2 mV to 21.7 mV, increases the compactness of deposited Li from 31.5% to 41.3%, and reduces inactive Li from 45.18% to 10.86% and SEI-Li from 31.04% to 12.49%, respectively. Due to the synergetic effects, Cu/NMC111 cell attains average coulombic efficiency (avg. CE) of 98.4% and capacity retention (CR) of 51.2% after 60 cycles at 0.2 mA cm-2, while the cell with EC/DEC at 25 °C offers avg. CE of 92.8% with CR of 40.4% after 15 cycles. Here, the moisture and temperature sensitivity of the LiPF6 salt in the carbonate electrolyte and poor passivation formation are problematic for the enhancement of the cycling stability of the AFLMBs.
In the final work, the interface instability of LMBs and AFLMBs, in particular, has been resolved by developing a functional dual-salt electrolyte consisting a mixture of LiDFOB and LiPO2F2 in a mixture of EC/DEC (1:1 v/v). Here, the dual-salt (0.8LDF/0.2LPOF) in EC/DEC was designed and about 1% TMSP additive was used to form ionic conductivity of the electrolyte and stabilize the salts during cycling. Remarkably, the developed electrolyte can form robust CEI and SEI layers at the cathode and Cu current collector interfaces due to the prior redox decomposition of LDF and LPOF salts during formation cycles. The deposited Li in the Cu/NMC111 cell containing 0.8LDF/0.2LPOF or 0.8LDF/0.2LPOF + 1% TMSP is significantly compacted and uniform. Therefore, the cell with 0.8LDF/0.2LPOF electrolyte attained an avg. CE of 97.97% with CR of 49.57% after 60 cycles at 25 °C and 0.2 mA cm-2 current density, while the cell with 0.8LDF/0.2LPOF + 1% TMSP achieved avg. CE of 98.09% and CR of 61.55% after the same cycle number and cycling conditions.
In general, we used anode-free Cu/NMC111 configuration as a tool to intensively investigate the interfacial reactions and overall interface phenomena in the AFLMBs, which helps to design a suitable electrolyte for boosting the cycling stability of the LMBs in general.

Table of Contents

摘要    i
Abstract    iii
Acknowledgment    vii
Table of Contents    ix
Index of Figures    xiii
Index of Tables    xxiii
Index of Schemes    xxv
Index of Units and Abbreviations    xxvii
Chapter 1:     General Background    1
1    Energy Sources and Storage Systems    1
2    Energy Storage Systems    2
3    Batteries as Electrochemical Energy Storage System    3
Chapter 2:     Lithium Metal Battery as Electrochemical Energy Storage System    7
1    Lithium Metal Battery and its Components    7
1.1    Cathode Materials    8
1.2    Electrolytes    10
1.3    Electrolyte Additives    13
1.4    Anode Materials    15
2    Lithium Metal Battery Challenges    15
2.1    Li Dendrite Growth and Dead Li Formation    17
2.2    High Volume Change    20
2.3    Instability of SEI Layers    20
2.4    Interfacial Reactions    21
2.4.1    Interfacial Side Reactions at the Cathode Side    22
2.4.2    Interfacial Side Reactions at the Anode Side    24
3    Approaches for Suppression of Interfacial Side Reactions    26
3.1    Artificial SEI Engineering on the Current Collectors    27
3.2    Electrolyte Engineering    30
3.2.1    Electrolyte Formulation Using Additives    30
4    Anode free Li-metal Battery as a Tool to Study Interfacial Reactions    35
5    Anode free Li-metal Battery as a Tool to Develop Carbonate-based Electrolytes    41
6    Motivation and Objectives of the study    46
6.1    Motivation of the Study    46
6.2    Objectives of the Study    47
Chapter 3:     Experimental Section and Characterization    49
1    Chemicals and Reagents    49
2    Cathode Material Preparation    50
3    Anode Current Collector Preparation    50
4    Electrolyte Preparation    50
5    Online Electrochemical Mass Spectrometry (OEMS) Designing    52
6    Physicochemical Properties    55
7    Electrochemical Measurements    56
8    Morphological Evolution of in situ Deposited Li    56
9    SEI Components Characterization    57
10    Dead Li Quantification    57
Chapter 4:    Decoupling of Interfacial Reactions at Anode and Cathode by Combining Online Electrochemical Mass Spectroscopy with Anode-free Li-metal Battery    59
1    Introduction    59
2    Results and Discussion    61
2.1    Gas Formation Analysis of Cu/NMC111 Full-cells at 25 °C    61
2.2    Gas Formation Analysis of Cu/NMC111 Full-cells at 40 and 60 °C    70
2.3    Gas Formation Analysis During Electrochemical Reduction of EC/DEC and EC/EMC Electrolytes    73
2.4    Gas Formation Analysis of Li/NMC111 Half-cells at 25 °C    76
2.5    Surface Composition Characterization    81
3    Summary    84
Chapter 5:    Evolution of Interfacial Phenomena Induced by Electrolyte Formulation and Hot Cycling in Anode-free Li-metal Battery    85
1    Introduction    85
2    Results and Discussion    86
2.1    Electrolyte Optimization    86
2.2    Interfacial Phenomena    89
2.2(a)    Evolution of Early Stage Li Nucleation    90
2.2(b)    Compactness of In Situ Deposited Li    93
2.2(c)    Evolution of Inactive Lithium    98
2.2(d)    Electrolyte Decomposition    101
2.2(e)     Evolution of SEI Compositions    105
2.3    Electrochemical Performance    110
2.3(a)    Li/Cu half-cells Performance    110
2.3(b)    Cu/NMC111 Anode-free full-cells Performance    111
3    Summary    116
Chapter 6:       Stabilizing the Electrode/electrolyte Interfaces Enabled by Functional Dual-salt Electrolyte for Long Cycling of Anode-free Li-metal Battery    117
1    Introduction    117
2    Results and Discussion    118
2.1    Optimization of Dual-salt electrolytes    118
2.2    Li/Cu half-cells Performance    124
2.3    Cu/NMC111 full-cells Performance    126
2.4    Origins of Irreversible Coulombic Efficiency    129
2.5    Surface Morphology Characterization    133
2.6    Evolution of Passivation Layer Formation    137
3    Summary    147
Chapter 7:    Conclusions and Future Outlooks    149
1    Conclusion    149
2    Future Outlooks    151
References    153
List of Publication    177


                                

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