Developing Ester-Based Fluorinated Electrolyte with LiPO2F2 as an Additive for High-Rate and Thermally Robust Anode-Free Lithium Metal Battery

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研究生：	Boas Tua Hotasi Boas Tua Hotasi
論文名稱：	Developing Ester-Based Fluorinated Electrolyte with LiPO2F2 as an Additive for High-Rate and Thermally Robust Anode-Free Lithium Metal Battery Developing Ester-Based Fluorinated Electrolyte with LiPO2F2 as an Additive for High-Rate and Thermally Robust Anode-Free Lithium Metal Battery
指導教授：	黃炳照 Bing Joe Hwang
口試委員:	蘇威年 Wei Nien Su 吳溪煌 She Huang Wu
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	102
中文關鍵詞：	anode-free lithium metal battery 、linear esters 、lithium difluorophosphate (LiPO2F2) 、ionic conductivity 、rate capability 、thermal stability
外文關鍵詞：	anode-free lithium metal battery, linear esters, lithium difluorophosphate (LiPO2F2), ionic conductivity, rate capability, thermal stability
相關次數：	點閱：372 下載：0
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空間任務、軍事要求和便攜式應用需要高能量密度、長循環壽命、高倍率能力和極低溫耐受性的能量存儲。1 M LiPF6 的FEC/TTE/EMC (FTE 352) 電解液已被證明可以提高無陽極鋰金屬電池 (AFLMB) 的循環壽命、安全性和能量密度，因為它具有高氧化穩定性、不易燃性和形成的能力富含氟化鋰 (LiF) 的固體電解質中間相 (SEI)。然而，在實際應用中必須考慮電解質的倍率性能、寬溫度範圍和熱穩定性。在本論文中，開發了1 M LiPF6 的FEC/TTE/EMC/MA酯基氟化電解液以及二氟磷酸鋰(LiPO2F2)為添加劑，及其最佳配方為體積比1/5/2/2和1wt%添加量（FTEM 1522 + 1 LPF）。該電解液具有高離子電導率、高氧化性穩定性 (>5 V)、高倍率能力和低溫 (0 oC) 的耐受性。這種電解液運用在無陽極電池中，室溫下提供 97.5% 的平均庫倫效率，0 oC 下可達 96%；相較於參考電解質1 M LiPF6 的FEC/TTE/EMC (FTE 352)的平均庫倫效率，在 0 oC為則為94.4%。這種電解液在 2 mA/cm2 的電流密度下也能保持 80% 的容量保持率，遠高於參考電解液的60%容量保持率。

Energy storage with high energy density, long cycle life, high rate capability, and extreme low-temperature tolerance is required for space missions, military requirements, and man-portable applications. The electrolyte of 1 M LiPF6 in FEC/TTE/EMC (FTE 352) has been demonstrated to increase cycle life, safety and energy density of anode-free lithium metal battery (AFLMB) due to its high oxidative stability, nonflamability and capability to form lithium fluoride (LiF) rich solid electrolyte interphase (SEI). However, rate capability, wide temperature range and thermal stability of electrolytes must be taken into consideration for practical applications. In this work, 1 M LiPF6 in FEC/TTE/EMC/MA (1/5/2/2 vol. ratio) + 1wt.% LiPO2F2 (FTEM 1522 + 1 LPF) was developed, which has high ionic conductivity, high oxidative stability (>5 V), high rate capability, and tolerance of extremely low temperature (0 oC). This electrolyte delivers average coulombic efficiency of 97.5% at room temperature and 96% at 0 oC using an anode-free configuration, while the average coulombic efficiency of reference electrolyte, 1 M LiPF6 in FEC/TTE/EMC (FTE 352) is 94.4% at 0 oC. This electrolyte also holds capacity retention of 80% under a current density of 2 mA/cm2, while the reference electrolyte’s retention capacity is 60%.

中文摘要    i
Abstract    ii
Acknowledgments    iii
Table of Contents    iv
List of Figures    vii
List of Tables    xi
List of Units and Abbreviations    xi
Chapter 1 Introduction    1
1. Energy Sources    1
2. Battery as Electrochemical Energy Storage Devices    1
3. Lithium Secondary Battery    3
3.1. Graphite Anode Lithium-ion Battery    4
3.2. Silicon Anode Lithium-ion Battery    4
3.3. Lithium Metal Anode Battery    5
4. Basic Components of Lithium Metal Batteries    6
4.1. Cathode Materials    6
4.2. Separators    7
4.3. Electrolytes    7
5. Organic Liquid Electrolyte and Its Components    8
5.1. Solvents    8
5.2. Salts    10
5.3. Electrolyte Additives    12
Chapter 2 Fundamentals of Anode-Free Lithium Metal Battery    14
1. Working Principle of Anode-free Lithium Metal Battery    14
2. Challanges of Anode-free Lithium Metal Battery    15
2.1. Low Lithium Plating Binding Energy    15
2.2. Interfacial Reactions    16
2.3. Dendrite Formation    17
2.4. Limited Active Material    18
3. Approaches    19
3.1. Current Collector Engineering    19
3.2. Artificial Lithiophilic Coating    20
3.3. Testing Protocols    21
3.4. Liquid Electrolyte Formulation    23
4. Motivations and Objectives of the Study    30
4.1. Motivations    30
4.2. Objectives    31
Chapter 3 Experimental and Characterization    33
1. Chemical and Reagents    33
2. Materials Preparation    34
2.1. Cathode Material    34
2.2. Anode Current Collector Material    34
2.3. Electrolyte Preparation    34
3. Electrochemical Measurements    36
4. Conductivity and Viscosity Measurements    37
5. Anode Morphology Observation    38
6. Surface Characterization    39
Chapter 4 Result and Discussion    41
1. Electrolyte Optimization    41
1.1. Solvent Optimization    41
1.2. Effect of LiPO2F2 Towards Cu||NMC111 Cyclic Performances    43
2. Electrochemical Measurement at Room Temperature    45
2.1. Electrolyte’s Physical Properties    45
2.2. Room Temperature Electrochemical Stability of Cu||NMC111    48
2.3. Plating Stripping Morphology of Different Electrolytes    52
2.4. Electrochemical Stability of Li||NMC111    53
3. Electrochemical Measurements at High Rate and Lower Temperature    56
3.1. Polarization at High Current Density and Impedance    56
3.2. SEI Composition of Different Electrolytes    59
3.3. Cyclic Stability of Cu||NMC111 at Wide Temperature (0 oC)    60
3.4. Plating Stripping Morphology at 0 oC    62
Chapter 5 Conclusions and Future Outlooks    63
1. Conclusions    63
2. Future Outlooks    64
References    66

                                

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