Enhancing Cycling Performance of Anode-free Lithium Metal Rechargeable Secondary Battery

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研究生：	Addisu Alemayehu Assegie Addisu Alemayehu Assegie
論文名稱：	Enhancing Cycling Performance of Anode-free Lithium Metal Rechargeable Secondary Battery Enhancing Cycling Performance of Anode-free Lithium Metal Rechargeable Secondary Battery
指導教授：	黃炳照 Bing-Joe Hwang
口試委員:	Wei-Nien Su Wei-Nien Su Shawn D. Lin Shawn D. Lin Nae-Lih Wu Nae-Lih Wu Tse-Chuan Chou Tse-Chuan Chou Hsisheng Teng Hsisheng Teng She-huang Wu She-huang Wu
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：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	192
中文關鍵詞：	Anode-free battery 、lithium metal 、spin coating 、polyethylene oxide 、copper anode 、chemical vapor deposition 、multilayer graphene 、lithium nitrate additive 、lithium dendrite 、dead lithium
外文關鍵詞：	Anode-free battery, lithium metal, spin coating, polyethylene oxide, copper anode, chemical vapor deposition, multilayer graphene, lithium nitrate additive, lithium dendrite, dead lithium
相關次數：	點閱：356 下載：0
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Abstract
Inventing new materials and battery design to enable rechargeable lithium battery with higher capacity, cycle life, efficiency, and energy density is of paramount importance. In fulfilling these principles’ Lithium metal is the most promising anode material in lithium metal battery due to its highest theoretical capacity (3860 mAh/g), lowest reduction potential (-3.04 V) vs Li/Li+(V) and lowest density (0.534 g/cm3). To realize lithium metal rechargeable secondary battery, tremendous research efforts exerted and a remarkable progress has been made. However, the safety challenge, low Coulombic efficiency, shallow cycling conditions, and poor cycle life limit the practical application. To overcome those bottleneck challenges and effectively use lithium metal anode, an anode-free lithium metal battery designed. The new battery architecture constructed in discharge state by pre-storing lithium in the cathode and lithium metal anode generated in-situ on copper current collector while charging. Realizing such a battery is an effective strategy to boost energy density, minimize cost and ease cell fabrication with safety. However, like lithium metal battery in-situ plated lithium grow to moss and whiskers like lithium dendrites on bare copper current collector upon cycling resulting from uneven Li deposition and inability of solid electrolyte interface (SEI) to control the stress exerted by dendritic Li growth. The formation of lithium dendrite induces low Coulombic efficiency, infinite volume expansion, electrolyte decomposition and even penetration of separator and short circuiting cell. To realize a dendrite free high energy density in-situ plated battery new strategies such as nanostructured current collector anode, using stable SEI layer forming additives, high concentration electrolytes, optimizing electrolyte solvent and using lithium rich or pre-lithiated cathodes to compensate lithium loss can be implemented. Our strategy will allow the newly battery design to gain widespread acceptance in electric vehicles, electronics, communication devise as a result of its simplicity to scale up, low cost, increase safety and a means to potential market.

In our first work, copper current collector coated with polyethylene oxide (PEO) film to stabilize lithium deposition and enhance cycle life. More importantly, the PEO film coating reinforces solid electrolyte interface (SEI) layer, encapsulate lithium film on copper and regulate the inevitable reaction of lithium with electrolyte. The modified electrode showed stable cycling of lithium with an average Coulombic efficiency of ~100% over 200 cycles and low voltage hysteresis (~30 mV) at a current density of 0.5 mA/cm2. Moreover, the anode-free battery proved experimentally by integrating it with the LiFePO4 cathode into a full cell configuration (Cu@PEO/LiFePO4). The new cell demonstrated stable cycling with average Coulombic efficiency of 98.6% and 49% capacity retention at 100th cycle. In contrary a capacity retention of ~35% obtained when bare copper paired with the same cathode. These impressive enhanced cycle life and capacity retention results from the synergy of PEO film coating and high electrode-electrolyte interface compatibility. Our result opens up a new route to realize the anode-free batteries by modifying the copper anode with PEO polymer to achieve ever demanding yet safe interfacial chemistry and controlled dendrite formation.

The second motivation of this dissertation focus on engineering copper current collector with ultra-thin graphene layer with chemical vapor deposition (CVD) method as artificial layer to suppress lithium dendrite. Multilayer graphene film with superior strength, stability, and flexibility to facilitate uniform lithium-ion flux makes it an excellent choice to stabilize electrode interface. The new designed copper electrode with size higher than cathode size paired with commercial LiFePO4 cathode (mass loading ~12 mg/cm2), and ensures the first cycle discharge capacity of 147 and 151 mAh/g for bare and multilayer graphene protected electrode respectively which then alleviate the big hurdle (initial capacity loss) in an in-situ plated battery. After 100 round trip cycles, bare and multilayer graphene film protected copper retain ~ 46 and 61 % of their initial capacity respectively in an ether-based electrolyte at 0.1C rate.

In final work, the viability of rechargeable in-situ plated lithium metal battery on bare copper anode demonstrated by using lithium bis(trifluoromethanesulfonyl)imide(LiTFSI) salt in dimethoxy ethane(DME)/1,3-dioxolane (DOL) solvent and 4 wt % LiNO3 additive. The reduction of LiNO3 into lower order nitrite LixNOx and lithium nitride (Li3N) facilitate the formation of robust solid electrolyte interface (SEI) layer with high mechanical strength and stability. By using Cu/LiFePO4 cell without any pre-lithiation, the feasibility of anode-free lithium metal battery could deliver areal capacity of ~1.60 mAh/cm2 in its first cycle and retains about 0.863 mAh/cm2 capacity even at 100th cycles. In contrary, Cu/LFP cell in ether electrolyte without LiNO3 showed a rapid capacity fading. Moreover, by using a 4 wt % graphite composite in LiFePO4 cathode the 100th and 200th cycle capacity retention improved to 65.6 % and 33 % of its initial capacity respectively when cycled at 0.2 mA/cm2.

Table of Contents
摘要    i
Abstract    iii
Acknowledgments    vi
Table of Contents    viii
List of Figures    xiv
List of Tables    xxvii
List of Units and Abbreviations    xxviii
Chapter 1: Introduction    1
1 Alternative Energy Sources    1
2 Batteries as Energy Storage Devise    3
3 Lithium Secondary Batteries    4
3.1 Cathode Material    6
3.2 Layered Structure    6
3.3 Spinel Structured Cathode    7
3.4 Olivine Structure    7
3.5 Lithium Battery Anodes    8
4 Lithium Secondary Battery Electrolytes    12
4.1 Liquid Electrolyte    13
4.2 Ionic Conductivity    13
4.3 Electrolyte Solvent    14
4.4 Electrolyte Stability    14
5 SEI Formation    15
6 Al Corrosion    16
7 Hydrolysis Stability    17
8 Electrolyte Additives    17
Chapter 2: Opportunities and Challenges of Lithium Metal Batteries    19
1    Lithium Metal Batteries    19
2    Challenges of Lithium Metal Battery    21
3    Theory of Lithium Dendrite Growth    22
4    Effects of Li Dendrite    24
5    Lithium Dendrite Characterization    25
6    Strategies to Utilize Lithium Metal as Anode    26
6.1    Optimizing Li Salts    28
6.2    Optimizing Electrolyte Solvent    30
6.3    Electrolyte Additive    31
6.4    Separator Modification    34
6.5    Electrode Engineering    36
7    Materials to Battery Component Engineering    37
7.1    Polymers in Anode Electrode Structuring    37
7.2    Inorganic-organic Composite Material Coating    41
8    Solid Electrolyte    44
9    Anode-free Lithium Metal Battery    47
10    Motivation and Objectives of the Study    55
10.1    Motivation    55
10.2    Objectives    56
Chapter 3: Experimental Section and Characterization    58
1 General Experimental Section    58
1.1 Chemicals and Reagents    58
2 Electrode Fabrication    61
2.1 Cathode Fabrication    61
2.2 Nano-structured Anode Fabrication    61
3 Structure Characterization of Modified Anode    66
3.1 PEO Film Characterization    66
3.2 Graphene Film Characterization    67
4 Electrochemical Measurement and Characterization    67
4.1 Electrochemical Measurement    67
4.2 Lithium Morphology Characterization    68
5 SEI Characterization    68
Chapter 4: Polyethylene Oxide Film Coating Enhances Lithium Cycling Efficiency of an Anode-free Lithium Metal Battery    70
1 Introduction    70
2 Results and Discussion    75
2.1 Modified Electrode Morphology and Thickness Evolution    75
3 Half-cell Electrochemical Performance    80
3.1 Li/Cu-cell Electrochemical Impedance Spectroscopy    88
3.2 SEM of Li Morphology on Cu Collected from Li/Cu Cell    89
4 Full-cell Electrochemical Characterization    91
4.1 Full Cell Cyclic Voltammetry Test    92
4.2 Anode-free Cells Electrochemical Cycling Performance    94
4.3 Full-cell Electrochemical Impedance Spectroscopy    99
5 Morphology Characterization of Full-cell Anode    100
6 Summary    103
Chapter 5: Multilayer Graphene Stabilized Lithium Deposition for Anode-free Lithium Metal Battery    104
1 Introduction    104
2 Results and Discussion    109
2.1 Graphene Film Characterization    109
3 Half-cell Plating and Stripping Test    112
3 Lithium Morphology Characterization on Copper using Li-Cu cell    115
4 Anode-free Full Cell Electrochemical Characterization    117
5 Full Cell Morphology Characterization    123
6 Summary    126
Chapter 6: Lithium Nitrate Additive Stabilized In-situ Plated Lithium Metal on Copper Foil Anode    127
1 Introduction    127
2 Results and Discussions    131
2.1 Morphology of Lithium Deposited on Copper Electrode    131
2.2 Electrochemical Test    132
3 SEI Characterization    141
4 Summary    147
Chapter 7: Conclusions and Perspectives    148
1 Conclusions    148
2 Perspectives    151
References    154
Appendices    182
Approach I    183
Approach II    189
Approach III    190
List of Research Papers    191
Conference Presentations    192


                                

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