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研究生： Semaw Kebede Merso
Semaw Kebede Merso
論文名稱： 無陽極金屬電池之銅集流體表面修飾用以抑制鋰枝晶生長並穩定固態電解質界面
Copper Current Collector Surface Modification for Suppressing the Li Dendrite Growth and Stabilizing the Solid Electrolyte Interphase of Anode-Free Lithium Metal Batteries
指導教授： 黃炳照
Bing-Joe Hwang
牟中原
Chung-Yuan Mou
口試委員: 黃炳照
Bing-Joe Hwang
吳溪煌
She-Huang Wu
蘇威年
Wei-Nien Su
王迪彥
Di-Yan Wang
牟中原
Chung-Yuan Mou
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： 2023
畢業學年度： 111
語文別： 英文
論文頁數： 205
中文關鍵詞： 無陽極 、SrF2 納米顆粒 、雙功能界面層 、鋰成核 、富含 LiF 的 SEI 、Li-Sr 合金 、鋰枝晶生長 、固態電解液界面 、無陽極袋式電池 、緻密沉積 、SrF2/PVDF-HFP 、Li-Sr/Li-Sn 合金 、GaN/PVDF-HFP 、Li-Ga 合金 、Li3N 富含的 SEI
外文關鍵詞： anode-free, SrF2 nanoparticles, bifunctional interfacial layer, Li nucleation, LiF-rich SEI, Li-Sr alloy, Lithium dendrite growth, solid electrolyte interphase, anode-free pouch cells, compact deposition, SrF2/PVDF-HFP, Li-Sr/Li-Sn alloys, GaN/PVDF-HFP, Li-Ga alloy, Li3N-rich SEI
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    • 摘要
    鋰金屬因其極高的理論比容量（3860 mAh g-1）、最低的氧化還原電位（-3.04 V vs. 標準氫電極）和輕量化的密度（0.534 g cm-3）而被視為未來最具潛力的陰極材料之一。然而，鋰金屬直接作為陰極的應用通常受到安全性問題、鋰枝晶生長、鋰金屬反應性強、體積變化大、固態電解質界面不穩定、持續腐蝕、短路和循環壽命短等挑戰的限制。除了追求更高能量密度外，鋰金屬的固有挑戰也促使研究人員設計了無陽極（最初無鋰）可充電鋰金屬電池（AFLMBs）於「零過剩鋰」的概念。無陽極鋰金屬電池因其極高的能量密度，因在陽極無初始鋰的簡易結構而受到關注，降低了電池重量，簡化了製造過程，並解決了安全性問題。然而，由於裸銅表面的疏水和非均勻特性，直接在其上沉積鋰會遇到高的成核能障，導致循環過程中鋰的非均勻沉積和嚴重的鋰枝晶生長。此外，AFLMBs由於電解液分解而導致固態電解質界面（SEI）不穩定。在第一部分中，由於裸銅的疏鋰特性和循環過程中的電解液分解，AFLMBs會出現嚴重的鋰枝晶生長和不穩定的固態電解質界面。因此，本論文成功地設計了使用氟化鍶（SrF2）納米顆粒作為雙功能塗層材料（Cu@SrF2）的銅電流收集器，以實現富含LiF的SEI和Li-Sr合金複合層的雙重功能。因此，這種原位衍生的雙功能複合層具有抑制鋰枝晶生長、防止不活性鋰的形成和降低電解液分解的能力，同時通過形成Li-Sr合金層，並儲存鋰在該合金層其下沉積，由於原位衍生的界面層的協同效應，Cu@SrF2電極表面呈現出緻密且無枝晶的形態。Cu@SrF2 // NCM111無陽極電池表現出優異的性能，在60個循環中實現了其初始放電容量的51.0%，平均庫倫效率（CE）為98.6%，相較於裸銅無陽極電池（BCu // NCM111）。此外，「原位形成的雙功能界面層」的概念也在使用相同方法的鋰金屬陽極上得到證明，展示了它在鋰金屬電池中的潛在應用。SrF2包覆的鋰金屬（Li@SrF2）電極在對稱和半電池中展示了優異的高容量和高電流密度的可逆性，並在全電池（Li@SrF2 // NCM111）中表現出優越的性能。此方法同時實現了均勻的鋰成核和富含LiF的SEI層的形成，為實現AFLMBs和LMBs具有更長壽命和更高庫倫效率奠定了基礎。在第二部分中，本研究更揭露了一種雙層保護層（Cu-Sn@SFPH）電極，底層為鍍錫銅（Cu-Sn），頂層則是由聚偏二氟乙烯-共-六氟丙烯（PVDF-HFP）強化的氟化鍶（SrF2）納米顆粒。原位衍生的富含LiF的SEI是快速Li+傳輸的穩定緩衝區，而親鋰的Li-Sn和Li-Sr合金層則作為均勻Li沉積的成核種子。因此，Cu-Sn@SFPH電極表面實現了緻密且無枝晶的Li沉積。Cu-Sn@SFPH // Li電池中的Cu-Sn@SFPH電極在0.5 mA cm-2電流密度和2 mAh cm-2容量下，表現出卓越的循環穩定性，超過3200小時。Cu-Sn@SFPH // NCM111無陽極軟包電池展示出優異的性能，相較於裸銅無陽極軟包電池（Cu // NCM111），在120個循環中實現了其初始放電容量的72.1%，平均庫倫效率（CE）為99.9%，使用1.5 M LiFSI in DME/TTE（1：4體積比）作為電解質。在實際應用條件下，搭配NCM正極和稀薄電解質，這種策略為AFLMBs帶來了有前景的未來。論文的最終部分，揭露以利用PVDF-HFP增強的氮化鎵（GaN）對銅電流收集器進行改性（Cu@GNPH），以實現原位形成的離子和電子導電層，促進橫向Li沉積並穩定SEI的形成。因此，原位衍生的Li-Ga合金層促進了Li的橫向生長(不易生成枝晶)，而Li3N富含的SEI層則促進了均勻的離子通量和快速動力學，從而抑制了Li枝晶生長。Cu@GNPH電極由於具有親鋰性的GaN和PVDF-HFP材料的共同作用，實現了均勻且緻密的Li沉積以及長期循環穩定性。Cu@GNPH // NCM523無陽極軟包電池在1.5 M LiFSI in DME/TTE（1：4體積比）作為電解質的情況下，相較於裸銅無陽極電極軟包電池（Cu // NCM523），在100個循環中也可實現了初始放電容量的70 %，平均庫倫效率（CE）為99.8%。

    Abstract
    Lithium (Li) metal is regarded as the brightest future anode material among all candidates owning to its extraordinarily high theoretical specific capacity (3860 mAh g-1), lowest redox potential (-3.04 V vs. standard hydrogen electrode), and low gravimetric density (0.534 g cm-3). Nevertheless, the direct use of Li metal as an anode is usually impeded by safety issues, severe Li dendrite growth, harsh reactivity of Li metal, high volume change, and unstable solid electrolyte interphase, continuous corrosion, short-circuiting, and short cycle life. Aside from pursuing higher energy density, the inherent Li metal challenges triggered the researchers to design anode-free (initially Li less) rechargeable Li metal batteries (AFLMBs) that relied on the zero-excess Li concept. Anode-free lithium metal batteries have gained prominence recently because of their extremely high energy density and their simplicity in that the cells are built with no initial Li in the anode, decreasing the cell weight as well as simplifying the manufacturing process and addressing safety issues. However, because of the lithiophobic and inhomogeneous characteristics of the bare Cu surface, direct deposition of Li on it encounters a high nucleation energy barrier, resulting in non-uniform Li deposition and severe Li dendrite growth during cycling. Furthermore, the AFLMBs suffer from unstable solid electrolyte interphase (SEI) owing to electrolyte decomposition.
    In the first part, the AFLMBs suffer from severe Li dendrites growth and unstable solid electrolyte interphase because of the lithiophobic characteristics of the bare Cu and the electrolyte decomposition upon cycling, respectively. As a result, we successfully designed the Cu current collector using strontium fluoride (SrF2) nanoparticles as bifunctional coating material (Cu@SrF2) to achieve the dual function of LiF-rich SEI and Li-Sr alloy composite layer upon plating. Thus, the in-situ derived dual-functional composite layer demonstrates the ability to inhibit the growth of Li dendrites while preventing the formation of inactive Li and decomposition of electrolyte, as well as storing Li via the formation of the Li-Sr alloy layer and enabling Li to deposit beneath it. Because of the synergetic effect of the in-situ derived interfacial layer, the Cu@SrF2 electrode surface attains compact and dendrite-free morphology. The Cu@SrF2 electrode cell (Cu@SrF2//NCM111) demonstrates superior performance, which attains 51.0% of its initial discharge capacity with an average Coulombic efficiency (CE) of 98.6% for 60 cycles in comparison to the bare Cu electrode cell (BCu//NCM111). Furthermore, the notion of an "in-situ formed bifunctional interfacial layer" has been proven on a lithium metal anode using the same approach, demonstrating its potential applications in lithium metal batteries. The SrF2-coated Li (Li@SrF2) electrode also demonstrates excellent Li reversibility at high capacities and current densities in symmetric and half-cells, and exhibits outstanding performance in full-cells (Li@SrF2//NCM111). This approach enables both homogeneous Li nucleation and the formation of LiF-rich SEI layers at the same time, paving the way for the realization of AFLMBs and LMBs with longer lifetimes and higher CE.
    In the second part, we efficiently developed a dual-coated protective layer (Cu-Sn@SFPH) electrode with Sn-coated Cu (denoted as Cu-Sn) as a bottom layer and SrF2 nanoparticles strengthened by poly (vinylidene fluoride)-co-hexafluoropropylene (PVDF-HFP) as the top layer. The in-situ derived LiF-rich SEI is a stable buffer zone for fast Li+ transfer, while the lithiophilic Li-Sn and Li-Sr alloy layers serve as nucleation seeds for uniform Li deposition. Thus, the Cu-Sn@SFPH electrode surface attains compact and dendrite-free Li deposition. The Cu-Sn@SFPH electrode cell (Cu-Sn@SFPH//Li) exhibits remarkable cyclability for over 3200 h at a current density of 0.5 mA cm–2 and capacity of 2 mAh cm–2. The Cu-Sn@SFPH electrode pouch cell (Cu-Sn@SFPH//NCM111) demonstrates outstanding performance that achieves 72.1% of its initial discharge capacity with an average CE of 99.9% for 120 cycles in comparison to the bare Cu pouch cell (Cu//NCM111) using 1.5 M LiFSI in DME/TTE (1:4 in volume) as an electrolyte. Under practical conditions, with NCM cathodes and a lean electrolyte, this strategy offers a promising future for AFLMBs.
    In the final work, we modified a Cu current collector using GaN with the integration of PVDF-HFP (Cu@GNPH) to attain the in-situ formed ionic and electronic conductive layers which promote the lateral Li deposition as well as stabilize the SEI during cycling. Thus, the in-situ derived Li-Ga alloy layer promotes the horizontal growth of Li, and the Li3N-rich SEI layer facilitates the uniform ionic flux and fast kinetics, thereby suppressing the Li dendritic growth. The Cu@GNPH electrode achieves homogenous and compact Li deposition as well as long-term cycling stability owing to the combined impact of lithiophilic GaN and PVDF-HFP materials. The anode-free pouch cell (Cu@GNPH//NCM523) of the Cu@GNPH electrode demonstrates superior performance that achieves 70 % of its initial discharge capacity with an average CE of 99.8% for 100 cycles when compared to the bare Cu electrode pouch cell (Cu//NCM523) using 1.5 M LiFSI in DME/TTE (1:4 in volume) as an electrolyte.

    Table of Contents 摘要 i Abstract iii Acknowledgments vii Table of Contents ix List of Schemes xxii List of Tables xxiii Index of Abbreviations, Nomenclatures, and Units xxv Chapter 1: General Background of the Study 1 1.1 Introduction to Energy Sources and Storage Systems 1 1.2 Rechargeable Batteries as an Electrochemical Energy Storage Device 3 Chapter 2: Challenges and Strategies for Realization of Lithium Metal Batteries 9 2.1 Fundamentals of Lithium Metal Batteries 9 2.2 Challenges of Li Metal Anode 10 2.2.1 Li Dendrite Growth and Dead Li Formation 12 2.2.2 Infinite Volume Changes 13 2.2.3 Instability of Solid Electrolyte Interphase Layers 14 2.2.4 High Reactivity of Li Metal 15 2.3 Possible Strategies to Alleviate the Issues of Lithium Metal Batteries 16 2.3.1 Designing of Artificial Protection Layers 18 2.3.1.1 Organic Polymer Coatings 18 2.3.1.2 Inorganic Coating Materials 20 2.3.1.3 Organic-Inorganic Hybrid Coating Layers 21 2.3.2 Electrode Design 23 2.3.2.1 3D Structural Hosts 24 2.3.2.2 Surface Modification with Lithiophilic Materials 25 2.3.3 Electrolyte Engineering 28 2.3.3.1 Functional Electrolyte Additives 29 2.3.3.2 Solvents and Conducting Salts 33 2.3.3.3 Solid Electrolytes 35 2.4 The Progress of Anode-Free Lithium Metal Batteries 38 2.5 Motivation and Objectives of the Study 52 2.5.1 Motivation 52 2.5.2 Objectives of the Study 53 Chapter 3: Experimental Section 55 3.1 Chemicals and Reagents 55 3.2 Synthesis of SrF2 Nanoparticles 57 3.3 Electrode Preparation 58 3.3.1 Cu Current Collector Preparation 58 3.3.2 Fabrication of SrF2-Coated Cu Electrode 58 3.3.3 Fabrication of SrF2-coated Li Metal Anode 59 3.3.4 Fabrication of Sn-Coated Cu and SrF2/PVDF-HFP-Coated Sn-Cu Electrodes 59 3.3.5 Fabrication of GaN/PVDF-HFP-Coated Cu Electrode 60 3.3.6 Cathode Preparation 61 3.4 Electrolyte Preparation 61 3.5 Electrochemical Measurements 62 3.6 Materials Characterization 64 Chapter 4: An In-Situ Formed Bifunctional Layer for Suppressing the Li Dendrite Growth and Stabilizing the Solid Electrolyte Interphase Layer of Anode-Free Lithium Metal Batteries 67 4.1 Introduction 67 4.2 Results and Discussion 70 4.2.1 Characterization of As-Synthesized Materials 70 4.2.2 Characterization of Electrodes 72 4.2.3 Interfacial Composite Layer Formation During Cycling 75 4.2.4 Electrochemical Stability of Electrodes 80 4.2.5 Morphological Evaluation of Electrodes 83 4.2.6 Performance and Electrochemical Impedance Spectroscopy Evaluation of the Cu@SrF2 Electrodes in Anode-Free Cells 89 4.2.7 The Potential Applicability of SrF2 Nanoparticles in Lithium Metal Batteries 92 4.2.7.1 Performance Evaluation of Li@SrF2 Electrodes 92 4.2.7.2 Morphological Evaluation of the Li@SrF2 Electrodes 95 4.2.7.3 Interfacial Layers Formation in Li@SrF2 Electrodes 96 4.2.7.4 Cycling Stability of Li@SrF2 Electrodes 99 4.3 Summary 105 Chapter 5: Multiple Protective Layers for Suppressing Li Dendrite Growth and Improving the Cycle Life of Anode-Free Lithium Metal Batteries 107 5.1 Introduction 107 5.2 Results and Discussion 110 5.2.1 Fabrication and Characterization of the Electrodes 110 5.2.2 Multiple Layer Formation 112 5.2.3 Cycling Stability of Electrodes 117 5.2.4 Morphological Evolution of the Electrodes 120 5.2.5 Electrochemical Performance of Electrodes in Pouch-Type Cells 122 5.3 Summary 127 Chapter 6: Lithiophilic and Li3N-rich SEI Composite Layers for Inhibiting the Growth of Li Dendrites and Long-Life Pouch Cells in Anode-Free Lithium Metal Batteries 129 6.1 Introduction 129 6.2 Results and Discussion 132 6.2.1 Preparation and Characterization of the Electrodes 132 6.2.2 In-Situ Composite Layer Formation 133 6.2.3 Electrochemical Stability of Electrodes 136 6.2.4 Morphological Evaluation of Electrodes 138 6.2.5 Electrochemical Performance of Electrodes in Pouch-Type Cells 141 6.3 Summary 145 Chapter 7: Conclusions and Future Perspectives 147 7.1 Conclusions 147 7.2 Future Perspectives 149 References 151 List of Publication 173

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