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研究生： Bikila
Bikila Alemu Jote
論文名稱： 使用預置鋰與電解液改良以提高無陽極鋰金屬電池之循環壽命
Electrolyte Modification and Prelithiation to Improve the Cycle-life of Anode-Free Lithium Metal Batteries
指導教授： 黃炳照
Bing-Joe Hwang
蘇威年
Wei-Nien Su
口試委員: 黃炳照
Bing-Joe Hwang
吳乃立
Nae-Lih Wu
潘俊仁
Chun-Jern Pan
蘇威年
Wei-Nien Su
吳溪煌
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： 2022
畢業學年度： 110
語文別： 英文
論文頁數： 155
中文關鍵詞： 無陽極鋰金屬電池 、碳酸二乙酯 、雙添加劑 、硝酸鋰 、過氧化鋰 、NMC811 、鋰庫存 、電化學性能 、預置鋰 、鋰枝晶 、固體電解質界面膜
外文關鍵詞： Anode-free lithium metal battery, DEC, Dual additives, LiNO3, Li2O2, NMC811, Li inventory, Electrochemical performance, Prelithiation, Lithium dendrite, Solid electrolyte interface
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    • 鋰金屬電池 (Lithium metal batteries, LMBs) 以金屬鋰為陽極在這其中備受期待。鋰金屬電池是高能量密度二次電池的主要競爭對手，其具有最大的理論電容量（3860 mAh g-1）和最低的電化學電位（-3.04 V vs. 標準氫電極）。然而，理論上，無陽極電池（anode-free battery）的想法可能會提供更大的能量密度。無陽極鋰金屬電池（Anode-free lithium metal battery, AFLMB）作為儲能裝置，由於其易於組裝、低成本和擁有更高的能量密度，目前吸引了大量人員研究著。然而，鋰枝晶的生成、安全性和庫侖效率低等問題一直困擾著它的發展。
    為了緩解這些問題，在本論文的第一項研究中，配製了由1.0 M二氟草酸硼酸鋰（LiDFOB）和0.05 M六氟磷酸鋰（LiPF6）溶在體積比為2:2:1的氟代碳酸乙烯酯（FEC）、1,1,2,2四氟乙基-2,2,3,3四氟丙基醚（TTE）與碳酸乙烯酯（DEC）中之混合電解液。在系統為Cu||Li電池和Cu||LiNi0.5Mn0.3Co0.2O2 (NMC532) 電池的測試中，所配製的電解液相對於使用FEC/TTE（體積比為2:3）的電解液具有更好的性能。經過35圈循環後，基於DEC和基於FEC/TTE的電解液的容量保持率分別為45% 和8%。此外，在相同的循環中比較了兩種電解液的平均庫侖效率，DEC的庫侖效率為98.07%，而FEC/TTE (v:v = 2:3) 的庫侖效率僅為92.23%。DEC的添加會提高離子導電率，在陽極部分提供了更多的鋰（Li），開發了富含LiF的固體電解質界面膜（SEI），所有這些都有助於延長電池的使用壽命。根據溶劑的增效作用設計電解液，為未來解決 AFLMB電池問題的方法提供了新的思路。
    具有裸銅箔、富鎳陰極和碳酸酯電解液體系的無陽極鋰金屬電池可以為下世代能量存儲的潛力裝置。然而，在碳酸酯電解液中，富鎳（NMC811）正極的容量衰減相對較快。開發一種解決方案提供額外鋰庫存以減輕由於鋰含量有限，所導致的AFLMB短循環性能問題，這一點至關重要。在第二項工作中，為了增補此問題，我們使用硝酸鋰（LiNO3）作為正極添加劑。LiNO3旨在提供鋰庫存以減輕永久性鋰消耗，同時還在沉積的鋰表面上形成穩定的固體電解質界面膜（SEI）。我們發現，在AFLMB架構中，LiNO¬3在高壓操作期間會分解，有利於產生更好的SEI（由LiF和Li3N組成）以及更好的LiF和Li3N組成之陰極-電解質界面膜（CEI）。在30圈循環後，有硝酸鋰添加劑的電池之庫侖效率（97.69%）明顯高於沒有添加劑的電池（89.25%）。
    無陽極鋰金屬電池裝置仍然面臨著有限的循環壽命和界面問題，阻礙了它們於高性能的用途。這是由於電池固體電解質界面膜（SEI）、電極和電解質在運行期間消耗有限的AFLMB鋰而發生的變化。在這裡，我們報導了由過氧化鋰（Li2O¬2）添加劑和LiNO3添加劑組成的雙添加劑，並用富鎳材料製成了複合正極。雙添加劑電化學分解可增加過量鋰的供應，同時也為電池形成穩定的SEI，這有助於離子的傳輸，並使Cu||LiNi0.8Mn0.1Co0.1O2電池有出色的循環性能，在0.5C倍率測試條件下、於50圈循環時，仍維持出40%的容量保持率。相較之下，一般正極在循環第25圈後，則僅有1.64%的容量保持率。這項研究揭示了簡易正極添加劑的運用方式，以及對延長電池壽命可產生的效果，特別是可用於無陽極電池的應用以補償鋰損失，並為開發更好的添加劑以促進電化學儲能提供了途徑。

    Lithium (Li) metal batteries (LMBs) are promising devices with metallic lithium as an anode. They are a prominent competitor for high-energy-density rechargeable batteries, which have the largest theoretical capacity (3860 mAh g-1) and the lowest electrochemical potential (-3.04 V vs. standard hydrogen electrode). However, theoretically, anode-free cell ideas might deliver even greater energy density. The anode-free lithium metal batteries (AFLMBs) are a form of energy storage device that is now attracting substantial research due to their easy configuration, low cost, and increased energy density. Anode-free lithium metal batteries, which have a bare copper foil, Ni-rich cathode, and carbonated-electrolytes system, could be great energy storage for future generations. However, in a carbonate electrolyte, the capacity degradation of Ni-rich (NMC811) cathodes is relatively quick. Moreover, the issues such as dendritic type lithium creation, safety, and low Coulombic efficiency attenuate its beneficial aspects.
    The thesis is dedicated to mitigating these concerns. In the first work of this thesis, the electrolyte formulated consists of 1.0 M lithium difluoro (oxalate) borate (LiDFOB) and 0.05 M lithium hexafluorophosphate (LiPF6) in a mixture of solvents which are fluoroethylene carbonate/1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether/ diethyl carbonate (FEC/TTE/DEC) with (2:2:1 by volume). The formulated electrolyte gives improved performance in Cu||Li and Cu||LiNi0.5Mn0.3Co0.2O2 (NMC532) cells relative to the FEC/TTE-based electrolyte (in 2:3 by volume). After 35 cycles, DEC-based and FEC/TTE-based electrolytes retain roughly 45% and 8% of their initial discharge capacity, respectively. Furthermore, the average Coulombic efficiencies of the two electrolytes are compared at the same cycles, and the DEC-based has a Coulombic efficiency of 98.07%, whereas the cell with FEC/TTE-based electrolyte has a Coulombic efficiency of only 92.23 %. The addition of DEC improves ionic conductivity, the provision of more lithium (Li) on the anode part, and the development of LiF-richer solid electrolyte interphase (SEI), all of which contribute to prolonging the battery's lifespan. Electrolyte designing depending on the synergetic effect of the solvents provides a new perspective for future approaches to addressing AFLMB battery issues.
    It is critical to developing a solution to increase the lithium inventory in addition to the positive electrode to mitigate the issue of AFLMBs' short cycling performance due to low lithium. In the second work, to supplement NMC811, we use lithium nitrate (LiNO3) as an additive for the cathode. The LiNO3 is intended to provide lithium inventory to mitigate ongoing lithium depletion while also causing stable solid electrolyte interphase (SEI) to form on the deposited lithium surface. We find that the LiNO3 decomposes during high voltage operation in our AFLMB architecture, favoring the production of a better SEI (consists of LiF and Li3N) and better cathode-electrolyte interphase (CEI) of LiF and Li3N composition. The cell with the lithium nitrate additive has a substantially higher Coulombic efficiency (97.69 %) than the one without the additive (89.25 %) after 30 cycles. This work proposes a new way of prolonging the lifespan of AFLMB.
    Despite significant research into AFLMBs, these devices still face limited cycle life and interfacial issue that prevents them from being used for high-performance purposes. This is due to evolution within the battery solid electrolyte interphases (SEIs), electrodes, and electrolytes during the operation that consumes limited lithium of AFLMBs. Here we report dual additives comprising a lithium peroxide (Li2O2) additive and LiNO3 additive and make a composite cathode with Ni-rich material. The dual additives electrochemical decomposition results in a supply of excess lithium and also in the formation of stable SEI for the cell, which helps in the transport of ions and enables superior cycling of Cu||LiNi0.8Mn0.1Co0.1O2 cell that exhibited the capacity retention of 40% after 50 cycles under 0.5 C-rate test conditions. The cell with a bare cathode exhibit the capacity retention of only 1.64% at the 25th cycle. This research sheds light on previously unknown additive effects upon fabrication with positive electrodes in anode-free batteries to compensate for lithium loss and provides the path for developing better additives to advance electrochemical energy storage.

    中文摘要. iii Abstract... vi Acknowledgements ix List of figures xiii List of tables xix Index of units and abbreviations xx Chapter 1: Energy sources and batteries 1 1.1 Different types of energy sources 1 1.2 Rechargeable batteries 3 1.2.1 Electrolytes 3 1.2.2 Cathode Materials 5 1.2.3 Anode Materials 7 1.3 Lithium metal battery 8 Chapter 2: Challenges and approaches of prelithiation techniques 13 2.1 Anode prelithiation 15 2.2 Cathode prelithiation 15 2.2.1 Electrochemical lithiation 16 2.2.2 Prelithiation by using additives 17 2.3 Anode-free lithium metal battery and Li compensation 21 2.4 Motivation and objectives of the study 36 2.4.1 Motivation 36 2.4.2 Objectives 37 Chapter 3: Experimental section and characterization 39 3.1 Chemicals and reagents 39 3.2 Electrode preparation 41 3.2.1 Cathode material 41 3.2.2 Bare current collector 43 3.3 Electrolyte preparation 43 3.4 Electrochemical tests and characterizations 44 Chapter 4: Effect of diethyl carbonate solvent with fluorinated solvents as electrolyte system for anode-free battery 47 4.1 Introduction 47 4.2 Results and discussion 49 4.2.1 Li-Cu cell performance 49 4.2.2 Cu||NMC532 cell performance 51 4.2.3 Surface morphology and compositions 56 4.3 Summary 60 Chapter 5: Lithium nitrate as a surplus lithium source for anode-free cell with Ni-rich (NMC811) cathode 61 5.1 Introduction 61 5.2 Results and discussion 63 5.2.1 Structure and cyclic voltammetry 63 5.2.2 Cu||NMC811 and Li||NMC811 cell performance 65 5.2.3 Surface morphology and conductivity 69 5.2.4 Gas evolution and surface compositions 71 5.3 Summary 77 Chapter 6: Investigating the effect of dual additives on Ni-rich cathode material in anode-free battery….. 79 6.1 Introduction 79 6.2 Results and discussion 82 6.2.1 Optimization, structure and cyclic voltammetry 82 6.2.2 Cu||NMC811 cell performance 87 6.2.3 Surface morphology 90 6.2.4 Gas evolution and surface compositions 93 6.3 Summary 97 Chapter 7: Conclusions and future outlooks 99 7.1 Conclusions 99 7.2 Future outlooks 100 References 103

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