鋰電池電解質可以說是整個鋰電池的心臟，其重要性是可以直接影響電池的充放電效能、工作溫度、循環壽命以及電池的安全性。隨著人類對於更高能量的儲能裝置需求之下，具有高能量密度的鋰金屬電池被認為是極具潛力的研究主題。因此，開發高循環充放電效能且具穩定性的電解質應用於鋰金屬電池可具有相當大的價值與意義。本論文藉由低毒性腈類溶劑、雙鋰鹽電解質以及抑制枝晶鋰生成的膠態高分子來進行抗腐蝕、高效能與高穩定壽命的鋰金屬電池電解質研究開發。
本論文第一章介紹鋰金屬電池、鋰電池電解質以及膠態高分子在鋰電池的應用。第二章詳細介紹本文中電池相關的材料製備、分析儀器、電化學系統以及實驗方法。
在第三章中，本研究使用3-甲氧基丙基腈(3-methoxypropionitrile, MPN)作為含雙(三氟甲基磺醯)氨基鋰鹽(Lithium bis(trifluoromethanesulfonyl)imide, LiTFSI)的電解質溶劑，並在LiNi0.6Mn0.2Co0.2O2) || Li 鋰金屬鈕扣電池進行循環充放電測試後，確認該溶劑可有效的抑制電池正極鋁箔集電材料的腐蝕，並且有效改善鋰電池的循環壽命。藉由線性掃描伏安法來驗證鋁箔在電解質加入3-甲氧基丙基腈溶劑後可增加氧化反應電位以及其安定性。經過X射線光電子能譜儀(X-ray photoelectron spectroscopy, XPS)分析後，驗證了鋁箔上具有氮化鋁(aluminium nitride passivation, AlN)鈍化層的生成，可保護鋁箔表面且改善電池容量維持率。
在第四章中，本論文中開發了臨場電化學光學顯微鏡系統來探討鋰金屬表面生成枝晶鋰的機制，並清楚觀察到使用傳統商業化的六氟磷酸鋰碳酸酯電解質下枝晶鋰的生成，以及使用LiTFSI-LiPF6雙鹽電解質下可有效抑制枝晶鋰的現象。除此之外，使用傳統電解質下，鋰金屬電極表面會累積 Dead lithium 產物、出現表面孔蝕及氣體產物生成；然而，本文在臨場電化學光學顯微鏡結果中發現LiTFSI-LiPF6雙鹽電解質可以明顯有效改善這些問題。本研究亦藉由電化學阻抗圖譜分析、離子導電度計的量測、鋰金屬對稱電極電池與鋰金屬半電池循環的測試結果來探討各電解質在鋰金屬電極表面的影響。
在第五章中，本研究藉由拉曼光譜更進一步分析不同濃度單鹽與LiTFSI-LiPF6雙鹽電解質中並探討鋰離子與溶劑分子的作用關係。由電化學阻抗圖譜數據的奈奎斯特圖分析得知，雙鹽電解質使鋰金屬表面具有較低的固態電解質介面阻抗及電荷轉移阻抗，可改善LiNi0.6Mn0.2Co0.2O2) || Li鋰金屬半電池的充放電效率表現。此外，LiTFSI-LiPF6雙鹽電解質在鋰金屬半電池在500次長循環下，具有68 %的電池容量保持率，明顯高於傳統的六氟磷酸鋰碳酸酯電解質。
在第六章中，聚乙二醇二丙烯酸酯高分子搭配醚類或是碳酸酯類電解液組成的膠態高分子電解質，可設計為膠態高分子電解質改質層鋰金屬電極表面。透過臨場電化學光學顯微鏡觀測結果得知，膠態高分子改質層能有效抑制鋰金屬表面產生枝晶鋰、孔蝕、及死鋰堆積的問題。將膠態高分子電解質改質層應用於鋰對稱電池，可增加鋰離子轉移數；並在Li||LiNi0.6Mn0.2Co0.2O2電池循環充放電時，維持充電的起始過電壓，進而提升電池容量保持率與電池循環壽命。

Lithium-metal batteries are considered as a promising candidate to replace the present state of the art lithium-ion technology. Thus, developing high-performance and stable electrolytes for batteries containing lithium metal rather than graphitic carbon is significant. This thesis investigates corrosion-resistant, high-performance, and long-lifetime electrolytes for lithium-metal batteries by developing a novel nitrile solvent, dual-lithium salt electrolytes, and a dendrite-suppression gel polymer layer.
A general background about lithium-metal batteries and electrolytes is provided in Chapter 1. A detailed explanation of battery preparation and experimental methods is presented in Chapter 2.
Chapter 3 of this thesis investigates the use of the nitrile-based solvent (3-methoxypropionitrile) within the lithium electrolyte, thereby effectively suppressing aluminium current collector corrosion during LiNi0.6Mn0.2Co0.2O2 || Li cell cycling. The oxidation stability window expands with the use of nitrile-based electrolyte, as verified through linear sweep voltammetry. The aluminium nitride passivation layer was characterised via X-ray photoelectron analysis, and the addition of 3-methoxypropionitrile was found to improve capacity retention.
Chapter 4 discusses lithium dendrite formation in conventional carbonate electrolytes and demonstrates the dendrite suppression using dual-salt electrolytes via in situ optical microscopy observation. Dead lithium accumulation and gas evolution were observed in the carbonate-based electrolytes; however, LiTFSI-LiPF6 dual-salt electrolytes effectively addressed these problems during cell cycling. Ionic conductivity, electrochemical impedance spectroscopy, symmetric lithium cells cycling and LiNi0.6Mn0.2Co0.2O2||Li half cells performance were compared and analysed for 1–4 M of single and dual electrolytes.
Chapter 5 studies lithium-ion solvation in LiTFSI-LiPF6 dual-salt electrolytes via Raman spectroscopy analysis and compares the results with those of single-salt electrolytes. Nyquist plots indicated that the dual-salt electrolytes exhibited lower SEI-layer resistance and charge transfer resistance, which explains the effect of a lower resistance SEI layer formation on the Li metal surface. In addition, the improved rate capacity performance in LiNi0.6Mn0.2Co0.2O2||Li cells with these dual-salt electrolytes can be attributed to the effect of low RCT and low desolvation energy. An improved capacity retention of 68 % in the 2 M LiTFSI and 1 M LiPF6 dual-salt electrolyte compared to 29% of 1M LiPF6 electrolyte could be obtained after 500 long-cycle at 0.5C in LiNi0.6Mn0.2Co0.2O2||Li cells.
In Chapter 6, the design of a poly(ethylene glycol) diacrylate-derived gel polymer containing ether-based or carbonate-based electrolytes is discussed for use as a gel polymer-modified layer (GPL) to effectively suppress the lithium dendrite formation, pitting holes, and dead lithium accumulation on the lithium metal surface. The GPL increases the lithium-ion transference number (t+) in conventional liquid electrolytes and results in low cell charge voltages in the lithium metal anode of Li||LiNi0.6Mn0.2Co0.2O2, which enhances the capacity retention and prolongs cell lifetime.

摘要 I
Abstract III
致謝 V
Table of Contents VIII
List of Figures XI
List of Tables XVIII
Chapter 1 Introduction 1
1.1. Introduction of Li metal batteries 1
1.2. Challenges of lithium metal batteries 3
1.3. Electrolyte salts for LMBs 4
1.3.1 Lithium hexafluorophosphate (LiPF6) 5
1.3.2 Imide-based lithium salts 7
1.3.3 Other lithium salts 8
1.4. Electrolyte solvents for LMBs 9
1.4.1 Carbonate-based solvents 10
1.4.2 Ether-based electrolytes 12
1.4.3 Nitrile-based electrolyte 14
1.5. Electrochemical cell for in situ optical microscopic observation during electrodeposition and dissolution 15
1.6. Blended lithium salts electrolyte for LMBs 18
1.7. PEO-based gel polymer layer for Li metal anode 19
1.8. Aim of this work 21
Chapter 2 Experimental Methods 23
2.1 Cell preparation 23
2.1.1 LiNi0.6Mn0.2Co0.2O2 cathode preparation 23
2.1.2 Liquid electrolytes preparation 24
2.1.3 Gel polymer electrolytes preparation 25
2.2 Electrochemical characterisation techniques 26
2.2.1 Linear sweep voltammetry (LSV) 26
2.2.2 Coin cell assembly and cycling 28
2.2.3 Electrochemical impedance spectroscopy (EIS) 29
2.2.4 Lithium-ion transference number 33
2.2.5 Synchronised electrochemical/optical microscopy (in situ OM) 34
2.3 Material characterisation 36
2.3.1 Karl-Fisher titration (KFT) 36
2.3.2 Ionic conductivity measurement 37
2.3.3 Scanning electron microscope (SEM) 38
2.3.4 X-ray photoelectron spectroscopy 38
2.3.5 Raman spectroscopy 39
2.3.6 Fourier-transform infrared (FTIR) spectroscopy 40
Chapter 3 Aluminium current collector corrosion suppression in Li-ion cells using 3-Methoxypropionitrile co-solvent 41
3.1. Overview of this chapter 41
3.2. Results and discussion 42
3.2.1. Electrolyte characterisation 42
3.2.2. Surface analysis by X-ray photoelectron spectroscopy 47
3.2.3. Protection mechanism 51
3.2.4. Cycling performance of LiNi0.6Mn0.2Co0.2O2||Li cells 53
3.3. Summary 59
Chapter 4 In situ observation of imide-based dual-salt electrolytes enabling lithium dendrite suppression in lithium-metal batteries 60
4.1. Overview 60
4.2. Results and discussion 61
4.3.1 Lithium dendrite formation and depletion observed by in situ OM 61
4.3.2 In situ OM observation of lithium dendrites in LiPF6 carbonate-based electrolytes 64
4.3.3 In situ OM observation of lithium dendrites in LiTFSI ether-based electrolytes 66
4.3.4 Lithium dendrite suppression in LiTFSI-LiPF6 dual-salt electrolyte 68
4.3.5 Ionic conductivity measurements of the electrolytes 74
4.3.6 Electrochemical impedance spectroscopy analysis 76
4.3.7 Li || Li cell cycling in dual-salt electrolyte 81
4.3.8 Electrochemical performance of Li || LiNi0.6Mn0.2Co0.2O2 cells 83
4.3. Summary 84
Chapter 5 Investigation of lithium-ion solvation in dual-salt electrolytes and rate capability of lithium metal batteries 86
5.1 Overview of this chapter 86
5.2 Results and discussion 87
5.2.1 Raman spectroscopy analysis of dual-salt electrolytes 87
5.2.2 Li-ion transference number of dual-salt electrolytes 92
5.2.3 Rate capability of LiNi0.6Mn0.2Co0.2O2||Li cells with dual-salt electrolytes 99
5.2.4 Long-cycling performance of Li∥LiNi0.6Mn0.2Co0.2O2 cells 101
5.3 Summary 104
Chapter 6 Investigating dendrite suppression gel polymer layer for upgrading conventional electrolytes in lithium metal batteries 105
6.1 Overview of this chapter 105
6.2 Result and discussion 106
6.2.1 Characterisation of the gel polymer layer 106
6.2.2 In situ optical microscopy of GPL-coated lithium 112
6.2.3 Li ion transference number of gel polymer electrolytes 115
6.2.4 Cycling performance of LiNi0.6Mn0.2Co0.2O2 || Li cells 118
6.2.5 GPLs and electrodes compatibility in LMBs 122
6.2.6 Enhanced cycling performance of Lithium Metal Batteries in nitrile-based electrolytes by GPL coating on lithium metal 124
6.3 Summary 126
Chapter 7 Conclusions and furtherwork 127
Chapter 8 References 130
DECLARATION 163
CURRICULUM VITAE 163

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