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研究生： Bizualem Wakuma Olbasa
Bizualem Wakuma Olbasa
論文名稱： 高濃度水系電解液在鋅金屬電池的電化學性能強化與反應機制研究
Study on Electrochemical Performance Enhancement and Reaction Mechanism of Concentrated Aqueous Electrolyte in Zinc Metal Battery
指導教授： 黃炳照
Bing-Joe Hwang
蘇威年
Wei-Nien Su
吳溪煌
She-Huang Wu
口試委員: 黃炳照
BING-JOE HWANG
蘇威年
WEI-NIEN SU
吳溪煌
SHE-HUANG WU
吳乃立
Nae-Lih Wu
鄧熙聖
Hsisheng Teng
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： 2021
畢業學年度： 109
語文別： 英文
論文頁數： 191
中文關鍵詞： 水性電解液 、鋅離子電池 、濃電解液 、穩定性 、電化學測是 、電解質發展 、鋅枝晶 、鈍化層
外文關鍵詞： Aqueous electrolyte, Zn ion battery, concentrated electrolyte, stability, electrochemical test, electrolyte development, zinc dendrite, passivation layer
相關次數： 點閱：321  下載：0 
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    • 具備高能量密度，安全性和相容性的材料是改善下一代儲能材料之關鍵因素。鋅金屬被視為鋅電池之理想負極材料是因為具備高能量密度 (5855 mAh/cm3) 、安全性、豐富的地球蘊藏量以及低的還原電位 (相對於SHE為 -0.76 V) 。然而，鋅電池循環時所產生的枝晶生長、腐蝕、鈍化和低庫倫效率等問題限制了鋅金屬電池之實際應用。為了克服這些問題，研究人員提出了許多不同的策略，包括電解液改質，添加電解液添加劑，於陽極鋅金屬的表面上形成人工鈍化層，隔離膜設計等。因此，找到一個能有效穩定陽極鋅金屬的電解液並開發有效的操作方法是克服陽極鋅金屬實際應用的之重要因素。
    本研究的第一份工作是高濃度硫酸鋅電解液之研究，於4.2 M ZnSO4中加入0.1 M MnSO4電解液添加劑。此開發的電解液達成了穩定的鋅沉積/溶解過程中無樹突狀枝晶之產生，在Zn||Cu電池系統中充放電循環1000小時以上仍有99% 的平均庫侖效率，相較於低濃度的硫酸鋅電解液 (2 M ZnSO4 + 0.1 M MnSO4) 是充放電循環少於400小時並 ~97％ 的平均庫侖效率。此次開發的電解液有這種傑出的表現是由於其獨特電解液溶液結構中的協同效應，所形成的陽離子-陰離子聚集體改善了溶劑化/去溶劑化之過程並且MnSO4 電解液添加劑之功能是因為靜電屏蔽機制。因此，電解液添加劑還能作為減少MnO2陰極於電解液中的溶解。
    本研究的第二份工作探討高濃度水系混合電解液(4 M Zn(CF3SO3)2 + 2 M LiClO4)，如何穩定水系雙離子電池系統中之鋅金屬陽極。此開發的電解液系統於高電流密度下可達到鋅沉積/溶解過程中無樹突狀枝晶之產生，並有著傑出的~100％平均庫侖效率。經由更詳細的分析包括同步輻射光源之臨場TXM、 XRD和非臨場XPS證明了緻密且穩定的鈍化層生成，此鈍化層除了於鋅沉積/溶解的過程促進均勻的電流分佈，更進一步避免了新生成的鋅沉積與高濃度混合電解液直接的反應。因此，電位窗口的拓寬是來由於抑制了水的副反應發生。使用高濃度混合水系電解液在Zn||LiFePO4電池系統中達成了穩定的效能，經過285圈充放電循環後，有著99％以上的CE和90％以上的電容量保持率。相對地，在相同系統中，使用低濃度混合水系電解液 (1 M Zn(CF3SO3)2 + 2 M LiClO4) 在170圈充放電循環中的電容量保持率不到65％。 因此，利用高濃度混合水系電解液能夠實現可逆性極高的陽極鋅金屬。此開發的電解液的有益效用可以歸因於其獨特的溶劑化結構，進而形成源自於陰離子鹽的緻密、穩定鈍化層，這與在低濃度電解液中的行為不同。
    本研究的第三份工作，超高濃度混合水系電解質 (4 M Zn(CF3SO3)2 + 2 M LiClO4 + 5 M LiCF3SO3, HCHAE) 之研究，於先前第二份工作中所開發的電解液中加入了水溶性高的三氟甲磺酸鋰 (LiCF3SO3)。添加了額外的高水溶性的鋰鹽可以增強陽離子-陰離子對的聚集體，進而減少電解液中自由溶劑分子的存在而抑制了電化學反應中水的活性。此設計的電解液在Zn||Cu電池系統中可達到鋅沉積/溶解過程中無樹突狀枝晶之產生，並有著傑出的~100％平均庫侖效率。此外，在Zn||Zn對稱電池系統中，於長圈數的循環下也有著高穩定性的鋅沉積/溶解過程並且低極化電位。獨特的電解液溶劑化結構之形成表示了所開發的超高濃縮混合電解液的特色能增進陽極鋅金屬的穩定性。由於抑制了水的副反應發生，因此相較於第二份工作所開發的高濃度水系電解液有著更寬的電位窗口。此開發的超高濃度水系電解液的有益效用可以歸因於其獨特的溶劑化結構，進而形成源自於陰離子鹽的緻密、穩定鈍化層，這與在低濃度電解液中的行為不同。此開發的 HCHAE有穩定且好的效能，於Zn||LiFePO4電池系統中經過155圈充放電循環後，有著99％以上的CE和95％以上的電容量保持率。獲得高效能電容量表現可以歸因於溶劑化結構和開發的電解質。
    因此，大部分保護陽極鋅金屬的策略，本研究特別著重在電解液改質（電解液添加劑、高濃度電解液、雙離子電解液系統），以更深入地了解水系電解液，及研究可逆性金屬陽極的基本機制。高濃度混合水系電解液可大幅拓寬和穩定系統的電位勢窗，進而改善水系鋅離子電池的能量密度。

    A high energy density, safety, and compatibility of electrodes are the key parameters for the improvement of next-generation energy storage materials. A Zn metal is considered as the most promising ideal anode material in zinc metal battery owing to its high volumetric energy density (5855 mAh/cm3), safety, a highly abundant resource, and lower reduction potential (-0.76 V vs. SHE). However, various challenges such as dendrite growth, corrosion formation, passivation, and low coulombic efficiency while cycling limits the practical application of zinc metal batteries. Numerous strategies have been made by different research scholars to overcome those challenges by electrolyte formulation, introducing electrolyte additives, forming an artificial passivation layer on the surface of Zn metal anode, designing separators, using concentrated electrolytes, and the others. Hence, finding an effective electrolyte that stabilizes the Zn metal anode and developing effective operational tools are the parameters to solve the challenges raised by the practical applications of zinc metal anode technology.
    In our first work, concentrated aqueous zinc sulfate electrolyte, 4.2 M ZnSO4 in the presence of 0.1 M MnSO4 electrolyte additives have been investigated. The developed electrolyte attains stable Zn plating/stripping with dendritic-free morphology achieving more than 99% average coulombic efficiency cycling for more than 1000 h compared to diluted aqueous zinc sulfate electrolyte (2 M ZnSO4 + 0.1 M MnSO4) achieving ~97% average coulombic efficiency cycling for less than 400 h using Zn||Cu cell configuration. The outstanding performance obtained while using the developed concentrated electrolyte shows the synergistic effect of the unique solution structure of an electrolyte due to the formation of aggregated cation-anion ion-pairs that enhances the solvation/desolvation process and function of the MnSO4 electrolyte additive due to electrostatic shielding mechanism. Accordingly, the electrolyte additives are also used to decrease the dissolution of the MnO2 cathode into an electrolyte.
    The developed concentrated electrolyte achieves a stable performance using Zn||MnO2 full-cell and ~89% capacity retention at 1200 cycle number using 938 mA/g current density.
    In our second work, the role of concentrated hybrid aqueous electrolyte (4 M Zn(CF3SO3)2 + 2 M LiClO4) on stabilizing Zn metal anode for aqueous hybrid battery system was investigated. The designed electrolyte system attains dendrite-free morphology while Zn plating/stripping achieving excellent ~100% average coulombic efficiency at high current density. Scientific investigations including the synchrotron-based in-operando TXM and XRD, as well as ex-situ XPS, suggests that the dense and stable in-situ formed passivation layer facilitates homogeneous current distribution during Zn plating/stripping and further prevents direct contact of freshly deposited Zn from the electrolyte when concentrated hybrid aqueous electrolyte was used. Thus, the water-related side-reactions were suppressed, leading to the widening of the electrochemical potential window. In a hybrid Zn||LiFePO4 configuration, the cell with concentrated hybrid aqueous electrolyte delivers a stable performance achieving more than 99% CE and more than 90% capacity retention after 285 cycle number. In contrast, the cell with dilute hybrid aqueous electrolyte (1 M Zn(CF3SO3)2 + 2 M LiClO4) gave less than 65% capacity retention at 170 cycles. Hence, concentrated hybrid aqueous electrolyte allows an exceedingly reversible Zn metal anode and realizes. The developed electrolyte's beneficial effects can be ascribed to its unique solvation structure, leading to a dense and stable salt anion-derived passivation layer, which is different from the one obtained in the dilute electrolyte.
    In our third work, a highly concentrated hybrid aqueous electrolyte (4 M Zn(CF3SO3)2 + 2 M LiClO4 + 5 M LiCF3SO3, HCHAE) was investigated by adding highly water-soluble Lithium trifluoromethanesulfonate (LiCF3SO3) to the previously developed electrolyte under our second work. Further addition of highly soluble lithium salt enhances the aggregation of cation-anion ion-pairs by further decreasing the presence of free solvent molecules and suppressing water-activity while the electrochemical process.
    The designed electrolyte system attains dendrite-free morphology while Zn plating/stripping achieving excellent ~100% average CE using Zn||Cu cell configurations. Highly stable Zn plating/stripping in lower potential polarization for longer cycle number was achieved using Zn||Zn symmetric cell also. The unique solvation structure of an electrolyte formed shows unique characteristics of the developed highly concentrated hybrid electrolyte that enhances the stabilizing property of the Zn metal anode. Thus, the water-related side-reactions were suppressed, leading to the widening of the electrochemical potential window compared to the previously developed concentrated hybrid aqueous electrolyte. The developed highly concentrated hybrid aqueous electrolyte's advantageous effects can be ascribed to its unique solvation structure, leading to a dense and stable salt anion-derived passivation layer, which is different from the one obtained in the dilute electrolyte. The developed HCHAE achieves a stable high performance using Zn||LiFePO4 cell configuration, with more than 99% CE and more than 95% capacity retention after 155 cycle number. The obtained high-performance capacity can be explained due to the solvation structure and the developed electrolyte.
    Therefore, among a widespread Zn metal anode protection strategy, using electrolyte formulation for instance we have comprehensively examined the role of electrolyte additives, the effect of highly concentrated electrolytes, and the role of hybrid ion-containing electrolyte systems to achieve a profound understanding and to explain the fundamental mechanism of Zn metal anodes’ reversible reaction in aqueous solutions. The concentrated hybrid ion aqueous-based electrolyte system significantly enlarges the electrochemical stability window of the system which can improve the energy density of aqueous-based ZIBs.

    中文摘要 i Abstract iv Acknowledgment vii Table of Contents ix Index of Figures xiii Index of Tables xxii Index of Units and Abbreviations xxiii Chapter 1 Introduction 1 1.1. Backgrounds of the study 1 1.2. Rechargeable aqueous zinc-ion battery (AZIB) 3 1.3. Fundamental development of aqueous-based electrolyte for ZIBs 5 Chapter 2 Advantages and Challenges of Zinc Metal Batteries 11 2.1. Advantages of zinc metal batteries 11 2.2. Challenges of Zn metal anode 11 2.2.1. Fundamentals of Zn dendrite formation and growth in aqueous electrolyte 12 2.2.2. Shape changes 13 2.2.3. Fundamentals of Zn corrosion formation 14 2.2.4. Fundamentals of Zn surface passivation 14 2.3. Approaches to solving the challenges of Zn metal anode 15 2.3.1. Zn surface modification/protective layer coating 16 2.3.2. Structural design of Zn metal anode surface 19 2.3.3. The fundamental effect of electrolytes for modification of Zn anode for ZIBs 19 2.4. Motivation and objectives of the study 42 2.4.1. Motivation 42 2.4.2. Objectives 43 Chapter 3 Experimental Section 44 3.1. Chemicals and reagents 44 3.2. Synthesis and preparations of electrodes 45 3.2.1. Synthesis of α-MnO2 cathode materials 45 3.2.2. Preparation of electrodes and current collectors 46 3.2.3. Preparation of electrolytes 47 3.3. Electrochemical measurement and characterization technique 48 3.3.1. Electrochemical investigation 48 3.3.2. Characterization 49 Chapter 4 Highly Stable and Long-Cycling with a Dendrite-Free Zn Metal Anode in an Aqueous Zn-Ion Battery Using Concentrated Electrolytes 51 4.1. Introduction 51 4.2. Results and discussion 53 4.2.1. Investigating effect of electrolyte concentration on electrochemical performance 53 4.2.2. Effect of electrolyte concentration on the solution structure 58 4.2.3. Morphological investigation for Zn plating/stripping 65 4.2.4. Investigation of surface chemistry and its composition using XPS 70 4.2.5. Investigation of electrochemical performance using MnO2 cathode material 73 4.3. Summary 79 Chapter 5 Highly Reversible Zn Metal Anode Stabilized by Dense and Anion-Derived Passivation Layer Obtained from Concentrated Hybrid Aqueous Electrolyte for Zinc-Hybrid Batteries 80 5.1. Introduction 80 5.2. Results and discussion 83 5.2.1. Electrochemical performance investigation for half-cells 83 5.2.2. Morphological evaluation of Zn plated and/or stripped onto the Cu substrate 91 5.2.3. Schematic representation for solution structure and mechanistic insight 93 5.2.4. Morphological evaluation of Zn plating/stripping using in-operando TXM 95 5.2.5. Investigation of Zn||Cu cell using synchrotron-based in-operando XRD 99 5.2.6. Investigation of in-situ formed passivation layer composition using XPS 102 5.2.7. Electrochemical investigation of Zn||LFP hybrid battery system 106 5.3. Summary 116 Chapter 6 Highly Concentrated Hybrid Aqueous Electrolyte for Stabilizing Zn Metal Anode and Improving its Electrochemical Performance for Hybrid Battery 117 6.1. Introduction 117 6.2. Results and discussion 121 6.2.1. Electrochemical performance for Zn||Zn symmetric cell 121 6.2.2. Morphological evaluation of Zn plated/stripped onto/out the Cu substrate 130 6.2.3. Schematic representation for solution structure of the developed electrolyte 132 6.2.4. Investigation of surface composition using XPS 136 6.2.5. Electrochemical investigation of Zn||LFP hybrid battery system 139 6.3. Summary 141 Chapter 7 Conclusions and Future Outlooks 142 7.1. Conclusions 142 7.2. Future outlook 145 Reference 147 List of Research Papers 162 Conference/workshop presentations 164

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