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研究生： Fekadu Wubatu Fenta
Fekadu Wubatu Fenta
論文名稱： 水系可充電鋅離子電池的錳基氧化物正極材料設計及其性能與反應機制之研究
Manganese-Based Oxide Cathodes for Aqueous Rechargeable Zinc-Ion Batteries: Design, Performance, and Reaction Mechanism Study
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: 吳乃立
Nae-Lih Wu
鄧熙聖
Hsisheng Teng
黃炳照
BING-JOE HWANG
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： 2021
畢業學年度： 109
語文別： 英文
論文頁數： 161
中文關鍵詞： 水系鋅離子電池 、水系電解質 、錳基氧化物正極 、離子摻雜
外文關鍵詞： Aqueous Zn-Ion Batteries, Aqueous Electrolyte, Manganese-based Oxide Cathodes, Ion Doping
相關次數： 點閱：244  下載：0 
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    • 由於日益增加的能源危機和環境問題，尋求高效的可充電電池在近年來獲得研究人員的極大關注。儘管過去鋰離子電池（LIBs）已被用作重要的儲能裝置，然而它們的有機電解質之易燃特性和鋰金屬資源稀缺問題正是使人們尋找其他替代可充電電池的動力。
    使用水性電解質的水系可充電電池由於其高安全性、環保和水性電解質的高離子傳導性而受到極大關注。特別是偏酸性電解質的水性可充電鋅離子電池（ZIBs），由於其成本低、理論電容量高（820 mAh g-1）與氧化還原電勢相對較低（-0.76 V vs. SHE），因此與LIBs相比，使用鋅金屬作為負極被認為很有潛力。到目前為止，水系ZIBs的效能研究上已顯示出可觀的進步，但仍有一些問題需要克服，如高性能正極材料的設計是提高能量密度的主要挑戰之一。
    錳基材料是具有不同多晶型的二氧化錳，如-MnO2、-MnO2、-MnO2、 -MnO2和其他低價態錳氧化物（MnO、Mn2O3、Mn3O4），在水系ZIBs中表現出良好的電化學性能，因為其在地球上的豐度高、能量密度高、成本低以及多價晶體結構的結果。然而，由於它們的低電導率、結構穩定性高、結構轉變和自身氧化還原反應引起的錳溶解，使它們在電池循環過程中造成嚴重的電容量衰減。在這項研究中，我們專注於通過金屬摻雜來改善錳基氧化物正極材料的性能並研究其儲能機制。
    在這項工作中，摻雜Cu0.09MnO將設計成水系ZIBs的高容量正極材料。電化學機制研究結果表明，初始的Cu0.09MnO奈米球(nanospheres) 於H+/Zn2+離子的共遷入/遷出轉化為Cu0.01MnO2.nH2O奈米花(nanoflowers)，然後在Cu-MnO2.nH2O和ZnCu-MnO2.nH2O / MnOOH之間進行可逆相變。利用不同的非臨場表徵技術系統地研究Cu0.044MnO的基本相變化和活化的Cu-MnO2.nH2O的儲能機制。結果表明，活化的Cu-MnO2.nH2O具有錳空位，這會明顯誘發Cu-MnO2.nH2O晶格中的氧化還原反應以進行電荷補償。結果顯示，Zn / Cu-MnO2.nH2O電池在0.5C時可提供320 mAh g-1的高比容量，且具有長圈數循環壽命，值得一提的是，在1C下1000次循環中可保持70％的電容量。此外，探討了在沒有MnSO4添加劑下Cu-MnO電極的電化學特性及結構演變，除電容量衰退快速外，證明了與加入MnSO4添加劑後相似的行為。
    在第二項工作中，我們通過-MnO2的結構工程設計了Ag0.4Mn8O16，並通過Ag +摻入ZIBs正極材料，證明其電化學性能的提升和儲能機制。在材料製備上，銀奈米粒子很好地分散在Mn-MnO2的奈米棒中，從而導致更大的表面積，更小的奈米棒和在Ag0.4Mn8O16結構中所產生的氧空位。觀察到H+ / Zn2+離子的共遷入/遷出和Ag+的氧化/還原以及在Ag0.4Mn8O16和ZnxMn8O16/MnOOH之間的可逆相變/轉化反應。結果顯示，Zn/Ag0.4Mn8O16電池具有出色的電化學性能，例如優異的倍率性能：與-MnO2相比（在0.1 A g-1時為227 mAh g-1），0.1 A g-1時的高比容量是306 mAh g-1和1 A g-1時的800次循環的長期循環壽命。
    最後，研究鉀離子（K+）濃度對電子電導率和離子擴散率的影響。-MnO2中更多的K+不僅通過使用Mn3+ / Mn4+混合物增加電子躍遷以增強電子電導率，並通過穿隧擴張來改善離子擴散率。

    The search for high efficient rechargeable batteries has attracted researcher’s great attention due to the increasing energy crisis and environmental concerns. Although lithium-ion batteries (LIBs) have been employed as crucial energy storage devices recently, their use of flammable organic electrolytes and scarce resources are driving the search for alternative rechargeable batteries.
    Aqueous rechargeable batteries employing water-based electrolytes are drawing tremendous attention owing to their high safety, environmentally friendly, and ionic conductivity of aqueous electrolytes. Particularly, aqueous rechargeable zinc-ion batteries (ZIBs) using mild acidic electrolytes are considered promising compared to LIBs due to low cost, high theoretical capacity (820 mAh g-1), and relatively low redox potential (-0.76 V vs SHE) of Zn metal anode. So far, aqueous ZIBs have been shown considerable progress, but there are still issues that should be overcome. The design and development of high-performance cathodes are one of the main problems to boost energy density.
    Manganese-based materials such as MnO2 with different polymorphs (-MnO2,-MnO2, -MnO2, -MnO2) and other lower valance manganese oxides (MnO, Mn2O3, Mn3O4) have revealed good electrochemical performance in aqueous ZIBs as a result of their high abundance on earth, high energy density, low cost, and multi-valent crystal structures. However, they undergo capacity fading during cycling because of their low conductivity, low structural stability, structural transformations, and manganese dissolution caused by the disproportionation reaction. In this study, we focus on improving the performance and elucidating the energy storage mechanism of manganese-based oxide cathodes through transition metal doping for ZIBs.
    In the first work, Cu doped and manganese/oxygen-deficient Cu0.09MnO is designed as high capacity cathode for aqueous ZIBs. Electrochemical mechanism investigation results show that the initial Cu0.09MnO nanospheres are transformed to Cu0.01MnO2.nH2O nanoflowers for co-insertion/extraction of H+/Zn2+ ions followed by reversible phase transformation between Cu-MnO2.nH2O and ZnCu-MnO2.nH2O/MnOOH. The underlying phase transformation of Cu0.044MnO and the energy storage mechanism of the activated Cu-MnO2.nH2O are systematically investigated with different ex-situ characterization techniques. The activated Cu-MnO2.nH2O has manganese vacancies, which remarkably triggers lattice oxygen redox reaction in Cu-MnO2.nH2O for charge compensation. As a result, the Zn/Cu-MnO2.nH2O batteries delivered a high specific capacity of 320 mAh g-1 at 0.5C and long-term cycling life with 70% capacity retention over 1000 cycles at 1C. In addition, the electrochemical properties and structural evolution of Cu-MnO electrodes were investigated without MnSO4 additive, demonstrating similar behavior with that of MnSO4 additive except the capacity fades rapidly.
    In the second work, we designed Ag0.4Mn8O16 by structural engineering of -MnO2 via Ag+ incorporation for ZIBs cathode material and demonstrate the electrochemical performance and energy storage mechanism. The sliver species are well dispersed in the tunnels of -MnO2, which results in higher surface area, smaller nanorods, and oxygen vacancies in Ag0.4Mn8O16 structure. The H+/Zn2+ insertion/extraction and Ag+ reduction/oxidation accompanied by the reversible phase transformation/conversion reaction between Ag0.4Mn8O16 and ZnxMn8O16/MnOOH are observed. As a result, Zn/Ag0.4Mn8O16 batteries delivered an excellent electrochemical performance such as impressive rate capability, high specific capacity of 306 mAh g-1 at 0.1 A g-1, and long-term cycling life over 800 cycles at 1 A g-1 compared to -MnO2 (227 mAh g-1 at 0.1 A g-1).
    Lastly, the role of tunnel potassium (K+) concentration on the electronic conductivity and ion diffusivity was investigated. The more tunnel K+ in -MnO2 not only enhances the electronic conductivity through increasing electron hopping using Mn3+/Mn4+ mixtures but also improves ion diffusivity via tunnel expansion.

    摘要 i Abstract v Acknowledgment viii Table of contents ix Index of figures xiii Index of tables xix List of units and abbreviations xxi Chapter 1: General background 1 1.1. Energy sources and their storage systems 1 1.2. Rechargeable batteries 1 1.3. Aqueous rechargeable zinc-ion batteries (ZIBs) 3 1.4. Components of aqueous ZIBs 5 1.5. Device structure and working principles of aqueous ZIBs 5 1.6. Challenges of aqueous ZIBs 7 1.7. Anode materials 8 1.8. Aqueous electrolytes 9 1.9. Current collectors 10 1.10. Cathode materials 10 1.10.1. Manganese-based cathodes 11 1.10.2. Vanadium (V)-based cathodes 12 1.10.3. Prussian Blue, organic compound, and other types of cathode materials 14 Chapter 2: Electrochemistry and Zn2+ storage mechanism of manganese-based oxide cathodes 15 2.1. Introduction 15 2.2. Energy storage mechanism in manganese oxide cathode materials 16 2.2.1. Zn2+ insertion/extraction mechanism 16 2.2.2. Chemical conversion reaction mechanism 17 2.2.3. H+ and Zn2+ Co-insertion/extraction Mechanism 19 2.2.4. Dissolution-deposition reaction mechanism 20 2.3. Challenges of Mn-based oxide cathode materials 23 2.4. Strategies to improve stability and performance of Mn-based cathodes 24 2.4.1. Nanostructure design 24 2.4.2. Pre-intercalation of ions and molecules 25 2.4.3. Electrolyte additive 27 2.4.4. Surface coating 28 2.4.5. Defect engineering 29 2.5. Motivation and objectives 35 2.5.1. Motivation 35 2.5.2. Objectives of the study 36 Chapter 3: Materials, experimental methods, and characterization techniques 37 3.1. Chemicals and reagents 37 3.2. Experimental section 39 3.2.1. Synthesis of Cu-MnO nanospheres 39 3.2.2. Synthesis of Ag0.4Mn8O16 nanorods 39 3.2.3. Synthesis of -MnO2 nanofibers 40 3.3. Cathode preparation 40 3.4. Materials characterization 41 3.5. Electrochemical measurement 42 Chapter 4: Electrochemical transformation reaction of Cu-MnO in aqueous rechargeable zinc-ion batteries for high performance and long cycle life 43 4.1. Introduction 43 4.2. Results and discussion 45 4.2.1. Synthesis and characterization of Cu-MnO nanospheres 45 4.2.2. Phase transformation of Cu-MnO Nanospheres 53 4.2.3. Energy storage mechanism of Zn/Cu-MnO2.H2O batteries 61 4.2.4. Electrochemical tests 66 4.2.5. Summary 73 Chapter 5: Structural engineering of -MnO2 cathode by Ag+ incorporation for high capacity aqueous zinc-ion batteries 75 5.1. Introduction 75 5.2. Results and Discussion 77 5.2.1. Morphological and structural characterization of Ag0.4Mn8O16 nanorods 77 5.2.2. Electrochemical performance of Ag0.4Mn8O16 cathode 83 5.2.3. Energy storage mechanism 89 5.2.4. Summary 96 Chapter 6: The role of tunnel K+ concentration on the performance of -MnO2 cathode materials for rechargeable aqueous zinc-ion batteries 97 6.1. Introduction 97 6.2. Results and discussion 98 6.2.1. Structural and morphological characterization of -MnO2 nanofibers 98 6.2.2. Electrochemical tests 101 6.2.3. Energy storage mechanism 105 6.2.4. Summary 107 Chapter 7: Conclusions and perspectives 109 7.1. Conclusions 109 7.2. Perspectives 111 Reference 113 List of research papers 133 Conference presentations 134 Award 135

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