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研究生： 吳岱璇
Tai-Hsuan Wu
論文名稱： 鹵化物固態複合正極的平台優化及其固態電池性能衰退現象
The platform optimization of halide solid-state composite cathodes and the degradation phenomenon of solid-state battery performance
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
學位類別： 碩士
Master
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： 中文
論文頁數： 134
中文關鍵詞： 鹵化物固態電解質 、硫化物固態電解質 、複合正極 、全固態電池 、介面反應 、乾式成膜
外文關鍵詞： halide solid electrolyte, sulfide solid electrolyte, composite cathode, all- solid-state battery, interface reaction, dry film process
相關次數： 點閱：500  下載：4 
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  •  上一筆

    • 固態電池（All-solid-state battery, ASSB）是一種較新的高能量密度電池技術，相對於傳統鋰離子電池（Lithium-ion battery, LIB）更安全且具有更高能量密度，具有巨大的應用前景。本研究聚焦於優化鹵化物複合正極，以提升全固態電池的性能和穩定性。
    第一部分，以高電容量的層狀結構的多晶富鎳過渡金屬氧化物（LiNi0.8Mn0.1Co0.1O2, NMC811）的正極活性材料配合界面穩定性較佳的鹵化物固態電解質作為主要材料，鹵化物複合正極的優化過程首先從固態全電池組成的優化開始，以確保有穩定的平台觀測，包括正極集電材料的優化改為碳塗層鋁箔、負極材料選擇較高的電導率集電材的Li/Cu，以及複合正極組成增加導電碳至3 wt%提升導電度，結合以上的優化條件組成全固電池，在首圈充電中，電容量為214.21 mAh/g，放電電容量為177.85 mAh/g，達到了83.02%的庫倫效率。在20個循環中，平均庫倫效率為98.21%，在首圈充電時，面電容達到了4.53 mAh/cm2，顯示其具有高效的電化學性能，但衰退的現象仍清楚可見，第20圈電容量維持率降低至72.55%。
    第二部分，利用X射線吸收光譜（XAS）技術研究NCM811和LIC之間的界面相互作用，研究結果顯示，高電位下NMC811的Ni離子會被LIC還原為較低的價態，通過計算平均價態，可以更直接地比較還原程度，進行傅立葉轉化為R-space進行晶格空間分析，發現混合過LIC的NMC811各元素之鍵長縮短，並降低了Ni-O的強度比例，證實了除了高電位下價數降低的還原現象，LIC與多晶NMC811不同程度混合也會導致晶體結構的變化。
    最後部分，利用XANES及XRF mapping的量測，在負極端發現了正極材料中的過渡金屬訊號，如同液態電池的cross-talk的現象，並隨著循環圈數的增加，在XRF mapping可以看到沉積的分布量與範圍隨之增加，並且遷移於全固態電池各層之間，透過XANES及XPS可以發現，大部分Ni都是以2+和3+的價態沉積於負極端，這些實驗結果對於複合正極的衰退有了更多不同面向的認識，以利在日後進一步研究複合正極的性能衰退機制。

    Solid-state batteries (SSBs) are a relatively new battery technology with higher energy density and improved safety than conventional lithium-ion batteries (LIBs). They hold great potential for various applications. This study focuses on optimizing halide composite cathode to enhance the performance and stability of all-solid-state batteries (ASSBs).
    In the first part, a promising cathode electrode material nickel-rich lithium transition metal oxides (LiNi0.8Mn0.1Co0.1O2, NMC811) with layer structure and high capacity, is combined with halide solid electrolyte with superior interface stability as the main material. The optimization process of the halide composite cathode begins with optimizing the composition of the solid-state full cell to ensure a stable observation platform. This includes optimizing the positive electrode current collector material by using carbon-coated aluminum foil, selecting anode electrode material with a higher conductivity current collector such as Li/Cu, and increasing the conductive carbon content in the composite cathode to 3 wt% to enhance conductivity. By combining these optimization conditions, a full solid-state battery is fabricated, which exhibits a capacity of 214.21 mAh/g during the initial charging and a discharge capacity of 177.85 mAh/g, achieving 83.02% coulombic efficiency. After 20 cycles, the average coulombic efficiency is 98.21%. The surface capacity during the initial charging reaches 4.53 mAh/cm2, demonstrating its feasibility and potential for solid-state batteries. However, the degradation phenomenon is still evident, with the capacity retention rate decreasing to 72.55% after the 20th cycle.
    In the second part, X-ray Absorption Spectroscopy (XAS) is employed to investigate the interface interaction between active material NCM811 and the halide solid electrolyte. The research findings reveal that Ni ions in NMC811 are reduced to lower oxidation states by the solid electrolyte under high potentials. The average oxidation states are calculated to compare the reduction extent directly. Fourier transformation of XAS data into R-space is performed for lattice spatial analysis, which indicates shortened bond lengths of various elements and a decrease in the Ni-O intensity ratio in NMC811 mixed with the solid electrolyte. This confirms the reduction phenomenon observed at high potentials and reveals that the mixture of the solid electrolyte with poly-crystalline NMC811 can also induce changes in the crystal structure.
    In the final part, XANES and XRF mapping measurements are conducted to investigate the phenomenon of cross-talk between the transition metals in the active material NMC811 and the anode electrode in the ASSB. With increasing cycle numbers, XRF mapping reveals an increase in the distribution and range of deposited transition metals, resembling the cross-talk behavior observed in liquid batteries. Furthermore, the transition metals migrate between different layers of the solid-state battery. XANES and XPS analyses indicate that most deposited Ni exists in the 2+ and 3+ states at the anode side. These experimental results provide further insights into the performance degradation mechanisms of the composite cathode electrode and facilitate future research in this area.

    摘要 I Abstract III 致謝 V 目錄 VII 圖目錄 XI 表目錄 XXII 第 1 章 緒論 1 1.1 前言 1 1.2 商業化鋰離子二次電池 2 1.3 全固態鋰離子電池 3 1.4 全固態電池的挑戰極為來發展性 5 第 2 章 全固態電池的電極設計 11 2.1氧化物正極材料 11 2.1.1 鈷酸鋰正極材料(LCO) 11 2.1.2 錳酸鋰正極材料(LMO) 12 2.1.2 磷酸鋰鐵正極材料(LFP) 13 2.1.3高鎳三元正極材料(NMC) 16 2.2 固態電解質 22 2.2.1 硫化物電解質 23 2.2.2 鹵化物電解質 25 2.3 固態複合正極 27 2.3.1 複合正極中之分解反應 27 2.3.2鹵化物複合正極 29 2.4全固態複合正極濕試膜與乾式膜 32 2.4.1固態複合正極溼式成膜 32 2.4.2固態複合正極乾式成膜 34 2.5 合金型態之負極 36 2.6 研究動機與目的 39 第 3 章 實驗方法 41 3.1 儀器設備 41 3.2 實驗藥品 42 3.3 實驗步驟及實驗儀器 43 3.3.1 濕式複合正極黏著劑配製 43 3.3.2 濕式複合正極塗布 43 3.3.3 乾式複合正極膜製備 45 3.3.3 固態電池 47 3.4 電化學測試 49 3.4.1 充放電測試 49 3.4.2 交流阻抗分析 49 3.4.3 線性掃描伏安法分析 50 3.5 儀器分析與原理 51 3.5.1 X-ray繞射分析(XRD) 51 3.5.3 X光射線光電子光譜(XPS) 51 3.5.4 X光射線吸收光譜(XAS) 52 第 4 章 鹵化物複合正極平台建立及優化 55 4.1固態全電池組成優化 56 4.1.1正極之集電材料優化 56 4.1.2 負極材料選擇與比較 58 4.1.3 鹵化物複合正極之導電碳比例優化 63 4.2鹵化物固態乾式複合正極膜優化 64 4.2.1濕式製程的問題與挑戰 64 4.2.1乾式固態複合正極膜製程之平台建立 65 4.2.2乾式固態複合正極膜全固態電池應用 72 4.3鹵化物複合正極反應分析 75 4.3.1 LIC與NMC811混合之XRF與XANES的介面鑑定分析 75 4.3.2 LIC與NMC811混合之XAS與R-space的鑑定分析 81 4.4 鹵化物複合正極之cross-talk現象 89 第 5 章 結論 99 第 6 章 未來展望與建議 101 參考資料 102

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