鋰離子電池是廣泛應用於日常生活的可充電電池設備，具有體積小、能量密度高、無記憶效應等優點，在筆記型電腦、手機、電動車等產品中常見使用。鋰離子電池的負極材料主要有石墨和矽兩類。石墨具有高穩定性和低成本等優勢，但其理論電容量相對較低 (372 mA h g−1)。矽則具有高理論電容量 (4000 mA h g−1)，但在充放電過程中會出現體積變化大的問題，導致循環穩定性差。負極材料的研究重點在於提高能量密度、循環穩定性和充放電速率。本研究以新穎氧化物作為鋰離子電池負極材料，進行合成和材料鑑定，並通過電化學性能測試評估其性能。並對新材料的儲能機制進行研究，以了解其在充放電過程中的鋰化/脫鋰機制以及材料結構的變化情況。透過這些研究，希望能夠開發出具有高能量密度、良好循環穩定性和快速充放電速率的新型負極材料，以提升鋰離子電池的性能和應用範圍。
本論文中第一部份首次合成含鎳之多釩酸鹽Na6[NiV14O40]作為負極材料於高能量密度儲鋰應用。Na6[NiV14O40]以適合低成本大規模生產的簡單溶液法製備，其半電池電容量高達700 mA h g−1，在循環400次後仍未衰退，顯示其出色的循環穩定性。本研究使用臨場X光吸收光譜、X光繞射、穿透式X光顯微鏡和密度泛函理論計算研究其電荷儲存機制，其中V5+在鋰化過程中被還原為V2+，證實Na6[NiV14O40]為一種嵌入型負極材料。此外，Na6[NiV14O40]在循環過程中保持其非晶結構，故體積膨脹/收縮程度相當微小，因此具有良好的循環穩定性。Na6[NiV14O40]//LiFePO4鋰離子全電池具有高達300 W h kg−1之能量密度，而Na6[NiV14O40]//膨脹中間相碳球 (expanded mesocarbon microbeads) 鋰離子電容在175.7與7774.2 W kg−1之功率密度下可分別提供218.5和47.9 W h kg−1之能量密度。
第二部分根據過去的研究指出(Mg, Co, Ni, Cu, Zn)O高熵氧化物作為鋰離子電池之負極材料具有優異的循環穩定性，並歸因於高熵穩定效應與非活性Mg之貢獻。本研究合成具有不同Mg含量之(Mg, Co, Ni, Cu, Zn)O，並以循環伏安法和恆電流充放電測量分析不同非活性元素含量對其電化學性質之影響。接著進一步以臨場同步輻射穿透式X光顯微鏡觀察其鋰化/脫鋰過程中材料形態的變化。希望透過研究非活性Mg的作用，有助於開發用於鋰離子電池之高熵氧化物電極。
第三部分中為拓展不同結構高熵氧化物作為鋰離子電池負極材料之研究，本研究採用簡單的固態燒結方法合成新穎的單相尖晶石結構高熵氧化物 (Ni0.2Co0.2Mn0.2Fe0.2Ti0.2)3O4 (NCMFT)。NCMFT在100 mA g−1的電流密度下具有約 560 mA h g−1之電容量，並在100次循環後仍保有100%電容量。利用臨場X光吸收近邊結構和非臨場X光光電子能譜分析，了解NCMFT負極在鋰化和脫鋰過程中之氧化還原反應，證實其中部分陽離子屬於置換型機制，而Ti則屬嵌入型反應。此外，以臨場X光繞射和非臨場穿透式電子顯微鏡用於分析置換反應過程中的結構變化，並以臨場穿透式X光顯微鏡觀察NCMFT負極的體積變化行為。藉由上述分析方法，對NCMFT負極的儲能機制進行全面的研究，以了解高熵氧化物在儲能應用之機制。

Lithium-ion batteries are widely used rechargeable battery devices in everyday life, known for their small size, high energy density, and lack of memory effect. They are commonly used in products such as laptops, smartphones, and electric vehicles. Graphite and silicon are commonly used anode materials in lithium-ion batteries. Graphite offers advantages such as high stability and low cost, but its theoretical capacity is relatively low (372 mA h g−1). On the other hand, silicon has a high theoretical capacity (4000 mA h g−1), but it suffers from significant volume changes during charging and discharging, leading to poor cycling stability. Research on anode materials focuses on improving energy density, cycling stability, and charge/discharge rate. This study employed novel oxides as anode materials for lithium-ion batteries. The synthesis and material characterization were conducted, followed by electrochemical performance testing to evaluate their capabilities. The energy storage mechanism of the new materials was also investigated to understand the lithiation/delithiation process and the structural changes during charge and discharge. These investigations aim to develop new anode materials with high energy density, good cycling stability, and fast charge/discharge rates, thereby enhancing the performance and application range of lithium-ion batteries.
In the first part, this study synthesized a nickel-containing heteropolyvanadate, Na6[NiV14O40], as an anode material for lithium storage, offering high energy density. Na6[NiV14O40] was prepared using a solution method suitable for low-cost, large-scale production. The prepared half-cell exhibited a high capacity of 700 mA h g−1 and demonstrated excellent cycle stability, maintaining its capacity without fading after 400 cycles. The charge storage mechanism was investigated using in situ X-ray absorption spectroscopy, X-ray diffraction, transmission X-ray microscopy, and density functional theory calculations. These analyses revealed that V5+ was reduced to V2+ during lithiation, confirming that Na6[NiV14O40] functions as an intercalation-type anode material. Additionally, Na6[NiV14O40] maintained its amorphous structure, with negligible volume expansion or contraction observed during cycling. In full-cell tests, Na6[NiV14O40]//LiFePO4 lithium-ion batteries exhibited a high energy density of 300 W h kg−1. When applied to lithium-ion capacitors, Na6[NiV14O40]//expanded mesocarbon microbeads demonstrated energy densities of 218.5 and 47.9 W h kg−1 at power densities of 175.7and 7774.2 W h kg−1, respectively.
The second part of the study builds upon previous studies indicating that (Mg, Co, Ni, Cu, Zn)O high-entropy oxide exhibits excellent cycling stability as anode material for lithium-ion batteries, attributed to the high-entropy stabilization effect and the inactive Mg. This stability is attributed to the combined effects of high-entropy stabilization and the inactive Mg contribution. In this study, (Mg, Co, Ni, Cu, Zn)O with varying Mg contents was synthesized, and the influence of inactive element ratios on their electrochemical properties was analyzed using cyclic voltammetry and galvanostatic charge-discharge measurements. Furthermore, the morphological changes of the materials during the lithiation/delithiation process were observed using an operando synchrotron transmission X-ray microscope. Investigating the role of inactive Mg is expected to contribute to the development of high-entropy oxide electrodes for lithium-ion batteries.
In the third part, we investigate high-entropy oxides with diverse structures as anode materials for lithium-ion batteries. This study employed a simple solid-state sintering method to synthesize a novel high-entropy oxide, (Ni0.2Co0.2Mn0.2Fe0.2Ti0.2)3O4 (NCMFT), with a single-phase spinel structure. NCMFT demonstrated a capacitance of approximately 560 mA h g−1 at a current density of 100 mA g−1, along with exceptional capacity retention of 100% after 100 cycles. Through operando X-ray absorption near-edge structure and ex-situ X-ray photoelectron spectroscopy analysis, the redox reaction of NCMFT anode during lithiation/delithiation was comprehended, confirming its involvement in the conversion mechanism. Operando X-ray diffraction and ex-situ transmission electron microscopy were used to analyze the structural changes during the displacement reaction. In addition, the volume change behavior of the NCMFT negative electrode was observed using a field transmission X-ray microscope. By conducting the aforementioned analyses, the energy storage mechanism of the NCMFT anode was systematically investigated, thereby providing fundamental analytical methods for comprehending the energy storage applications of high-entropy oxides.

摘要 I
Abstract III
致謝 VI
目錄 VIII
圖目錄 XII
表目錄 XIX
第1章 緒論 1
1.1 研究背景 1
1.2 研究動機 1
第2章 文獻回顧與原理簡介 3
2.1 鋰離子電池介紹 3
2.2 鋰離子電容介紹 3
2.3 鋰離子電池負極材料 5
2.4 多金屬氧酸鹽 7
2.5 高熵氧化物 12
第3章 實驗方法 23
3.1 實驗架構 23
3.2 實驗藥品 26
3.3 材料合成 27
3.3.1 Na6[NiV14O40] 27
3.3.2 (Mg, Co, Ni, Cu, Zn)O 28
3.3.3 (Ni, Co, Mn, Fe, Ti)3O4 29
3.4 電池組裝 30
3.4.1 電極製備 30
3.4.2 freestanding電極製備 30
3.4.3 鈕扣型電池組裝 30
3.4.4 開洞鈕扣型電池組裝 32
3.4.5 軟包型電池組裝 32
3.4.6 全電池組裝 33
3.5 材料特性分析方法 34
3.5.1 X光繞射分析 34
3.5.2 熱重分析 34
3.5.3 傅立葉轉換紅外光譜儀 34
3.5.4 感應耦合電漿放射光譜儀 34
3.5.5 場發射掃描式電子顯微鏡 35
3.5.6 穿透式電子顯微鏡 35
3.5.7 X光吸收光譜 36
3.6 電化學性質量測方法 36
3.6.1 循環伏安法 36
3.6.2 恆電流充放電測試 37
3.6.3 恆電位間歇滴定技術 37
3.6.4 全電池測試 38
3.6.5 電化學阻抗頻譜分析 38
3.7 模擬計算分析方法 38
3.8 電池臨場/非臨場量測及分析方法 39
3.8.1 非臨場X光光電子能譜分析 39
3.8.2 非臨場掃描式電子顯微鏡 39
3.8.3 非臨場穿透式電子顯微鏡 39
3.8.4 臨場X光吸收光譜 39
3.8.5 臨場X光繞射分析 40
3.8.6 臨場穿透式X光顯微鏡 40
第4章 結果與討論 41
4.1 含鎳之多金屬釩酸鹽做為鋰離子儲能元件負極之應用與機制探討 42
4.1.1 Na6[NiV14O40]之材料分析鑑定 42
4.1.2 Na6[NiV14O40]之電化學性質表現 45
4.1.3 Na6[NiV14O40]之儲能機制探討 48
4.1.4 Na6[NiV14O40]之全電池測試 59
4.1.5 Na6[NiV14O40]研究總結 62
4.2 以臨場穿透式X光顯微鏡探討高熵氧化物 (Mg, Co, Ni, Cu, Zn)O 負極中非活性元素含量之影響 63
4.2.1 不同非活性元素比例(Mg, Co, Ni, Cu, Zn)O之材料分析鑑定 63
4.2.2 不同非活性元素比例(Mg, Co, Ni, Cu, Zn)O之電化學性質表現 66
4.2.3 不同非活性元素比例(Mg, Co, Ni, Cu, Zn)O之臨場TXM分析 71
4.2.4 不同非活性元素比例(Mg, Co, Ni, Cu, Zn)O之研究總結 75
4.3 尖晶石高熵氧化物(Ni, Co, Mn, Fe, Ti)3O4 作為鋰離子電池負極材料之性質與機制探討 76
4.3.1 NCMFT之材料分析鑑定 76
4.3.2 NCMFT之電化學性質量測與分析 85
4.3.3 NCMFT之鋰化/脫鋰價態分析探討 89
4.3.4 NCMFT之鋰化/脫鋰結構分析探討 95
4.3.5 NCMFT之鋰化/脫鋰體積變化分析 98
4.3.6 NCMFT之研究總結 101

第5章 未來展望 103
研究發表 104
參考資料 106

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