鋰離子電池具有高能量密度和長循環壽命，因此被認為是理想的儲能系統。然而，傳統鋰離子電池含有可燃的有機電解質，使其增加了爆炸和火災的風險，故全固態鋰離子電池在近年來引起了廣泛的關注。使用固態電解質可有效避免有機液態電解質燃燒及爆炸的危險性，並提升電池的性能。石榴石型 (Garnet-type) 氧化物Li7La3Zr2O12為常見的固態電解質材料，其中摻雜Ta的Li6.4La3Zr1.4Ta0.6O12具有高離子傳導率，然而其易於與空氣中的H2O和CO2反應，在接觸空氣後離子傳導率會明顯衰減。為解決現今商業化鋰離子電池之安全性問題，並提升電池之能量密度，本研究合成具有高離子傳導率之固態電解質，包含高熵石榴石固態電解質以及四元石榴石固態電解質，後續進行材料分析與電化學分析，並以磷酸亞鐵鋰 (LiFePO4) 之正極材料組成全電池做測試，以探討固態電解質材料組裝成全電池之可行性。
在本研究第一部分中，成功地使用固態燒結法合成新型的石榴石高熵氧化物，Li6.4La3Zr0.4Ta0.4Nb0.4Y0.6W0.2O12 (LLZTNYWO)，作為鋰離子電池的固態電解質，並以掃描式電子顯微鏡、X光繞射分析、穿透式電子顯微鏡、交流阻抗分析、循環伏安法分析以及恆電流充放電等材料與電性分析以了解其材料之表面結構、結晶性以及電化學特性。將Ta、Nb、Y以及W置換Zr，可顯著提高其離子傳導率，並且具有較高的空氣穩定性及較低的燒結溫度。相比單一元素掺雜的Li6.6La3Zr1.6Ta0.4O12 (6.57 × 10−5 S cm−1) 、Li6.6La3Zr1.6Nb0.4O12 (2.19 × 10−5 S cm−1) 和Li6.2La3Zr1.6W0.4O12 (1.16 × 10−4 S cm−1)，LLZTNYWO具有1.16 × 10−4 S cm−1的高離子傳導率。此外，它在與等摩爾的Li5.8La3Zr0.4Ta0.4Nb0.4Y0.4W0.4O12 (1.95 × 10−5 S cm−1) 比較時也表現出更高的離子傳導率。由於石榴石結構在大氣下之不穩定性，會與空氣中之水與二氧化碳反應而生成碳酸鋰，造成離子傳導率降低，然而LLZTNYWO在大氣下存放30天後仍維持極佳的離子傳導率，並未衰減，顯示其出色的空氣穩定性。此外， LZTNYWO表現出高達6 V的電化學穩定範圍和優異的電化學穩定性。與磷酸亞鐵鋰組成之全電池後，於0.1C (17 mA g−1)電流密度下之電容量高達163 mAh g−1，且經過250圈充放電循環後仍能維持79.8%之電容量保持率。顯示其為一種有潛力的鋰離子電池固態電解質。
本研究第二部分以固態燒結法製備四元石榴石結構氧化物， Li6.5La3Zr0.5Ta0.5Nb0.5Y0.5O12 (LLZTNYO)，作為鋰離子電池的固態電解質，並以掃描式電子顯微鏡、X光繞射分析、穿透式電子顯微鏡、交流阻抗分析、循環伏安法分析以及恆電流充放電等材料與電性分析以了解其材料之表面結構、結晶性以及電化學特性。相比單掺雜的Li6.5La3Zr1.5Ta0.5O12 (2.44 × 10−5 S cm−1) 、Li6.5La3Zr1.5Nb0.5O12 (2.62 × 10−5 S cm−1) 和Ta與Nb共同摻雜的Li6 La3ZrTa0.5Nb0.5O12 (1.78 × 10−4 S cm−1)，LLZTNYO具有1.98 × 10−4 S cm−1的高離子傳導率。本研究為了驗證中熵石榴石結構之空氣穩定性，亦量測存放不同天之離子傳導率，LLZTNYO在大氣下存放30天後仍維持極佳的離子傳導率，並未出現明顯之衰退現象，代表其具有良好的空氣穩定性。此外，中熵石榴石結構亦具有寬廣的穩定電化學窗範圍和對Li金屬優異的電化學穩定性。與磷酸亞鐵鋰組成之全電池後，於0.1C (17 mA g−1)電流密度下之電容量高達167 mAh g−1，且經過10圈充放電循環後仍能維持等值之電容量。表明它是一種有潛力的鋰離子電池固態電解質。

Due to their high energy density and long cycling life, lithium-ion batteries are considered an ideal choice for energy storage systems. However, the use of organic liquid electrolytes increases the risk of explosion and fire. Therefore, all-solid-state lithium-ion batteries have gained significant attention as they eliminate the hazards of combustion and explosions associated with liquid electrolytes, while enhancing battery performance. Garnet-type oxides are commonly used as solid electrolyte materials. The commonly used Ta-doped garnet oxide, Li7La3Zr2O12, is susceptible to reactions with CO2 and H2O in air, leading to a significant decrease in its ionic conductivity.
To address the safety issues and improve the energy density of commercial lithium-ion batteries, this study focuses on synthesizing high ionic conductivity solid electrolyte materials, specifically high-entropy garnet and ternary-doped garnet-type solid electrolytes. The materials are then analyzed using techniques such as scanning electron microscopy, X-ray diffraction analysis, transmission electron microscopy, electrochemical impedance spectroscopy, cyclic voltammetry, and galvanostatic charge-discharge measurements to understand their surface structure, crystallinity, and electrochemical properties. Ta, Nb, Y, and W are used as substitutes for Zr, which significantly enhance ionic conductivity, possess high stability in air, and have a lower sintering temperature. In comparison to singly doped Li6.6La3Zr1.6Ta0.4O12 (6.57 × 10−5 S cm−1), Li6.6La3Zr1.6Nb0.4O12 (2.19 × 10−5 S cm−1), and Li6.2La3Zr1.6W0.4O12 (1.16 × 10−4 S cm−1), LLZTNYWO exhibits higher Li-ion conductivity at 1.16 × 10−4 S cm−1. Furthermore, it demonstrates higher ionic conductivity compared to equimolar Li5.8La3Zr0.4Ta0.4Nb0.4Y0.4W0.4O12 (1.95 × 10−5 S cm−1). One notable challenge with garnet-based electrolytes is their instability in air, leading to reactions with atmospheric moisture and CO2 to form lithium carbonate. However, LLZTNYWO exhibits excellent air stability, maintaining its high ionic conductivity for 30 days in an air atmosphere without any decay. Additionally, LLZTNYWO demonstrates a wide electrochemical window of up to 6 V vs. Li/Li+ and excellent electrochemical stability against Li metal. When assembled into full cells with lithium iron phosphate (LiFePO4) as the cathode material, LLZTNYWO shows a high capacity of 163 mAh g−1 at a current density of 17 mA g−1 and retains 79.8% of its capacity after 250 charge-discharge cycles. These results indicate that LLZTNYWO is a promising solid electrolyte for lithium-ion batteries.
In the second part of this study, ternary-doped garnet structures were prepared using solid-state sintering. Specifically, Li6.5La3Zr0.5Ta0.5Nb0.5Y0.5O12 (LLZTNYO) was synthesized as a solid electrolyte for lithium-ion batteries. The material was then analyzed using scanning electron microscopy, X-ray diffraction analysis, transmission electron microscopy, alternating current impedance analysis, cyclic voltammetry, and constant current charge-discharge measurements to understand its surface structure, crystallinity, and electrochemical properties. Compared to single-doped Li6.5La3Zr1.5Ta0.5O12 (2.44 × 10−5 S cm−1)、and Li6.5La3Zr1.5Nb0.5O12 (2.62 × 10−5 S cm−1), as well as Li6 La3ZrTa0.5Nb0.5O12 co-doped with Ta and Nb (1.78 × 10−4 S cm−1), the LLZTNYO exhibits a comparable high ion conductivity of 1.98 × 10−4 S cm−1. This study aimed to verify the air stability of the LLZTNYO. Hence, we measured its ion conductivity after storing it for different periods. After being stored in atmospheric conditions for 30 days, the LLZTNYO maintained excellent ion conductivity without significant degradation, indicating its good air stability. This demonstrates its outstanding air stability. Additionally, the LLZTNYO garnet structure also exhibits a wide and stable electrochemical window of up to 6 V when cycled with a Li/Li+ reference electrode, showcasing excellent electrochemical stability towards Li metal. When used as a solid electrolyte in a full lithium-ion battery configuration with lithium iron phosphate, it exhibited a high capacity of 167 mAh g−1 at a current density of 0.1C (17 mA g−1), and maintained a consistent capacity after 10 charge-discharge cycles. This indicates its potential as a solid-state electrolyte for lithium-ion batteries.

目錄
摘要 I
Abstract III
致謝 VI
目錄 VII
圖目錄 XI
表目錄 XVII
第一章 研究目的 1
1.1 研究背景 1
1.2 研究動機 2
第二章 文獻回顧與原理簡介 5
2.1 鋰離子電池 5
2.1.1 鋰離子電池工作原理與簡介 6
2.2 固態鋰離子電池 8
2.3 鋰離子電解質 11
2.3.1 有機液態電解質 11
2.3.1.1 有機液態電解質溶劑 12
2.3.1.2 有機液態電解質鋰鹽 13
2.3.2 陶瓷固態電解質 14
2.3.3 高分子固態電解質 22
2.3.4 離子液體電解質 26
2.4 以多元摻雜石榴石結構組裝全固態鋰電池 26
第三章 實驗流程與研究方法 30
3.1 實驗架構 30
3.2 實驗藥品 31
3.3 固態電解質之合成 33
3.4 介面添加劑之製備 34
3.5 電池組裝 35
3.5.1 極片製備 35
3.5.2 鈕扣電池組裝 35
3.6 材料電化學分析法 37
3.6.1 交流阻抗分析 (Electrochemical Impedance Spectroscopy, EIS) 37
3.6.2 定電壓直流電極化分析 (Wagner’s DC Polarization Technique) 39
3.6.3 循環伏安法 (Cyclic Voltammetry, CV) 40
3.6.4 恆電流充放電測試 (Galvanostatic Charge Discharge measurement, GCD) 40
3.7 材料特性分析法 41
3.7.1 場發射掃描式電子顯微鏡 (Field Emission Scanning Electron Microscopy, FESEM) 41
3.7.2 X光繞射分析 (X-Ray Diffraction, XRD) 41
3.7.3 穿透式電子顯微鏡 (Transmission Electron Microscopy, TEM) 42
3.7.4 X光吸收光譜 (X-Ray Absorption Spectroscopy, XAS) 42
3.7.5 感應耦合電漿光學發射光譜儀 (Inductively coupled plasma-optical emission spectrometry, ICP-OES) 43
第四章 結果與討論 45
4.1 高熵五元石榴石結構應用於全固態鋰離子電池電解質材料之研究 45
4.1.1 高熵石榴石結構之材料分析與鑑定 46
4.1.1.1 高熵石榴石結構之晶體結構鑑定 46
4.1.1.2 高熵石榴石結構之表面形貌分析 53
4.1.1.3 高熵石榴石結構之元素分析 57
4.1.2 高熵石榴石結構之電化學性質分析 59
4.1.2.1 高熵石榴石結構之交流阻抗分析 59
4.1.2.2 高熵石榴石結構之定電壓直流電極化分析 71
4.1.2.3 高熵石榴石結構之循環伏安法測試分析 72
4.1.2.4 高熵石榴石結構之恆電流充放電測試分析 73
4.1.3 結果討論 77
4.2 中熵四元石榴石結構氧化物應用於全固態鋰離子電池電解質材料之研究 78
4.2.1 四元石榴石結構之材料分析與鑑定 79
4.2.1.1 四元石榴石結構之晶體結構鑑定 79
4.2.1.2 四元石榴石結構之表面形貌分析 84
4.2.1.3 四元石榴石結構之元素 86
4.2.2 四元石榴石結構之電化學性質分析 86
4.2.2.1 四元石榴石結構之交流阻抗分析 87
4.2.2.2 四元石榴石結構之定電壓直流電極化分析 96
4.2.2.3 四元石榴石結構之循環伏安法測試分析 97
4.2.2.4 四元石榴石結構之恆電流充放電測試分析 99
4.2.3 結果討論 101
第五章 結論 102
第六章 未來展望 103
研究發表 104
參考資料 108



圖目錄
圖 1 1、石榴石結構與空氣中H2O與CO2反應示意圖[27] 3
圖 2 1、鋰離子電池充放電結構組成與電流方向示意圖 7
圖 2 2、全固態鋰離子電池結構示意圖 9
圖 2 3、以不同結構分類之固態鋰離子電解質與其離子傳導率在室溫下的比較[61] 15
圖 2 4、Li10GeP2S12 結構 16
圖 2 5、Perovskite晶格結構 17
圖 2 6、Garnet晶格結構 20
圖 2 7、石榴石結構與空氣中H2O與CO2反應示意圖[27] 20
圖 2 8、NASICON晶格結構 22
圖 2 9、PEO中的離子傳導過程[124] 23
圖 2 10、鋰離子在結晶區的傳遞[125] 23
圖 2 11、有序陶瓷與高熵陶瓷之離子傳導機制示意圖[151] 28
圖 3 1、高熵石榴石結構作為全固態鋰離子電池固態電解質之實驗架構 31
圖 3 2、合成LLZO之流程 34
圖 3 3、全電池組裝之示意圖。 36
圖 3 4、電化學穩定窗之半電池示意圖 36
圖 3 5、對稱電池組裝之示意圖 36
圖 3 6、量測夾具圖 38
圖 3 7、變溫量測設備裝置 39
圖 4 1、LLZTO、LLZNO、LLZTWO、LLZTNYWO以及LLZTNYWO_E之XRD圖 48
圖 4 2、LLZTO、LLZNO、LLZTWO、LLZTNYWO以及LLZTNYWO_E之XRD Rietveld精修數據 49
圖 4 3、(a) HR-TEM圖與Fast Fourier transform (FFT) 圖譜 (b) HR-TEM圖與晶面間距 (c) 亮場影像 (BF image) (d) 高角度環形暗場像 (High-angle annular dark-field image, HAADF image) 51
圖 4 4、在LLZTNYWO中Zr位置元素之Zr/Nb/Y K-edge and Ta/W L-edge 傅立葉轉換EXAFS圖 52
圖 4 5、燒結前之粉末顆粒SEM影像：(a) LLZTO、(b) LLZNO、(c) LLZWO以及(d) LLZTNYWO 54
圖 4 6、LLZTNYWO在1100 °C下燒結24小時後之結果 54
圖 4 7、研磨後之燒結錠片SEM 500倍影像：(a) LLZTO、(b) LLZNO、(c) LLZWO以及(d) LLZTNYWO；研磨後之燒結錠片SEM 5000倍影像：(e) LLZTO、(f) LLZNO、(g) LLZWO以及 (h) LLZTNYWO 56
圖 4 8、SEM與EDS影像：(a) LLZTO、(b) LLZNO、(c) LLZWO、(d) LLZTNYWO以及 (e) LLZTNYWO_E 57
圖 4 9、LLZTNYWO之高倍STEM-EDS分析 58
圖 4 10、LLZTNYWO之低倍STEM-EDS分析 58
圖 4 11、在25、40、60以及80 °C下量測 (a) LLZTO、(b) LLZNO、(c) LLZWO、(d) LLZTNYWO以及 (e) LLZTNYWO_E的Nyquist plots 61
圖 4 12、LLZTO、LLZNO、LLZWO、LLZTNYWO與LLZTNYWO_E在25到80 °C下之離子傳導率比較圖 62
圖 4 13、LLZTO、LLZNO、LLZWO、LLZTNYWO與LLZTNYWO_E在25到80 °C下之Arrhenius圖 64
圖 4 14、暴露在空氣下1、3、5、10、15、20以及30天下量測 (a) LLZTO、(b) LLZNO、(c) LLZWO、(d) LLZTNYWO以及 (e) LLZTNYWO_E的Nyquist plots 68
圖 4 15、LLZTO、LLZNO、LLZWO、LLZTNYWO與LLZTNYWO_E在暴露不同天下之離子傳導率比較圖 70
圖 4 16、LLZTNYWO之DC直流極化曲線，定電壓 = 1.5 V 71
圖 4 17、Li/solid electrolyte/Stainless steel(SS) 電池在25 °C下量測以1 mV s−1掃描速率下之CV圖：(a) LLZTO、(b) LLZNO、(c) LLZWO以及 (d) LLZTNYWO 73
圖 4 18、恆電流循環測試圖 (Galvanostatic cycling test)，鋰金屬的沉積與溶解時間為1小時：(a) LLZTO、(b) LLZNO、(c) LLZWO以及 (d) LLZTNYWO 74
圖 4 19、恆電流充放電測試圖 (a) Li//LLZTNYWO//LiFePO4 之全固態電池在電壓範圍為 2–3.8 V vs. Li/Li+ (b) Li//liquid electrolyte//LiFePO4 電池在電壓範圍為 2–4 V vs. Li/Li+ 之測試數據 76
圖 4 20、在17 mA g−1電流密度下 (0.1C) 之恆流充放電之循環性能圖 76
圖 4 21、LLZTO、LLZNO、LLZTNO以及LLZTNYO之XRD圖 81
圖 4 22、LLZTO、LLZNO、LLZTNO以及LLZTNYO之XRD Rietveld精修數據 82
圖 4 23、在LLZTNYO中Zr位置元素之Zr/Nb/Y K-edge與Ta/W L-edge 傅立葉轉換EXAFS圖 83
圖 4 24、研磨後之燒結錠片SEM 500倍影像：(a) LLZTO、(b) LLZNO、(c) LLZTNO以及(d) LLZTNYO；研磨後之燒結錠片SEM 10k影像：(e) LLZTO、(f) LLZNO、(g) LLZTNO以及(h) LLZTNYO 85
圖 4 25、SEM與EDS影像：(a) LLZTO、(b) LLZNO、(c) LLZTNO以及 (d) LLZTNYO 86
圖 4 26、在25、40、60以及80 °C下量測 (a) LLZTO、(b) LLZNO、(c) LLZTNO以及 (d) LLZTNYO的Nyquist plots 88
圖 4 27、LLZTO、LLZNO、LLZTNO與LLZTNYO在25到80 °C下之離子傳導率比較圖 89
圖 4 28、LLZTO、LLZNO、LLZTNO與LLZTNYO在25到80 °C下之Arrhenius圖 90
圖 4 29、暴露在空氣下1、10、20以及30天下量測 (a) LLZTO、(b) LLZNO、(c) LLZTNO以及 (d) LLZTNYWO_E的Nyquist plots 93
圖 4 30、LLZTO、LLZNO、LLZTNO與LLZTNYO在暴露不同天下之離子傳導率比較圖 95
圖 4 31、LLZTNYO之DC直流極化曲線，定電壓 = 1.5 V 96
圖 4 32、Li/solid electrolyte/Stainless steel (SS) 電池在25 °C下量測以1 mV s−1掃描速率下之CV圖：(a) LLZTO、(b) LLZNO、(c) LLZTNO以及 (d) LLZTNYO 98
圖 4 33、恆電流循環測試圖 (Galvanostatic cycling test)，鋰金屬的吸附與脫附時間為1小時：(a) LLZTO、(b) LLZNO、(c) LLZTNO以及 (d) LLZTNYO 99
圖 4 34、恆電流充放電測試圖 (a) Li//LLZTNYO//LiFePO4 之全固態電池在電壓範圍為 2–3.8 V vs. Li/Li+ (b) Li//liquid electrolyte//LiFePO4 電池在電壓範圍為 2–3.8 V vs. Li/Li+ 之測試數據 100




表目錄
表 2 1、石榴石結構固態氧化物電解質之特性比較 19
表 2 2、陶瓷固態電解質之種類與特性比較 29
表 3 1、實驗藥品列表 31
表 4 1、高熵石榴石結構之摻雜比例與燒結參數 46
表 4 2、LLZTO、LLZNO、LLZTWO、LLZTNYWO以及LLZTNYWO_E之XRD Rietveld精修結果與晶格常數 49
表 4 3、LLZTNYWO之ICP-OES數據 59
表 4 4、LLZTO、LLZNO、LLZWO、LLZTNYWO與LLZTNYWO_E在不同溫度下量測之阻抗數據，代號g與gb分別代表grain與grain boundary 65
表 4 5、LLZTO、LLZNO、LLZWO、LLZTNYWO與LLZTNYWO_E在不同天量測之阻抗數據，代號g與gb分別代表grain與grain boundary 69
表 4 6、四元石榴石結構之摻雜比例與燒結參數 79
表 4 7、LLZTO、LLZNO、LLZTNO以及LLZTNYO之XRD Rietveld精修結果與晶格常數 82
表 4 8、LLZTO、LLZNO、LLZTNO與LLZTNYO在不同溫度下量測之阻抗數據，代號g與gb分別代表grain與grain boundary 91
表 4 9、LLZTO、LLZNO、LLZTNO與LLZTNYO在不同天量測之阻抗數據，代號g與gb分別代表grain與grain boundary 94

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