博碩士論文 106324026 詳細資訊




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姓名 許偉倫(Wei-Lun Hsu)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 利用旋轉塗佈法製備固態電解質應用於鋰離子電池
(Preparation of Solid Electrolyte Li7La3Zr2O12 by Spin Coating Method for Lithium-Ion Batteries)
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摘要(中) 本實驗第一部分,使用旋轉塗佈法製備固態電解質,此方法的優點為控制其薄膜的厚度、增加Li+ 的擴散通道,使Li+ 更加地容易傳送。固態電解質是由PEO、LiTFSI、Ga-doped LLZO混合而成的,而我們嘗試尋找旋轉塗佈法的最佳參數: 轉速1000 rpm、時間60秒、每滴溶劑150 μL、層數15層。而隨著固態電解質的濃度增加,可以有效地抑制電壓的抖動,故電解質的最佳比例則是PEO: LiTFSI : LLZO = 1:1:2。
我們沿用第一部分的最佳參數,第二部分則是比較五種LLZO製備固態電解質應用於鋰離子電池,而與其它種類的LLZO相比,Li6.25Ga0.25La3Zr2O12有最好的電化學性質,其0.1C下電容值約有120 mAh/g,庫倫效率約有97%,且發現粒徑大小會部分影響電化學性質,因為在固態電解質Li+ 傾向於在 LLZO 相中傳遞,所以我們降低固態電解質中的粒徑大小,便能夠使Li+ 更加容易地穿透,進而造成電化學性質提高。我們選擇填充物Al2O3取代LLZO,但卻得到很差的電化學性質,這邊推測為高分子主鏈運動不易,導致導電度不佳,故結過顯示填充物無法取代LLZO,固態電解質是必要的存在。
實驗第三部分,我們加入離子液體在固態電解質和鋰金屬之間,藉此降低其界面阻抗,並選擇三種不同摻雜的LLZO比較其電化學性質,而Li6.25Ga0.25La3Zr2O12加入離子液體1M LiTFSI/PMPTFSI有最好的電化學性質,其0.1C下電容值約有148 mAh/g,庫倫效率約有97%。以0.5C下作200圈循環壽命測試,維持率高達96% (137.48/143.21 mAh/g, 200th/1st )。
摘要(英) A single-phase Li7La3Zr2O12 (LLZO) solid electrolyte is synthesized using a solid-state reaction method. The influences of doping elements (Ga, Ta, and Mg) on the properties of LLZO are investigated. In addition, a hybrid electrolyte, composed of Ga-doped (or Ta-doped) LLZO, LiTFSI, and poly(ethylene oxide) was prepared, using the spin coating method. The LLZO/LiTFSI/PEO ratio of slurry and number of layers were changed to compare their electrochemical properties. As compared to LLZO pellet electrolyte, the hybrid electrolyte shows a higher ionic conductivity and a better charge-discharge performance in Li/LiFePO4 cells.
We compare different kinds of LLZO and find out that Li6.25Ga0.25La3Zr2O12 has the best electrochemical properties. The charge is about 120 mAh/g and coulombic efficiency is also 97%. It was found that the particle size will affect the electrochemical performance. The Li+ ion tends to pass through the LLZO phase in the solid electrolyte, by reducing the particle size Li+ ion can penetrate more easily.
The huge interface impedance still possesses a great challenge toward a better performance. We add the ionic liquid between the solid electrolyte and lithium metal to decrease the interface impedance. Li6.25Ga0.25La3Zr2O12-1M LiTFSI/PMPTFSI demonstrates good charge and discharge performance.The charge reaches up to 148 mAh/g and coulombic efficiency is also 97 %. The cycle retention at 0.5C is about 96% during the 200 cycles.
關鍵字(中) ★ 固態電解質
★ 鋰電池
★ 正極材料
關鍵字(英) ★ solid electrolytes
★ Li-ion batteries
★ cathode materials
論文目次 摘要 i
Abstract ii
誌謝 iii
總目錄 iv
圖目錄 viii
表目錄 xiv
第一章 緒論 1
1-1 研究背景 1
1-2 研究動機 2
第二章 文獻回顧 4
2-1 固態電解質 4
2-1-1傳導機制 4
2-1-2混合型的固態電解質 6
2-1-2-1 Polymer/Liquid Hybrid Electrolytes with Organic Liquids 6
2-1-2-2 Polymer/Liquid Hybrid Electrolytes with Ionic Liquids 9
2-1-2-3 Polymer/Polymer Coordinating Electrolytes 11
2-1-2-4 Polymer/Inorganic Composite Electrolytes 16
2-1-3固態陶瓷電解質結構 28
2-2 Li7La3Zr2O12 的發展與應用 30
2-2-1 Li7La3Zr2O12 分析 30
2-2-2 Li7La3Zr2O12 不同元素摻雜 34
2-3 Li7La3Zr2O12 應用於鋰電池 41
2-3-1錠狀(pellet)固態電解質 41
2-3-2混合的固態電解質(hybrid) 45
第三章 實驗方法與步驟 60
3-1 實驗藥品及材料 60
3-2 電池製備 63
3-2-1 工作電極塗佈 63
3-2-2 固態電解質薄膜製備 63
3-2-3 電解液的配置 64
3-2-4鈕扣型電池製備 64
3-3材料分析與鑑定 65
3-3-1 X光繞射分析 (X-ray diffraction,XRD) 65
3-3-2場發式掃描電子顯微鏡 (Field Emission Gun Scanning Electron Microscope, FEI, Inspect F50) 65
3-3-3 動態光散射粒徑分析儀 (Dynamic Light Scattering) 65
3-3-4線性掃描伏安法 (Linear scan voltammetry) 65
3-3-5連續循環充放電測試 (Charge and Discharge Test) 66
3-3-6交流阻抗 (electrochemical impedance spectroscopy, EIS) 66
第四章 結果與討論 67
4-1旋轉塗佈法(spin coating)的最佳參數 67
4-1-1 LiPF6-EC/DEC的基本性質 67
4-1-2 Spin coating 電解質的比例 72
4-2摻雜不同元素Li7La3Zr2O12的比較 80
4-2-1 摻雜不同元素Li7La3Zr2O12的基本性質 80
4-2-2 摻雜不同元素Li7La3Zr2O12的電化學性質 84
4-3固態電解質加入離子液體對電池性能的影響 99
4-3-1離子液體的基本性質 99
4-3-2 Li7La3Zr2O12 加入離子液體的電池性能 107
第五章 結論 125
第六章 附錄 126
第七章 參考文獻 129
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86. Rangasamy, E., J. Wolfenstine, and J. Sakamoto, The role of Al and Li concentration on the formation of cubic garnet solid electrolyte of nominal composition Li7La3Zr2O12. Solid State Ionics, 2012. 206: p. 28-32.
87. Cao Yang et al., Densification and lithium ion conductivity of garnet-type Li7-xLa3Zr2-xTaxO12 (x=0.25) solid electrolytes. Chin. Phys. B Vol. 22, No. 7 (2013).

88. Wu, J.-F., et al., Gallium-doped Li7La3Zr2O12 garnet-type electrolytes with high lithium-ion conductivity. ACS applied materials & interfaces, 2017. 9(2): p. 1542-1552.
89. Maoyi Yi et al., High Li-ion conductivity of Al-free Li7-3xGaxLa3Zr2O12 solid electrolyte prepared by liquid-phase sintering. Journal of Solid State Electrochemistry. February 2019.
90. Ahn, C.-W., et al., Electrochemical properties of Li7La3Zr2O12-based solid state battery. Journal of Power Sources, 2014. 272: p. 554-558.
91. Li, Y., et al., Hybrid Polymer/Garnet Electrolyte with a Small Interfacial Resistance for Lithium-Ion Batteries. Angewandte Chemie International Edition, 2017. 56(3): p. 753-756.
92. Hyun Woo Kim et al., Hybrid solid electrolyte with the combination of Li7La3Zr2O12 ceramic and ionic liquid for high voltage pseudo-solid-state Li-ion batteries, Journal of Materials Chemistry A-2016.
93. Shuang‑Jie Tan et al., Recent Advancements in Polymer‑Based Composite Electrolytes for Rechargeable Lithium Batteries. Electrochemical Energy Reviews. May 2018.
94. Choi, J.-H., et al., Enhancement of ionic conductivity of composite membranes for all-solid-state lithium rechargeable batteries incorporating tetragonal Li7La3Zr2O12 into a polyethylene oxide matrix. Journal of Power Sources,2015. 274: p. 458-463.
95. Wenqiang Zhang et al., A durable and safe solid-state lithium battery with a hybrid electrolyte membrane. Nano Energy 45 (2018) 413–419.
96. Jae-Yeong Park et al., Effect of solvated ionic liquids on the ion conducting property of composite membranes for lithium ion batteries. Res Chem Intermed. May 2018
97. Kun (Kelvin) et al., Toward garnet electrolyte–based Li metal batteries: An ultrathin, highly effective, artificial solid-state electrolyte/metallic Li interface. Science Advance. April 2017.
98. Gulin Vardar,William J. Bowman, Structure, Chemistry, and Charge Transfer Resistance of the Interface between Li7La3Zr2O12 Electrolyte and LiCoO2 Cathode. Chem. Mater. 2018.
99. 1eng, J., M. Tang, and Y.Y. Hu, Lithium Ion Pathway within Li7La3Zr2O12- Polyethylene Oxide Composite Electrolytes. Angewandte Chemie, 2016.128(40): p. 12726-12730.
100. Yun-Chae Jung et al., Ceramic separators based on Li+-conducting inorganic electrolyte for high-performance lithium-ion batteries with enhanced safety. Journal of Power Sources 293 (2015) 675-683.
101. Hyun Woo Kim et al, Hybrid solid electrolyte with the combination of Li7La3Zr2O12 ceramic and ionic liquid for high voltage pseudo-solid-state Li-ion batteries. J. Mater. Chem. A. August 2016.
102. Hanyu Huo, Ning Zhao, Jiyang Sun, Fuming Du, Yiqiu Li, Xiangxin Guo, Composite electrolytes of polyethylene oxides/garnets interfacially wetted by ionic liquid for room-temperature solid-state lithium battery. Journal of Power Sources 372 (2017) 1–7,2017.
103. Y.F. Liang, S.J. Deng, Y. Xia, X.L. Wang, X.H. Xia, J.B. Wu, C.D. Gu, J.P. Tu. A superior composite gel polymer electrolyte of Li7La3Zr2O12- poly(vinylidene fluoride-hexafluoropropylene) (PVDF-HFP) for rechargeable solid-state lithium ion batteries. Accepted Manuscript, 2018.
104. Fei Chen, All-Solid-State Lithium Battery Fitted with Polymer Electrolyte Enhanced by Solid Plasticizer and Conductive Ceramic Filler. Journal of The Electrochemical Society, 165 (14) A3558-A3565 (2018).
105. Da Hye Kim, Min Young Kim, Seung Hoon Yang, Fabrication and Electrochemical Characteristics of NCM-Based All-Solid Lithium Batteries using Nano-grade Garnet Al-LLZO Powder. Accepted Manuscript, 2019.
106 Yali Luo, Xueyan Li, Electrochemical Properties and Structural Stability of Ga- and Y- co-doping in Li7La3Zr2O12 Ceramic Electrolytes for Lithium-ion Batteries. Accepted Manuscript, 2019.

107. Maoyi Yi, Tao Liu, Xiangnan Wang, Jingyun Li, High densification and Li-ion conductivity of Al-free Li7-xLa3Zr2-xTaxO12 garnet solid electrolyte prepared by using ultrafine powders. Accepted Manuscript, 2019.
108. Yang Li, Wei Zhang, Qianqian Dou, Ka Wai Wong and Ka Ming Ng, Li7La3Zr2O12 ceramic nanofiber-incorporated composite polymer electrolytes for lithium metal batteries. Journal of Materials Chemistry A,2019.
109. Da Hye Kim, Min Young Kim, Fabrication and Electrochemical Characteristics of NCM-Based All-Solid Lithium Batteries using Nano-grade Garnet Al-LLZO Powder. Accepted Manuscript, 2019.
110. Zeya Huang, Wanying Pang, A dopamine modified Li6.4La3Zr1.4Ta0.6O12 /PEO solid-state electrolyte: enhanced thermal and electrochemical properties. Journal of Materials Chemistry A,2019.
指導教授 李岱洲(Tai-Chou Lee) 審核日期 2019-8-16
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