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論文名稱 Title |
無還原添加劑水熱合成磷酸鋰鐵 Hydrothermal Synthesis of Lithium Iron Phosphate without Reducing Additives |
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系所名稱 Department |
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畢業學年期 Year, semester |
語文別 Language |
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學位類別 Degree |
頁數 Number of pages |
84 |
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研究生 Author |
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指導教授 Advisor |
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召集委員 Convenor |
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口試委員 Advisory Committee |
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口試日期 Date of Exam |
2014-06-16 |
繳交日期 Date of Submission |
2014-06-23 |
關鍵字 Keywords |
還原劑、正極材料、鋰離子二次電池、磷酸鋰鐵、水熱法 reducing additive, Cathode material, Hydrothermal process, Lithium-ion secondary battery, Lithium iron phosphate |
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統計 Statistics |
本論文已被瀏覽 5688 次,被下載 0 次 The thesis/dissertation has been browsed 5688 times, has been downloaded 0 times. |
中文摘要 |
本研究針對水熱法合成磷酸鋰鐵進行改良,成功研究出無需額外還原性添加劑,並可於大氣環境下合成出純相磷酸鋰鐵的方法。利用X光繞射儀(X-ray diffraction, XRD)確認此磷酸鋰鐵為橄欖石斜方晶系結構,並由拉曼(Raman spectroscopy)、化學分析能譜儀(Electron Spectroscopy for Chemical Analysis, ESCA)判讀樣品中是否存在三價鐵不純物,而材料表面型態變化則以掃描式電子顯微鏡(Scanning electron microscopy, SEM)和穿透式電子顯微鏡(Transmission electron microscopy, TEM)進行觀察,並藉元素分析儀(Elemental analyzer, EA)分析樣品各元素比例是否符合理論。得到磷酸鋰鐵粉體後,在多項電化學測試,例如經過循環伏安法(Cyclic Voltammetry, CV)可看到材料本身具有良好的可逆性,且可由交流阻抗測試(AC-impedance)觀察到材料本身電荷轉移阻抗小,而在定電流0.2C充放電下,材料所表現出的電容量為80mAh/g。 |
Abstract |
LiFePO4 is successfully prepared by hydrothermal synthesis in air without extra reducing additives. The structure and morphology of the resulting LiFePO4 powders were shown by X-ray diffraction (XRD),scanning electron microscope (SEM), and a transmission electron microscope (TEM).The XRD results demonstrate that LiFePO4 powder has an orthorhombic olivine-type structure with a space group of Pnma. Raman spectroscopy and electron spectroscopy for chemical analysis (ESCA) reveal the impurity of Fe3+ in samples. The chemical composition of the LiFePO4 powders was characterized by elemental analysis (EA). Among the conditions, the electrochemical results show the energy capacity is 84 mAh g−1 at 0.2 C-rate. |
目次 Table of Contents |
論文審定書 i 誌謝 ii 中文摘要 iii Abstract iv 目錄 v 圖目錄 x 表目錄 xiv 第一章. 緒論 1 1-1. 前言 2 1-2. 研究動機 2 第二章. 文獻回顧 4 2-1. 一次與二次電池發展 5 2-1-1. 一次電池介紹 5 2-1-2. 二次電池介紹 6 2-2. 鋰離子二次電池工作原理 7 2-3. 鋰離子二次電池正極材料 9 2-3-1. LiCoO2, 鈷酸鋰 9 2-3-2. LiNiO2, 鎳酸鋰 10 2-3-3. LiMn2O4, 錳酸鋰 11 2-3-4. LiFePO4, 磷酸鋰鐵 11 2-4. 磷酸鋰鐵合成方法 13 2-4-1. 固態反應法 14 2-4-2. 機械活化法 14 2-4-3. 微波法 15 2-4-4. 水熱法合成磷酸鋰鐵 15 第三章. 實驗方法 17 3-1. 實驗藥品與器材 18 3-2. 實驗步驟 19 3-2-1. 不同鐵源比例調整 19 3-2-2. 零價鐵的反應機制探討 19 3-2-3. 高溫管狀爐鍍碳鍛燒 20 3-2-4. 半電池組裝 21 3-3. 粉體分析鑑定儀器介紹 23 3-3-1. X光繞射儀(XRD) 23 3-3-2. 拉曼光譜儀(RS) 23 3-3-3. 場發射掃描式電子顯微鏡(SEM) 24 3-3-4. 穿透式電子顯微鏡(TEM) 24 3-3-5. 化學分析電子能譜儀(ESCA) 25 3-3-6. 元素分析儀(EA) 25 3-4. 電化學測試儀器介紹 27 3-4-1. 循環伏安法測試(CV) 27 3-4-2. 交流阻抗測試(AC-impedance) 28 3-4-3. 充放電及倍率效能測試(Charge-discharge & c-rate performance) 29 第四章. 結果與討論 30 4-1. 不同鐵源比例調整 31 4-1-1. X光繞射分析 31 4-1-2. 掃描式電子顯微鏡 32 4-1-3. 穿透式電子顯微鏡 34 4-1-4. 拉曼光譜分析 38 4-1-5. 元素分析 40 4-1-6. 化學分析能譜儀 41 4-2. 零價鐵的反應機制探討 43 4-2-1. X光繞射分析 43 4-2-2. 掃描式電子顯微鏡 45 4-2-3. 穿透式電子顯微鏡 48 4-2-4. 拉曼光譜分析 51 4-2-5. 元素分析 52 4-2-6. 化學分析能譜儀 53 4-2-7. 反應機制的推導 54 4-3. 電化學分析 55 4-3-1. 循環伏安法分析 56 4-3-2. 交流阻抗分析 58 4-3-3. 定電流充放電測試 60 4-3-4. 倍率放電測試 61 第五章. 結論 63 第六章. 參考文獻 66 |
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