動力鋰電池陰極材料磷酸亞鐵鋰目前工業上遭遇之問題與研究

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研究生：	黃楷斌 Kai-Pin Huang
論文名稱：	動力鋰電池陰極材料磷酸亞鐵鋰目前工業上遭遇之問題與研究
指導教授：	費定國 Ting-Kuo Fey
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程與材料工程學系 Department of Chemical & Materials Engineering
論文出版年：	2014
畢業學年度：	102
語文別：	中文
論文頁數：	137
中文關鍵詞：	鋰離子電池、磷酸亞鐵鋰、陰極材料
外文關鍵詞：	Lithium ion battery, LiFePO4, cathode material
相關次數：	點閱：8 下載：0
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磷酸亞鐵鋰具有低成本、低汙染、良好熱穩定性與長循環壽命等優點，因此成為近年最受矚目的鋰離子電池陰極材料之一。本論文有四大主題，目的是研究LiFePO4商業化發展上遇到的問題，包含材料中磁性雜質的存在、較低的工作電壓與電容量、以及材料吸水劣化等問題。
吾人首先以磁選的方式，製備一系列含有不同磁性雜質含量的樣品，並以新式磁導儀量化磁性雜質對電性的影響，非常適合作為工業上的品管工具，純化後不含磁性雜質的LiFePO4/C，其0.5 C的初始電容量高達151 mAh g-1，自放電率在所有樣品中最低，一週後在0.5 C條件測試下仍有高於97%的電容量維持率，5 C長循環測試下，500次後仍有92%的電容量維持率。
為了提升材料電壓，吾人以流變相法配合錳(Mn)與釩(V)的添加，合成LiFexMnyVzPO4/C複合材料，其中LiFe0.6Mn0.2V0.2PO4/C展現良好的電化學性能，0.5 C充放電條件下，放電電容量達153 mAh g-1。由於電壓的提升，此材料能量密度達520 Wh kg-1，比 LiFePO4/C高出約15%，且碳含量僅3.4 wt.%，比LiFe1-xMnxPO4/C於一般文獻上報導的5~10%低，此可增加工業上電芯製作時的加工性。
承上述V添加的改質經驗，吾人成功合成出Li2Fe0.9V0.1PO4/C複合材料，該材料理論電容量高達220 mAh g-1，吾人於本論文報導的結果中，其0.5 C的放電電容量已達161 mAh g-1，在4.6-2.0電壓範圍內，可承受20 C之充放電速率，並具有良好的熱穩定性，具有成為下世代陰極材料的潛力。
為瞭解水氣對置放不同濕度環境LiFePO4的影響，吾人測試商用LiFePO4含水量、粒徑、比表面積與放電電容量隨時間的變化，含水量與比表面積隨時間有增加的趨勢，且比表面積的增加具有不可逆的特性，粒徑與鈕扣型電池的電容量隨時間幾乎沒有變化，但軟包電芯的放電電容量卻會因受水氣造成材料的脫鋰現象而下降。

Olivine-structured lithium iron phosphates (LiFePO4) become a promising cathode material because of its low cost, low toxicity, remarkable thermal stability and long operation life. In order to overcome the obstacles hindering the commercial development of LiFePO4, there are four topics in this study, including the presence of magnetic impurities, lower work voltage and discharge capacity, and property deterioration upon exposure to humid air.
First, we produced a series of samples containing different amounts of magnetic impurities by magnetic selection, and applied a new alternative current magnetic susceptibility device to quantify the impact of magnetic impurities on LiFePO4/C composites, which is a useful quality control tool for practical lithium battery applications. The magnetic impurity-removed LiFePO4/C composites exhibited the best discharge capacity of 151 mAh g-1 at 0.5 C and excellent cycle performance with a capacity retention of 97% after 500 cycles at 5 C. Self-discharge experiments showed that the purified LiFePO4/C maintains 97% residual capacity after a week at 0.5 C, which is better than the others containing magnetic impurities.
In order to increase the work voltage, LiFexMnyVzPO4/C composites were prepared by a rheological phase method with the addition of Mn and V. The LiFe0.6Mn0.2V0.2/C composites deliver the best initial discharge capacity of 153 mAh g-1 at 0.5 C. Due to the increase of voltage, the energy density of LiFe0.6Mn0.2V0.2/C is 520 Wh kg-1, which is 1.15 times higher than LiFePO4/C. The carbon content is 3.4 wt.%, which is lower than 5~10 wt.% as stated by the previous reports. Lower carbon content leads to better processability of pouch cells in industry.
According to the above modification method, we synthesized Li2Fe0.9V0.1PO4/C composites, whose theoretical capacity is 220 mAh g-1. This work shows that the Li2Fe0.9V0.1PO4/C composites delivered an initial discharge capacity of 161 mAh g-1 at 0.5 C, and can sustain a 20 C-rate between 4.6 and 2.0 V. Besides, Li2Fe0.9V0.1PO4/C shows excellent thermal stability, which has been recognized as the most promising positive cathode.
To better realize the moisture effect on LiFePO4/C in different humidity, we measured the water content, particle size, specific surface area and discharge capacity of commercial LiFePO4/C dependent time. The water content and specific surface area increase with time, and the change of surface area is irreversible. The particle size and discharge capacity of coin cells do not change with time, but the discharge capacity of pouch cells decreases due to the delithiation caused by moisture.

中文摘要………………………………………………………………………………………I
英文摘要………………………………………………………………………………………II
致謝……………………………………………………………………………………………III
目錄……………………………………………………………………………… ……………IV
圖目錄…………………………………………………………………………………………VII
表目錄…………………………………………………………………………………………XI
第一章    緒論…………………………………………………………………………1
1-1前言………………………………………………………………………………………1
1-2鋰電池的發展……………………………………………………………………2
1-3鋰離子電池陰極材料發展與簡介…………………………………3
1-4研究目的及架構…………………………………………………………………8
第二章    文獻回顧……………………………………………………………… 10
   2-1磷酸亞鐵鋰(LiFePO4)應用於鋰離子電池…………10
   2-2磷酸亞鐵鋰的結構………...………………………………………11
   2-3磷酸亞鐵鋰的充放電模型…………………………………………13
   2-4磷酸亞鐵鋰的合成方法………………………………………………16
  2-5磷酸亞鐵鋰的改質…………………………………………………………16
      2-5-1添加高導電性塗佈層………………………………………16
      2-5-2掺雜不同金屬改質……………………………………………22
2-6磷酸亞鐵鋰的磁性………………………..……………………………………25
2-7提升磷酸亞鐵鋰的電壓與電容量………..………….……………28
2-8水分對磷酸亞鐵鋰的影響.………….……………………………………32
第三章    實驗方法……………………………………………………………………36
  3-1實驗儀器設備……………………………………………………………………36
  3-2實驗藥品……………………………………………………………………………37
  3-3實驗步驟……………………………………………………………………………38
3-3-1 LiFePO4磁選實驗……………………..……………………………38
3-3-2高電壓LiFexMnyMzPO4/C複合材料實驗………………40
3-3-3高容量Li2Fe1-xVx P2O7/C複合材料實驗…………42
3-3-4 水份對LiFePO4/C影響實驗……………….……………………44
  3-4材料鑑定分析………………………………………………………………………44
      3-4-1X光繞射（X-ray Diffraction, XRD）分析…………………44
      3-4-2掃描式電子顯微鏡 （Scanning Electron Microscope, SEM）觀測……44
      3-4-3高解析穿透式電子顯微鏡……………………………………45
      3-4-4拉曼光譜（Raman Spectroscopy）鑑定………………45
      3-4-5微分掃描熱卡儀（Differential Scanning Calorimeter, DSC）檢測………46
      3-4-6熱重量分析儀/熱差分析儀(Thermogravimetric Analyzer / Differential Thermal Analyzer, TGA/DTA)測試………………………………46
      3-4-7總有機碳（Total Organic Carbon, TOC）分析………………46
      3-4-8四點探針（Four-Point probe）導電度儀……………………………46
3-4-9 電量法卡式水份計 (Coulometric Karl Fischer Moisturemeter) …………47
3-4-10交流磁導率量測儀 (Magnetosusceptometer) ……………………………48
3-4-11 X光吸收光譜 (X-ray Absorption Spectroscopy, XAS) …48
3-4-12 感應耦合型電漿 (Inductively-Coupled Plasma, ICP)………48
  3-5材料電化學特性分析…………...…………………………………………….48
      3-5-1電池性能測試……………………………………………………………48
      3-5-2慢速循環伏安分析(Slow scan cyclic voltammetry)……51
      3-5-3電化學交流阻抗(Electrochemical A/C impedance)分析…51
第四章    結果與討論…………………………………….……………………………………52
  4-1 LiFePO4磁選實驗………………………………………….………………………52
      4-1-1 X光繞射(XRD)結構分析…………………………………………52
      4-1-2交流磁導率分析………………………………………………….……………55
      4-1-3電池性能測試………………………………………………………….………57
      4-1-4慢速循環伏安測試……………………………………………….……………63
      4-1-5交流阻抗測試……………………………………………………….…………66
      4-1-6大型磁選機實驗……………………………………………….………………67
  4-2高電壓材料實驗……...…………………………………………..……………………69
      4-2-1添加不同金屬(M)合成LiFe0.7Mn0.2M0.1PO4/C……………………………….69
      4-2-2煆燒溫度對LiFe0.7Mn0.2V0.1PO4/C電池性能影響………70
      4-2-3錳(Mn)劑量對LiFe0.9-xMnxV0.1PO¬4/C電池性能影響………71
      4-2-4釩(V)劑量對LiFe0.8-yMn0.2VyPO4/C電池性能影響……………72
      4-2-5碳源添加量對LiFe0.7Mn0.2V0.2PO4/C電池性能影響……………73
      4-2-6最佳參數………………………………………………………………………75
      4-2-7 X光繞射結構(XRD)分析…………………….………………76
4-2-8掃描電子顯微鏡(SEM)鑑定………….……....……..……………79
4-2-9穿透式電子顯微鏡(TEM)分析………………….………………….……81
4-2-10微分掃描熱卡儀 (DSC)分析…………………...……………..…83
4-2-11拉曼光譜鑑定…………...……………..……………………………….……85
4-2-12電池長循環測試..……………..……………………………………….……87
4-2-13特徵曲線測試……..………………………….……………………….…….88
4-3高容量材料鑑定分析..………………………………………...……………….89
4-3-1熱重量分析儀/熱差分析儀(TGA/DA)測試………………………..89
4-3-2 X光繞射(XRD)結構分析………………..…………………………….……...91
4-3-3掃描電子顯微鏡(SEM)鑑定……..…………………………….……………...91
4-3-4穿透式電子顯微鏡(TEM)分析……………….…………………..…………...93
4-3-5電池放電電容量測試…….………………………………………..…………..96
      4-3-6特徵曲線測試.…………………………………………..……………….…….97
      4-3-7電池長循環測試………………………………….……..……………….…….98
      4-3-8碳含量、導電度測定……..……………………………………………..…….99
      4-3-9微分掃描熱卡儀(DSC)測試……………………………………………..…….99
  4-4水氣對LiFePO4/C的影響……………………………………………..………..……101
      4-4-1 LiFePO4吸水速率………………………………………………………..,,,…101
      4-4-2 LiFePO4烘箱去水實驗…………………………………………………….…102
      4-4-3含水量對LiFePO4粒徑與比表面積的影響………………………………….103
      4-4-4 LiFePO4烘箱去水後之表面積……………………………………………….104
      4-4-5含水量對LiFePO4電池放電電容量影響…………………………………….105
      4-4-6 X光吸收光譜 (XAS) ………………………………………………….…….107
第五章    結論……………………………………………………………………………...…109
第六章    參考文獻…………………………………...………………………………………112
第七章    附錄………………………………...………………………………………………120

                                

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