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研究生： 王智憲
Wang, Chih-Shian
論文名稱： 後熱處理對噴霧法LiMn2O4正極材料之充放電特性效應探討
Effect of Post-treatment on Charge-discharge Capacity of Spray-drying LiMn2O4 Electrode Material
指導教授： 方滄澤
Fang, Tsang-Tse
呂傳盛
Lui, Truan-Sheng
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2004
畢業學年度： 92
語文別： 中文
論文頁數： 74
中文關鍵詞： 噴霧乾燥 、鋰錳氧
外文關鍵詞： Spray-drying, LiMn2O4
相關次數： 點閱：69  下載：5 
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    • 　　利用噴霧乾燥法並配合後續熱處理可合成單相之LiMn2O4粉末，因此熱處理條件對粉末特性的影響相當重要。本研究藉由控制煆燒溫度、時間及氣氛獲得不同LiMn2O4粉末，並進行循環充放電測試(0.3C，截止電壓為3.0及4.3V)，以探討煆燒條件對LiMn2O4粉末充放電特性的影響。
    　　經由BET及XRD分析，可知當增加煆燒溫度及時間時，會使得LiMn2O4粉末的表面積下降及晶格常數增加，其中以煆燒溫度的影響較為顯著。而充放電測試結果顯示以700℃，5小時的煆燒條件所得到的放電電容量最佳(約125mAh/g)，且在15次充放電循環後其循環效率維持在95%左右。
    　　本研究同時將LiMn2O4粉末在900℃氧氣氛圍下進行煆燒，以改善高溫煆燒所造成的氧損失，並進行充放電測試。實驗結果顯示通入氧氣進行煆燒可增加初始放電電容量，但無法改善循環效率劣化。

    　　A spray-drying method has been developed to synthesize ultrafine LiMn2O4 powders. For the purpose to acquire completely spinel LiMn2O4 powders, a post heat treatment, calcination, should be performed. In this study, parameters of heat treatment including atmospheres, holding temperature and time were controlled to obtain the powders with superior discharge capacity. The cyclic discharge tests were performed at a 0.3C rate between 3.0V and 4.3V.
    　　Through analyzing by XRD and BET, it could be found that the lattice constant was enlarged and the surface area was reduced with increasing holding temperature and holding time. The effect of holding time was tremendous. The recommended optimal parameters are calcining at 700℃ for 5h. The samples thus produced exhibit an initial discharge capacity of 125mAh/g and the capacity retention of 95% after 15 cycles.
    　　To reduce oxygen deficiency while calcination at high temperatures, parts of the powders were calcined under flowing oxygen circumstance at 900℃. It can be found that calcinations with oxygen can raise the initial discharge capacity, however, capacity fading after cyclic discharge can not be improved.

    中文摘要………………………………………………………… Ⅰ 英文摘要………………………………………………………… Ⅱ 誌謝……………………………………………………………… Ⅲ 總目錄…………………………………………………………… Ⅳ 表目錄…………………………………………………………… Ⅶ 圖目錄…………………………………………………………… Ⅷ 第一章 緒論……………………………………………… 1 1-1 鋰離子電池簡介……………………………………… 1 1-2 研究大綱及目的…………………………………… 2 第二章 理論基礎與文獻回顧………………………… 5 2-1 鋰離子電池的工作原理……………………………… 5 2-2 鋰離子電池的理論電容量…………………………… 5 2-3 鋰離子電池的系統構造……………………………… 6 2-4 陰極材料的合成方法………………………………… 7 2-4-1 噴霧乾燥法……………………………………… 7 2-4-2 噴霧乾燥原理…………………………… 8 2-4-2-1 簡介……………………………………………… 8 2-4-2-2 原理……………………………………………… 9 2-5 尖晶石型態鋰錳氧材料……………………………… 11 第三章 實驗方法…………………………………………… 22 3-1 實驗藥品與器材……………………………………… 22 3-2 陰極材料粉末之合成……………………………… 22 3-3 陰極材料粉末性質分析……………………………… 23 3-3-1 X粉末繞射分析……………………………… 23 3-3-2 掃描式電子顯微鏡(SEM)之分析……………… 23 3-3-3 熱重分析………………………………………… 23 3-3-4 表面積測量……………………………………… 24 3-3-5 感應耦合電漿質譜分析(ICP)…………………….. 24 3-4 充放電測試……….……………………………………… 24 第四章 結果與討論………………………………………… 31 4-1 LiMn2O4粉末之煆燒溫度效應…….…..………………… 31 4-1-1 LiMn2O4粉末合成與粉末X光繞射分析……… 31 4-1-2 LiMn2O4粉末之熱重分析……………………… 32 4-1-3 煆燒溫度對晶格常數的影響…………………… 32 4-1-4 LiMn2O4之比表面積與表面型態……………… 33 4-1-5 煆燒溫度對LiMn2O4充放電性質之影響……… 33 4-2 固定700℃下LiMn2O4粉末之煆燒時間效應…………… 34 4-2-1 LiMn2O4粉末X光繞射分析…………………… 34 4-2-2 煆燒時間對晶格常數的影響…………………… 35 4-2-3 LiMn2O4之比表面積與表面型態……………… 35 4-2-4 煆燒時間對LiMn2O4充放電性質之影響………36 4-3 高溫煆燒氣氛效應…………………………………… 37 4-3-1 LiMn2O4粉末X光繞射、晶格常數分析…… 37 4-3-2 不同煆燒氣氛下SEM表面型態觀察…………… 37 4-3-3 不同煆燒氣氛對LiMn2O4充放電性質之影響… 38 4-4 噴霧法製程對充放電影響因素…………………… 38 第五章 結論…………………………………………………. 66 第六章 參考文獻…………………………………………… 67

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