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研究生： 黃庭緯
Huang, Ting-Wei
論文名稱： 利用磁控濺鍍在鋁箔上成長LiCoO2正極薄膜及電化學性質之研究
Growth and Electrochemical Properties of RF-sputter Cathode LiCoO2 Thin Film on Al foil
指導教授： 黃肇瑞
Huang, Jow-Lay
共同指導教授: 劉全璞
Liu, Chuan-Pu
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： 2021
畢業學年度： 109
語文別： 中文
論文頁數： 134
中文關鍵詞： 鋰鈷氧化物 、氮化鈦 、磁控濺鍍 、鋰離子薄膜電池 、退火 、擴散現象 、擴散阻障層
外文關鍵詞： Li-ion thin film battery, LiCoO2, RF-sputtering, interdiffusion, diffusion barrier, TiN
相關次數： 點閱：139  下載：0 
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    • 薄膜電池具有固態電池高安全性以及高能量密度等相關優勢，且由於各層都是以薄膜形式為主，因此可降低固態電池界面阻抗高等問題，可作為可撓式3C裝置或者是微機電裝置的供電來源。在正極材料當中，鋰鈷氧化物(LiCoO2, LCO)具有高理論電容量(140 mAh/g)、高工作電壓(〜4.2 V)以及循環穩定性高等優勢，因此適合作為薄膜電池的正極選擇。LiCoO2薄膜電池研究中，文獻探討製程參數對於LCO微結構的影響所得的結果較為不一；此外，發現基板為鋁時電容量較低，分析薄膜與基板間相互擴散可能為原因，然而幾乎沒有任何相關研究。因此，本研究將以磁控濺鍍成長LiCoO2薄膜，觀察製程參數對於薄膜微結構及電池性能的影響，以及觀察基板與薄膜是否有相互擴散現象，並探討擴散現象對於電池性能影響，最後，運用TiN阻障層嘗試避免擴散現象發生。
    本研究第一部份為磁控濺鍍參數對於LCO薄膜微結構的影響，從結果中可得藉由高濺鍍功率及基板升溫可先形成較穩定的LCO結晶相，並透過降低工作距離以增加薄膜中鋰離子含量進而降低鈷氧化物的生成。此外，發現Ar/O2氣體比例不同能夠影響LCO的結晶方向，當Ar/O2比例較低時，能夠使LCO從(003)方向轉變為(101)方向，此為較高電容量的結晶取向。最後，在此部分採用100W、濺鍍壓力10mtorr、Ar/O2為1/1，工作距離7cm及基板溫度250°C為最佳的LCO成長條件。
    研究第二部分為退火對於LCO薄膜影響，其結果可得退火氣氛會影響第二相的生成，並可推測LCO薄膜退火時微結構變化的過程；而較高溫及較長時間退火下可得最佳的LCO結晶性。最後以600°C、四小時並於大氣退火可得最佳的LCO結晶性，且可得到最高的電池電容量表現。在此部分也發現在高溫退火時有擴散現象發生，並由XPS、XRD、EDS分析可能形成LiAlO2和LiCo1-xAlxO2等第二相，為可能導致電容量相較於理論值較低的原因；但擴散現象卻對於貼合性部分有較好的幫助，進而提升長循環充放電下的庫倫效率。
    研究第三部分為TiN阻障層影響，從結果可得TiN可完全阻擋LCO與Al之間的相互擴散，且晶體分析上可發現Ti離子並不會擴散進入LCO中，且在電性測量上電阻率經過退火後幾乎無明顯差別，證明TiN可有阻障能力及維持良好的導電性，因此預期電性結果會有更好的表現。

    LiCoO2 (LCO) is successfully deposited by RF-sputtering on Al foil. By understanding the influence of sputtering and annealing parameters to the film, specific orientation, low second phase and high crystallinity LCO thin film can be prepared. The XRD shows high LCO (101) orientation, and Raman spectra result shows low Co3O4 second phase. The SEM image shows no crack appear after annealing, so short circuit will not occur during battery cycling. Furthermore, interdiffusion is also studied in this research. LiAlO2 layer forms during sputtering, and then Al will diffuse into LCO and substitute Co to become LiCo1-xAlxO2 after annealing through TEM, EDS, XRD and XPS result. The battery discharge capacity is 80 mAh/g after annealing, but due to LiCo1-xAlxO2, it is still lower than practical capacity (140 mAh/g). However, interdiffusion increases coulombic efficiency and enhances long-term cycling performance. TiN can be used as diffusion barrier, and diffusion between LCO and Al can be prevented and maintain conductivity.

    摘要 I Extended Abstract III 致謝 XIII 總目錄 XV 表目錄 XIX 圖目錄 XX 第一章 緒論 1 1.1 前言 1 1.2 研究動機 1 第二章 文獻回顧 3 2.1 鋰離子電池發展與介紹 3 2.2 鋰離子電池分類 5 2.3 鋰離子薄膜電池 6 2.3.1 薄膜電池製備方式 6 2.4 鋰離子電池工作原理 8 2.5 鋰離子正極材料 10 2.6 鋰鈷氧化物正極材料 13 2.6.1 鋰鈷氧化物（LiCoO2, LCO）晶體結構 13 2.6.2 電化學特性 14 2.7 磁控濺鍍LiCoO2正極薄膜研究近況 16 2.7.1 薄膜厚度 16 2.7.2 薄膜結晶取向 19 2.7.3 濺鍍參數影響—瓦數 22 2.7.4 濺鍍參數影響—工作壓力 24 2.7.5 濺鍍參數影響—Ar/O2 27 2.7.6 濺鍍參數影響—基板取向 30 2.8 退火對於LiCoO2薄膜的影響 32 2.8.1 退火氣氛 32 2.8.2 退火溫度 36 2.8.3 退火時間 40 2.9 活性材與基板之擴散現象研究 42 2.9.1 薄膜電池擴散現象研究簡述 42 2.9.2 正極薄膜的擴散研究簡述 47 2.9.3 鋰鈷氧薄膜擴散現象研究 55 2.9.4 LiCoO2薄膜電池現況 57 第三章 實驗方法與分析設備 59 3.1 實驗材料 59 3.2 實驗設計 59 3.3 實驗流程 60 3.3.1 基板前處理 60 3.3.2 LiCoO2薄膜濺鍍 60 3.3.3 LiCoO2薄膜退火 62 3.3.4 TiN擴散阻障層薄膜製程 63 3.3.5 LCO/TiN/Al substrate 製備 63 3.4 材料鑑定分析 64 3.4.1 X-ray 繞射分析儀 64 3.4.2 拉曼光譜分析儀(Raman spectroscopy) 65 3.4.3 高解析場發射掃描式電子顯微鏡(FE-SEM) 66 3.4.4 高解析穿透式電子顯微鏡(Ultrahigh Resolution Analytical Electron Microscopy:HR-AEM) 67 3.4.5 電子能譜化學分析儀(Electron Spectroscopy for Chemical Analysis:ESCA) 68 3.4.6 四點探針(Four point probe) 69 3.5 鈕扣型半電池測試 70 3.5.1 半電池組裝 70 3.5.2 活性材重量估算方式 70 3.5.3 半電池充放電循環壽命測試 70 3.5.4 dQ/dV分析 70 第四章 結果與討論 71 4.1 薄膜濺鍍 71 4.1.1 濺鍍瓦數(sputtering power) 71 4.1.2 濺鍍工作壓力以及Ar/O2比例 74 4.1.3 工作距離(Working distance) 及不同Ar/O2比例薄膜探討 80 4.1.4 As-deposited薄膜電池測試 93 4.2 薄膜退火 96 4.2.1 退火氣氛 96 4.2.2 退火溫度 99 4.2.3 退火時間 101 4.2.4 介面擴散現象觀察與分析 105 4.2.5 薄膜退火電池表現 115 4.3 TiN擴散阻障層對LiCoO2薄膜影響 122 4.3.1 濺鍍生成TiN薄膜 122 4.3.2 LiCoO2/TiN/Al 薄膜介面分析 123 4.3.3 四點探針量測 126 第五章 結論 127 參考資料 129

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