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研究生： 賴冠杰
Lai, Kuan-Chieh
論文名稱： 銳鈦礦二氧化鈦奈米管在鋰離子電池陽極的應用
Anatase TiO2 Nanotubes as Anodes for Lithium Ion Batteries
指導教授： 鄧熙聖
Teng, Hsisheng
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2015
畢業學年度： 103
語文別： 中文
論文頁數： 85
中文關鍵詞： 鋰離子電池 、二氧化鈦 、奈米管 、石墨烯 、負極
外文關鍵詞： Lithium ion batteries, TiO2, Nanotubes, Reduced graphene oxide, Anode
相關次數： 點閱：114  下載：0 
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    • 本研究以水熱法合成二氧化鈦奈米管，並且藉由添加氧化石墨烯(GO)與冷凍乾燥處理，得到二氧化鈦奈米管與石墨烯(f-TNT/RGO)的複合材料。藉由組成半電池進行測試，並與TNT、TNT/RGO、f-TNT比較其性能，以分析f-TNT/RGO之優勢。
    由XRD與Raman分析得知所合成的二氧化鈦晶相為銳鈦礦以及少量的TiO2-B，同時藉由Raman與FTIR分析確認GO的還原。接著由TEM與SEM圖觀察石墨烯以及冷凍乾燥對二氧化鈦奈米管的影響，分別造成團聚顆粒以及奈米管之間的分散，再藉由氮氣吸脫附曲線搭配BET分析確認冷凍乾燥可令表面積顯著增加(TNT由166增至279 m2/g，TRGO由200增至278 m2/g)。組裝半電池進行循環伏安測試分析，出現銳鈦礦與TiO2-B的氧化/還原峰，且與充放電測試一起顯示經冷凍乾燥的樣品(f-TNT與f-TNT/RGO)，鋰離子主要由在1.75-1V的表面嵌入與界面儲存所貢獻。
    電池性能方面，f-TNT/RGO有最好的充放電表現，在1 C與30 C分別有239和155 mA h g-1的電容量。由阻抗分析得知f-TNT/RGO有較低之電荷傳遞阻力值，此結果肇因於(1)較高的電解液的接觸面積，(2) RGO與二氧化鈦界面的擬電容，(3) RGO提供較好的電子傳遞能力。在高速(30 C)長效穩定性測試方面，進行100圈充放電測試後，f-TNT/RGO具有100%的維持率，且在200圈後，維持率仍有94 %。圖4-14 顯示近年以二氧化鈦與碳之複合材料，其半電池在不同充放電速率下的結果，可更清楚瞭解本研究之表現。

    This study reports an anatase TiO2 nanotubes (TNT) and reduced graphene oxide (RGO) hybrid that is synthesized via an in situ hydrothermal process followed freezing dry treatment (f-TNT/RGO). The structure and performances are compared with TNT, f-TNT and TNT/RGO. The f-TNT/RGO were characterized by XRD, Raman, FTIR, TEM, SEM, BET and TGA, indicating the coexistence of anatase and minor TiO2-B with the reduction of GO. The structure and anchoring to RGO are confirmed, showing the vary difference between the product with/without RGO and especially freezing dry, each affects the agglomeration of particles and separation between tubes, which contribute to BET surface area. The dramatic incensement of f-TNT/RGO (278 m2g-1) comes from the pores in the network of tubes. The discharge curve and broad feature of CV below 1.7 V display the surface and interfacial Li+ storage from TiO2 with high surface area after freezing dry. The f-TNT/RGO exhibits better rate performance, 239 and 155 mA h g-1 can be obtained at 1 and 30 C. The AC impedance analysis leads to the lower charge transfer resistance of f-TNT/RGO, which is due to (1) high surface area which can afford more Li+ flow; (2) the interfacial Li+ storage (pseudo-capacity) and (3) a faster electron transport attributed to the RGO. 100 % retention of its value at the fifth cycle can be obtained after 100 cycles at 30 C, and retain at 94 % after another 100 cycles.

    中文摘要 I 英文摘要 II 誌謝 IX 本文目錄 X 表目錄 XIII 圖目錄 XIV 第一章 緒論 1 　　1-1 前言-電池發展與介紹 1 　　1-2 鋰電池與鋰離子二次電池 4 　　　　1-2.1 裝置構造 5 　　　　1-2.2 工作原理 5 　　1-3 電解質 7 　　　　1-3.1 液態有機電解質 7 　　　　1-3.2 固態高分子電解質 9 　　　　1-3.3 膠態高分子電解質 9 　　1-4 電極材料 11 　　　　1-4.1 正極材料 11 　　　　1-4.2 負極材料 13 　　1-5 研究動機與目的 19 第二章 理論說明與文獻回顧 21 　　2-1 二氧化鈦負極材料介紹 21 　　　　2-1.1 二氧化鈦介紹 21 　　　　2-1.2 銳鈦礦型二氧化鈦的嵌鋰機制 23 　　2-2 二氧化鈦奈米管 25 　　　　2-2.1 二氧化鈦奈米管合成方法 26 　　　　2-2.2 水熱法合成機制 28 　　2-3 二氧化鈦負極材料改質 29 第三章 實驗方法與儀器原理介紹 32 　　3-1 實驗藥品 32 　　3-2 實驗儀器設備 33 　　3-3 樣品製備 34 　　　　3-3.1 二氧化鈦奈米管 34 　　　　3-3.2 二氧化鈦奈米管與石墨烯複合材料 35 　　　　3-3.3 冷凍乾燥 35 　　3-4 實驗分析儀器與裝置分析儀器原理簡介 37 　　　　3-4.1 穿透式電子顯微鏡(Transmission Electron Microscope, TEM) 37 　　　　3-4.2 掃描式電子顯微鏡 (Scanning Electron Microscope, SEM) 38 　　　　3-4.3 物理吸附分析 (Brunauer-Emmett-Teller, BET) 41 　　　　3-4.4 X光繞射分析(Xray Diffraction, XRD) 43 　　　　3-4.5 拉曼光譜分析(Raman Spectrum) 45 　　　　3-4.6 傅立葉轉換紅外線光譜(Fourier Transform Infrared Spectroscopy, FTIR) 47 　　3-5 電化學測試 49 　　　　3-5.1 電極製作 49 　　　　3-5.2 鈕扣型電池(coin-cell)組裝 49 　　　　3-5.3 循環伏安法(cyclic voltammetry, CV) 50 　　　　3-5.4 半電池阻力測試 50 　　3-6 半電池性能測試 51 　　　　3-6.1 充放電測試 51 　　　　3-6.2 長效性測試 51 　　3-7 實驗流程 52 第四章 結果與討論 53 　　4-1 二氧化鈦奈米管物理分析與鑑定 53 　　　　4-1.1 XRD與Raman分析 53 　　　　4-1.2 FTIR分析 58 　　　　4-1.3 TEM與SEM分析 59 　　　　4-1.4 氮氣吸脫附結果分析 65 　　　　4-1.5 TGA分析 67 　　4-2 半電池電化學測試 69 　　4-3 電池性能測試 70 　　　　4-3.1 充放電測試 70 　　　　4-3.2 界面阻力測試 74 　　　　4-3.3 長效測試 75 　　　　4-3.4 文獻比較 76 第五章 結論與建議 78 參考文獻 79

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