以水熱法製備水系鈉離子電池NaTi2(PO4)3負極材料

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藍瑋宣(Wei-hsuan Lan) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

以水熱法製備水系鈉離子電池NaTi2(PO4)3負極材料
(The sodium ion battery negative material NaTi2(PO4)3 prepared by hydrothermal method to apply in aqueous systems)

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摘要(中)

本研究以水熱法合成鈉超離子導體(NASICON)-磷酸鈉鈦，藉改變合成參數，如反應體積、反應時間、前驅物濃度及界面活性劑濃度，可獲得奈米顆粒；並添加不同比重之碳源進行碳包覆，增進其導電性，以利後續電池性能量測。經X光繞射儀(XRD)分析得知: 水熱法合成可獲得結晶性良好之磷酸鈉鈦；掃描式電子顯微鏡(SEM)觀察: 磷酸鈉鈦粉末之平均粒徑範圍約為100 ~ 500 nm。經碳包覆後，由拉曼(Ramam)光譜分析偵測出碳特徵訊號、熱重分析(TGA)得知包覆後碳含量依碳源添加量不同約3 wt%、6wt%，穿透式電子顯微鏡(TEM)觀察可確認碳包覆及其形貌。先後以三極式電化學系統量測循環伏安曲線、二級式鈕扣電池量測鈉離子電池之性能。最佳合成參數及碳包覆含量之樣品其於不同充放電速率(0.2、0.5、1、2、5C)下展現出優異電容量(121、114、110、102、67mAh/g)、庫倫效率除首圈外，皆高達99%以上、放電電容量維持率亦維持在95%以上；經200次充放電循環測試後，仍保持約82%之放電電容量，且由電化學交流阻抗分析表明，阻值無明顯上升，顯示以水熱法合成之鈉超離子導體(NASICON)-磷酸鈉鈦在作為水系鈉離子電池負極材料極具潛力。

摘要(英)

Nano particle of sodium titanium phosphate belonging to sodium super-ionic conductor (NASICON)-type were successfully prepared by hydrothermal method under different synthetic parameters. With appropriate carbon-coating can improve material conductivity thus possibly suitable for making negative electrodes of sodium-ion batteries. From X-ray diffraction (XRD), which results revealed well crystalline structure of NaTi2(PO4)3 by hydrothermal method. Examination by field-emission scanning electron microscope (FE-SEM), the powders indicated their particle size in the range from 100 nm to 500 nm depending upon the experimental conditions. After coating by carbon, Raman spectroscopy demonstrated the D-band and G-band of carbon. The result of thermal gravimetric analysis (TGA) displayed that the carbon content was about 3wt%, 6wt% depending upon content of carbon source. The presence of carbon coating could be directly observed through by transmission electron microscope. Standard three-electrode cell was employed to conduct the cyclic voltammetry; two-electrode system via a coin cell was carried out for the test of battery performance, respectively. The optimal results revealed that C-coated nanoparticle NaTi2(PO4)3/C exhibited excellent electrochemical performance with high specific capacities (121, 114, 110, 102, 67mAh/g), high coulomb efficiency (99%) except first cycle and well discharge capacity retention (95%) at different charge/discharge rate (0.2, 0.5, 1, 2, 5C). A delivery of ~82% discharge capacity retention after 200 cycles and no obvious fading for impedance indicated that sodium titanium phosphate nano powders prepared in this work provided a potential material to prepare the anode used in aqueous sodium ion battery.

關鍵字(中)

★ 水熱法
★ 磷酸鈉鈦
★ 負極
★ 鈉離子電池
★ 鈉超離子導體

關鍵字(英)

★ Hydrothermal
★ NaTi2(PO4)3
★ anode
★ sodium ion battery
★ NASICON

論文目次

摘要 i
Abstract ii
誌謝 iii
目錄 iv
表目錄 x
圖目錄 xi
一、緒論 1
1-1前言 1
1-2 鈉離子電池發展背景 3
1-3鈉離子電池基本工作原理 4
1-4研究動機與目的 5
二、文獻回顧 8
2-1負極材料種類 8
2-1-1 碳材 8
2-1-2 金屬化合物 10
2-1-3 合金 13
2-2磷酸鈉鈦介紹 14
2-2-1 製程方法 14
2-2-2 電極材料應用 15
2-3奈米化 17
2-4界面活性劑 19
2-4-1界面活性劑之性質及種類 20
2-4-2 P123非離子型界面活性劑 21
三、研究方法 24
3-1實驗規劃 24
3-2實驗藥品 24
3-3 NaTi2(PO4)3合成條件 25
3-4實驗步驟 26
3-4-1前驅物溶液調配 26
3-4-2材料合成 27
3-4-3反應後產物洗淨、烘乾 27
3-4-4界面活性劑去除 27
3-4-5磷酸鈉鈦之碳包覆 28
3-4-6電極製備 28
3-5 材料鑑定分析 28
3-5-1場發射掃描式電子顯微鏡 28
3-5-2 X光粉末繞射儀 29
3-5-3高解析掃描穿透式電子顯微鏡 30
3-5-4拉曼光譜分析 31
3-5-5同步熱重分析儀 32
3-6 材料電化學分析 32
3-6-1量測系統 32
3-6-2循環伏安法 32
3-6-3充放電速率測試材料電化學性質 33
3-6-4充放電壽命 34
3-6-5電化學阻抗分析 34
四、結果 36
4-1材料合成 37
4-1-1不同水熱反應體積影響 37
4-1-1-1 XRD繞射晶體結構分析 38
4-1-1-2 FE-SEM表面形貌及粒徑大小觀察 38
4-1-2不同水熱反應時間影響 39
4-1-2-1 XRD繞射晶體結構分析 40
4-1-2-2 FE-SEM表面形貌及粒徑大小觀察 40
4-1-3不同前驅物濃度影響 41
4-1-3-1 XRD繞射晶體結構分析 42
4-1-3-2 FE- SEM表面形貌及粒徑大小觀察 42
4-1-4不同界面活性劑濃度影響 43
4-1-4-1 XRD繞射晶體結構分析 44
4-1-4-2 FE-SEM表面形貌及粒徑大小觀察 44
4-2碳包覆鑑定 45
4-2-1 Raman光譜分析 46
4-2-2 TGA熱重分析 47
4-2-3 TEM穿透式電子顯微鏡 47
4-2-3-1相鑑定 47
4-2-3-2晶粒形貌觀察 48
4-2-3-3碳包覆形貌觀察 48
4-3電化學性質量測 49
4-3-1循環伏安法 49
4-3-2表面形貌及粒徑大小對電池性能之影響 49
4-3-2-1放電電壓對電容量曲線圖 49
4-3-2-2充放電可逆性 50
4-3-2-3放電電容量維持率與充放電庫倫效率 51
4-3-3碳包覆含量對電池性能之影響 51
4-3-3-1放電電壓對電容量曲線圖 51
4-3-3-2循環壽命測試 52
4-3-3-3電化學交流阻抗分析 53
五、討論 54
5-1材料合成 54
5-1-1不同水熱反應體積影響 54
5-1-1-1 XRD繞射晶體結構分析 54
5-1-1-2 FE-SEM表面形貌及粒徑大小觀察 54
5-1-2 不同水熱反應時間影響 55
5-1-2-1 XRD繞射晶體結構分析 55
5-1-2-2 FE-SEM表面形貌及粒徑大小觀察 56
5-1-3 不同前驅物濃度影響 57
5-1-3-1 XRD繞射晶體結構分析 57
5-1-3-2 FE-SEM表面形貌及粒徑大小觀察 58
5-1-4 不同界面活性劑濃度影響 58
5-1-4-1 XRD繞射晶體結構分析 58
5-1-4-2 FE-SEM表面形貌及粒徑大小觀察 59
5-2碳包覆鑑定 61
5-2-1 Raman光譜分析 61
5-2-2 TGA熱重分析 61
5-2-3 TEM穿透式電子顯微鏡 62
5-2-3-1相鑑定 62
5-2-3-2晶粒形貌觀察 63
5-3電化學性質量測 64
5-3-1循環伏安法 64
5-3-2表面形貌及粒徑大小對電池性能之影響 64
5-3-2-1放電電壓對電容量曲線圖 64
5-3-2-2充放電可逆性 66
5-3-2-3放電電容量維持率與充放電庫倫效率 67
5-3-3碳包覆含量對電池性能之影響 67
5-3-3-1放電電壓對電容量曲線圖 67
5-3-3-2循環壽命測試 68
5-3-3-3電化學交流阻抗分析 70
六、結論 72
七、未來展望 75
八、參考文獻 76

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指導教授

林景崎(Jing-chie Lin)

審核日期

2014-8-11

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