臺灣博碩士論文加值系統

本研究為探討在醇系溶液中合成磷酸鋰鐵 (LiFePO4) 三維材料之顆粒生長情形是值得研究，於不同 pH 值及鋰源比例的添加條件下，利用共沉澱法改變酸鹼值能適當地改變 LiFePO4 的溶解度，進而影響材料晶相與結晶度及控制晶粒大小，再以葡萄糖及煤煙 (生物碳) 作為碳源進行包覆碳層，分別獲得磷酸鋰鐵–葡萄糖 (LFP–CG) 及磷酸鋰鐵–煤煙 (LFP–CS) 複合材料，且在碳塗層改質方法上探討碳源添加比例及煅燒溫度對材料之影響。LiFePO4 及煤煙之微結構及表面化學可藉由 XRD、TEM、SEM、EDS、FTIR 與 EA 等儀器分析。在電化學性能測試，則組裝成 CR2032 型鈕扣型電池，其測試結果在 pH 7 時，可有效提高 LiFePO4 的充放電電容量。在不同速率充放電分析時，提高合成 LFP-CS 之煅燒溫度有助於高速率充放電下之電容量表現。透過循環伏安法測試，LFP-CG 擁有較小電阻值，得到鋰離子在正極表面嵌入嵌出機制速率較佳。本研究以 soot 作碳塗層之 LiFePO4 複合材料可保持良好的循環性能。SEM 分析結果顯示，中性 pH 值之材料顆粒由小於 100 nm球型粒子互相堆疊成 200–400 nm 顆粒，整體材料粒徑均勻。這項研究解釋 4 種不同 pH 下及 2 種不同碳源，對電化學性能影響外，還探討材料晶體表徵特性之差異，係來自鋰源比例及 pH 差異的重要作用。

A three-dimensional lithium iron phosphate (LiFePO4, LPF) was synthesized via alcoholic-based approach for making cathode material. The crystal phase, crystallinity and grain size of LFP can be controlled with different pH values and various lithium hydroxide monohydrate (LiOH ．H2O) molar ratio using co-precipitation method. Glucose and soot (biochar) were used as carbon sources coating on LFP to form carbon layers. Lithium iron phosphate-glucose (LFP–CG) and lithium iron phosphate-soot (LFP–CS) composites were obtained, thus the carbon coating layers could be affected by carbon source contect and calcination temperature. The microstructures of LFP were observed by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscope (SEM), Energy Dispersive Spectrometer (EDS), Fourier-Transform Infrared spectroscopy (FTIR) and Elemental Analysis (EA). The electrochemical characteristics of LFP–C were assembled in CR2032 type coin cell. The results showed the charge/discharge capacity of LFP–C cathode material could be enhanced effectivity as pH 7. Moreover, in different charge/discharge rate tests, high rate capacity performance of the LFP–CS could be improved with higher calcination temperature. However, in cyclic voltammetry tests, LFP–CG showed a lowest resistance and high lithium ion intercalation/deintercalation mechanism rate. In this study, LiFePO4 composite with soot as carbon layer could keep a great cyclic performance The results of SEM showed the material particle size with appropriate pH value was folded up into particle size 200-400 nm by 100 nm spherical particles, and performed uniform particle size. In this study, the electrochemical behaviors of LFP were not only illustrated effects of four pH values and two carbon sources but also demonstrated the important role of lithium source molar ratio and pH value in surface chemistry.

摘要 i
Abstract ii
致謝 iv
目錄 v
表目錄 ix
圖目錄 xi
第一章 緒論 1
1.1 研究緣起 1
1.2 研究目的 3
1.3 研究架構 4
第二章 文獻回顧 5
2.1 鋰離子二次電池之工作原理 5
2.2 鋰離子電池正極材料 6
2.2.1 鈷酸鋰(LiCoO2) 7
2.2.2 鎳酸鋰(LiNiO2) 8
2.2.3 錳酸鋰(LiMn2O4) 9
2.2.4 三元正極材料(Ternary cathode material) 9
2.2.5 磷酸鋰鐵(LiFePO4) 10
2.3 磷酸鋰鐵充放電模型 11
2.4 磷酸鋰鐵的合成 14
2.5 磷酸鋰鐵正極材料之研究現況 21
2.5.1 縮小顆粒粒徑 24
2.5.2 元素摻雜 25
2.5.2.1 金屬摻雜 25
2.5.2.2 非金屬摻雜 28
2.5.3 添加導電塗層 30
2.5.3.1 非金屬氧化物塗層 30
2.5.3.2 導電聚合物塗層 31
2.5.3.3 碳塗層 32
2.6 生物碳(biochar)中之煤煙(soot) 36
2.7 磷酸鋰鐵/煤煙(LiFePO4/soot)複合材料 37
第三章 實驗方法與程序 40
3.1 實驗藥品與儀器 40
3.1.1 實驗藥品 40
3.1.2 實驗器材與儀器 41
3.2 實驗程序 43
3.2.1 磷酸鋰鐵前驅物之製備 43
3.2.2 碳源加入磷酸鋰鐵之製備 45
3.2.3 磷酸鋰鐵正極極片之製備 46
3.2.4 CR2032型鈕扣電池之組裝 46
3.3 特性分析 48
3.3.1 材料性質 48
3.3.1.1 X-ray繞射光譜儀(X-ray Diffraction,XRD) 48
3.3.1.2 掃描式電子顯微鏡(Scanning Electron Microscope,SEM) 48
3.3.1.3 穿透式電子顯微鏡(Transmission Electron Microscopy,TEM) 49
3.3.1.3 能量散射光譜分析儀(Energy Dispersive Spectrometer,EDS) 49
3.3.1.4 元素分析儀(Elemental Analysis,EA) 49
3.3.1.5 傅里葉紅外光譜(Fourier Transform Infrared Spectrometer,FTIR) 49
3.3.2 電化學分析50
3.3.2.1 定電流充放電性質分析 50
3.3.2.2 循環伏安法分析(Cyclic Voltammetry,CV) 50
第四章 結果與討論 51
4.1 控制鋰源比例及添加碳塗層對磷酸鋰鐵複合材料電化學性影響 52
4.1.1 以葡萄糖作碳塗層之磷酸鋰鐵複合材料充放電測試 52
4.1.2 以煤煙作碳塗層之磷酸鋰鐵複合材料充放電測試 55
4.1.3 不同碳源及煅燒溫度之磷酸鋰鐵複合材料充放電測試 60
4.2 變速率性能測試 63
4.2.1 葡萄糖作碳源之變速率性能測試 63
4.2.2 煤煙作碳源之變速率性能測試 64
4.2.3 不同碳源及煅燒溫度之變速率性能測試 66
4.3 循環充放電測試 67
4.3.1 低速率循環性能測試 67
4.3.2 高速率循環性能測試 69
4.4 循環伏安法分析 71
4.4.1 葡萄糖作碳源之循環伏安法分析 71
4.4.2 煤煙作碳源之循環伏安法分析 73
4.4.3 不同碳源及煅燒溫度之循環伏安法分析 77
4.4.4 多次數循環之循環伏安法分析 78
4.3 材料微結構特性分析結果 81
4.3.1 XRD分析 81
4.3.2 SEM與EDS分析 83
4.3.2.1 葡萄糖作為碳源之SEM與EDS分析 83
4.3.2.2 煤煙作為碳源之SEM與EDS分析 88
4.3.2.3 不同碳源之磷酸鋰鐵複合材料對照分析(Maping Analysis) 94
4.3.3 TEM分析 96
4.3.4 EA分析 99
4.3.5 FTIR分析 99
第五章 結論與建議 102
5.1 結論 102
5.2 建議 105
參考文獻 106

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