以有機金屬框架結合乙醇輔助水熱法製備鐵摻雜鋰鎳錳氧高電壓正極 應用於鋰離子電池之研究

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劉嘉翰(Jia-Han Liu) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

以有機金屬框架結合乙醇輔助水熱法製備鐵摻雜鋰鎳錳氧高電壓正極應用於鋰離子電池之研究
(Ethanol-Assisted Hydrothermal Synthesis of High Voltage Fe-Doped LiNi0.5Mn1.5O4 Positive Electrode Using Metal-Organic Framework for Lithium-Ion Battery)

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至系統瀏覽論文 (2028-6-30以後開放)

摘要(中)

無鈷尖晶石正極材料LiNi0.5Mn1.5O4(LNMO)由於低成本、高工作電壓、優異的能量密度(690 Wh/kg)，以及良好的熱穩定性而受到廣泛的關注。然而，其高工作電壓(4.7 V vs Li/Li+)會加速商用電解液劣化，容易導致長時間循環壽命衰減，使得實際可行性備受挑戰。為了解決這些問題，我們提出一種創新的方式結合乙醇輔助水熱和金屬有機框架(基於PTA的MOFs)作為前驅物，合成出LNMO複合正極。如此一來，金屬離子便可以成功與有機配體排列整齊，同時乙醇輔助水熱法進一步改善LNMO顆粒的分散性與降低顆粒尺寸。而為了實現最佳電化學性能，因此我們使用不同的水熱溫度(T=100、120、140、160 °C)來定義出最佳參數，並加以合成。接著，透過在 MOF 的 Ni-Mn 前驅體中摻雜 Fe，以三金屬前驅體煅燒形成 Fe 摻雜 LNMO (LiNi0.5-xMn1.5-xFe2xO4 (x=0, 0.03, 0.05 , 0.1, 0.15))來增加結構穩定性。結果證實，這種新穎的合成方法是製備高性能LNMO正極之可行策略，不同水熱溫度讓LNMO前軀物擁有不同的顏色和粒徑大小。此外，合成之LNMO表面會自然生成出無定質的Li2CO3層(厚度約1 nm)，以保護材料免受電解液之過度反應，並有效輔助Li+擴散進行。在所有樣品中，LNMO-120°C具有最小的顆粒大小和均勻的粒徑分佈，在0.2 C下，具有最佳的142.5 mAh/g之實際電容量，並在1 C速率下第200次循環後之電容保持率為80.1%。與原始LNMO正極不同，摻雜Fe之尖晶石材料減少了常見的LixNi1-xO雜質相，並具有令人滿意的循環穩定性， LiNi0.45Fe0.1Mn1.45O4樣品顯示出最出色的循環穩定性(在1 C下200圈循環後之電容保持率為96.7%)，成功大幅改善了商用LNMO所存在的結構穩定性問題。另外，也具備極佳的倍率性能，即使在5 C下，其容量仍達到118.9 mAh/g，並通過GC-MS證實Fe摻雜能有效去抑制並減緩電解液中有機酯EC與DEC劣化成其他副產物。

摘要(英)

The cobalt-free spinel positive electrode LiNi0.5Mn1.5O4 (LNMO) is receiving extensive attention for lithium-ion batteries due to its low cost, high operating voltage (4.7 V vs. Li/Li+), superior energy density (690 Wh/kg), and good thermal stability. However, its high operating voltage hampers its stability with commercial electrolytes, leading to capacity decay during long-term charge-discharge cycling. This makes its practical viability challenging.
To solve these problems, we combined ethanol-assisted hydrothermal and metal−organic frameworks (PTA-based MOFs) as precursors to synthesize high-voltage LNMO composite positive electrode. In this way, the metal ions can be successfully aligned by organic ligands, meanwhile the ethanol-assisted hydrothermal process improves the dispersity of LNMO particles with reduced particle size. Since selecting the appropriate hydrothermal temperature is crucial to achieve optimal electrochemical performance, we used different hydrothermal temperatures (T=100, 120, 140, 160°C) for synthesis. In order to further enhance structural stability, Fe was doped in the Ni-Mn precursors of MOF, and the trimetallic precursor is calcinated to form Fe-doped LNMO (LiNi0.5-xMn1.5-xFe2xO4 (x=0, 0.03, 0.05, 0.1, 0.15)).
The results confirm that the novel synthesis method is a feasible strategy to fabricate high-performance LNMO positive electrodes. Various hydrothermal temperatures give rise to different colors and particle size of the LNMO precursors. In addition, it is confirmed by XPS that an amorphous Li2CO3 layer formed on the surface of the as-synthesized LNMO, which can protect the material from overreaction and effectively assist Li+ diffusion. Among the samples, the LNMO-120°C is the smallest with uniform size distribution and has the best discharge capacity (142.5 mAh/g at 0.2 C) and cycling stability with a capacity retention of 80.1 % after 200 cycles at 1 C. Different from the parent LNMO material, the Fe-doped spinel one has reduced rock-salt-type impurity phase and satisfactory cycling stability and rate performance. Among all the samples, the LiNi0.45Fe0.1Mn1.45O4 sample shows the best cycling stability (capacity retention of 96.7 % after 200 cycles at 1 C) and rate capability with a capacity of 118.9 mAh/g even at 5 C.

關鍵字(中)

★ 高電壓正極
★ 金屬有機框架
★ Fe摻雜
★ Li2CO3表面塗層
★ 鋰離子電池

關鍵字(英)

★ High-voltage positive electrode
★ Metal−Organic Frameworks
★ Fe-doped
★ Li2CO3 coating
★ Lithium-ion battery

論文目次

摘要 i
Abstract iii
誌謝 v
目錄 vii
圖目錄 xi
表目錄 xvi
第一章、序論 1
1-1能源議題現況及儲能發展 1
1-2鋰離子產業之發展及未來趨勢 4
1-3鋰離子電池的組成與工作原理 6
1-4鋰離子電池的組成材料 8
1-4-1正極材料 8
1-4-2負極材料 12
1-4-3電解質 14
1-4-4隔離膜 15
1-4-5集電體 16
1-4-6黏著劑 17
1-5研究動機 19
第二章、文獻回顧 21
2-1 LiNi0.5Mn1.5O4 (LNMO)正極材料 21
2-2 開發新型LNMO正極材料之合成方式(Novel synthesis method) 24
2-2-1 乙醇輔助水熱法(Ethanol-assisted hydrothermal method) 28
2-2-2 高分子輔助法之有機金屬框架(MOF) 30
2-3 過渡金屬(Transition Metal, TM)摻雜 34
第三章、實驗方法 37
3-1 實驗架構 37
3-2實驗藥品與儀器 39
3-2-1 實驗藥品 39
3-2-2 實驗材料 40
3-2-3 實驗儀器 41
3-3實驗方法與步驟 42
3-3-1活性物質之製備 42
3-3-2 LNMO及Fe-doped LNMO碳纖維紙集電體之極片製備 44
3-3-3 CR2032 鈕扣型電池製備 44
3-4電極材料分析與電化學分析 46
3-4-1熱重分析儀 (Thermogravimetric Analyzer, TGA) 47
3-4-2高解析場發掃描式電子顯微鏡(Field Emission Scanning Electron Microscope, FE-SEM) 47
3-4-3 X光繞射分析儀(X-ray Diffraction, XRD) 48
3-4-4傅立葉轉換紅外線光譜儀(Fourier-transform infrared spectroscopy, FTIR) 48
3-4-5 X 射線光電子能譜儀(X-ray Photoelectron Spectroscopy, XPS) 49
3-4-6感應耦合電漿質譜儀(Inductively Coupled Plasma Mass Spectrometry, ICP-MS) 49
3-4-7 動態光散射儀(Dynamic Light Scattering, DLS) 50
3-4-8 充放電性能測試分析 (Charge/Discharge Test) 50
3-4-9 循環伏安分析 (Cyclic Voltammetry, CV) 51
3-4-10 EIS阻抗分析(Electrochemical Impedance Spectroscopy, EIS) 52
3-4-11 高解析氣相層析質譜分析 (High Resolution Gas Chromatograph Mass Spectrometer , HRGC-MS) 52
3-4-12 高解析穿透式電子顯微鏡(Transmission Electron Microscopy, HR-TEM) 53
第四章、結果與討論 54
4-1 不同水熱溫度以合成LNMO正極材料之前驅物 54
4-1-1 LNMO前驅物之顏色與表面型態分析 54
4-1-2 LNMO前驅物之粒徑分布分析 56
4-1-3 LNMO前驅物之XRD圖譜分析 59
4-1-4 LNMO前驅物之FTIR光譜分析 61
4-1-5 LNMO前驅物之ICP-MS定量分析 63
4-2 比較MOF保留/去除對於LNMO正極材料之影響 64
4-2-1 XRD圖譜分析 64
4-2-2電化學分析-充放電與循環穩定性測試 66
4-2-3有機配體之熱重分析 68
4-3不同水熱溫度合成LNMO正極材料 69
4-3-1 LNMO之表面型態分析 69
4-3-2 LNMO之粒徑分布分析 71
4-3-3 LNMO之XRD圖譜分析 73
4-3-4 LNMO之電化學分析-充放電與循環穩定性測試 75
4-3-5 LNMO之電化學分析-快速充放電測試 78
4-4 鐵摻雜對於LNMO正極材料前驅物之影響 80
4-4-1 Fe-doped LNMO前驅物表面型態分析 80
4-4-2 Fe-doped LNMO前驅物XRD圖譜分析 82
4-4-3 Fe-doped LNMO前驅物FTIR光譜分析 83
4-4-4 Fe-doped LNMO前驅物ICP-MS定量分析 84
4-5鐵摻雜對於LNMO正極材料之影響 86
4-5-1 Fe-doped LNMO之表面型態分析 86
4-5-2 Fe-doped LNMO之XRD圖譜分析 91
4-5-3 Fe-doped LNMO之FTIR分析 94
4-5-4 Fe-doped LNMO之XPS分析 95
4-5-4 Fe-doped LNMO之HR-TEM分析 100
4-5-5 Fe-doped LNMO之電化學分析-充放電與循環穩定性測試 103
4-5-6 Fe-doped LNMO之電化學分析-快速充放電測試 106
4-5-7 Fe-doped LNMO之電化學分析-循環伏安法分析 108
4-5-8 Fe-doped LNMO之電化學分析-電化學阻抗分析 110
4-5-9 與商用電極之電性比較-Li2CO3表面塗層與Fe摻雜LNMO 115
4-6電解液劣化分析 117
第五章、結論與未來展望 123
5-1 結論 123
5-1-1 不同水熱溫度合成LNMO正極材料 123
5-1-2 鐵摻雜對於LNMO正極材料之影響 125
5-2 未來展望 127
參考文獻 128

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指導教授

劉奕宏(Yi-Hung Liu)

審核日期

2023-8-11

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