臺灣博碩士論文加值系統

本研究利用示差掃描熱量分析儀(DSC)，以非恆溫反應動力學探討合成馬來醯亞胺線性添加劑( Living@ MI )和馬來醯亞胺/雙馬來醯亞胺支狀添加劑( Living@ BMI/MI )，合成反應溫度、反應放熱量以及藉由自由模型法求得反應活化能，並利用核磁共振(NMR)鑑定Living@ BMI/MI、Living@ MI添加劑的化學結構，而熱重分析(TGA)和動態光散射(DLS)，分別為測試Living@ BMI/MI以及Living@ MI添加劑耐熱性質以及Living@ BMI/MI添加劑具有Microgel顆粒性質。
另一方面的研究，將Living@ BMI/MI、Living@ MI添加劑應用於鋰離子電池，作為鋰離子電池添加劑，探討對於LiNi0.5Co0.2Mn0.3O2正極材料的影響，利用正極半電池，進行充放電(C/DC)、交流阻抗圖譜(EIS)以及循環伏安(CV)以上測試，分析這兩種添加劑添加至正極材料後，對於電池性能、電池內部阻抗以及電化學性質的影響，並通過掃描式電子顯微鏡(SEM)、能量分散光譜(EDS)，了解經充放電後的電極極片表面型態及元素組成，最後再藉由示差掃描熱量分析儀(DSC)測試電極材料的熱穩定性。本研究的實驗結果，在正極材料中添加1wt%的Living@ BMI/MI可以最有效改善正極半電池於常溫電池循環壽命衰退以及電化學反應性質，而高溫環境的充放電測則是添加1 wt%的Living@ MI表現最為優異，在電極材料的熱穩定性為0.5%的Living@ BMI/MI耐熱性質較佳。

This study used a differential scanning calorimeter (DSC) to investigate the maleimide additive (Living@ MI) and bismaleimide / maleimide additive (Living@ BMI/MI) with non-isothermal kinetics that can be understanded the reaction temperature, exotherm. the study also used the free model method to know the activation energy, and identification of chemical structure of Living@ BMI/MI, Living@ MI additive by nuclear magnetic resonance (NMR), and thermogravimetry Analysis (TGA) and dynamic light scattering (DLS), respectively, for testing Living@BMI/MI and Living@MI additive heat-resistant properties and Living@BMI/MI additive Microgel particle properties.
On the other hand, Living@BMI/MI and Living@MI additives were applied to lithium-ion batteries, We want to know the effect of LiNi0.5Co0.2Mn0.3O2 cathode material. The cathode be made to the half-cell, It was used for charging. Discharge test (C/DC), Electrochemical Impedance Spectroscopy (EIS), and cyclic voltammetry (CV) tests were performed to analyze the effects of the two additives added to the positive electrode material. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to understand the surface morphology and elemental composition of the electrode after charge and discharge. Finally, the thermal stability of the electrode material was tested by differential scanning calorimetry (DSC). . The experimental results of this study, adding 1wt% of Living@BMI/MI to the positive electrode material can most effectively improve the cycle life degradation and electrochemical reaction properties of the positive half cell at room temperature, while the charge and discharge test in the high temperature environment is to add 1 wt. % Living@ MI is the most excellent, and the heat resistance of Living@BMI/MI with 0.5% thermal stability of the electrode material is better.

摘要 I
Abstract II
致謝 III
目錄 IV
圖目錄 VIII
表目錄 XI
第一章、研究背景 1
1.1鋰離子電池 1
1.1.1正極材料 2
1.1.2電解質 2
1.1.3隔離膜 2
1.1.4負極材料 3
第二章、研究動機 4
第三章、文獻回顧 8
3.1隔離膜斷開技術 8
3.1.1微孔高分子隔離膜 9
3.1.2不織布纖維隔離膜 11
3.1.3無機複合隔離膜 12
3.2電解質安全性改善 13
3.2.1穩定的鋰鹽 14
3.2.2路易斯鹼穩定劑 14
3.2.3阻燃添加劑 16
3.3塗層技術保護正極材料 17
3.4表面活物修飾 23
第四章、研究介紹 26
4.1 Living@ BMI / MI反應機制 27
4.2 Living@ MI反應機制 28
第五章、實驗藥品和設備 29
第六章、實驗樣品製備 30
6.1 NMR樣品製備 30
6.1.1 [ BMI / MI [ 1 / 1 ( mol / mol )] / NMP ] 30
6.1.2 [ MI / NMP ] 30
6.1.3 [ BMI / NMP ] 30
6.2 DLS樣品製備 30
6.2.1 [ BMI / MI [ 1 / 1 ( mol / mol )] / NMP ] 30
6.2.2 [ MI / NMP ] 31
6.2.3 [ BMI / NMP ] 31
6.3 DSC樣品製備 31
6.3.1 [ BMI / MI [ 1 / 1 ( mol / mol )] / NMP ] 31
6.3.2 [ MI / NMP ] 31
6.3.3 [ BMI / NMP ] 32
6.3.4 [ BMI / MI [ 1 / 1 ( mol / mol )] / HQ / NMP ] 32
6.3.5 [ MI / HQ / NMP ] 32
6.3.6 [ BMI / HQ / NMP ] 32
6.4 GPC樣品製備 32
6.4.1 [ BMI / MI [ 1 / 1 ( mol / mol )] / NMP ] 32
6.4.2[ MI / NMP ] 33
6.4.3 [ BMI / NMP ] 33
6.5 TGA樣品製備 33
6.5.1 [ BMI / MI [ 1 / 1 ( mol / mol )] / NMP ] 33
6.5.2 [ MI / NMP ] 33
6.5.3 [ BMI ] 34
6.5.4 [ MI ] 34
6.6 Living@添加劑製備 34
6.6.1 [ BMI / MI [ 1 / 1 ( mol / mol )] ] 34
6.6.2 [ MI ] 34
6.6.3 [ BMI ] 34
6.7 電極漿料製備 35
6.7.1 [ LiNi0.5Co0.2Mn0.3O2 ] 35
6.7.2 [ Living@ BMI / MI - 0.5% / LiNi0.5Co0.2Mn0.3O2 ] 35
6.7.3 [ Living@ BMI / MI - 1% / LiNi0.5Co0.2Mn0.3O2 ] 35
6.7.4 [ Living@ BMI - 0.5% / LiNi0.5Co0.2Mn0.3O2 ] 35
6.7.5 [ Living@ BMI - 1% / LiNi0.5Co0.2Mn0.3O2 ] 35
6.7.6 [ Living@ MI - 0.5% / LiNi0.5Co0.2Mn0.3O2 ] 36
6.7.7 [ Living@ MI - 1% / LiNi0.5Co0.2Mn0.3O2 ] 36
6.8 電極極片製備 36
6.9 鈕扣型電池(coin cell)組裝 37
第七章、結果與討論 38
7.1 Living@添加劑合成熱化學分析 38
7.1.1 馬來醯亞胺與雙馬來醯亞胺非恆溫動力學 38
7.1.2 馬來醯亞胺非恆溫動力學 40
7.1.3 雙馬來醯亞胺非恆溫動力學 41
7.2 非恆溫動力學以自由模型法分析 42
7.2.1 非恆溫動力學雙馬來醯亞胺活化能分析 43
7.2.2 非恆溫動力學馬來醯亞胺活化能分析 44
7.2.3 非恆溫動力學馬來醯亞胺與雙馬來醯亞胺活化能分析 45
7.3 Living@添加劑反應機制探討 47
7.3.1 馬來醯亞胺與雙馬來醯亞胺反應機制分析 47
7.3.2 馬來醯亞胺反應機制分析 47
7.4 Living@添加劑NMR結構分析 48
7.4.1 Living@ BMI / MI 氫譜結構分析 49
7.4.2 Living@ MI 氫譜結構分析 50
7.4.3 PMI / MI 氫譜結構分析 51
7.5 Living@ BMI / MI添加劑 DLS粒徑分析 52
7.6 Living@添加劑耐熱性質分析 53
7.8 循環伏安(CV)分析 55
7.8.1 Bare NCM523 55
7.8.2 Living@ MI 56
7.8.3 Living@ BMI/MI 57
7.8.4 Living@ BMI/MI不同添加量對於CV分析的影響 59
7.9第一圈充放電曲線分析 60
7.10常溫充放電循環壽命圖 62
7.10.1 Living@ BMI/MI、Living@ MI與Living@ BMI分析 62
7.10.2 Living@ BMI/MI、Living@ MI與STOBA分析 63
7.11常溫Living@添加劑(1-50圈)充放電曲線 64
7.12常溫Living@添加劑(1-50圈)交流阻抗圖譜分析 66
7.12.1 NCM523 66
7.12.2 Living@ BMI/MI - 0.5% 67
7.12.3 Living@ BMI/MI - 1% 69
7.12.4 Living@ MI - 0.5% 70
7.12.5 Living@ MI - 1% 71
7.13 高溫(55oC)充放電循環壽命圖 72
7.13.1 Living@ BMI/MI、Living@ MI與STOBA分析 72
7.14 高溫(55oC)Living@添加劑充放電曲線分析 73
7.15 高溫(55oC)Living@添加劑交流阻抗圖譜分析 75
7.16 Living@ BMI/MI添加劑於不同充放電速率分析 77
7.17 [ Living@ 添加劑 / NCM523 ] SEM分析 78
7.17.1 NCM523 78
7.17.2 Living@ BMI/MI - 0.5% 79
7.17.3 Living@ BMI/MI - 1% 80
7.18 [ Living@添加劑 / NCM523 ] EDS分析 81
7.19正極極片DSC分析 82
第八章、結論 83
參考文獻 84
圖片參考 88

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