新穎光聚合及熱聚合黏著劑應用於鋰離子 電池三元系正極材料性能探討

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蔣泓璟(Hung-Ching Chiang) 查詢紙本館藏

畢業系所

化學學系

論文名稱

新穎光聚合及熱聚合黏著劑應用於鋰離子電池三元系正極材料性能探討

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至系統瀏覽論文 (2027-7-31以後開放)

摘要(中)

傳統鋰電池的製備常使用Poly(vinylidene difluoride) (PVDF)當作黏著劑以固定活性材料與導電物質。並以N-Methyl-2-pyrrolidone (NMP)做為溶劑，與活性物質及導電粒子混和，將漿料塗佈於鋁片上。含NMP的極板在烘箱經過長時間(10-24小時)高溫烘烤，去除溶劑以完成成極片。由於NMP有毒，所以回收過程必須有額外的溶劑回收系統，並且需要大量的烘烤設備，以及烘烤過程中需消耗大量的電力、時間成本，不符合環境友善及節能減碳的環保概念。
因此也有越來越多人朝著綠色環保這方面去改善鋰電池的製作過程，像是水性黏著劑黏著劑的開發，以減少現有溶劑NMP的使用，但使用水性黏著劑還是有遇到幾個問題像是去除水分的烘乾過程過長以及電容量、壽命低下等問題。
有鑑於此，本論文主要是使用光聚合高分子、熱聚合高分子取代傳統的電極黏著劑(PVDF)以解決傳統鋰電池，極片烘乾時間過長、使用有毒溶劑、耗時耗能的問題。
首先黏著劑方面，分成光聚合黏著劑以及熱聚合黏著劑。光聚合黏著劑將DE單體與G3E單體進行光聚合反應、熱聚合反應則是將DP單體與G3E單體進行熱聚合反應。組成Li[Ni1/3Mn1/3Co1/3]O2/Li半電池測試，利用電子掃描顯微鏡(SEM)、X-射線光電子光譜(XPS)、循環伏安法(CV)及電化學阻抗頻譜(EIS)進行探討。實驗數據證實此兩款黏著劑確實參與SEI的形成且能夠減少電解液以及鋰鹽的消耗還有分解，我們認為此兩款黏著劑可以緊密包覆電極，避免正極持續與電解液反應，讓電池能夠長圈數循環後仍能繼續維持良好的電量。光聚合黏著劑、熱聚合黏著劑，與傳統黏著劑相比，電池電容量在經過100圈充放電後，分別是、104.6(mAh/g)、120.1(mAh/g)、107.9(mAh/g)，電容保持率分別是76.6%、81.9%、64.3%，光聚合以及熱聚合黏著劑在電容量、高倍率充放電、壽命的表現都優於傳統鋰電池。

摘要(英)

In the preparation of traditional lithium batteries, Poly (vinylidene difluoride) (PVDF) is often used as binder to fix active materials and conductive substances. And N-Methyl-2-pyrrolidone (NMP) is used as a solvent, mixed with active material and conductive particles, and the slurry is coated on the aluminum foil. The battery plate that containing NMP is baked at high temperature for a long time (10-24 hours) in an oven to remove solvent. However, NMP is toxic, the recycling process must have an additional solvent recovery system, and a large number of baking equipment is required, and the baking process consumes a lot of electricity and time costs, which does not correspond to the environmental protection concept of environmental friendliness and energy saving and carbon reduction.
In view of this, this thesis mainly uses photo-curing polymer and thermal-curing polymer to replace the traditional electrode binder (PVDF) to solve the problem of traditional lithium battery manufacturing.
First of all, in terms of adhesives, it is divided into photo-curing binder and thermal-curing binder. In the photo-curing binder, the DE monomer and the G3E monomer are subjected to photopolymerization reaction. In the thermal-curing binder, the DP monomer and the G3E monomer are subjected to thermalpolymerization reaction. Composition Li[Ni1/3Mn1/3Co1/3]O2/Li half-cell test using scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) discuss. The experimental data confirm that the two binders are indeed involved in the formation of SEI and can reduce the consumption and decomposition of electrolyte and lithium salts. Compared with traditional binder, photopolymerized binder and thermally polymerized binder have a battery capacity of 104.6(mAh/g), 120.1(mAh/g), 107.9(mAh/g) after 100 cycles of charge and discharge, respectively. ), the capacitance retention is 76.6%, 81.9%, 64.3%, photopolymerized and thermally polymerized binder have enough performance to match or even surpass traditional lithium batteries.
Finally, we also used XPS, CV, and EIS to confirm that these two binder can tightly coat the electrodes to prevent the positive electrode from continuously reacting with the electrolyte, so that the battery can continue to maintain a good power after a long cycle.

關鍵字(中)

★ 鋰電池
★ 黏著劑
★ 光聚合高分子
★ 熱聚合高分子

關鍵字(英)

★ lithium batteries
★ binder
★ photo-curing polymer
★ thermal-curing polymer

論文目次

目錄

摘要 i
Abstract iii
目錄 v
圖目錄 ix
表目錄 xvi
第一章緒論 1
1-1 前言 1
1-2 鋰離子電池基本原理 3
1-3 光聚合、熱聚合之介紹 4
1-4 研究動機 5
第二章文獻回顧 7
2-1 黏著劑簡介 7
2-2 黏著劑種類與材料特性 8
2-2-1 羧甲基纖維素(Carboxymethylcellulose，CMC) 12
2-2-2 丁苯橡膠(Styrene-Butadiene Rubber，SBR) 18
2-2-3 聚四氟乙烯（Polytetrafluoroethylene，PTFE） 20
2-3 光聚合、熱聚合高分子材料簡介 23
2-4 固態鈍化層介面簡介 31
2-4-1 Solid Electrolyte Interphase (SEI)固態鈍化層介面介紹 31
2-4-2 Cathode Electrolyte Interphase(CEI) 正極電解質界面介紹 35
2-5 層狀氧化物(正極材料)電容量損失成因 38
2-6 研究動機與設計 41
第三章實驗 43
3-1 實驗藥品、器材與儀器設備 43
3-1-1 實驗藥品 43
3-1-2 實驗器材 45
3-1-3 實驗儀器設備 45
3-2 實驗方法 46
3-2-1 黏著劑聚合方式 46
3-2-2 正極極片製備 47
3-2-3 鈕扣型半電池製備 49
3-3 實驗儀器原理及介紹 50
3-3-1 超高解析場發射掃描式電子顯微鏡(CFE-SEM) 50
3-3-2 超高解析穿透式電子顯微鏡(TEM) 51
3-3-3 X-光光電子能譜儀(XPS) 52
3-4 鋰電池效能及電化學特性分析 53
3-4-1 電池充放電測試 53
3-4-2 循環伏安法分析(CV) 53
3-4-3 交流阻抗分析儀(AC Impedance) 54
第四章結果與討論 57
4-0 寡聚物以及單體的選用 57
4-0-1 變速率充放電 57
4-1 光聚合黏著劑應用於鋰離子電池 60
4-1-1 光聚合黏著劑之反應鑑定 60
4-1-2 光聚合黏著劑之變速率測試圖 61
4-1-3 光聚合黏著劑之循環壽命測試 62
4-1-4 循環伏安法測試 64
4-1-5 掃描式電子顯微鏡(SEM)之電極表面型態分析 65
4-1-6 穿透式電子顯微鏡(TEM)之電極型態分析 67
4-1-7 交流阻抗測試 69
4-1-8 半電池極化分析 72
4-2 熱聚合黏著劑應用於鋰離子電池 74
4-2-1 熱聚合黏著劑之變速率測試圖 74
4-2-2 熱聚合黏著劑之循環壽命 75
4-2-3 循環伏安法測試 76
4-2-4 掃描式電子顯微鏡(SEM)之電極表面型態分析 78
4-2-5 穿透式電子顯微鏡(TEM)之電極型態分析 79
4-2-6 交流阻抗測試 81
4-2-7 半電池極化分析 83
4-3 光聚合以及熱聚合黏著劑比較 85
4-3-1 製備方式 85
4-3-2 黏度差異 87
4-3-3 變速率以及循環壽命的表現 87
4-3-4 循環伏安法測試 90
4-3-5 掃描式電子顯微鏡(SEM)之電極表面型態分析 92
4-3-6 穿透式電子顯微鏡(TEM)之電極型態分析 94
4-3-7 交流阻抗測試 96
4-3-8 電池極化分析 99
4-3-9 X-光光電子能譜儀(XPS)之鈍化層探討 100
4-3-10 示意圖 108
4-3-11 成本及能量消耗評估 109
第五章結論與未來展望 114
參考文獻 116

圖目錄
圖 1- 1鋰電池近年成本變化[4] 2
圖 1- 2環境友善的鋰電池 [8] 2
圖 1- 3鋰離子電池放電時的工作原理圖[15] 3

圖 2- 1黏著劑的未來研究方向以及理想條件[19] 9
圖 2- 2黏著劑的種類 10
圖 2- 3黏著劑與活性材料間的作用示意圖(a)黏彈體(b) PVDF[20] 13
圖 2- 4顯示了具有 LiFePO4陰極和 PVDF 和水性粘合劑電池的第一個循環[20] 14
圖 2- 5用LiFePO4/graphite製備的全電池在 60 °C 下，高倍率充放電的表現[20] 14
圖 2- 6 LiNi0.4Mn1.6O4的XRD (a)無浸泡水中 (b)浸泡於水中[21] 16
圖 2- 7具有CMC黏著劑或是PVDF黏著劑的LiNi0.4Mn1.6O4電極，在不同速率下充放電的電容比較[21] 17
圖 2- 8用(a)CMC/CB 和 (b)PVdF/CB/碳纖維的SEM[21] 17
圖 2- 9 CuO負極使用不同黏著劑的充放電曲線 (a)PVDF (b) SBR+CMC，(d)兩者長圈數循環壽命[22] 19
圖 2- 10充放電前後的電極完整程度，充放電前(左)，充放電後(右) [22] 20
圖 2- 11兩種黏著劑 (a)室溫下(20°C)的醬料黏度 (b) 溫度範圍從20 °C 至 90 °C的黏度變化 [23] 22
圖 2- 12使用(a)PTFE (b)PVDF 製備的 LiFePO4/C電極的SEM圖，以及(c)PTFE (d)PVDF製備電極的示意圖 [23] 22
圖 2- 13由PVDF和PTFE製備的正極在(c)變速率充放電的穩定性(b)0.2C下，長圈數的循環穩定性 [23] 23
圖 2- 14PAA-BP之光交聯機制反應[28] 26
圖 2- 15充放電60圈極片厚度比較，(a)未經光交聯與(b)經光交聯之極片斷面SEM圖[28] 27
圖 2- 16壽命表現比較圖[28] 27
圖 2- 17 (a) PAA+CMC，熱聚合前 (b) PAA+CMC，熱聚合後(c) PAA 與-Si-OH 在加熱後，形成共價鍵[52] 29
圖 2- 18(a) PVDF與矽顆粒的相互作用示意圖 (b) c-PAA-CMC 與矽顆粒的相互作用示意圖[52] 29
圖 2- 19對於不同類型黏著劑，以0.1C的速率，充放電100圈，的電容表現[52] 30
圖 2- 20常見的電解液添加劑[35] 34
圖 2- 21 SEI沉積在電極表面機制圖[34] 35
圖 2- 22電池經過充放電後，Cathode-Electrolyte Interphase(CEI)形成示意圖[44] 37
圖 2- 23循環前、浸泡電解液24hr、100圈循環後 (a) C1s (b) O2p 的XPS圖[44] 37
圖 2- 24高解析度的cryo-EM (a)充放電前 (b)100圈充放電後，NMC電極表面沒有明顯的鈍化層形成[44] 38
圖 2- 25NMC811 與鋰金屬組成的半電池，的第一個循環[50] 40
圖 2- 26 Li x Ni0.8Mn0.1Co0.1O2中的鋰擴散係數與鋰含量的關係[50] 40
圖 2- 27光固化示意圖 41

圖 3- 2(a)光聚合反應式 (b)熱聚合反應式 46
圖 3- 3光聚合極片製備 48
圖 3- 4熱聚合極片製備 49
圖 3- 5鈕扣型半電池組裝順序[53] 50
圖 3- 6循環伏安法分析圖[54] 54
圖 3- 7鋰離子電池等校電路模組示意圖 56

圖 4- 1不同年黏著劑比例的變速率充放電 58
圖 4- 2不同比例黏著劑的電性表現 59
圖 4- 3光聚合黏著劑共聚反應之ATR-IR圖譜光聚合黏著劑共聚反應之ATR-IR圖譜 61
圖 4- 4不同比例光聚合黏著劑之變速率充放電圖 62
圖 4- 5不同比例光聚合黏著劑之循環壽命圖 63
圖 4- 6 (左)PVDF(右)光聚合黏著劑之循環伏安圖 64
圖 4- 7左半部分為PVDF，右半部分為DE:G3E (8:2)，在充放電前(0 圈)與充放電後(125 圈)的SEM 66
圖 4- 8以PVDF黏著劑製備的電極的TEM，及元素分析(Ni、Mn、Co、F、C) 67
圖 4- 9光聚合黏著劑(DE+G3E)製備的電極TEM以及元素分析(Ni、Mn、Co、C) 68
圖 4- 10等效電路圖 69
圖 4- 11四種不同黏著劑比例經過 (a) 0圈 (b) 3圈 (c) 125圈充放電後之交流阻抗圖譜 70
圖 4- 12不同組成之充放電曲線圖(a)PVDF (b)DE:G3E(3:7) (c)DE:G3E(4:6) (d)DE:G3E(5:5) (e)DE:G3E(8:2) 73
圖 4- 13不同比例熱聚合黏著劑之變速率充放電圖 74
圖 4- 14不同比例熱聚合黏著劑之循環壽命圖 75
圖 4- 15(左)PVDF(右)熱聚合黏著劑之循環伏安圖 77
圖 4- 16左半部分為PVDF，右半部分為DP:G3E(10:0)，在充放電前(0 cycle)與充放電後(125 cycle)的SEM 78
圖 4- 17以PVDF黏著劑製備的電極的TEM，及元素分析(Ni、Mn、Co、F、C) 80
圖 4- 18熱聚合黏著劑DP:G3E (10:0)的TEM以及元素分析(Ni、Mn、Co、C) 80
圖 4- 19等效電路圖 81
圖 4- 20圖 4- 11四種不同黏著劑比例經過 (a) 0圈 (b) 3圈 (c) 125圈充放電後之交流阻抗圖譜 82
圖 4- 21不同組成之充放電曲線圖(a)PVDF (b)DP:G3E(3:7) (c) DP:G3E (5:5) (d) DP:G3E (8:2) (e) DP:G3E(9:1) (f) DP:G3E (10:0) 84
圖 4- 22傳統電極製備 86
圖 4- 23熱聚合電極製備 86
圖 4- 24光聚合電極製備 86
圖 4- 25光聚合黏著劑(粉)、熱聚合黏著劑(藍)、傳統黏著劑(綠)，變速率充放電 88
圖 4- 26光聚合黏著劑(粉)、熱聚合黏著劑(藍)、傳統黏著劑(綠)，循環壽命測試 88
圖 4- 27 PVDF、光聚合黏著劑、熱聚合黏著劑之循環伏安圖 90
圖 4- 28三種黏著劑在充放電前(0 cycle)、充放電後(125 cycle)，的SEM比較 93
圖 4- 29 PVDF黏著劑製備的電極TEM，及元素分析(Ni、Mn、Co、F、C) 94
圖 4- 30 光聚合黏著劑(DE+G3E)製備的電極TEM以及元素分析(Ni、Mn、Co、C) 95
圖 4- 31 熱聚合黏著劑DP:G3E(10:0)的TEM以及元素分析(Ni、Mn、Co、C) 95
圖 4- 32光聚合、熱聚合、傳統黏著劑經過0圈、3圈、125圈後的交流阻抗圖譜 97
圖 4- 33不同組成之充放電曲線圖 100
圖 4- 34含有高濃度水溶性電解質的石墨電極，經過循環後SEI層的高解析O 1s, F 1s 的XPS縱深分析 102
圖 4- 35經過3圈充放電跟125圈充放電的電極XPS比較圖(O1s) 102
圖 4- 36經過3圈充放電跟125圈充放電的電極XPS比較圖(P2p) 103
圖 4- 37 LiPF6的水解機制 104
圖 4- 38 經過3圈充放電跟125圈充放電的電極XPS比較圖(F1s) 105
圖 4- 39 經過3圈充放電跟125圈充放電的電極XPS比較圖(C1s) 106
圖 4- 40(a)光聚合黏著劑(b)熱聚合黏著劑(c)傳統黏著劑與活性材料表面作用力示意圖 108

表目錄
表 1- 1水性黏著劑的優點[18] 11
表 1- 2各種黏著劑的優缺點 12
表 1- 3 LiNi0.4Mn1.6O4 (立方晶系Fd-3m)有無浸泡於水的晶格常數、晶體尺寸[21] 16

表 2- 1各極片組成比例 48

表 3- 1不同比例光聚合黏著劑之循環壽命統計表 63
表 3- 2不同黏著劑三圈氧化峰位置 65
表 3- 3四種不同比例的黏著劑，在經過0圈、3圈、125圈後測量之阻抗值 71
表 3- 4不同比例熱聚合黏著劑之循環壽命統計表 76
表 3- 5不同黏著劑三圈氧化峰位置 77
表 3- 6五種不同比例的黏著劑，在經過0圈、3圈、125圈後測量之阻抗值 83
表 3- 7不同黏著劑的黏度測試 87
表 3- 8不同黏著劑之電容保持率 89
表 3- 9不同黏著劑三圈氧化峰位置 91
表 3- 10光聚合、熱聚合、傳統黏著劑經過0圈、3圈、125圈後的Rs、Rct值 97
表 3- 11 不同黏著劑的原料成本、溶劑成本 110
表 3- 12 每顆電池的黏著劑、溶劑成本 110
表 3- 13 不同溶劑的比熱容、汽化熱、分子量以及每片極片所使用的溶劑莫爾數 111
表 3- 14 烘乾不同溶劑的時間、耗電量 112
表 3- 15 不同黏著劑之比較 112

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指導教授

諸柏仁(Po-Jen-Chu)

審核日期

2022-7-27

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