鋰離子電池新型添加劑之合成及其應用｜國立臺灣科技大學博碩士論文系統

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研究生：	廖禮葳 Lee-Wei Liao
論文名稱：	鋰離子電池新型添加劑之合成及其應用 Synthesis and Applications of New Additives for Lithium Ion Batteries
指導教授：	黃炳照 Bing-Joe Hwang
口試委員:	江志強 Jyh-Chiang Jiang 蘇威年 Wei-Nien Su 陳景翔 Ching-Hsiang Chen
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2014
畢業學年度：	102
語文別：	中文
論文頁數：	160
中文關鍵詞：	碳酸丙烯酯、共遷入、高分歧化聚合物、固體電解質界面、熱穩定性
外文關鍵詞：	Propylene carbonate, Cointercalation, Hyper branch polymer, SEI layer, Thermal stability
相關次數：	點閱：278 下載：8
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本研究開發兩種不同功能添加劑之應用 (一)抑制PC電解液於充放電過程中與鋰離子共遷入碳材電極中之現象，並使電池能有效運作。(二)高分歧化聚合物(Hyper branched Polymaleimide, HBPM)應用於鋰離子電池陰極之熱穩定型添加劑。
根據理論計算，研發出可抑制PC電解液於充放電過程中與鋰離子共遷入碳材材料電極中之現象之新型添加劑。當添加量為2wt.%時，能有效抑制共遷入現象，並維持穩定有效率的充放電。當添加量為1wt.%時，無法有效阻止共遷入現象，電池無法正常運作。而當添加量超過5wt.%以上，雖然能夠有效抑制共遷入現象，讓電池能順利進行充放電，卻無法維持穩定的電容量。
HBPM 經過電化學程序後，會於陰極材料鋰鈷氧(LiCoO2)表面上形成固態電解質介面(solid electrolyte interface，SEI )，此新的SEI層能有效提升原本鋰鈷氧於電池系統中的熱穩定性及安定性；此外，藉由將HBPM上未與maleimide反應之OH官能基與小分子Acyl chloride反應，電化學表現有了好的改善；由DSC結果測試，熱裂解溫度及放熱量皆隨著HBPM的導入而延遲。

In this work, the development of two different additives serving differing functions were fabricated and investigated.。(I) The inhibition of the co-intercalation of PC solvent with Li-ions into graphite electrode allowing for practical use within a PC-solvent containing battery system。(II) Hyper branched polymaleimide (HBPM) used as an cathode additive to alleviate thermal runway。
Based on criteria established by theoretical calculations, new additives were fabricated to inhibit PC solvent and Li ion co-intercalation into graphite electrode during the charge and discharge process. The addition of 2 wt% of the additives can effectively suppress the co-intercalation phenomenon maintain stable charge/discharge while the addition of only 1wt.% showed relatively poor performance and stability . With the addition of more than 5wt.%, there is adequate suppression of the co-intercalation phenomenon but a reduction of stability occurs.
After electrochemical cycling, HBPM forms as a new SEI layer on the surface of lithium cobalt oxide, which enhances the thermal stability and reduction of exothermic reactions of lithium cobalt oxide in the battery system as evidenced by DSC. In addition, the use of Acyl chloride to reduce the OH functional groups of the maleimide shows to have greatly enhanced the electrochemical performance and stability during battery operation.

摘要..........................................................................................................Ⅱ
Abstract.....................................................................................................Ⅲ
致謝..........................................................................................................Ⅳ
目錄..........................................................................................................Ⅴ
圖目錄..................................................................................................ⅩⅠ
表目錄..................................................................................................ⅩⅦ
第一章 緒論..............................................................................................1
1-1 前言 ..................................................................................................1
1-2 鋰離子電池的演進與發展.................................................................2
1-3 二次鋰離子電池之組成與機制.........................................................5
1-4 二次鋰離子電池之各元件介紹 .......................................................7
1-4-1 正極(陰極).......................................................................................7
1-4-2負極(陽極)......................................................................................10
1-4-3 隔離膜...........................................................................................12
1-4-4 電解液...........................................................................................13
1-5 研究動機與目的 .............................................................................17
1-5-1用於抑制PC共遷入現象之新型添加劑.........................................17
1-5-2熱穩定型添加劑 ...........................................................................18
第二章 文獻回顧 .................................................................................21
2-1 電解液添加劑 …............................................................................21
2-1-1 SEI (Solid electrolyte interface，固液電解質界面) ....................24
2-1-2 還原型添加劑 .............................................................................27
2-1-3 反應型添加劑 .............................................................................30
2-1-4 正極保護添加劑 .........................................................................36
2-2 安全性改質的技術及進展 ............................................................33
2-2-1 電極材料本身的熱穩定性..........................................................38
2-2-1-1負極與電解液之間的反應......................................................38
2-2-1-2 正極與電解液之間的反應....................................................39
2-3 電池安全機制 ...............................................................................42
2-4 樹枝狀高分子 ...............................................................................47
第三章 實驗方法 ................................................................................52
3-1 實驗儀器設備 ...............................................................................52
3-2 實驗藥品器材 ..............................................................................54
3-3 材料鑑定分析 ..............................................................................56
3-3-1 掃瞄式電子顯微鏡分析（SEM）............................................56
3-3-2 能量散佈分析儀(EDS) ............................................................57
3-3-3 微分掃描熱卡分析儀(DSC).....................................................57
3-3-4 核磁共振儀分析（NMR） ....................................................59
3-3-5 傅立葉轉換紅外線光譜儀(FTIR) ...........................................60
3-3-6 高解析光電子能譜儀(XPS) ....................................................61
3-3-7 熱重量分析儀 (TGA) .............................................................63
3-3-8 膠體滲透層析儀(GPC) ...........................................................63
3-4 材料電化學特性分析 ................................................................64
3-4-1 電池性能測試 .........................................................................64
3-4-2 循環伏安分析 .........................................................................64
3-4-3 交流阻抗分析 .........................................................................65
3-5實驗步驟 ......................................................................................68
3-5-1新型添加劑之合成.................................................................68
3-5-1-1 4-(chloromethyl)-1,3,2-dioxathiolane 2-oxide之合成…..68
3-5-1-2 4,5-bis(chloromethyl)-1,3,2-dioxathiolane 2-oxide之合成..70
3-5-2熱穩定型樹枝狀高分子聚合物材料之合成步驟 .................71
3-5-2-1 N-(4-carboxyphenyl)maleamic acid 單體之合成 ..............71
3-5-2-2 N-(4-carboxyphenyl)maleimide 單體之合成 ...................71
3-5-2-3 N-[4-(chlorocarbonyl)phenyl]maleimide 之合成…….......73
3-5-2-4 Hyperbranched polyester- maleimide terminated 之合....74
3-5-2-5 Hyper branched polyester- maleimide terminated尾端OH基再封端…………………………………………………………………….75
3-5-3 陰極(正極)極片之製備 ..........................................................77
3-5-4 陽極電解液之製備...................................................................79
3-5-5 硬幣型電池之組裝...............................................................79
第四章 結果與討論.............................................................................82
4-1新型添加劑之合成鑑定與性質分析.............................................82
4-1-1 4-(chloromethyl)-1,3,2-dioxathiolane 2-oxide之鑑定 .............83
4-1-2 4,5-bis(chloromethyl)-1,3,2-dioxathiolane 2-oxide之鑑………………………………………………………………….85
4-1-3 新型添加劑之電化學分析…………………….……….…87
4-1-3-1 MCMB電極-純PC電解液之充放電圖譜分析..............................................................................................87
4-1-3-2  MCMB電極-Monochloride additive充放電圖譜分析…..88
4-1-3-3  MCMB電極-dichloride additive充放電圖譜分析..............89
4-1-4 循環伏安分析...........................................................................90
4-1-5 交流阻抗分析 ..........................................................................93
4-1-6 SEM分析 .................................................................................. 94
4-1-7 XRD結構分析.............................................................................96
4-1-8新型添加劑於不同組成條件之電解液下之電化學分析……..97
4-2 熱穩定型高分子材料之合成鑑定與性質分析 ......................101
4-2-1 N-(4-carboxyphenyl)maleamic acid材料的合成鑑定與性質分析 .....................................................................................................101
4-2-1-1 N-(4-carboxyphenyl)maleamic acid單體的DSC結果 .....................................................................................................101
4-2-1-2 N-(4-carboxyphenyl)maleamic acid 單體的IR圖譜 ....................................................................................................101
4-2-1-3 N-(4-carboxyphenyl)maleamic acid 單體的NMR圖譜 .................................................................................................103
4-2-2 N-(4-carboxyphenyl)maleimide單體材料的合成鑑定與性質分析 ................................................................................................ 105
4-2-2-1 N-(4-carboxyphenyl)maleimide單體材料的DSC測試結果 ............................................................................................... 105
4-2-2-2 N-(4-carboxyphenyl)maleimide單體材料的IR分析結果 ............................................................................................... 106
4-2-2-3 N-(4-carboxyphenyl)maleimide單體材料的NMR分析結果 ................................................................................................ 107
4-2-3 N-[4-(chlorocarbonyl)phenyl]maleimide單體材料的合成鑑定與性質分析 ........................................................................................ 110
4-2-3-1 N-[4-(chlorocarbonyl)phenyl]maleimide單體材料的DSC測試結果 .................................................................................................... 110
4-2-3-2 N-[4-(chlorocarbonyl)phenyl]maleimide單體材料的IR分析結果 ................................................................................................... 111
4-2-3-3 N-[4-(chlorocarbonyl)phenyl]maleimide之NMR測試 ................................................................................................. 112
4-2-4 樹枝狀高分子的合成鑑定與性質分析 ...........................115
4-2-4-1樹枝狀高分子之NMR分析結果 .................................... 118
4-2-5 Hyperbranched polymaleimide (HBPM) 之電化學性質與電性表現 ................................................................................................. 121
4-2-5-1 Hyper branched polymaleimide的充放電曲線圖……….121
4-2-6 Hyper branched polymaleimide不同添加量對電池的熱穩定性分析 ................................................................................................. 124
第五章 結論.................................................................................. 126
5-1 新型添加劑............................................................................. 126
5-2 熱穩定型高分子材料 ........................................................... 126
未來展望 ....................................................................................... 128
參考文獻 ....................................................................................... 132

                                

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