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研究生： 李冠霆
Lee, Kuan-Ting
論文名稱： 聚偏二氟乙烯衍生高分子之合成鑑定與其於鋰電池之應用
Synthesis and Characterization of Polyvinylidene Fluoride Derivatives Used for Lithium Batteries
指導教授： 郭炳林
Kuo, Ping-Lin
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2017
畢業學年度： 105
語文別： 中文
論文頁數： 129
中文關鍵詞： 聚偏二氟乙烯 、磺酸根 、腈基 、黏著劑 、鋰電池
外文關鍵詞： polyvinylidene fluoride, sulfonate, nitrile group, binder, lithium battery
相關次數： 點閱：78  下載：4 
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    • 本研究以原子轉移自由基聚合法，成功合成出側鏈帶有不同長度磺酸根及腈基的聚偏二氟乙烯接枝高分子P-g-sPGMA及P-g-sPGMA-PAN，並將其作為導離子型高分子黏著劑，應用於鋰電池正極磷酸鋰鐵材料中。此高分子黏著劑，於電解液中有良好電化學穩定性，且側鏈上的磺酸根及腈基，能幫助電極材料提升分散性，並增進鋰離子傳導速率，減少電池極化現象。本實驗將以循環伏安法、電化學阻抗頻譜法、電池充放電測試、循環壽命測試、及180 °剝離力測試，鑑定高分子黏著劑之特性及電化學表現性，並與商業用黏著劑聚偏二氟乙烯作比較。以P-g-sPGMA 及P-g-sPGMA-PAN製備的電極材料，由於能在負極形成穩定且緻密的SEI層，因此有著相對較小的界面阻抗。其側鏈導離子官能基，由於能幫助鋰離子嵌入遷出電極，因此可得到較穩定之充放電平台。與PVDF相比，使用P-g-sPGMA 及P-g-sPGMA-PAN的電極材料，有著更優異的循環穩定性與電容維持率，儘管接枝導離子官能基後，其附著力不如PVDF，但仍不影響其在循環壽命上的表現性。

    In this study, the polyvinylidene fluoride (PVDF) grafted with sulfonates (P-g-sPGMA) and nitrile groups (P-g-sPGMA-PAN) has been synthesized through atom transfer radical polymerization (ATRP) and applied as the ionic conductivity binder for a lithium ion phosphate (LiFePO4) cathode of a lithium battery. These two types of grafted polymers exhibit strong chemical stability in electrolyte. Sulfonic and nitrile side chains can help to improve the dispersion of cathode materials and enhance the ionic conductivity and Li+ ion diffusion due to the charge delocalization over the sulfonic and nitrile chains. The performances are evaluated by cyclic voltammetry, electrochemical impedance spectroscopy, charge-discharge testing, cycle testing, 180° peel testing, and compared with the cathode prepared with PVDF binder. The electrodes prepared with P-g-sPGMA and P-g-sPGMA-PAN binder form the relatively smaller resistance due to the stable and compact SEI layer formed on the Li electrode. The ionic side chains are beneficial to lithium ion intercalation and de-intercalation of the cathode during charging-discharging, therefore the cell prepared with P-g-sPGMA and P-g-sPGMA-PAN show lower charge plateau potential and higher discharge potential. Compared with PVDF, the electrode with ionic binder exhibits better cycling stability and rate capability. Meanwhile, although the adhesion strength of electrodes prepared with ionic binders are less than that with PVDF, it does not influence the cycling stability.

    中文摘要 I Abstract II 誌謝 XIV 目錄 XV 表目錄 XX 圖目錄 XXI 第一章 緒論 1 1.1 前言 1 1.2 鋰電池簡介 3 1.3 鋰電池基本工作原理 5 1.4 電極材料 7 1.5 電解質 11 1.6 黏著劑 13 1.7 研究動機 15 第二章 文獻回顧 17 2.1 非水性黏著劑 17 2.2 水性黏著劑 19 2.2.1 羧甲基纖維素（CMC） 19 2.2.2 聚丙烯酸（PAA） 23 2.2.3 海藻酸鈉（SA） 25 2.3 功能型高分子黏著劑 27 2.3.1 導電型高分子黏著劑 27 2.3.2 導離子型高分子黏著劑 28 2.3.3 穩定電極結構型高分子黏著劑 30 2.3.4 鋰硫電池黏著劑 33 2.4 鋰金屬負極的型態變化與SEI的形成 36 2.5 原子轉移自由基聚合法 (ATRP) 43 2.5.1 ATRP簡介 43 2.5.2 ATRP構成要素 44 2.5.3 ATRP反應機制 45 2.5.4 ATRP之應用 46 第三章 實驗 49 3.1 實驗藥品與材料 49 3.2 實驗儀器與設備 51 3.3 樣品製備 53 3.3.1 鋰式牛磺酸（LiAES）之製備 53 3.3.2 聚偏二氟乙烯接枝高分子之製備 53 3.3.3 聚偏二氟乙烯接枝高分子之磺酸化 55 3.4 材料性質分析與鑑定 58 3.4.1 傅立葉轉換紅外光譜儀（FT-IR） 58 3.4.2 核磁共振光譜儀（1H NMR） 58 3.4.3 熱重分析儀（TGA） 59 3.4.4 示差掃描熱量分析儀（DSC） 59 3.4.5 掃描式電子顯微鏡（SEM） 60 3.4.6 剝離力測式（Peeling Test） 60 3.4.7 高分子於電解液中穩定性測試（Polymer Stability） 61 3.4.8 鋰金屬表面型態分析 61 3.5 鋰離子電池之製備與組裝 63 3.5.1 LiFePO4正極極片製作 63 3.5.2 鈕扣型電池組裝 63 3.6 電化學測試 65 3.6.1 電池充放電能力測式（C-rate Test） 65 3.6.2 電池循環壽命測試（Cycle Life Test） 65 3.6.3 電化學阻抗頻譜法（EIS） 65 3.6.4 離子傳導度（Ionic Conductivity） 68 3.6.5 循環伏安法（Cyclic Voltammetry） 69 第四章 結果與討論 70 4.1 聚偏二氟乙烯衍生高分子之合成與鑑定 70 4.1.1 傅立葉轉換紅外光譜分析 70 4.1.2 核磁共振光譜分析 72 4.2 熱重分析 76 4.3 熱轉移性質 80 4.4 黏著劑於電解液中穩定性測試 82 4.5 電極表面與截面型態 85 4.6 循環伏安法分析 91 4.7 離子傳導度 95 4.8 電化學阻抗頻譜分析 97 4.9 鋰離子電池充放電測試 101 4.10 鋰離子電池循環壽命測試 105 4.11 鋰金屬形態變化及其表面SEI之形成 112 4.12 剝離力測試 115 第五章 結論 120 第六章 參考文獻 122

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