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研究生： 陳彥名
Chen, Yen-Ming
論文名稱： 氧化石墨烯量子點提昇膠態鋰離子電池之研究
Graphene Oxide Quantum Dots for High Performance Gel-state Lithium Ion Batteries
指導教授： 鄧熙聖
Teng, Hsi-Sheng
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： 149
中文關鍵詞： 鋰離子電池 、聚丙烯腈 、膠態高分子電解質 、氧化石墨烯量子點
外文關鍵詞： lithium-ion battery, gel polymer electrolyte, poly(acrylonitrile), filler, graphene oxide quantum dots, cluster ions
相關次數： 點閱：151  下載：5 
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    • 本研究以聚丙烯腈(Poly(acrylonitrile-co-vinyl acetate) (PAV))高分子為主架構，混摻Poly(methyl methacrylate) (PMMA)高分子，並添加氧化石墨烯量子點(GOQDs)強化性能，再經過靜電紡絲方法製備出高分子薄膜，最後將其浸泡於有機電解液(LE)中24小時，即可得到本研究之膠態高分子電解質。此外本研究進一步探討三種不同尺寸之氧化石墨烯量子點(QD11、QD7、QD3)對整體電解質系統之影響，其所形成之膠態電解質稱作GPE-PAVM:QD11、GPE-PAVM:QD7與GPE-PAVM:QD3。
    首先在氧化石墨烯量子點的測試上，經由TEM、AFM與Mott Schottky測試，鑑定其形貌、粒徑大小與半導體性質。結果顯示本研究之氧化石墨烯量子點具有P-type 半導體特性，且尺寸都相當微小、分散性也相當好，因此對於提升整體系統吸引負離子(PF6¯)的接觸面積有相當程度的增加。接著藉由NMR、拉曼測試與鋰離子遷移常數分析，針對膠態高分子電解質系統內離子、溶劑分子、高分子官能基間交互作用進行探討。進而發現加入GOQDs的高分子電解質GPE-PAVM:QDx ( x = 3 or 7)可增加吸引PF6¯的數量，將溶劑中的離子團(Cluster ions)分散，並減少鋰離子與溶劑分子的配位數，使鋰離子所受到的阻力大為減小，加速鋰離子的傳遞。此性質也對電化學穩定電位窗、導離子度都有所提升。其中最小尺寸氧化石墨烯量子點(QD3)因為具有最大的接觸面積，因此其所形成的膠態高分子電解質(GPE-PAVM:QD3)則具有最好的效果。在半電池阻力分析及壓降分析，可以得知GPE-PAVM:QD3系統皆具有較低阻力值，此結果可證實其對於鋰離子傳遞的幫助甚大。本研究之電池性能測試是使用磷酸鋰鐵搭配鋰金屬組裝成半電池測試，比較SLE (商用隔膜)、GPE-PAVM (未加入GOQDs)、GPE-PAVM:QD11、GPE-PAVM:QD7與GPE-PAVM:QD3的差異。在高速充放電(20 C-rate) 時GPE-PAVM:QD3仍擁有52.1 mAh g-1之高放電量。在高速(5 C-rate)長效穩定性測試方面，進行500圈長效充放電測試後，GPE-PAVM:QD3半電池仍可穩定維持完美100%的效能。

    This study incorporates graphene oxide quantum dots (GOQDs) into a gel polymer electrolyte (GPE) designed for lithium ion batteries (LIBs). The GPE comprises poly(acrylonitrile-co-vinyl acetate) copolymer (PVA) blending poly(methyl methacrylate) (PMMA) as a host swelled by a liquid electrolyte (LE) of 1 M LiPF6 in a carbonate solvent. The present study finds that the QD3, PVA, and PMMA incorporated GPE-PAVM:QD3 system have excellent performance because it has strongly interaction with PF6− anions to effectively disperse the cluster ions and decreased the solvation degree of Li+ that accelerate the transport of Li+ ion. GPE-PAVM:QD3 has a high Li+ transference number (0.77). Immobilization of PF6− anions also leads to the formation of stable solid-electrolyte interface (SEI) layers in a half-cell Li / electrolyte / PAV+LiFePO4 battery, which exhibits low SEI and overall resistances. The Li / electrolyte / PAV+LiFePO4 battery delivers high capacity of 52 mAh g−1 even at 20 C and presents 100% capacity retention after 500 charge−discharge cycles at 5 C, respectively.

    第一章緒論 1 1-1前言-電池發展與介紹 1 1-3鋰電池與鋰離子二次電池 3 1-3.1 裝置構造 4 1-3.2 工作原理 4 1-4電解質 6 1-4.1 液態有機電解質 6 1-4.2 固態高分子電解質 8 1-4.3 膠態高分子電解質 11 1-4.4固態鋰陶瓷電解質 12 1-5電極材料 14 1-5.1 正極材料 14 1-5.2 負極材料 18 1-6不同電池系統 20 1-6.1鋰硫電池 20 1-6.2鋁電池 23 1-6.3鈉/鎂電池 25 1-6.4鋰空氣電池 28 1-7常見鋰離子電池專有名詞與計算 30 1-7.1理論電容計算 30 1-7.2鋰電池專有名詞 31 1-7.3電池組串並聯計算 32 1-8全球鋰電池商業概況 34 1-9研究動機與目的 37 第二章理論說明與文獻回顧 38 2-1聚丙烯腈性質與回顧 38 2-2電紡絲技術(Electrospinning) 40 2-3導離子度 43 2-4 正離子遷移常數 45 第三章實驗方法與儀器原理介紹 48 3-1 實驗藥品 48 3-2 實驗儀器設備 49 3-3 氧化石墨烯量子點製備 51 3-4 膠態高分子電解質製備 52 3-5鈕扣型電池(coin-cell)組裝 54 3-6實驗分析儀器與裝置分析儀器原理簡介 55 3-6.1掃描式電子顯微鏡(Scanning Electron Microscope, SEM) 55 3-6.2 穿透式電子顯微鏡(Transmission Electron Microscope, TEM ) 57 3-6.3核磁共振光譜儀(Nuclear Magnetic Resonance, NMR) 58 3-6.3拉曼光譜分析(Raman Spectrum) 62 3-6.4半導體–電解質之介面分析(Semiconductor-Electrolyte Interfance) 64 3-7電化學測試 67 3-7.1 導離子度(Ionic conductivity, σ) 67 3-7.2 線性掃描伏安法(Linear sweep voltammogram, LSV) 67 3-7.3 鋰離子遷移常數 (Lithium transference number, tLi+) 67 3-7.4電池阻力測試 68 3-8電池性能測試 69 3-8.1 LiFePO4正極之極片製作 69 3-8.2 LiFePO4半電池 69 3-9實驗流程 70 第四章結果與討論 71 4-1氧化石墨烯量子點物理分析與鑑定 73 4-1.1 TEM與AFM分析 73 4-1.2 半導體性質分析 76 4-2膠態高分子電解質內部分析 77 4-2.1 高分子膜形貌 77 4-2.2 SEM分析 80 4-2.3 TGA分析 81 4-2.4 NMR分析 83 4-2.5 Raman分析 85 4-3膠態高分子電解質電化學分析 89 4-3.1 離子傳導度(Ionic conductivity) 89 4-3.2 鋰離子遷移數(Lithium transference number, tLi+) 94 4-3.3電化學穩定度量測 98 4-4 Li｜LiFePO4半電池性能測試 100 4-4.1 LiFePO4半電池充放電測試 100 4-4.2 LiFePO4半電池界面阻力測試 105 4-4.3 LiFePO4半電池voltage drop分析 108 4-4.4 LiFePO4半電池長效測試 110 4-4.5 PVDF+LiFePO4半電池性能測試 112 4-4.6 電池短路性能測試 114 4-4.7 Ragone plot 116 4-5 文獻比較 118 第五章結論與建議 121 參考文獻 123

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