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研究生：	梁育豪 Liang, Yu-Hao
論文名稱：	鋰離子於聚丙烯腈共聚物膠態高分子電解質之傳導行為探討 Study on the conductivity behaviour of lithium ion in the plasticized polymer electrolyte based on polyacrylonitrile copolymer
指導教授：	陳志勇 Chen, Chuh-Yung
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2008
畢業學年度：	96
語文別：	中文
論文頁數：	141
中文關鍵詞：	膠態高分子電解質、聚丙烯腈共聚合物、導電度、鋰離子
外文關鍵詞：	plasticized polymer electrolyte, lithium ion, conductivity, copolymer of polyacrylonitrile
相關次數：	點閱：89 下載：3
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本研究主要是將不同極性基引入polyacrylonitrile (PAN)中形成共聚物，以應用於膠態高分子電解質之研究，本文總共製備三種不同之共聚物：(1)Copoly(AN–PEGMEM)，以側鏈含–CH2–O–CH2–基的單體Poly(ethylene glycol)methyl ether methacrylate (PEGMEM)與AN單體進行共聚合；(2) Block copoly(AN–PEG)：利用尾端基含Poly(ethylene glycol) (PEG)鏈段的起始劑聚合AN單體。(3) Copoly(AN–GMA-IDA)：製備含螯合基單體(2-methylacrylic acid 3-(bis-carboxymethylamino-2-hydroxy-propyl ester) (GMA-IDA)，再與AN單體進行共聚合。
將各共聚物混合鋰鹽及塑化劑製備成各種不同組成的膠態高分子電解質，並由紅外線光譜儀(Fourier-transform infrared spectroscopy；FT-IR)及固態核磁共振儀(7Li magic-angle spinning NMR；7Li MAS NMR)確認各系統與鋰離子作用之官能基與引入之極性基對鋰鹽解離能力的影響。而由熱插微分掃描分析儀(Differential scanning calorimetry；DSC)觀察到不同的高分子基材對於塑化劑-propylene carbonate (PC)的運動性有不同的影響。在鋰鹽加入後，鋰離子與PC及高分子間的作用力也會使PC的運動性下降，且依高分子的組成不同其變化的趨勢亦會不同。
就導電度方面而言，copoly(AN–PEGMEM)及block copoly(AN–PEG)皆可於polymer/PC 50:50 wt.%組成下使導電度達10–3 Scm–1，而copoly(AN–GMA-IDA)則須於polymer/PC 20:80 wt.% 組成才能使導電度達到10–3 Scm–1。此外，copoly(AN–PEGMEM)雖然可於copoly(AN–PEGMEM)/PC 50:50 wt.%的組成下使導電度達10–3 Scm–1，但由於其側鏈基團影響而造成其成膜性及機械強度都較其他兩系統差；block copoly(AN–PEG)系統除了可於block copoly(AN–PEG)/PC 50:50 wt.%的組成下使導電度達10–3 Scm–1外，並兼具一定的機械強度。copoly(AN–GMA-IDA)則須於polymer/PC 20:80 wt.%組成才能使導電度達10–3 Scm–1等級。但GMA-IDA單元導入膠態高分子中時，其可幫助此系統即使於高塑化劑含量下仍可維持與鋰電極界面的穩定性及保持一定的機械強度。此外，可透過改變塑化劑使copoly(AN–GMA-IDA)於polymer/EC 40:60 wt.%組成下即可使導電度接近10–3 Scm–1。所以，此系統也是可應用於鋰電池中的膠態高分子電解質。

Three types of copolymer electrolytes were prepared in this study, including: (a) Copoly(AN–PEGMEM), a comb-like polymer was prepared by copolymerization of acrylonitrile (AN) and poly(ethylene glycol-methyl methacrylate) (PEGMEM); (b) Block copoly(AN–PEG), a block copolymer was synthesized by the macroinitiator method; and (c) Copoly(AN–GMA-IDA), a monomer (3-(bis-carboxymethylamino-2-hydroxy-propyl ester) (GMA-IDA) with a strong chelating group, iminodiacetic acid, was introduced into the PAN matrix by copolymerization.
All copolymers were mixed with plasticizer and lithium perchlorate (LiClO4) to form plasticized polymer electrolytes. 7Li magic-angle spinning NMR and Fourier-transform infrared spectroscopy elucidate the interactions between lithium ions and the unpaired electrons on the groups based on the plasticized polymer. Moreover, the results of the spectra indicate that the introduced polar groups promote dissociation of the lithium salt. Differential scanning calorimetry was used to study the thermal behavior of plasticized polymer electrolytes of different compositions. The polymer matrixes affect the mobility of plasticizer in the system. In Addition, the glassy transition temperature (Tg) of the plasticized polymer electrolytes increases with the doping of LiClO4, indicating interactions among lithium ions, the plasticizer-PC and the copolymer.
Furthermore, the conductivity of plasticized polymer electrolytes based on copoly(AN–PEGMEM) and block copoly(AN–PEG) is better than the conductivity of that based on polyacrylonitrile (PAN) with the same composition (polymer/plasticizer 50:50 wt.%). Notably, the highest conductivity of the copolymer/plasticizer 50:50 wt.% systems is close to that of the PAN/plasticizer 20:80 wt.% system (1.9010–3 Scm–1). Besides, the composition polymer/plasticizer 50:50 wt.% based on block copoly(AN–PEG) also has good mechanical strength. On the other hand, the copoly(AN–GMA-IDA) system needs more plasticizer (polymer/PC 20:80 wt.%) to improve the conductivity to 10–3 Scm–1. However, the GMA-IDA unit can improve the stability of interface between polymer electrolyte and lithium electrode and retain good mechanical strength, even through a system with high plasticizer content. Moreover, the conductivity of the copoly(AN–GMA-IDA)/plasticizer 40:60 wt.% composition was promoted to nearly 10–3 Scm–1 by using ethylene carbonate (EC) as plasticizer.

中文摘要．．．．．．．．．．．．．．．．．．．．．．．．．I
英文摘要．．．．．．．．．．．．．．．．．．．．．．．．III
致謝．．．．．．．．．．．．．．．．．．．．．．．．．．．V
目錄．．．．．．．．．．．．．．．．．．．．．．．．．．VII
表目錄．．．．．．．．．．．．．．．．．．．．．．．．．．．．X
圖目錄．．．．．．．．．．．．．．．．．．．．．．．．．XII
	
第一章、緒論．．．．．．．．．．．．．．．．．．．．．．．1
第二章、文獻回顧．．．．．．．．．．．．．．．．．．．．．5
  2-1、高分子電解質．．．．．．．．．．．．．．．．．．．5
    2-1-1、全固態高分子電解質．．．．．．．．．．．．．．5
    2-1-2、膠態高分子電解質．．．．．．．．．．．．．．．9
      2-1-2-1、膠態高分子電解質之高分子基材．．．．．．．9
      2-1-2-2、膠態高分子電解質之塑化劑．．．．．．．．．15
    2-1-3、無機複合高分子電解質．．．．．．．．．．．．．18
  2-2、離子源之種類．．．．．．．．．．．．．．．．．．．19
  2-3、高分子電解質的傳導機制．．．．．．．．．．．．．．20
    2-3-1、固態高分子電解質之機制．．．．．．．．．．．．20
    2-3-2、膠態高分子電解質之機制．．．．．．．．．．．．23
  2-4、PAN系列膠態高分子電解簡介．．．．．．．．．．．．27
  2-5、研究動機與大綱．．．．．．．．．．．．．．．．．．32
    2-5-1、研究動機．．．．．．．．．．．．．．．．．．．32
    2-5-2、大綱．．．．．．．．．．．．．．．．．．．．．32
第三章、實驗部分．．．．．．．．．．．．．．．．．．．．34
  3-1、藥品．．．．．．．．．．．．．．．．．．．．．．．34
  3-2、儀器．．．．．．．．．．．．．．．．．．．．．．．35
  3-3、實驗步驟．．．．．．．．．．．．．．．．．．．．．36
    3-3-1、Copoly(AN–PEGMEM)合成．．．．．．．．．．．．36
    3-3-2、Block copoly(AN–PEG)合成．．．．．．．．．．37
    3-3-3、Copoly(AN–GMA-IDA)合成．．．．．．．．．．．38
    3-3-4、膠態高分子電解質的製作．．．．．．．．．．．．40
    3-3-5、紅外線光譜分析(FT-IR) ．．．．．．．．．．．．40
    3-3-6、液態核磁共振光譜分析(NMR) ．．．．．．．．．．41
    3-3-7、固態核磁共振光譜分析( Solid State NMR) ．．．41
    3-3-8、微差熱掃描分析(DSC)．．．．．．．．．．．．．41
    3-3-9、交流阻抗分析(AC Impedance) ．．．．．．．．．41
    3-3-10、應力-應變測試．．．．．．．．．．．．．．．．42
第四章、結果與討論．．．．．．．．．．．．．．．．．．．43
  4-1、不同鋰鹽之研究及探討．．．．．．．．．．．．．．．43
    4-1-1、不同鋰鹽於膠態高分子電解質中之FT-IR研究．．．44
    4-1-2、不同鋰鹽於膠態高分子電解質中之13C CP/MAS NMR研究．．．．．．．．．．．．．．．．．．．．．．．．．．．48
    4-1-3、不同鋰鹽於膠態高分子電解質中之導電度研究．．．48
  4-2、不同高分子基材的導電行為之研究．．．．．．．．．．53
    4-2-1、高分子之合成及鑑定．．．．．．．．．．．．．．53
      4-2-1-1、梳狀共聚高分子copoly(AN–PEGMEM)的鑑定．．53
      4-2-1-2、Block copoly(AN–PEG)之合成及鑑定．．．．56
      4-2-1-3、Copoly(AN–GMA-IDA)之合成及鑑定．．．．．67
    4-2-2、膠態高分子之製備．．．．．．．．．．．．．．．73
    4-2-3、膠態高分子電解質之FT-IR分析．．．．．．．．．77
    4-2-4、膠態高分子電解質之7Li solid state MAS NMR分析．．．．．．．．．．．．．．．．．．．．．．．．．．．93
    4-2-5、膠態高分子電解質之DSC分析．．．．．．．．．．102
    4-2-6、膠態高分子電解質之導電度分析．．．．．．．．106
    4-2-7、Copoly(AN–GMA-IDA)膠態高分子電解質與鋰電極之界面穩定性分析．．．．．．．．．．．．．．．．．．．．．．109
  4-3、使用結晶性塑化劑Etheylene Carbonate(EC)於copoly(AN–GMA-IDA)電解質之研究．．．．．．．．．．．．．．．．．．118
    4-3-1、Copoly(AN–GMA-IDA)與EC之間的交互作用分析．．119
    4-3-2、Copoly(AN–GMA-IDA)與EC之膠態高分子導電度分析．．．．．．．．．．．．．．．．．．．．．．．．．．．120
第五章、總結．．．．．．．．．．．．．．．．．．．．．．127
未來工作建議．．．．．．．．．．．．．．．．．．．．．．129
參考文獻．．．．．．．．．．．．．．．．．．．．．．．．130
                                    

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