臺灣博碩士論文加值系統

超級電容器的電容量遠大於傳統電容器，而與電池相比，其擁有更理想的功率密度、更高的充放電效率，以及更長的使用壽命，使超級電容器成為具有潛力的能量儲存裝置。在眾多的電極材料之中，聚苯胺具有合成簡單、單體的成本低、導電機制易於控制，以及對環境污染較少等優點，使其常用來作為電極材料。但在充放電過程中，聚苯胺薄膜體積會膨脹，進而導致結構的破壞，造成循環穩定度不佳。因此，我們將異參茚并苯分子引入至聚苯胺骨架之中，設計並合成出星形聚合物SIP 與SIA 以及交聯聚合物CI，也合成以參茚并苯為核心之星形聚合物STP 作為對照，探討其對聚苯胺作為超級電容器電極材料的穩定度與電容值
之影響。
我們將聚苯胺和不同比例的聚合物進行表面形態的觀測，星形聚合物與聚苯胺有相似的顆粒堆疊，而交聯聚合物CI 則呈現明顯不同的球形奈米結構。在電化學表現方面，和聚苯胺相比，摻雜異參茚并苯分子後可在維持相同的循環穩定度下提升電容值和能量密度，此原因推測為異參茚并苯分子本身的結構有利於電荷傳遞，這可由和STP 聚合物的比較來佐證；此外，對於循環穩定度的表現無法有效改善，可能是因為表面積和孔洞體積並沒有形成適合離子進出的孔洞，導致穩定度無法提升，但電容值在1000 次掃描後仍比聚苯胺高出許多，能儲存更多的電荷，而有較佳的電化學表現。
根據此研究成果，對於超級電容器電極材料的改良，可以引入如異參茚并苯般具有π 共軛系統的分子；然而，若要改進材料穩定度，可能需要使分子擁有立體的三度空間結構，使其堆疊後能產生孔道，有助於降低離子進出以及高分子鏈體積膨脹所造成的影響，進而使新穎的聚苯胺材料在超級電容器領域上具有更好的應用價值。

Supercapacitors have emerged as a new kind of energy storage device with higher energy density than conventional capacitors and with superior power density
and cyclic stability than batteries. Among the electrode materials for supercapacitors, polyaniline has been a promising candidate because of its simple synthesis, low cost, controllable electrical conductivity, good redox reversibility, and high environmental stability. However, long-term charge/discharge processes cause structural breakdown and, thus, fast capacitance decay of polyaniline. To improve the performance of polyanilines in supercapacitors, we have introduced the two-dimensional isotruxene scaffold to polyaniline to form a series of new polyanilines, including star-shaped SIP and SIA, as well as crosslinked CI. We also synthesized truxene-incorporated star-shaped STP for comparison.
Our results indicate that the morphology of SIP and SIA is similar to that of polyaniline, which contains fibers and granules, but CI shows sphere morphology, attributable to its crosslinked structures. The isotruxene-incorporated polyanilines display higher specific capacitance than the parent polyaniline owing to strong electronic couplings among the branched arms. However, their cyclic stability is similar to parent polyaniline, presumably due to the unchanged intermolecular packing such that no channels are created for the movement of electrolyte ions during charge/discharge processes.
Our results show that introduction of large π-conjugated systems to polyaniline could enhance the electrochemical performance. However, to improve the operation stability, the materials might need to possess nonplanar structures, so that channels for penetration of ions could be generated to reduce the structural deformation. This work may be helpful for future modification and application of novel polyanilines as the electrode materials of supercapacitors.

謝誌.................................................................................................................................i
摘要...............................................................................................................................iv
Abstract ..........................................................................................................................v
目錄...............................................................................................................................vi
圖目錄...........................................................................................................................ix
表目錄..........................................................................................................................xii
附圖目錄.................................................................................................................... xiii
第一章 序論..................................................................................................................1
1-1 能源儲存.........................................................................................................1
1-2 超級電容器簡介.............................................................................................2
1-2-1 超級電容器原理...................................................................................2
1-2-2 超級電容器種類...................................................................................3
1-2-3 超級電容器電極材料分析...................................................................7
1-3 聚苯胺.............................................................................................................8
1-3-1 聚苯胺簡介及導電原理.......................................................................8
1-3-2 聚苯胺的聚合反應機制.....................................................................11
1-3-3 聚苯胺的奈米結構.............................................................................14
1-3-4 聚苯胺的合成方法.............................................................................15
1-3-5 寡聚物添加對聚苯胺奈米結構之影響.............................................17
1-4 聚苯胺在超級電容器上的應用...................................................................18
1-4-1 聚苯胺應用於超級電容器的限制.....................................................18
1-4-2 聚苯胺穩定度的改善方法.................................................................19
1-4-3 混合式超級電容器的利用.................................................................19
1-4-4 導電高分子的奈米結構與表面形態改善.........................................21
1-4-5 聚苯胺高分子鏈本質的改變.............................................................22
1-5 超級電容器的介面化學分析.......................................................................23
1-5-1 介面化學分析.....................................................................................23
1-5-2 掃描式電子顯微鏡.............................................................................24
1-5-3 穿透式電子顯微鏡.............................................................................24
1-5-4 BET 比表面積及孔徑分析儀............................................................25
1-6 超級電容器的電化學分析...........................................................................28
1-6-1 電化學分析介紹.................................................................................28
1-6-2 循環伏安法.........................................................................................29
1-6-3 恆電流充放電法.................................................................................30
1-6-4 電化學阻抗光譜.................................................................................31
1-7 共軛聚合物...................................................................................................33
1-7-1 一維與多維共軛聚合物.....................................................................33
1-7-2 異參茚并苯 (isotruxene) 及其衍生物............................................33
1-8 研究動機.......................................................................................................35
第二章 結果與討論....................................................................................................37
2-1 單體化合物之合成.......................................................................................37
2-1-1 合成策略分析.....................................................................................37
2-1-2 異參茚并苯及其衍生物之合成.........................................................38
2-1-3 參茚并苯及其衍生物之合成.............................................................42
2-2 含異參茚并苯骨架之聚苯胺的聚合與性質鑑定.......................................43
2-2-1 含異參茚并苯骨架之聚苯胺的聚合反應.........................................43
2-2-2 含異參茚并苯骨架之聚苯胺的鑑定.................................................45
2-2-3 含異參茚并苯骨架之聚苯胺的性質量測.........................................49
2-3 含異參茚并苯骨架之聚苯胺的奈米結構及表面形態...............................51
2-3-1 含異參茚并苯骨架之聚苯胺的SEM 影像圖..................................51
2-3-2 含異參茚并苯骨架之聚苯胺的TEM 影像圖..................................54
2-3-3 含異參茚并苯骨架之聚苯胺的奈米結構分析.................................56
2-4 含異參茚并苯骨架之聚苯胺的表面分析...................................................57
2-4-1 含異參茚并苯骨架之聚苯胺的氮氣吸附-脫附等溫曲線與孔徑尺寸分布................................................................................................57
2-5 含異參茚并苯骨架之聚苯胺的電化學分析...............................................58
2-5-1 含異參茚并苯骨架之聚苯胺的循環伏安法分析.............................59
2-5-2 含異參茚并苯骨架之聚苯胺的恆電流充放電法分析.....................63
2-5-3 含異參茚并苯骨架之聚苯胺的電化學阻抗光譜分析.....................67
2-5-4 含異參茚并苯骨架之聚苯胺的循環穩定度分析.............................69
2-5-5 含參茚并苯骨架之聚苯胺的電化學分析比較.................................71
2-5-6 含異參茚并苯骨架之聚苯胺進行循環穩定度掃描前後的SEM影像圖........................................................................................................73
2-6 含異參茚并苯骨架之聚苯胺的元素分析討論...........................................75
第三章 結論................................................................................................................77
第四章 實驗部分........................................................................................................79
4-1 實驗藥品與溶劑...........................................................................................79
4-2 實驗儀器與方法...........................................................................................82
4-2-1 化合物結構鑑定.................................................................................82
4-2-2 純化系統.............................................................................................84
4-2-3 化合物表面化學與熱穩定性質之量測.............................................84
4-2-4 超級電容器電極材料的電化學性質之量測.....................................85
4-3 實驗步驟.......................................................................................................86
4-3-1 異參茚并苯及其衍生物之合成..........................................................86
4-3-2 參茚并苯及其衍生物之合成..............................................................95
參考文獻......................................................................................................................99
附圖............................................................................................................................106

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