本實驗專注於水系鋅離子混合電容器之研究，首次使用奈米多孔核殼結構多壁奈米碳管/氧化石墨烯奈米帶（NP-MWCNT@GONR）作為正極材料，後續更進一步使用膠態電解質改善液態電解液的循環穩定性問題。研究內容分為三大部分，第一部分為將多壁奈米碳管（MWCNT）及其改質後的多壁奈米碳管/氧化石墨烯奈米帶（MWCNT@GONR）、奈米多孔核殼結構多壁奈米碳管/氧化石墨烯奈米帶（NP-MWCNT@GONR）的材料特性分析。第二部分是將這三種碳材作為水系鋅離子混合電容正極材料，測試在液態電解液系統中之電化學性能。第三部分為分析NP-MWCNT@GONR於膠態電解質系統中的表現，同時利用同步輻射技術驗證此系統的穩定性，並製成柔性可彎折、自修復特性的元件，測試其電性表現。
第一部分為利用場發射掃描式電子顯微鏡、穿透式電子顯微鏡、X光繞射儀、拉曼光譜分析、BET比表面積與孔徑分析以及X光光電子能譜進行材料分析。由材料分析結果可觀察到改質後具有高比表面積的NP-MWCNT@GONR為有潛力之鋅離子混合電容器正極材料。
第二部分將MWCNT、MWCNT@GONR與NP-MWCNT@GONR於液態電解液中進行循環伏安法、恆電流充放電測試、倍率與循環性能量測、電化學阻抗頻譜分析與Ragone plot分析。由結果可觀察到NP-MWCNT@GONR在1 A g−1¬¬的循環測試下其第1、2圈的電容量分別為111.4 mAh g−1和82.2 mAh g−1，200圈後之電容量維持率仍有86.5%，並且同時有相當高的能量密度與功率密度表現，在95 W kg−1下能量密度為90.09 Wh kg−1，而30.55 Wh kg−1下功率密度為19 kW kg−1。然而其在200圈後元件即失效，推測是鋅金屬的枝晶生長以及正極鋅沉積對整體系統產生影響，故後續使用黏度較高的膠態電解質系統，以抑制系統中鋅金屬過度生長。
實驗第三部分，我們利用冷凍乾燥法將NP-MWCNT@GONR正極以及鋅金屬負極製成膠態電解質系統元件並進行電化學分析。其有優於液態電解液系統的長程循環穩定性（2000圈後的電容量維持率為67.5%），由臨場穿透式X光顯微鏡分析結果觀察到膠態系統可有效抑制鋅枝晶，因此有效提升循環穩定性。最後將膠態電解質系統進行柔性彎曲、破壞以及自修復特性等測試，仍保有優異之電性表現。本研究顯示膠態電解質系統元件同時具有高電容量、高穩定性、高安全性和高回復性等四大特性，以及應用於可彎曲器件上之潛力與發展性。

Considering the growing demand for versatile electronics, excellent electrochemical performance energy storage devices along with low cost and high safety installation are in urgent need. Currently, lithium and sodium ion hybrid capacitors are considered as one of the very promising energy storage devices with high energy and power density which are benefitted from the combination of batteries and supercapacitors respectively. However, these type of hybrid capacitors are comparatively limited in wearable and flexible device applications because of their safety issues such as flammability and leakage problem. Here, we demonstrate a safe and versatile zinc-ion hybrid supercapacitor (ZHC) based on pristine and chemical-modified multiwalled carbon nanotube as the cathode, zinc trifluoromethanesulfonate as the electrolyte and Zn foil as the anode. The electrochemical performances such cyclic voltammetry (CV), galvanostatic charge/discharge (GCD) cycles, and electrochemical impedance spectroscopy (EIS) are studied by using BioLogic potentiostat VMP3.
We demonstrated three types of active materials for the cathode such as multiwalled carbon nanotube (MWCNT), multiwalled carbon nanotube at graphene oxide nanoribbons (MWCNT@GONR) and nanoporous-core-shell-structured multiwalled carbon nanotube at graphene oxide nanoribbons (NP-MWCNT@GONR). Due to the obvious large surface area of NP-MWCNT@GONR and the hollow framework that enhances the ion adsorption and desorption kinetics, the fabricated device delivered the highest capacity of 111.4 mAh g−1 and 82.2 mAh g−1 at first and second cycles at the current density of 1 A g−1. In addition, NP-MWCNT@GONR exhibited high energy density of 90.09 Wh kg−1 at 95 W kg−1, and high power density of 19 kW kg−1 at 30.55 Wh kg−1. The cyclic retention was 86.5% up to 200 cycles. However, the capacity gradually decreased after 200 cycles. In the zinc-ion hybrid capacitor, the capacity loss is mainly because of the severe zinc dendrite formation along with the deposition of zinc metal on anode.
In order to minimize the zinc dendrite formation, the performance was further analyzed in a gel electrolyte system, which is able to restrain the growth of zinc dendrite at high viscosity of electrolyte. In order to demonstrate the stability of the gel electrolyte, synchrotron radiation analysis was used. Freeze drying method was used after assembling the whole device with the gel electrolyte system. The output performance showed that the ZHC with gel electrolyte exhibited high electrochemical performance. The capacity for the first and second cycles were 85 mA h g−1 and 71.1 mAh g−1 respectively. The cycling retention of the ZIC with gel electrolyte was 86.4% after 200 cycles and 67.5% after 2000 cycles, which was comparatively larger than the ZHC with liquid electrolyte. A series of tests were conducted to check the versatile nature of gel type ZHC devices such as bending, cutting, and self-healing tests. This work provides new insights to develop next generation high performance energy storage devices.

摘要 I
Abstract III
致謝 V
目錄 X
圖目錄 XV
表目錄 XX
第1章 研究目的 1
1.1 研究背景 1
1.2 研究動機 2
第2章 文獻回顧與反應機制 5
2.1 鋅離子混合電容器發展與簡介 5
2.2 鋅離子混合電容器元件的儲電原理 6
2.3 鋅離子混合電容器的正極反應機制 7
2.3.1 電雙層反應 7
2.3.2 擬電容反應 8
2.4 鋅離子混合電容器之電極材料 9
2.4.1 鋅離子混合電容器之正極材料 9
2.4.2 鋅離子混合電容器之負極材料 11
2.5 鋅離子混合電容器之電解液以及電解質 13
2.5.1 液態電解液系統 13
2.5.2 膠態電解質系統 14
第3章 實驗方法 17
3.1 實驗架構 17
3.1.1 材料特性分析 17
3.1.2 液態電解液系統（Liquid electrolyte systems） 17
3.1.3 膠態電解質系統（Gel electrolyte systems） 18
3.2 實驗藥品 19
3.3 活性物質（Active material）合成 20
3.4 材料特性分析 21
3.4.1 場發射掃描式電子顯微鏡（Field Emission Scanning Electron Microscope, FESEM） 21
3.4.2 穿透式電子顯微鏡（Transmission Electron Microscope, TEM） 21
3.4.3 X光繞射儀（X-ray Diffraction, XRD） 22
3.4.4 拉曼光譜分析（Raman） 23
3.4.5 BET比表面積與孔徑分析（Brunauer–Emmett–Teller, BET） 23
3.4.6 X光光電子能譜（X-ray photoelectron spectrometer, XPS） 23
3.5 液態電解液系統（Liquid electrolyte systems） 24
3.5.1 極片製備 24
3.5.2 液態電解液製備 25
3.5.3 鈕扣電池組裝 25
3.6 膠態電解質系統（Gel electrolyte systems） 26
3.6.1 極片製備 26
3.6.2 膠態電解質前驅物合成 27
3.6.3 元件組裝與膠態電解質成形 27
3.6.4 加熱膠態成形法（Heating method） 28
3.6.5 冷凍乾燥法（Freeze drying method） 28
3.7 材料電化學性質量測 29
3.7.1 循環伏安法測試（Cyclic Voltammetry, CV） 29
3.7.2 恆電流充放電測試（Galvanostatic Charge/Discharge Test, GCD） 30
3.7.3 電化學阻抗頻譜分析（Electrochemical Impedance Spectroscopy, EIS） 30
3.8 同步輻射量測用之液態與膠態電解質系統 31
3.8.1 極片製備與元件組裝 31
3.8.2 穿透式X光顯微鏡分析（Transmission X-Ray Microscope, TXM） 31
第4章 結果與討論 33
4.1 多壁奈米碳管及其衍生物之材料分析與鑑定 33
4.1.1 場發射掃描式電子顯微鏡分析 33
4.1.2 穿透式電子顯微鏡 34
4.1.3 X光繞射分析 35
4.1.4 拉曼光譜分析 35
4.1.5 BET比表面積與孔徑分析 36
4.1.6 X光光電子能譜分析 38
4.2 以多壁奈米碳管及其衍生物作為水系鋅離子混合電容器正極於液態電解液系統（Liquid electrolyte systems）之研究 40
4.2.1 循環伏安法分析 40
4.2.2 恆電流充放電測試 45
4.2.3 電容量計算 46
4.2.4 倍率與循環性能（Rate and cycling performance） 47
4.2.5 電化學阻抗頻譜分析 49
4.2.6 Ragone plot分析 54
4.2.7 液態電解液系統長程循環失效原因 55
4.3 以奈米多孔核殼結構多壁奈米碳管/氧化石墨烯奈米帶作為水系鋅離子混合電容器正極於膠態電解質系統（Gel electrolyte systems）之研究 59
4.3.1 電容量計算 59
4.3.2 電化學阻抗頻譜分析 61
4.3.3 Ragone plot分析 62
4.3.4 循環性能 63
4.3.5 膠態電解質系統長程循環優異的原因 63
4.3.6 穿透式X光顯微鏡分析 65
4.3.7 柔性以及破壞測試 72
4.3.8 彎曲狀態下之循環伏安法分析 73
4.3.9 彎曲狀態下之恆電流充放電測試 76
4.3.10 彎曲狀態下之電容量計算 77
4.3.11 彎曲狀態下之循環性能 79
4.3.12 彎曲狀態下之電化學阻抗頻譜分析 80
4.3.13 自修復特性 81
第5章 結論 84
第6章 未來展望 86
本研究相關之發表 87
參考文獻 88

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