電容去離子系統是一項新穎且可替代傳統海水淡化的技術，是利用多孔性碳材超級電容器於水相電解液中有著電雙層特性，使其具有可逆性吸、脫附離子之能力。
參考電極可測量電極操作電壓，三極式電化學系統常見的銀/氯化銀鹽橋式參考電極並不適合應用在電容去離子的系統中，由於半鹹水的鹽類濃度稀薄，鹽橋中的離子會干擾離子去除量測。銀氯化物電極會與Cl -，Br -，I - 和CN- 產生反應。第一部分研究主要開發鈀氫化物參考電極並做電容去離子系統之電化學分析應用，故本研究使用以 -0.2 V (vs. Ag/AgCl)進行15分鐘陰極極化的鈀氫化物可替代銀/氯化銀鹽橋式參考電極，研究結果驗證出此參考電極可避免產生離子釋出和電極氧化而影響去離子效果評估，同時可測量離子在不同電壓操作的吸、脫附情形長達4小時的穩定。
第二部分主要探討電極材料的表面特性對電容去離子和逆向電容去離子系統之去除離子效能之影響。本研究藉由微波水熱法將氧化石墨烯混摻奈米碳管等進行改質，進而改變其表面官能基含量與活性碳作比較，並以電容去離子系統探討在8 mM NaCl水溶液中的離子吸附、脫附行為，並以電量平衡概念，透過不同電容器組裝找出最佳去離子效果之操作與組裝方式。證明透過鈀氫化物參考電極輔助於適當組裝和電位操作，以氧化石墨烯混摻奈米碳管與活性碳為非對稱式電容器，去離子效能提升至21.33 mg g-1；經部分還原再和活性碳組裝非對稱式電容器，具有最佳逆向電容去離子效能可達25.2 mg g-1。

This Thesis mainly focuses on the capacitive deionization (CDI) studies, which is an alternative and new technology for desalination process. The process utilizes the formation of electric double layer capacitance (EDLC) at the interfaces of porous carbon electrodes which can reversibly adsorb or desorb the salt ions from aqueous solution.
The reference electrode plays an important role in the CDI system. It can be used to understand the relationship between adsorption/ desorption of ions and working potential of various electrode materials by analyzing their electrochemical behavior. However, for the brackish water, it is not suitable to use the Ag/AgCl electrode as the reference electrode in the CDI system due to the extra release of ions from the salt bridge which can interfere the measurement of salt concentration. Furthermore, AgClx electrode can react with anions such as Cl-, Br-, I-, and CN-, thus, it is difficult to apply it in the CDI system.
The first part was developing β-PdHx as an alternate reference electrode for the CDI system. β-PdHx was fabricated by cathodic polarization at -0.2 V (vs. Ag/AgCl) for 15 min and was used as the reference electrode. The results confirmed that β-PdHx not only can avoid the interference of extra ions releasing from the silver electrode or ion exchange salt bridge, and also can operate stably for the electrochemical analysis of salt ions and electrode materials. Therefore, we can find one of the best CDI assembly and operation by using β-PdHx reference electrode.
The second part was investigation of the effects of surface properties of electrode materials on the deionization performance in the capacitive deionization and the invert capacitive deionization system. In this study, we use graphene oxide/carbon nanotubes composite (GO+CNT) which were modified by microwave hydrothermal in order to obtain the electrode materials with different content of oxidative functional group and compared with activated carbon for CDI studies. Sodium chloride (8 mM) was used as target solution for CDI treatment to find the relationship between the various electrode materials and adsorption/desorption of salt ions by using electrochemical analysis. Using β-PdHx reference electrode for CDI system, when the GO+CNT combined with activated carbon as asymmetric capacitors, the deionization efficiency was increased to 21.33 mg g-1. However, when the rGO+CNT and AC assembled asymmetric capacitors, it was found that the best invert capacitance deionization efficiency was 25.20 mg g-1.

中文摘要 I
Abstract II
誌謝 V
目錄 VII
圖目錄 XI
表目錄 XVI
第一章 緒論及理論基礎 1
1-1 電化學原理 1
1-1-1 電化學反應系統 1
1-1-2 參考電極的種類與應用 3
1-1-3 影響電化學系統之因素 7
1-2 電化學電容器 9
1-2-1 超級電容器之簡介與應用 9
1-2-2 超級電容器之儲能機制與分類 11
1-3 電容去離子技術基礎與應用 13
1-3-1 電容去離子與傳統的去離子技術比較 13
1-3-2 電容去離子技術和原理 15
1-3-3 電容去離子電極材料與特性 16
1-3-4 去離子系統的發展與參考電極的應用 20
1-3-5 逆向電容去離子技術 23
1-3-6 電容去離子效能基準 27
1-4 研究動機 29
第二章 實驗方法與儀器介紹 31
2-1 實驗藥品與儀器介紹 31
2-1-1 實驗藥品 31
2-1-2 實驗儀器 32
2-1-3 實驗流程 33
2-2 電極與電極材料製備 34
2-2-1 金屬鈦片基材之製備與處理 34
2-2-2 氧化石墨烯溶液之配製 34
2-2-3 以微波輔助水熱法合成還原氧化石墨烯 36
2-2-4 去離子系統工作電極之製備 36
2-3 電化學實驗 37
2-3-1 電容去離子系統裝置 37
2-3-2 循環伏安法 (Cyclic voltammetry, CV) 38
2-3-3 安培分析法 (Amperometry, i-t curve) 38
2-3-4 計時電位分析法 (Chronopotentiometry, CP) 39
2-3-5 開環路電壓測試 (Open Circuit Potential, OCP) 40
2-3-6 交流阻抗分析法 (A.C. Impedance, EIS) 40
2-4 製作電容去離子系統之參考電極 42
2-4-1 鈀氫化物參考電極的製作 42
2-4-2 銀氯化物參考電極的製作 42
2-5 材料分析儀器介紹 43
2-5-1 X光繞射分析 (X-ray Diffraction analysis, XRD) 43
2-5-2 掃描式電子顯微鏡 (Scan electron microscope, SEM) 45
2-5-3 電子能譜儀 46
2-5-4 拉曼光譜儀 46
2-5-5 比表面積與孔徑分析儀 (Surface area and porosity analyzer) 48
第三章 開發鈀氫化物參考電極應用於電容去離子系統 51
3-1 參考電極於電容去離子系統中的應用 52
3-2 氫原子於鈀絲上吸附電位特性探討 54
3-2-1 氫原子吸附反應之電位於循環伏安法特徵峰探討 54
3-2-2 氫原子吸附反應之不同下限電位的比較 55
3-2-3 不同陰極極化時間對氫原子吸附反應之影響 57
3-2-4 製作鈀氫化物參考電極並探討其穩定性 58
3-3 鈀氫化物參考電極應用於電容去離子系統 61
3-4 鈀氫化物參考電極應用於活性碳電容去離子系統 64
3-4-1 鈀氫化物參考電極對活性碳電化學分析 64
3-4-2 鈀氫化物參考電極對活性碳去離子效能分析 66
3-5 結論 70
第四章 電容去離子與逆向電容去離子之討論 71
4-1 氧化石墨烯作為電極之合成與材料分析 71
4-1-1 以X光繞射分析探討氧化石墨烯及其還原 72
4-1-2 以X 射線光電子能譜儀分析氧化石墨烯及其還原 73
4-1-3 以拉曼光譜儀分析電極材料特性 75
4-1-4 以掃描式電子顯微鏡分析電極材料特性 76
4-1-5 碳材料之氮氣吸脫附曲線表面積與孔洞分析 78
4-2 以電化學方法探討電極材料與材料表面官能基之關係 82
4-2-1 以循環伏安法探討兩電極於電容去離子系統中操作電位範圍 83
4-2-2 以循環伏安法和交流阻抗分析法探討兩電極材料零和電位 86
4-2-3 不同含氧官能基石墨烯混摻奈米碳管之電極材料在電容去離子系統特性比較 88
4-3 多孔性碳材料電容去離子系統之組裝 90
4-3-1 比較多孔性碳材料之組裝應用於電容去離子系統 90
4-3-2 正逆向電容去離子系統之離子移動情況討論 96
4-4 結論 98
第五章 總結與未來展望 99
5-1 總結 99
5-2 未來展望 100
參考文獻 101

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