本研究主要分為三部分，第一部分為普魯士藍類比物NaxCu[Fe(CN)6]的改質，透過溶液法將普魯士藍類比物中的其中一個氰鍵置換為4-氰基吡啶(C6H4N2)及鄰-甲苯胺(CH3C6H4NH2)官能基，合成改質前對照組NaCu[Fe(CN)6] (簡稱NaCuHCF)及KCu[Fe(CN)6] (簡稱KCuHCF)以及改質後實驗組NaxCu[Fe(CN)5(C6H4N2)] (簡稱NaxCuCNPFe)及NaxCu[Fe(CN)5(CH3C6H4NH2)] (簡稱NaxCuTolFe)並以此作為水系鈉離子電池的正極材料。在此實驗中，我們除了探討官能基對普魯士藍類比物的化學穩定性影響外，亦討論其在不同濃度及不同種類的電解液中(1 M Na2SO4、1 M NaClO4及17 m NaClO4)之電化學性質差異，並透過多種臨場量測驗證其反應機理。第二部分為利用溶膠凝膠法合成鈉離子超離子導體結構材料(Na super ionic conductor material, NASICON) NaTi2(PO4)3@carbon@reduced graphene oxide (NTP@C@RGO)，透過更改不同比例之檸檬酸、不同比例之氧化石墨烯及不同之燒結溫度，以期達到最佳電化學性能並作為水系鈉離子電池之負極材料。第三部分為結合第一、二部分實驗成果，組合成水系鈉離子全電池並測試其電池性質。
在第一部分普魯士藍類比改質物實驗中，首先進行官能基置換化學反應。產物透過掃描式電子顯微鏡、X光繞射光譜儀、拉曼光譜、紫外光-可見光吸收光譜及X光光電子能譜儀進行初步材料鑑定。接著藉由循環伏安法、定電流充放電測試進行電化學特性之研究。改質後之普魯士藍類比物於未經特殊處理的低濃度電解液1 M Na2SO4中，以1 A g−1電流密度下進行2000次充放電循環後，仍有近50%的電容量維持率，相較之下未經官能基改質的普魯士藍類比物之電容量維持率衰退至0%。此結果顯示出此種官能基改質對於提升其穩定性具有良好的作用。本研究亦於國家同步輻射中心進行臨場X光吸收光譜量測及臨場X光繞射圖譜量測，證實四種普魯士藍類比物儲能機制屬於鈉嵌入機制。其鐵元素於充放電過程中經歷Fe2+/Fe3+的可逆價態變化，銅元素則具Cu1+/Cu2+價態變化。
在第二部分，本研究以溶膠凝膠法合成NTP@C@RGO。經製程改善後之NTP@C@RGO負極材料具有良好的電化學性能。於0.025 A g−1電流密度下之電容量高達99 mAh g−1，於10 A g−1電流密度下則約為64 mAh g−1。
在第三部分，本研究結合普魯士藍類比改質物及NTP@C@RGO材料進行全電池應用探討。NaxCuCNPFe//NTP@C@RGO於4338 W kg−1功率密度下之能量密度為18.11 Wh kg−1，NaxCuTolFe//NTP@C@RGO於4742 W kg−1功率密度下之能量密度為11.87 Wh kg−1。此研究結果與其他普魯士藍類比物文獻相比具有更高的功率密度，顯示其在發展高安全性與快速充放電之儲能元件上具有相當大的潛力。

In this study, a Prussian blue analogue (PBA) (NaxCu[Fe(CN)6]) was modified by ligand substitutions (4–pyridinecarbonitrile (C6H4N2) and o-toludine (CH3C6H4NH2)). NaxCu[Fe(CN)5(C6H4N2)] (NaxCuCNPFe) and NaxCu[Fe(CN)5(CH3C6H4NH2)] (NaxCuTolFe) were utilized as cathode materials for aqueous sodium-ion batteries in the first part. The comparison group NaCu[Fe(CN)6] (NaCuHCF) and KCu[Fe(CN)6] (KCuHCF) were also synthesized and tested for comparison. These PBAs were tested in different electrolytes to investigate the influence of the ligand substitutions and electrolytes on electrochemical performances. To grasp a better understanding of the charge-discharge mechanisms of PBA cathodes, in-situ synchrotron experiments were applied. In the second part, NaTi2(PO4)3@carbon@reduced graphene oxide (NTP@C@RGO) was synthesized with a simple sol-gel method as an anode material for aqueous sodium ion batteries. In the third part, the full-cell aqueous sodium ion batteries were assembled and studied with PBAs and NTP@C@RGO as cathode and anode materials, respectively.
First, modified PBAs were characterized with field emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy, UV-Vis adsorption spectroscopy, and X-ray photoelectron spectroscopy. Then the electrochemical performance was tested with three-electrode setup in 1 M Na2SO4, 1 M NaClO4 and 17 m NaClO4 electrolytes. The modified material NaxCuCNPFe and NaxCuTolfe exhibited about 50% capacity retention after 2000 cycles in 1 M Na2SO4 without purging N2 gas or adjusting pH value. In comparison with the non-modified NaCuHCF and KCuHCF, which showed about 0% capacity retention after 2000 cycles, the improvement is significant.
In the second part, a simple sol-gel method was used to synthesize NTP@C@RGO. The amount of citric acid, ratios of NTP@C and graphene oxide, and sintering conditions were optimized. The optimized NTP@C@RGO anode material exhibited a high capacity of 99 mAh g−1 at 0.025 A g−1.
In the third part, the NaxCuCNPFe//NTP@C@RGO and NaxCuTolFe//NTP@C@RGO full cells in 17 m NaClO4 were assembled, and they exhibited high power densties up to 4338 W kg−1 (with an energy density of 18.11 Wh kg−1) and 4742 W kg−1 (with an energy density of 11.87 Wh kg−1), respectively. These results demonstrate that both NaxCuCNPFe and NaxCuTolFe are promising cathode materials for high-safety and high-power aquoues sodium ion batteries.

摘要 i
Abstract iii
致謝 v
目錄 vii
圖目錄 x
表目錄 xiv
第一章 緒論 1
第1.1節 研究背景與動機 1
第二章 文獻回顧與原理介紹 3
第2.1節 電池歷史簡介 3
第2.2節 水系鈉離子電池原理 4
第2.2.1節 層狀氧化物材料 7
第2.2.2節 鈉離子超導體結構氧化物(Na super ionic conductor, NASICON) 8
第2.2.3節 普魯士藍類比物 9
第2.3節 Water-in-salt 現象 12
第2.4節 普魯士藍類比物中的配位化學及π-反向回饋現象 14
第三章 實驗步驟與研究方法 15
第3.1節 實驗架構 15
第3.2節 實驗藥品 18
第3.3節 普魯士藍改質物之合成 19
第3.3.1節 Na3[Fe(CN)5NH3] ·3H2O之合成 19
第3.3.2節 NaxCuCNPFe之合成 20
第3.3.3節 NaxCuTolFe之合成 21
第3.3.1節 KCuHCF及NaCuHCF之合成 21
第3.4節 NTP@C@RGO之合成 23
第3.5節 電化學分析 26
第3.5.1節 循環伏安法 (Cyclic voltammetry, CV) 27
第3.5.2節 恆電流充放電測試 (Galvanostatic charge discharge measurement, GCD) 28
第3.6節 全電池組裝及其量測方法 29
第3.6.1節 極片製備 29
第3.6.2節 鈕扣電池 30
第3.7節 實驗儀器 31
第3.7.1節 電子掃描式顯微鏡 (Scanning Electron Spectroscopy, SEM ) 31
第3.7.2節 X光繞射分析(X-ray Diffraction, XRD) 31
第3.7.3節 拉曼光譜儀 (Raman Spectroscopy) 32
第3.7.4節 X光光電子能譜儀分析 (X-Ray Photoelectron Spectroscopy, XPS) 32
第3.7.5節 X光吸收能譜 (X-Ray Adsorption Spectroscopy, XAS) 33
第3.7.6節 紫外光可見光光譜光譜儀 (UV-Vis Spectroscopy) 34
第3.7.7節 恆電位儀 BioLogic potentiostat VMP3 34
第3.7.8節 臨場X光吸收光譜量測 35
第四章 結果與討論 37
第4.1節 以普魯士藍類比物及普魯士藍類比改質物作為鈉離子電池正極材料之研究 37
第4.1.1節 普魯士藍改質物材料性質分析 38
第4.1.2節 普魯士藍類比物臨場電化學量測 55
第4.2節 NTP@C@RGO負極材料分析 64
第4.2.1節 NTP@C@RGO參數比例調整 64
第4.2.2節 拉曼圖譜分析 70
第4.3節 以普魯士藍類比改質物正極材料與NTP@C@RGO負極材料應用於水系鈉離子全電池研究 72
第五章 結論 78
第六章 未來展望 80
本研究相關發表 81
參考文獻 82

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