電容去離子(Capacitive Deionization, CDI)是深具潛力的低能耗脫鹽技術，透過在兩個電極之間施加電壓從水溶液中去除離子。當溶液中存在多種離子時，CDI系統對每種離子的去除率不同，即CDI系統對離子之電吸附選擇性不同。本研究，利用三種電極材料：粒狀活性碳(GAC)、石墨烯/粒狀活性碳(rGO/GAC)和聚苯胺/粒狀活性碳(PANI/GAC)應用於CDI系統中，探討四種環境中常見陰離子(Cl-、NO3-、SO42-、H2PO4-)之電吸附情形。
研究發現離子價數顯著影響電吸附選擇性，離子價數越高，離子被CDI系統電吸附效果越好。在具有相同離子價的離子混合時，則是以水合比(hydration ratio即水合半徑與離子半徑的比)顯著影響電吸附選擇性，低水合比的離子表現出較高的電吸附選擇性，但研究中也發現磷酸不符合上述的規則。此外，初始濃度較高之離子，在電吸附初期，離子被電吸附的效率較高。
比較三種電極材料應用於CDI系統去除四種陰離子之吸附當量時，吸附當量由高至低的順序為SO42- > NO3- > Cl- > H2PO4-，符合離子價數高者電吸附效果較好(二價優於一價)，且水合比低者電吸附效果較好(水合比NO3- : 1.87、Cl- :1.99 )，但H2PO4-並不符合水合比原則，且在三種電極材料系統中電吸附表現皆為最差。
PANI/GAC複合材料，提高原GAC的比電容值(96.33 F/g)，且將中孔比率提升至91.74%，組成非對稱電容去離子系統後，針對SO42-和Cl-有較優異的電吸附表現，但對NO3-和H2PO4-去除效果不好，表示PANI/GAC複合材料對不同陰離子之電吸附選擇性。

Capacitive deionization (CDI) is an emerging low-energy desalination technology that removes ions from aqueous solutions by applying a voltage between two electrodes. When there are multiple ions in the solution, the removal efficiency of each ion by the CDI system is different, that is, the electrosorption selectivity of the CDI system for ions is different. In this study, three electrode materials employed: granular activated carbon (GAC), graphene/granular activated carbon (rGO/GAC) and polyaniline/granular activated carbon (PANI/GAC) were applied to CDI systems to explore the electrosorption of common anions (such as Cl-, NO3-, SO42-, H2PO4-) in the environment.
This study found that the ionic valence significantly affects the electrosorption selectivity. The higher the ionic valence, the better the ion electrosorption effect of the CDI system. When ions with the same ionic valence are mixed, the hydration ratio has significant impact on the electrosorption selectivity. Ions with low hydration ratios exhibit a higher electrosorption selectivity, but our study also found that phosphoric acid does not meet the above mentioned rules. In addition, the higher the initial concentration of ions, the higher the removal efficiency of the ion in the early stage of electrosorption.
In comparison of three electrode materials employed in CDI systems to remove four anions, the order of electrosorption equivalent from high to low is SO42- > NO3- > Cl- > H2PO4-. Divalent ion has better performance than that of monovalent ion, and those with lower hydration ratio have better electrosorption effect (hydration ratio NO3-: 1.87, Cl-: 1.99). However, H2PO4- does not agree with the principle of hydration ratio, and the electrosorption performance of H2PO4- is the worst among four anions.
Addition of PANI to GAC can improve the specific capacitance of the original GAC (96.33 F/g), and increase the mesopore ratio to 91.74%. An asymmetric PANI/GAC//GAC CDI system showed that it had excellent electrosorption performance for SO42- and Cl, but the removal efficiency of NO3- and H2PO4- was not good, indicating the electrosorption selectivity of PANI/GAC composites to different anions.

目錄
第一章	緒論	1
1.1	研究緣起	1
1.2	研究目的	2
第二章	文獻回顧	3
2.1	電容去離子技術	3
2.2	電極材料之特性	5
2.2.1	活性碳	6
2.2.2	石墨烯	7
2.2.3	導電性高分子	8
2.3	電容去離子的選擇性吸附	11
第三章	研究材料與方法	12
3.1	實驗架構	12
3.2	實驗藥品與設備	14
3.2.1	實驗藥品	14
3.2.2	實驗設備	16
3.3	電極材料製備	17
3.3.1	粒狀活性碳(Granular activated carbon, GAC)之製備	17
3.3.2	氧化石墨烯(Graphene oxide, GO)之製作	17
3.3.3	石墨烯 (Reduced Graphene Oxide, rGO)之製備	18
3.3.4	聚苯胺(Polyaniline, PANI)之製作	18
3.3.5	聚苯胺/活性碳複合材料(PANI/GAC)之製備	18
3.4	電容去離子系統電極製備	19
3.4.1	粒狀活性碳電極	19
3.4.2	石墨烯/活性碳複合電極	19
3.4.3	聚苯胺/活性碳複合電極	19
3.5	實驗分析方法	20
3.5.1	X射線繞射分析(X-ray Diffraction, XRD)	20
3.5.2	掃描式電子顯微鏡分析(Scanning Electron Microscope , SEM)	20
3.5.3	表面積及孔徑分析(BET)	20
3.5.4	接觸角測定 (Contact Angle, CA)	20
3.5.5	循環伏安法(Cyclic Voltammetry, CV)	21
3.5.6	電化學阻抗譜分析(Electrochemical impedance spectroscopy, EIS)	22
3.5.7	離子層析儀(Ion Chromatograph, IC)	22
3.6	電容去離子實驗(Capacitive deionization Experiment, CDI)	23
3.6.1	非對稱電容去離子系統(Asymmetric CDI system)	24
第四章	結果與討論	27
4.1	粒狀活性碳應用於電容去離子	27
4.1.1	粒狀活性碳表面特性分析	27
4.1.2	粒狀活性碳電化學特性分析	32
4.1.3	粒狀活性碳對單一陰離子的電吸附能力	37
4.1.4	粒狀活性碳對雙陰離子的選擇性	42
4.1.5	pH變化對粒狀活性碳對磷酸根的電吸附影響	49
4.1.6	粒狀活性碳對混合溶液的選擇性電吸附	53
4.2	石墨烯/粒狀活性碳(rGO/GAC)複合材料應用於電容去離子	58
4.2.1	石墨烯/粒狀活性碳(rGO/GAC)複合材料表面特性分析	58
4.2.2	石墨烯/粒狀活性碳(rGO/GAC)複合材料電化學特性分析	66
4.2.3	石墨烯/粒狀活性碳(rGO/GAC)複合材料對單一陰離子的電吸附能力	71
4.2.1	石墨烯/粒狀活性碳(rGO/GAC)複合材料對雙陰離子的選擇性	75
4.2.2	石墨烯/粒狀活性碳(rGO/GAC)複合材料對混合溶液的選擇性電吸附	80
4.3	聚苯胺/粒狀活性碳(PANI/GAC)複合材料應用於電容去離子	83
4.3.1	聚苯胺/粒狀活性碳(PANI/GAC)複合材料表面特性分析	83
4.3.2	聚苯胺/粒狀活性碳(PANI/GAC)複合材料電化學特性分析	88
4.3.3	聚苯胺/粒狀活性碳(PANI/GAC)複合材料對單一陰離子電吸附能力	93
4.3.4	聚苯胺/粒狀活性碳(PANI/GAC)複合材料對雙離子選擇性	97
4.3.5	聚苯胺/粒狀活性碳(PANI/GAC)複合材料對混合溶液的選擇性電吸附	102
4.4	綜合比較GAC、10% rGO/GAC與PANI/GAC 電極材料應用於CDI系統	105
4.4.1	比表面積與孔徑分佈比較	105
4.4.2	電化學性能比較	106
4.4.3	單一離子的電吸附能力比較	108
第五章	結論與建議	111

List of Figure
Figure 2.1.1 Principle of capacitive deionization	4
Figure 2.2.3.1 Chemical structures of PANI (a) generalized composition of PANI indicating the reduced and oxidized repeat units, (b) completely reduced polymer, (c) Half-oxidized polymer, and (d) fully oxidized polymer (MacDiarmid and Epstein 1994).	9
Figure 2.2.3.2 Scheme of proton doping in PANI (MacDiarmid and Epstein 1995).	10
Figure 1.1.1 Schematic experimental structure for CDI system.  13
Figure 3.6.1.1 The components of CDI system.	26
Figure 3.6.1.2 The schematic diagram of CDI batch-mode experiments.	26
Figure 4.1.1.1 SEM images of the granular activated carbon. (a) x2,000, (b) x10,000, (c) x30,000 and (d) x100,000.	29
Figure 4.1.1.2 Nitrogen adsorption(●)-desorption(○) isotherms of the granular activated carbon (GAC).	30
Figure 4.1.1.3 Pore size distribution of the granular activated carbon (GAC).	30
Figure 4.1.1.4 Contact angles of the granular activated carbon (GAC) (a) without (b) with 1 M KOH treatment.	31
Figure 4.1.2.1 Cyclic voltammograms of the granular activated carbon electrode in 1 M NaCl.	34
Figure 4.1.2.2 Specific capacitance (F/g) at different scan rates of the granular activated carbon electrode in 1 M NaCl.	34
Figure 4.1.2.3 The electrochemical impedance spectra (EIS) measured at frequency range of 1 Hz to 100 kHz of the granular activated carbon in 1 M NaCl.	35
Figure 4.1.3.1 Variation of different anions concentrations as a function of time using the granular activated carbon electrodes applied to CDI systems. Nitrate (●) has the highest removal efficiency, followed by chloride (○), sulfate (■) and phosphate (▲). Initial Cl- concentration = 1.77 mM; Initial NO3- concentration = 2.11 mM; Initial SO42- concentration = 2.17 mM; Initial H2PO4- concentration = 1.96 mM	39
Figure 4.1.3.2 Removal efficiency for individual anion using GAC electrodes within three cycles. Nitrate (●) has the highest removal efficiency, followed by chloride (○), sulfate (■) and phosphate (▲).	40
Figure 4.1.3.3 Variation of different anions concentrations as a function of time using the granular activated carbon electrodes applied to CDI systems. Nitrate (●) has the highest removal efficiency, followed by chloride (○), sulfate (■) and phosphate (▲). Initial Cl- concentration = 1.77 mM; Initial NO3- concentration = 2.11 mM; Initial SO42- concentration = 2.17 mM; Initial H2PO4- concentration = 1.96 mM.	40
Figure 4.1.4.1 Variation of Cl- (○) and NO3- (●) concentrations as a function of time using GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.07 mM; Initial NO3- concentration = 0.97 mM ; pH = 7.42.	45
Figure 4.1.4.2 Electrosorption limit of Cl- (○) and NO3- (●) concentrations as a function of time using GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.08 mM; Initial NO3- concentration = 1.00 mM ; pH = 7.45.	46
Figure 4.1.4.3 Variation of Cl- (○) and SO42- (■) concentrations as a function of time using GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.01 mM; Initial SO42- concentration = 1.01 mM.	47
Figure 4.1.4.4 Variation of Cl- (○) and H2PO4- (▲) concentrations as a function of time using the granular activated carbon electrodes applied to CDI systems. Initial Cl- concentration = 0.98 mM, Initial H2PO4- concentration = 0.99 mM, pH = 6.	48
Figure 4.1.5.1 Phosphoric acid species distribution.	50
Figure 4.1.5.2 Variation of different phosphate species concentrations as a function of time using GAC electrodes applied to CDI systems. H2PO4- (▲), HPO42- (△), and PO43- (◆).	51
Figure 4.1.6.1 Variation of 2 mM mixed anions concentrations as a function of time using GAC electrodes applied to CDI systems. Nitrate (●) has the highest removal efficiency, followed by sulfate (■), chloride (○) and phosphate (▲). Initial Cl- concentration = 0.56 mM; Initial NO3- concentration = 0.52 mM; Initial SO42- concentration = 0.52 mM; Initial H2PO4- concentration = 0.54 mM; pH = 6.5.	54
Figure 4.1.6.2 Variation of 2.5 mM mixed anions concentrations as a function of time using GAC electrodes applied to CDI systems. Nitrate (●) has the highest removal efficiency, followed by chloride (○), sulfate (■) and phosphate (▲). Initial Cl- concentration = 1.09 mM; Initial NO3- concentration = 0.52 mM; Initial SO42- concentration = 0.52 mM; Initial H2PO4- concentration = 0.51 mM; pH = 7.1.	56
Figure 4.2.1.1 XRD images of (a) GO and (b) rGO.	60
Figure 4.2.1.2 SEM images of rGO with magnification of (a) x500, (b) x3,000, (c) x10,000, (d) x30,000 and 10% rGO/GAC with magnification of (e) x5,000, (f) x 10,000, (g) x 30,000, and (h) x 50,000.	61
Figure 4.2.1.3 Nitrogen adsorption(●)-desorption(○) isotherms of (a) rGO and (b) 10% rGO/GAC.	63
Figure 4.2.1.4 Pore size distribution of (a) rGO and (b) comparison of 10% rGO/GAC(●) and GAC (○).	64
Figure 4.2.1.5 Figure 4.1.5 Contact angles of rGO (a) without (b) with 1 M KOH treatment and 10% rGO/GAC (c) without (d) with 1 M KOH treatment.	65
Figure 4.2.2.1 Cyclic voltammograms of (a) rGO and (b) 10% rGO/GAC in 1 M NaCl with various scan rates.	67
Figure 4.2.2.2 Cyclic voltammograms of three electrode materials in 1 M NaCl at scan rate of 1 mV/s, potential range -0.4 to 0.6 V.	68
Figure 4.2.2.3 Specific capacitance (F/g) of GAC (○), rGO (■) and 10% rGO/GAC (●) in 1 M NaCl at different scan rates.	68
Figure 4.2.2.4 The electrochemical impedance spectra (EIS) of rGO (○) and 10% rGO/GAC (●) in 1 M NaCl measured at frequency range of 1 Hz to 100 kHz.	69
Figure 4.2.3.1 Variation of different anions concentrations as a function of time using 10% rGO/GAC electrodes applied to CDI systems in individual anion solution. Chloride (○) has the highest removal efficiency, followed by nitrate (●), sulfate (■) and phosphate (▲). Initial Cl- concentration = 2.03 mM, initial NO3- concentration = 2.16 mM, initial SO42- concentration = 2.05 mM, initial H2PO4- concentration = 1.98 mM.	72
Figure 4.2.3.2 Removal efficiency for individual anion using 10% rGO/GAC electrodes within three cycles. Chloride (○) has the highest removal efficiency, followed by nitrate (●), sulfate (■) and phosphate (▲).	73
Figure 4.2.4.1 Variation of Cl- (○) and NO3- (●) concentrations as a function of time using rGO/GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.06 mM; Initial NO3- concentration = 1.02 mM.	77
Figure 4.2.4.2 Variation of Cl- (○) and SO42- (■) concentrations as a function of time using rGO/GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.05 mM; Initial SO42- concentration = 1.01 mM.	78
Figure 4.2.4.3 Variation of Cl- (○) and H2PO4- (▲) concentrations as a function of time using rGO/GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.06 mM, Initial H2PO4- concentration = 1.14 mM, pH = 6.	79
Figure 4.2.5.1 Variation of 2 mM mixed anions concentrations as a function of time using rGO/GAC electrodes applied to CDI systems. Nitrate (●) has the highest removal efficiency, followed by sulfate (■), chloride (○) and phosphate (▲). Initial Cl- concentration = 0.70 mM; Initial NO3- concentration = 0.52 mM; Initial SO42- concentration = 0.54 mM; Initial H2PO4- concentration = 0.64 mM.	81
Figure 4.3.1.1 SEM images of the polyaniline/granular activated carbon (PANI/GAC) composite with magnification of (a) x1,000, (b) x5,000, (c) and (d) x15,000.	84
Figure 4.3.1.2 Nitrogen adsorption (●) - desorption (○) isotherms of the polyaniline/ granular activated carbon (PANI/GAC) composite.	85
Figure 4.3.1.3 Pore size distribution of (a) the polyaniline/granular activated carbon (PANI/GAC) (●) composite and (b) comparison with original GAC (○).	86
Figure 4.3.1.4 Contact angles of the polyaniline/granular activated carbon (PANI/GAC) composite.	87
Figure 4.3.2.1 Cyclic voltammograms of the polyaniline/granular activated carbon (PANI/GAC) electrode in 1 M NaCl.	89
Figure 4.3.2.2 Cyclic voltammograms of PANI electrode in 1 M NaCl.	89
Figure 4.3.2.3 Cyclic voltammograms of three electrode materials in 1 M NaCl at scan rate of 1 mV/s, potential range -0.4 to 0.6 V.	90
Figure 4.3.2.4 Cyclic voltammograms of three electrode materials in 1 M NaCl at scan rate of 1 mV/s, potential range 0.4 to 0.5 V.	90
Figure 4.3.2.5 The electrochemical impedance spectra (EIS) measured at frequency range of 1 Hz to 100 kHz of the polyaniline/granular activated carbon (PANI/GAC) in 1 M NaCl.	91
Figure 4.3.3.1 Variation of different anions concentrations as a function of time using PANI/GAC applied to CDI systems. sulfate (■) has the highest removal efficiency, followed by chloride (○), Nitrate (●) and phosphate (▲). Initial Cl- concentration = 2.13 mM, initial NO3- concentration = 2.10 mM, initial SO42- concentration = 2.04 mM, initial H2PO4- concentration = 2.10 mM.	95
Figure 4.3.3.2 Variation of different anions concentrations as a function of time using PANI/GAC applied to CDI systems. sulfate (■) has the highest removal efficiency, followed by chloride (○), Nitrate (●) and phosphate (▲). Initial Cl- concentration = 2.13 mM, initial NO3- concentration = 2.10 mM, initial SO42- concentration = 2.04 mM, initial H2PO4- concentration = 2.10 mM.	95
Figure 4.3.4.1 Variation of Cl- (○) and NO3- (●) concentrations as a function of time using PANI/GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.16 mM; Initial NO3- concentration = 1.06 mM.	99
Figure 4.3.4.2 Variation of Cl- (○) and SO42- (■) concentrations as a function of time using PANI/GAC electrodes applied to CDI systems. Initial Cl- concentration = 1.06 mM; Initial SO42- concentration = 1.01 mM.	100
Figure 4.3.4.3 Variation of Cl- (○) and H2PO4- (▲) concentrations as a function of time using PANI/GACelectrodes applied to CDI systems. Initial Cl- concentration = 1.1 mM, Initial H2PO4- concentration = 0.98 mM.	101
Figure 4.3.5.1 Variation of 2 mM mixed anions concentrations as a function of time using PANI/GAC electrodes applied to CDI systems. Sulfate (■) has the highest removal efficiency, followed by nitrate (●), chloride (○) and phosphate (▲). Initial Cl- concentration = 0.64 mM, initial NO3- concentration = 0.56 mM, initial SO42- concentration = 0.55 mM, initial H2PO4- concentration = 0.74 mM, pH = 6.7.	103
Figure 4.4.2.1 The electrochemical impedance spectra (EIS) of electrode materials in 1 M NaCl measured at frequency range of 1 Hz to 100 kHz. GAC (○), 10% rGO/GAC (●) and PANI/GAC (▲).	107
Figure 4.4.3.1 Variation of different anions concentrations as a function of time using different electrode material (GAC (○), 10% rGO/GAC (●) and PANI/GAC (▲)) applied to CDI systems in individual (a) Cl-, (b) NO3-, (c) SO42-, and (d) H2PO4- solution.	109
Figure 4.4.3.2 Electrosorption capacity of different anions concentrations as a function using different electrode material.	110
 
List of Table
Table 3.2.1.1 Manufactures and purity of experimental chemicals.	14
Table 3.2.2.1 Manufacturers and models of equipment.	16
Table 4.1.1.1 Porosity characteristics of the granular activated carbon electrode (GAC).	29
Table 4.1.2.1 Specific capacitance at different scan rate of the granular activated carbon in 1 M NaCl.	35
Table 4.1.2.2 Impedance analyses of GAC in 1 M NaCl based on equivalent circuit model.	36
Table 4.1.3.1 Removal efficiency and electrosorption capacity of different anions using GAC electrodes for each cycle.	41
Table 4.1.4.1 Ionic properties of anions explored in this study (Pauling 1960, Montastruc et al. 2003, Kiriukhin and Collins 2002, Nightingale Jr 1959).	44
Table 4.1.4.2 Removal efficiency and electrosorption capacity of Cl- and NO3- in the Cl- and NO3- mixture using GAC electrodes applied to CDI systems.	45
Table 4.1.4.3 Removal efficiency limit and electrosorption capacity limit of Cl- and NO3- in the Cl- and NO3- mixture using GAC electrodes applied to CDI systems.	46
Table 4.1.4.4 Removal efficiency and electrosorption capacity of Cl- and SO42- in the Cl- and SO42- mixture using GAC electrodes applied to CDI systems.	47
Table 4.1.4.5 Removal efficiency and electrosorption capacity of Cl- and H2PO4- in the mixture of Cl- and H2PO4- using GAC electrodes applied to CDI systems.	48
Table 4.1.5.1 Removal efficiency and electrosorption capacity of different phosphate species using GAC electrodes for each cycle.	52
Table 4.1.6.1 Removal efficiency and electrosorption capacity of 2 mM mixed anions using GAC electrodes for each cycle.	55
Table 4.1.6.2 Removal efficiency and electrosorption capacity of 2.5 mM mixed anions using GAC electrodes for each cycle.	57
Table 4.2.1.1 Porosity characteristics of the granular activated carbon (GAC), graphene (rGO) and 10% rGO/GAC.	62
Table 4.2.2.1 Specific capacitance (F/g) of electrode materials in 1 M NaCl at different scan rates.	69
Table 4.2.2.2 Comparison of impedance of three electrode materials 1 M NaCl based on equivalent circuit model.	70
Table 4.2.3.1 Removal efficiency and electrosorption capacity of different anions using 10% rGO/GAC electrodes in individual anion solution for each cycle.	74
Table 4.2.4.1 Removal efficiency and electrosorption capacity of Cl- and NO3- in the Cl- and NO3- mixture using rGO/GAC electrodes applied to CDI systems.	77
Table 4.2.4.2 Removal efficiency and electrosorption capacity of Cl- and SO42- in the Cl- and SO42- mixture using rGO/GAC electrodes applied to CDI systems.	78
Table 4.2.4.3 Removal efficiency and electrosorption capacity of Cl- and H2PO4- in the mixture of Cl- and H2PO4- using rGO/GAC electrodes applied to CDI systems.	79
Table 4.2.5.1 Removal efficiency and electrosorption capacity of 2 mM mixed anions using rGO/GAC electrodes for each cycle.	82
Table 4.3.1.1 Porosity characteristics of the polyaniline/granular activated carbon (PANI/GAC) composite.	84
Table 4.3.2.1 Specific capacitance at different scan rate of the polyaniline- granular activated carbon in 1 M NaCl.	91
Table 4.3.2.2 Comparison of impedance of GAC and PANI/GAC in 1 M NaCl based on equivalent circuit model.	92
Table 4.3.3.1 Removal efficiency and electrosorption capacity of different anions using PANI/GAC electrodes for each cycle.	96
Table 4.3.4.1 Removal efficiency and electrosorption capacity of Cl- and NO3- in the Cl- and NO3- mixture using PANI/GAC electrodes applied to CDI systems.	99
Table 4.3.4.2 Removal efficiency and electrosorption capacity of Cl- and SO42- in the Cl- and SO42- mixture using PANI/GAC electrodes applied to CDI systems.	100
Table 4.3.4.3 Removal efficiency and electrosorption capacity of Cl- and H2PO4- in the mixture of Cl- and H2PO4- using PANI/GAC electrodes applied to CDI systems.	101
Table 4.3.5.1 Removal efficiency and electrosorption capacity of 2 mM mixed anions using PANI/GAC electrodes for each cycle.	104
Table 4.4.1.1 Porosity characteristics of Electrode materials.	105
Table 4.4.2.1 Comparison of impedance of three electrode materials in 1 M NaCl based on equivalent circuit model.	107
Table 4.4.3.1 Electrosorption capacity per pore volume (µN/cm3) of different anions using different electrode materials.	110

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