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Title Page

Abstract

Contents

Chapter 1. Introduction 14

1.1. Background and objective 14

1.2. Contents of each chapter 16

Chapter 2. Literature review 17

2.1. Seawater battery desalination 17

2.2. Membrane fouling by organic matter 18

2.3. Na metal electrode-based hybrid redox flow battery desalination 18

2.4. Response surface methodology 19

Chapter 3. Influence of organic matter on seawater battery desalination performance 20

Abstract 20

3.1. Introduction 20

3.2. Materials and methods 22

3.2.1. Experimental preparation 22

3.2.2. Cycle charging experiment 24

3.2.3. Fouling analysis of NASICON 26

3.2.4. Long-term charging experiment 27

3.2.5. Fouling analysis of AEM 28

3.3. Results and discussion 28

3.3.1. Cycle charging experiment 28

3.3.2. Fouling analysis on the NASICON membrane 32

3.3.3. Long-term charging experiment 35

3.3.4. Fouling analysis on the AEM in the long-term charging experiment 37

3.4. Conclusions 39

3.5. Supplementary information 40

Chapter 4. Optimization of a Redox Flow Battery desalination System: Experiment and modeling 47

Abstract 47

4.1. Introduction 47

4.2. Materials and methods 50

4.2.1. Experiment 50

4.2.2. RSM analysis of NRFDB-D experiment 53

4.3. Results and discussion 54

4.3.1. Experimental study on influencing factors 54

4.3.2. Specific energy consumption analysis 58

4.3.3. RSM analysis of the NRFDB-D system 62

4.4. Conclusion 69

4.5. Supplementary information 70

Chapter 5. Concluding remarks 72

References 74

List of Tables

Table 3.1. Information of the four types of artificial seawater. 24

Table 4.1. ANOVA table for the SEC₁ ; The input variables were the NaHCF concentration and the feed concentration. 63

Table 4.2. ANOVA table for the SEC₁ ; The input variables were the NaHCF concentration and the Salt removal rate. 64

Table 4.3. Optimized conditions and performance parameters of the NRFDB-D system, which aimed to optimize SEC by each feed concentration. SEC of the NRFDB-D system was compared with the... 67

Table 4.4. Optimized conditions and performance parameters of the NRFDB-D system, which aimed to optimize SEC by each salt removal rate. SEC of the NRFDB-D system was compared with the RO... 68

List of Supplementary Information Tables

Table 3.S1. Electrical conductivity of four types of artificial seawater before and after the cycle charging experiment. Note that EC is an acronym of electrical conductivity, and TDS is an acronym of... 40

Table 3.S2. Recorded voltage depending on the applied current before starting a charging cycle during the cycle charging experiment. The calculated electrical resistances of the SWB-D system are shown... 40

Table 3.S3. Estimation of the current efficiency of the SWB-D system in the absence of organic matter. Note that the square bracket, [], means that the inserted value is not a measured value but a value... 41

Table 3.S4. Energy consumptions of the SWB-D system at the third charging cycle. We assumed that the energy recovery rate was 80% regardless of fouling. 42

Table 4.S1. Current conditions for the SWB-D and the NRFDB-D systems converted into two current units 71

List of Figures

Fig.3.1. Illustrations of (a) SWB-D system and (b) SWB coin cell structure 23

Fig.3.2. Schematic of a batch SWB-D system. This SWB-D system includes two types of experimental setups for cycle charging and long-term charging experiments. The long-term charging... 25

Fig.3.3. Voltage profiles and charging capacity over three charging cycles when the desalination compartment was filled (a) with seawater, or with seawater containing (b) humic acid, (c) sodium... 29

Fig.3.4. Salt removal rate and charging capacity after each charging cycle when the desalination compartment was filled (a) with seawater, or with seawater containing (b) humic acid, (c) sodium... 31

Fig.3.5. Electrical resistance of the SWB-D system measured before the cycle charging experiment under the condition of (a) seawater only, and seawater with (b) humic acid, (c) sodium alginate, and (d)... 33

Fig.3.6. Cross-sectional SEM-EDS images and distributions of the ions detected on the NASICON membrane used for the cycle charging experiment under the conditions of (a) pristine, (b) seawater,... 35

Fig.3.7. Voltage profiles during long-term charging experiment. 36

Fig.3.8. Electrical resistance of AEM measured by using the four-electrode method after long-term charging experiment. 37

Fig.3.9. SEM-EDS images and detected ion distributions of an AEM used for the long-term charging experiment under the conditions of (a) pristine, (b) seawater, and seawater with (c) humic acid, (d)... 38

Fig.4.1. Diagram of the NRFDB-D system during the (a) charging and (b) discharging. During the charging, the desalination occurred in the desalination compartment where sodium and choline ions... 51

Fig.4.2. Schematic representation of a batch NRFDB-D system involving the charging and discharging processes. Both sides of the NASICON membrane were utilized simultaneously for the... 52

Fig.4.3. Charging voltage profiles at an applied current of 80 mA. Each voltage profile was obtained under various NaHCF concentration: 0.1 M, 0.2 M, 0.4 M, and 0.5 M. 55

Fig.4.4. Charging voltage profiles using 0.1 M NaHCF solution as the catholyte. Each voltage profile was obtained at applied current of 40, 60, 80, 100 and 120 mA. 56

Fig.4.5. (a) The difference in osmotic pressure between the NaHCF solution and the feedwater versus the feedwater flux passed through the AEM. (b) Reduction in the feedwater volume during charging... 58

Fig.4.6. SEC₂ (Wh/mol) and product volume after the desalination process. Product volume represents the final volume of the desalination compartment after completing the charging process. 59

Fig.4.7. Comparison of two SEC₁ values (kWh/m³): one based on the actual experiment and the other assuming an ideal water productivity calculated with all product volumes set at 150 mL 60

Fig.4.8. SEC₁ by each sequence under 40mA current condition (a) when osmosis occurred and (b) when osmosis was assumed to be absent. (c) SEC₁ of accumulated sequence under 40 mA current condition. 62

Fig.4.9. Response surface and contour plots for SEC₁ for the NRFDB-D system under 40mA current condition: (a) NaHCF concentration versus either feed concentration (26,000~35,064 mg/L) or (b)... 66

List of Supplementary Information Figures

Fig.3.S1. Illustration of four-electrode chamber for measuring electrical resistance of AEM. 43

Fig.3.S2. Photographs of NASICON membranes embedded in SWBs used for the cycle charging experiment under the conditions of (a) seawater, and seawater with (b) humic acid, (c) sodium... 43

Fig.3.S3. Results of the EIS analysis on the NASICON membrane used for the cycle charging experiment. The diameters of the colored circles represent the electrical resistance of the NASICON membrane. 44

Fig.3.S4. FTIR spectra of NASICON membranes. 45

Fig.3.S5. Photographs of NASICON membranes embedded on SWBs used for long-term charging experiments under the conditions of (a) seawater, and seawater with (b) humic acid, (c) sodium... 46

Fig.4.S1. Voltage profiles of the SWB-D system during charging with 0.2, 0.4, 0.6, 0.8 and 1.0 mA current applied. 70

Fig.4.S2. Comparison of the measured (x-axis) and predicted (y-axis) data for SEC for the NRFDB-D system under 40mA current condition: (a) NaHCF concentration versus feed concentration; (b)... 71

초록보기

 In addressing the water shortage problem, a seawater battery desalination (SWB-D) system has emerged as a promising electrochemical desalination technology, offering the dual benefits of generating drinking water and storing energy within the battery. Despite its potential, the practical application of the system is hindered by limited exploration of the organic matter impact and by higher energy consumption compared with conventional reverse osmosis (RO) systems. In response, this study first investigated the influence of organic matter on the membranes in terms of energy charging capacity and desalination performance through charging experiments and instrumental analysis. In order to address the excessive energy consumption, we also utilized a redesigned SWB-D system, termed a Na metal electrode-based hybrid redox flow battery desalination (NRFDB-D) system. The second phase of the investigation focuses on optimizing the NRFDB-D system by exploring catholyte concentration and osmosis through experiments and modeling, aiming to minimize specific energy consumption (SEC).

First, the organic fouling behavior in the SWB-D system was examined by individually dissolving three different types of organic matter—humic acid, sodium alginate, and bovine-serum-albumin (Chapter 3). The salt removal performance degraded with hydrophobic organics, while hydrophilic sodium alginate caused no decline. Continuous water flow mitigated the fouling behavior, and a large volume of saline water enabled longer charging. Electrical resistance increase was measured in the presence of organic matter using electrochemical impedance spectroscopy and the four-electrode method. Additionally, the presence of a fouling layer was identified using field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier-transform infrared spectrometry.

Second, the NRFDB-D system was investigated in terms of the catholyte concentration and the osmosis through experiment and modeling, achieving the minimum SEC (Chapter 4). The NRFDB-D experiment revealed the correlation between the catholyte concentration and the osmosis. Response surface methodology (RSM) analysis demonstrated optimal operating conditions in the NRFDB-D system, yielding the lowest SEC across various feedwater concentrations and salt removal rates. The optimized NRFDB-D system efficiently desalinated low-salt water (12,500 mg/L) and seawater (35,064 mg/L), exhibiting a lower SEC compared with the RO system. Additionally, utilizing the optimized NRFDB-D as a part of desalination (45% salt removal) could offset each system limitation, including concentrated brine generation and divalent ions removal in the feedwater.

These studies could be expected to contribute to the practical application of the desalination technologies using the SWB, thereby improving its performance as well as promoting environmental sustainability.

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