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Title Page 1

ABSTRACT 4

Contents 6

CHAPTER 1. INTRODUCTION 12

CHAPTER 2. LITERATURE REVIEW 19

2.1. Current technology for GenX treatment 19

2.2. Jet Plasma technology and plasma-catalysis 29

2.3 Reactive species and singlet oxygen (¹O₂) 32

CHAPTER 3. METHODOLOGY 36

3.1. Chemicals and reagents 36

3.2. Preparation of Catalysts 36

3.3. Argon (Ar) jet plasma configuration 37

3.4. GenX degradation experiments 39

3.5. Material and photoelectrochemical (PEC) characterization 45

3.6. Calculation of energy consumption for plasma-catalysis 51

CHAPTER 4. RESULTS AND DISCUSSION 52

4.1. GenX removal performance 52

4.2. Material Characterization 60

4.3. Photoelectrochemical analyses 81

4.4. Studies on reactive species and mechanism construction 98

CHAPTER 5. CONCLUSION 121

References 122

List of Publications and Papers Presented 130

List of Tables 11

Table 1. Benefits and drawbacks of various emerging treatment technologies for the removal of PFAS 21

Table 2. Kinetic rate constant (k₁) for degradation, synergistic factor (fₛyₙ) and...[이미지참조] 58

Table 3. XRD refinement quality parameters of the catalysts 64

Table 4. Cell size calculated from XRD refinement and kinetic rate constant (k₁... 67

Table 5. XPS analysis (O 1s and Ce³⁺/Ce⁴⁺ ratio) for each catalyst 72

Table 6. Moss-Schottky analysis parameters for each catalyst 85

Table 7. Calculated decay parameters of TRPL analysis for the prepared plasma-... 92

List of Figures 8

Figure 1. The percentages use of applied methods to remove GenX from... 24

Figure 2. Reactive species generated in the argon (Ar) jet plasma. (Takamatsu... 30

Figure 3. The generation of ¹O₂ through the energy transfer process. (Blacha-... 33

Figure 4. Orbital structure of oxygen molecule and reactive oxygen species 35

Figure 5. Current and voltage (I-V) curve for (a) plasma and (b)... 38

Figure 6. GenX degradation kinetics with plasma with different catalysts... 52

Figure 7. (a) Adsorption kinetics of GenX degradation, (b) point of zero charge... 54

Figure 8. 1ˢᵗ-order kinetic rate constant (min-¹) for each AOPs 55

Figure 9. Defluorination rate of each AOPs 57

Figure 10. 5 consecutive cycles of reusability test results with kinetic rate... 59

Figure 11. 5 consecutive cycle reusability kinetics for plasma/Ru(0.1%)- CBO 59

Figure 12. FESEM image of (a) CBO with (b) zoomed-in image 60

Figure 13. FESEM image of (a) Ru(0.1%)-CBO with (b) zoomed-in image 61

Figure 14. EDS mapping for Ru(0.1%)-CBO with (a)-(d) each element... 61

Figure 15. XRD spectra of the synthesized catalysts 63

Figure 16. Correlation between kinetic rate (min-¹) and the ratio of (120) facet... 66

Figure 17. XRD for Ru(0.1%)-CBO before and after GenX removal 68

Figure 18. XPS analysis of Bi 4f 73

Figure 19. XPS analysis of Ce 3d 74

Figure 20. XPS analysis of O 1s 75

Figure 21. XPS analysis of Ru 3d 76

Figure 22. Solid ESR analysis for CBO and Ru(0.1%)-CBO 77

Figure 23. XPS analysis of Bi 4f for Ru(0.1%)-CBO before and after GenX... 79

Figure 24. XPS analysis of Ce 3d for Ru(0.1%)-CBO before and after GenX... 79

Figure 25. XPS analysis of O 1s for Ru(0.1%)-CBO before and after GenX... 80

Figure 26. XPS analysis of Ru 3d for Ru(0.1%)-CBO before and after GenX... 80

Figure 27. UV-vis absorbance of the catalysts 82

Figure 28. Tauc plot estimation for (a) CBO, (b) Ru(0.05%)-CBO, (c)... 83

Figure 29. Mott-Schottky plot for (a) CBO, (b) Ru(0.05%)-CBO, (c) Ru(0.1%)-... 86

Figure 30. Photocurrent density for the catalysts 88

Figure 31. EIS analysis for the catalysts 88

Figure 32. Photoluminescence (PL) for CBO and Ru(0.1%)-CBO 90

Figure 33. Time-resolved photoluminescence (TRPL) for CBO and Ru(0.1%)-... 93

Figure 34. TRPL mapping for (a) CBO and (b) Ru(0.1%)-CBO 93

Figure 35. Estimated band positions of the catalysts 95

Figure 36. The correlations between k1 and (a) I(120)/I(111), (b) CeO₂ length,... 97

Figure 37. The concentration of (a) O₃ and (b) H₂O₂ with plasma combined... 102

Figure 38. Scavenger test for GenX degradation with (a) plasma and (b) plasma... 105

Figure 39. The inhibition rate of degradation by each scavenger for (a)... 106

Figure 40. Linear sweep voltammetry (LSV) plot for (a) CBO, and (b)... 107

Figure 41. Liquid ESR spin trap signal for plasma and plasma/Ru(0.1%)-CBO in... 111

Figure 42. Liquid ESR spin trap signal for plasma and plasma/Ru(0.1%)-CBO in... 111

Figure 43. Liquid ESR spin trap signal for plasma and plasma/Ru(0.1%)-CBO in... 112

Figure 44. Comparison of DMPO-·OH signal in the presence of e- and ¹O₂... 112

Figure 45. Terephthalic acid (TA) fluorescence as an ·OH probing: (a)... 115

Figure 46. Proposed mechanism for GenX degradation by plasma-catalysis and the structure of the catalyst... 118

Figure 47. EEO and G₅₀ for plasma and plasma/Ru(0.1%)-CBO[이미지참조] 120

초록보기

 GenX, the ammonium salt of hexafluoropropylene oxide dimer acid (HFPO-DA), has also been of concern not only because it also turned out to be distributed extensively in the aquatic system, but recent studies have implied that GenX could be potentially toxic to organisms in the system. Plasma system combining with catalyst can be beneficial for GenX degradation thanks to highly reactive species generated in the bulk through the system. In this study, GenX was degraded using argon (Ar) jet plasma with pristine bismuth oxide / cerium oxide composite (Bi₂O₃/CeO₂, 'CBO') and various ratios of ruthenium (Ru)-doped CBO as plasma-catalysts. Plasma-catalysis with 0.1% Ru-doped CBO achieved 74% degradation of GenX in 30 min, showing a significant synergistic effect (synergy factor: 1.7) compared to plasma (53%). Material characterizations indicated that Ru doping enhances the (120) facet of Bi₂O₃ and increases the electron density and oxygen vacancy (Ov) on CBO. PL and TRPL analyses suggested that the Ru doping leads to the introduction of Ov, thereby lowering the recombination. The contribution of reactive species revealed that hydroxyl radical (·OH) and singlet oxygen (¹O₂) is important to degrade GenX in both plasma and plasma-catalysis. Notably, it was confirmed that ¹O₂ formation on the catalyst surface is crucial to the overall ·OH production in the plasma-catalysis, leading to the synergistic effect. The energy consumption of plasma coupled with catalysis were found to be nearly twice as efficient as the sole plasma process, endorsing the economic feasibility of the synergistic effect in GenX degradation. Therefore, this study provides valuable insights into the role of ¹O₂ in achieving the synergistic effect and proves the economic feasibility of utilizing the plasmacatalysis for the degradation of GenX.

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