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제1장 서론 (Introduction) 16

1.1. 고분자 전해질 막 수전해의 분류 (Classification of polymer electrolyte membrane water electrolysis) 18

1.2. 음이온 교환막 수전해 (Anion exchange membrane water electrolysis: AEMWEs) 21

1.2.1. Basic principle of AEMFCs 21

1.2.2. Hydroxide ion transport mechanism in AEMWE 24

1.2.3. Typical polymer backbones and ion-conducting head group of anion exchange membranes 27

1.3. 연구 요약 (Research Summary) 32

1.3.1. 불소계 SEBS 기반 가교형 음이온 교환막의 개발 : 가교제효과에 대한 고찰 (Development of fluorinated SEBS-based anion exchange membranes: investigation of the various crosslinkers effect) 32

1.3.2. 향상된 용해도를 갖는 SEBS 고분자 기반의 세미(semi) 상호 침투 고분자 네트워크형 음이온 교환막의 개발 (Development of semi-interpenetrating polymer network-type anion exchange membranes based on SEBS polymer with improved solubility) 33

1.4. 참고문헌 (Reference) 36

제2장 불소계 SEBS 기반 가교형 음이온 교환막의 개발 : 가교제효과에 대한 고찰 (Development of fluorinated SEBS-based anion exchange membranes: investigation of the various crosslinkers effect) 41

2.1. 서론 (Introduction) 41

2.2. 결과 및 토의 (Result and discussion) 44

2.2.1. Synthesis and characterization of bromohexyl-pentafluoro-SEBS, (Br-Hex-F5-SEBS 2.2) 45

2.2.2. Fabrication and characterization of the 50x-SEBS membranes with different crosslinkers 50

2.2.3. Analysis of hydrogen bonding 55

2.2.4. IEC, water uptake, and swelling ratio 59

2.2.5. Mechanical and thermal properties 62

2.2.6. Morphological analysis 68

2.2.7. Hydroxide ion conductivity 75

2.2.8. Chemical stability 78

2.2.9. Single cell performance test 83

2.3. 결론 (Conclusion) 87

2.4. 참고문헌 (Reference) 89

제3장 향상된 용해도를 갖는 SEBS 고분자 기반의 세미(semi) 상호 침투 고분자 네트워크형 음이온 교환막의 개발 (Development of semi-interpenetrating polymer network-type anion exchange membranes based on SEBS polymer with improved solubility) 94

3.1. 서론 (Introduction) 94

3.2. 결과 및 토의 (Result and discussion) 101

3.2.1. Synthesis and characterization of triazole-incorporated dimethyl amine-functionalized SEBS, TDM-SEBS) 3.2 와 hexyl trimethyl quaternary ammonium-functionalized polycarbazole, HQA-PC 3.3 101

3.2.2. Fabrication of semi-IPN membrane with different penetrant (HQA-PC) composition 110

3.2.3. Ion exchange capacity (IEC), water uptake, swelling ratio and hydroxide ion conductivity 112

3.3. 향후 연구 진행 방향 (Future work and direction) 117

3.4. 참고문헌 (References) 118

제4장 Experimental 124

4.1. Materials 124

4.2. Technique of characterization and measurements 124

4.3. Synthesis 132

4.3.1. Synthesis of 6-bromohexanoyl SEBS (Br-Hex-CO-SEBS) 2.4 132

4.3.2. Synthesis of Br-Hex-F5-CO-SEBS 2.3 133

4.3.3. Reduction of Br-Hex-F5-CO-SEBS 2.3. to Br-Hex-F5-SEBS) 2.2 133

4.3.4. Fabrication of 50 mol% crosslinked SEBS membranes with different crosslinkers (50x-SEBS 2.1) 134

4.3.5. Synthesis of Br-SBS 3.4 134

4.3.6. Synthesis of Br-SEBS 3.5 135

4.3.7. Synthesis of N₃-SEBS 3.6 135

4.3.8. Synthesis of TDM-SEBS 3.2 136

4.4. Reference 137

ABSTRACT 138

표목차

Table 1.1. Types of water electrolysis according to conducting ion 20

Table 2.1. Gel fraction of the 50x-SEBSs membranes 52

Table 2.2. Density of the 50x-SEBSs membranes 57

Table 2.3. IEC, water uptake and swelling ratio of the 50x-SEBS membranes with different crosslinkers 62

Table 2.4. Ion cluster diameter and corresponding q value of 50x-SEBS membranes 74

Table 2.5. Hydroxide ion conductivity in water of 50x-SEBS membranes at different temperatures 76

Table 2.6. Comparison of the AEMWE single cell performance of TMHA-50x-SEBS and TDMAP-50x-SEBS with that of FAA-3-50 membrane at 1.8V and 2.0V 84

Table 3.1. Gel fraction of the xSEBS-nPC-IPN membranes 111

Table 3.2. IEC, water uptake, and swelling ratio of the xSEBS-nPC-IPN membranes with different penetrant (HQA-PC) compositions 114

Table 3.3. Hydroxide ion conductivity in water of xSEBS-nPC-IPN membranes at different temperatures 116

그림목차

Figure 1.1. Basic operation principles of an PEMWE and AEMWE 21

Figure 1.2. Schematic of typical cell configurations of AEMWE components 23

Figure 1.3. Annual AEMWE study published in the Journal Citation Report (JCR) 24

Figure 1.4. Schematic representation of hydroxide ion transport mechanism in AEMs 26

Figure 1.5. Typical solvation structure of hydroxide ion 27

Figure 1.6. Common polymer backbones for AEM 31

Figure 1.7. Common ion conducting group for AEM 31

Figure 1.8. Schematic image of crosslinked 50x-SEBS membranes with different crosslinkers 33

Figure 1.9. Schematic image of crosslinked xSEBS-nPC-IPN membranes with different penetrant compositions 35

Figure 2.1. Structure of the crosslinked Br-Hex-F5-SEBS polymer membranes (50x-SEBS) 44

Figure 2.2. ¹H NMR spectra of the (a) Br-Hex-CO-SEBS 2.4, (b) Br-Hex-F5-CO-SEBS 2.3, and 19F NMR spectra of the (c) Br-Hex-F5-CO-SEBS 2.3, and ¹H NMR spectra of the (d) Br-Hex-F5-SEBS 2.2 49

Figure 2.3. FT-IR spectra of the Br-Hex-CO-SEBS 2.4, Br-Hex-F5-CO-SEBS 2.3, and its reduced form, Br-Hex-F5-SEBS 2.2 50

Figure 2.4. Photographs of crosslinked 50x-SEBS membranes 2.1 with different crosslinkers 52

Figure 2.5. IR spectra of the 50x-SEBSs membranes 53

Figure 2.6. High resolution X-ray photoelectron spectroscopy of Br3d for 50x-SEBS membranes after crosslinking (a) DMA-50x-SEBS, TMHA-50x-SEBS (blue) and TDMAP-50x-SEBS (red)[이미지참조] 54

Figure 2.7. IR spectra of the DMA-50x-SEBS (black), TMHA-50x-SEBS (blue) and TDMAP-50x-SEBS (red) 56

Figure 2.8. Radial Distribution Functions (RDF) of (a) cationic group with H₂O, (b) cationic group with OH- of the 50x-SEBSs membranes[이미지참조] 58

Figure 2.9. (a) TGA graphs and (b) DSC graphs of 50x-SEBS membranes 64

Figure 2.10. (a) Stress-strain curves of 50x-SEBS membranes at 50% RH condition, (b) Young's modulus of the 50x-SEBS membranes compared with those of various SEBS AEMs... 66

Figure 2.11. Hydrogen permeability of 50x-SEBS membranes at room temperature under dry condition 68

Figure 2.12. (a-c) AFM surface images at 50 % RH condition and (d-f) AFM surface images dried in 50 % RH condition after treating membranes in water at 20℃ for 24 hours, and (g-i)... 70

Figure 2.13. SAXS profiles of 50x-SEBS membranes with different crosslinkers 74

Figure 2.14. (a) Normalized conductivity versus temperature of 50x-SEBS membranes in water, (b) comparison of the IEC vs normalized conductivity of the 50x-SEBS membranes... 77

Figure 2.15. Hydration number (λ) vs hydroxide ion conductivity at 20℃ to 80℃ of 50x-SEBS membranes 78

Figure 2.16. (a) Retention of hydroxide ion conductivity based on measured at 20℃ and, (b) IEC retention of 50x-SEBS membranes after being treated in 2M KOH at 80℃ 80

Figure 2.17. FT-IR spectra for three different sets of membranes before (fine line) and after (bold line) 2M KOH solution treatment at 80℃ for 864 hours (i.e., alkaline stability testing) 81

Figure 2.18. (a) Weight retention of 50x-SEBS membranes after treatment with Fenton's reagent for 120 hours at 60℃ and photographs of (b-e) DMA-50x-SEBS, (c-f) TMHA-50x-... 83

Figure 2.19. AEMWE Single cell performance of FAA-3-50, TMHA-50x-SEBS, and TDMAP-50x-SEBS membranes at 70℃ cell temperature with 1M KOH solution 85

Figure 2.20. Comparison of the AEMWE Single cell performance of TMHA-50x-SEBS, and TDMAP-50x-SEBS membranes with that of other commercialized AEMs 87

Figure 3.1. Schematic representation of the crosslinked-SEBS, interpenetrated with PC, semi-IPN membrane, xSEBS-PC-IPN, using crosslinked SEBS as a matrix, DBH as a crosslinker, and... 100

Figure 3.2. ¹H NMR spectra of (a) commercial SBS, (b) Br-SBS 3.4, (c) Br-SEBS 3.5, (d) N₃-SEBS 3.6 and (e) TDM-SEBS 3.2 107

Figure 3.3. ¹H NMR spectrum of bromo hexylated polycarbazole 3.7 and HQA-PC 3.3 109

Figure 3.4. Photographs of xSEBS-nPC-IPN membranes 3.1 with different PC compositions 111

Figure 3.5. IR spectra of the HQA-PC 3.3 and xSEBS-nPC-IPN membranes 112

Figure 3.6. Normalized conductivity versus temperature of xSEBS-nPC-IPN membranes in water 117

도식목차

Scheme 2.1. Synthetic route to the Br-Hex-CO-SEBS 2.4, Br-Hex-F5-CO-SEBS 2.3, and Br Hex-F5-SEBS 2.2 46

Scheme 3.1. Synthetic route to the crosslinked-SEBS-polycarbazole-based semi-IPN 3.1 102

Scheme 3.2. Synthetic route to TDM-SEBS 3.2 104

Scheme 3.3. Synthetic route to HQA-QC 3.3 104

Scheme 4.1. Schematic representation of the gas permeability measurement system. 131

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