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제1장 서론 11

제2장 이론 14

2.1. 졸-겔 공정 14

2.1.1. 졸-겔법 14

2.1.2. 졸-겔의 3가지 반응 20

2.1.3. 졸-겔 반응에 영향을 미치는 요인 22

2.2. 표면의 특성과 접촉각 29

2.3. 다양한 코팅방법 33

2.3.1. Spin-coating 33

2.3.2. Dip-coating 35

2.3.3. Roller-coating 37

2.3.4. Spray-coating 39

제3장 졸-겔법에 의해 TEOS와 MTMS으로부터 발수코팅제 제조 41

3.1. 실험 41

3.1.1. 재료 41

3.1.2. 실험방법 41

3.2. 분석 43

3.2.1. FT-IR분석 43

3.2.2. 접촉각 측정 43

3.2.3. 연필경도 43

3.2.4. 부착력 44

3.3. 결과 및 토론 45

3.3.1. MTMS/TEOS의 몰 비가 코팅 막의 물성에 미치는 영향 45

3.3.2. H₂O의 첨가량에 따라 코팅 막의 물성에 미치는 영향 56

3.3.3. NH₄OH의 첨가량에 따라 코팅 막의 물성에 미치는 영향 64

제4장 졸-겔법에 의해 MTMS와 TMES으로부터 발수코팅제 제조 73

4.1. 실험 73

4.1.1. 재료 73

4.1.2. 실험방법 73

4.2. 분석 75

4.2.1. FT-IR분석 75

4.2.2. 접촉각 측정 75

4.2.3. AFM 분석 75

4.2.4. 연필경도 76

4.2.5. 부착력 76

4.3. 결과 및 토론 77

4.3.1. TMES/MTMS의 몰 비가 코팅 막의 물성에 미치는 영향 77

4.3.2. H₂O의 첨가량에 따라 코팅 막의 물성에 미치는 영향 89

4.3.3. 옥살산(oxalic acid) 첨가량에 따라 코팅 막의 물성에 미치는 영향 95

제5장 졸-겔법에 의해 MTMS와 TMES으로부터 발수코팅제 제조에 미치는 촉매와 용매의 영향 102

5.1. 실험 102

5.1.1. 재료 102

5.1.2. 실험방법 103

5.2. 분석 105

5.2.1. FT-IR분석 105

5.2.2. 분산 안정성 측정 105

5.2.3. 접촉각 측정 105

5.2.4. 연필경도 106

5.2.5. 부착력 106

5.3. 결과 및 토론 107

5.3.1. 촉매의 종류가 발수 코팅 막에 미치는 영향 107

5.3.2. 용매의 종류가 발수 코팅 막에 미치는 영향 122

제6장 결론 135

6.1. 졸-겔법에 의해 TEOS와 MTMS으로부터 발수코팅제 제조 135

6.2. 졸-겔법에 의해 TEOS와 MTMS으로부터 발수코팅제 제조 136

6.3. MTMS와 TMES로부터 제조된 코팅 도막의 발수성에 미치는 촉매와 용매의 영향 137

참고문헌 138

ABSTRACT 142

Table 1. Various forms of alkoxides 23

Table 2. Various solvents used in the sol-gel method 25

Table 3. The composition of hydrophobic coating solutions with the... 47

Table 4. The Composition of hydrophobic coating solutions 57

Table 5. The Composition of hydrophobic coating solutions 65

Table 6. Properties of coating films on cold-rolled steel sheets 72

Table 7. The composition of hydrophobic coating solutions 80

Table 8. The composition of hydrophobic coating solutions with the... 90

Table 9. The composition of hydrophobic coating solutions prepared... 96

Table 10. Properties of coating films on cold-rolled steel sheets 101

Table 11. The composition of hydrophobic coating solutions with the... 110

Table 12. Properties of coating films on cold-rolled steel sheets 121

Table 13. The composition of hydrophobic coating solutions with the... 123

Table 14. Properties of coating films on cold-rolled steel sheets 134

Figure 1. Sol-Gel process. 15

Figure 2. Alkoxide sol-gel and Colloid sol-gel. 17

Figure 3. Sol-Gel process. 19

Figure 4. Hydrolysis reaction under acid catalyst. 26

Figure 5. Hydrolysis reaction under basic catalyst. 27

Figure 6. condensation reaction under acidic catalyst. 27

Figure 7. condensation reaction under basic catalyst. 28

Figure 8. hydrophilic surface and hydrophobic surface. 30

Figure 9. Equilibrium wet state of liquid. 32

Figure 10. 3 step process of spin-coating. 34

Figure 11. 3 step process of dip-coating. 36

Figure 12. process of roller-coating. 38

Figure 13. process of spray-coating. 40

Figure 14. Preparation process of hydrophobic coating solutions. 42

Figure 15. Photographs of hydrophobic coating solutions with the... 48

Figure 16. Surface images of cold-rolled steel sheets with the molar... 50

Figure 17. Contact angles of cold-rolled steel sheets with the molar... 52

Figure 18. FT-IR of hydrophobic coating solutions with the molar... 54

Figure 19. hydrophobic coating solutions with the moles of H₂O. 58

Figure 20. Surface images of cold-rolled steel sheets with the moles of... 60

Figure 21. Contact angles of surfaces of cold-rolled steel sheets with... 62

Figure 22. Hydrophobic coating solutions with the moles of ammonia. 66

Figure 23. Surface images of cold-rolled steel sheets with the moles of... 68

Figure 24. Contact angles of cold-rolled steel sheets with the moles of... 70

Figure 25. Preparation method of hydrophobic coating films. 74

Figure 26. Synthesis reaction of hydrophobic siloxane polymer. 78

Figure 27. Surface images of the cold-rolled steel sheets. 81

Figure 28. Contact angles of cold-rolled steel sheets with the molar... 83

Figure 29. FT-IR of hydrophobic coating solutions with the molar... 85

Figure 30. AFM results of cold-rolled steel sheets with the molar... 87

Figure 31. Surface images of the cold-rolled steel sheets with the... 91

Figure 32. Contact angles of cold-rolled steel sheets with the molar... 93

Figure 33. Surface images of the cold-rolled steel sheets with the... 97

Figure 34. Contact angles of cold-rolled steel sheets with the molar... 99

Figure 35. Preparation method of hydrophobic coating films. 104

Figure 36. Synthesis reaction equations of hydrophobic siloxane... 108

Figure 37. Photographs of hydrophobic coating solutions with the... 111

Figure 38. Dispersion stability of the hydrophobic coating solutions... 113

Figure 39. Surface images of the cold-rolled steel sheets with the... 115

Figure 40. Contact angles of cold-rolled steel sheets with the catalysts. 117

Figure 41. FT-IR of hydrophobic coating solutions with the catalysts. 119

Figure 42. Photographs of hydrophobic coating solutions with the... 124

Figure 43. Dispersion stability of the hydrophobic coating solution with... 126

Figure 44. Surface images of the cold-rolled steel sheets with the... 128

Figure 45. Contact angles of cold-rolled steel sheets with the solvents. 130

Figure 46. FT-IR of hydrophobic coating solutions with the solvents. 132

초록보기

In order to prepare a non-fluorine-based water-repellent agent, the experiment was carried out by changing the type of metal alkoxide, the functional group exhibiting substantially water repellency, the type of solvent, the amount of water, and the type of catalyst.

(1) A water repellent coating was prepared using TEOS as a precursor and MTMS as a functional group. The effect of the coating film was observed by changing the molar ratio of MTMS/TEOS, water, and the amount of ammonia as a catalyst. Water contact angle was 108° when the molar ratio of MTMS/TEOS was 10, the molar ratio of H₂O was 0.08 and the molar ratio of NH₄OH was 0.009.

(2) A water repellent coating was prepared using MTMS as a precursor and TMES as a functional group. At this time, the effect on the water-repellent coating film was changed by changing the molar ratio of TMES/MTMS, water, and the amount of oxalic acid. Water contact angle was 117° when the molar ratio of TMES/MTMS was 25, the molar ratio of H₂O was 5 and the molar ratio of oxalic acid 0.004.

(3) Starting materials MTMS and TMES were used, and the effects of catalyst type and solvent type were observed on the properties of the water-repellent coating. The hydrophobic solution prepared was stable in dispersion of the solution and suitable for coating under solvent was MEK and the catalyst was phosphoric acid. Water contact angle of the coating film was a high contact angle of 109°.