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제출문

요약문

SUMMARY

List of Table

List of Figure

표목차

그림목차

칼라

목차

I. 서론 16

1) 구조용 접착제의 개요 17

1. 구조용 접착제 17

2. 개발 목표 17

가. 적용 규격 17

3. 재료 20

가. 열 잠재성 경화제 4 20

나. 고무 변성 에폭시 수지 5,6 22

다. Poly(butylene terephthalate)-Poly(tetramethylene glycol) copolymer : PBT-PTMG 7 24

II. 국내외 기술개발 현황 26

III. 연구개발수행 내용 및 결과 27

1) 실험 27

1. 원재료 27

2. 기자재 28

가. 시편 제조용 기자재 28

나. 평가용 기자재 29

3. Al. 전처리 30

4. 접착제 시료 및 시편 준비 31

가. 접착액 제조 및 시료준비 31

5. 접착력 평가 방법 32

가. DMS 2169D 32

2) 실험방법(수행) 34

1. 배합비율 결정실험 34

가. Epoxy Resin 34

나. Hardener 34

다. Toughening agent 35

라. HW-810 배합 제조 36

2. 접착필름의 제조 36

가. Doctor blade 36

나. 연속식 접착필름 제조장치 36

3. 접착력 평가 37

가. 시편제조 37

나. 접착력 평가 38

3) 연구결과 39

1. 배합비율 결정 39

가. 에폭시 수지 39

나. 경화제 40

다. BPA(chain extender) 40

라. Toughening agent 41

2. HW-810 배합 42

4) 결론 43

IV. 연구개발목표 달성도 및 대외기여도 44

V. 연구개발결과의 활용계획 45

VI. 참고문헌 46

3차년도 연차보고서:접착제용 에폭시 수지의 강인화 특성 연구

3차년도 연차보고서:접착제용 에폭시 수지의 강인화 특성 연구 83

목차 84

표목차 88

그림목차 89

제1장 서론 92

제2장 실험 93

제1절 시료 93

제2절 Adhesive에서의 thickness effect 94

2-2-1. Epoxy part의 제조 94

2-2-2. Hardener part의 제조 94

2-2-3. Toughener 제조 94

2-2-3-1. CTBN／Epoxy 혼합물 제조 94

2-2-3-2. PBT-PTMG powder 제조 95

2-2-3-3. core-shell powder 제조 95

2-2-4. bulk 경화시편의 제조 95

2-2-5. adhesives 경화시편의 제조 95

2-2-5-1. 알루미늄 시편의 표면처리 95

2-2-5-2. tapered double cantilever joint 96

2-2-5-3. lap shear joint 96

제3절 적정 tack의 결정 96

제4절 기기 분석 97

2-4-1. 동적기계적 열분석 97

2-4-2. 주사전자현미경 관찰 97

2-4-3. 광학현미경 관찰 97

2-4-4. 기계적 물성 97

2-4-5. 표면 특성 98

제3장 결과 및 고찰 99

제1절 bulk 물성 99

3-1-1. Neat epoxy 99

3-1-2. PBT-PTMG toughened epoxy 100

3-1-3. Rubber(Ruber) toughened epoxy 101

3-1-3-1. adduct system(95-725 경화계) 102

3-1-3-2. simple mixing system(95-726 경화계) 102

3-1-3-3. 구조재용 접착제로서의 725,726 경화계의 문제점 103

3-1-3-4. 경화제 함량에 따른 simple mixing system에서의 강인화 현상 103

제2절 Adhesive 경화계 104

3-2-1. 알루미늄의 표면처리 106

3-2-2. Tapered double cantilever beam joint (thickness effect) 106

3-2-2-1. Neat epoxy 107

3-2-2-2. PBT-PTMG toughened epoxy 107

3-2-2-3. CTBN toughened epoxy 109

3-2-2-4. core-shell toughened epoxy 110

3-2-3. Lap shear joint(thickness effect) 110

3-2-3-1. Neat epoxy 111

3-2-3-2. PBT-PTMG toughened epoxy 112

3-2-3-3. CTBN toughened epoxy 114

3-2-3-4. core-shell toughened epoxy 115

3-2-4. Tapered double cantilever beam joint (formulation effect) 116

3-2-4-1. neat epoxy 116

3-2-4-2. PBT-PTMG toughened epoxy 117

3-2-4-3. CTBN toughened epoxy 117

3-2-5. lap shear test 118

3-2-5-1. Neat epoxy 118

3-2-5-2. PBT-PTMG toughened epoxy 119

3-2-5-3. CTBN toughened epoxy 119

제3절 적정 tack의 결정 120

제4장 결론 121

제1절 TDCB joint와 lap shear joint의 비교(thicknsess effect) 121

4-1-1. 두께에 따른 비교 121

4-1-2. 강인화제에 따른 비교 122

제2절 TDCB joint와 shear joint의 비교(formulation effect) 123

제5장 참고문헌[내용누락;p.78] 124

[title page etc.]

SUMMARY

Contents

I. Introduction 16

1) Introduction of structural adhesive film 17

1. Adhesive 17

2. Objects 17

가. Relative specifications 17

3. Materials 20

가. Thermal latent hardener 20

나. Rubber toughened epoxy 22

다. PBT-PTMG copolymer 24

II. Technical status domestic and overseas 26

III. Contents and results of the research(reseasch) 27

1) Experiments 27

1. Material 27

2. Supplies 28

가. Supplies for preparation 28

나. Supplies for evaluation 29

3. Al. surface preparation 30

4. Adhesive preparations 31

가. Specification preparations 31

5. Evaluations methods for adhesive strength 32

가. DMS 2169D 32

2) Experiments 34

1. Mixture ratios 34

가. Epoxy resins 34

나. Hardener 34

다. Toughening agent 35

라. HW-810 36

2. Adhesive film preparations 36

가. Doctor blade 36

나. Pilot plant for continuos(continous) adhesive film 36

3. Evaluations 37

가. Adhesive preparations 37

나. Adhesive strength 38

3) Results 39

1. Mixture ratios 39

가. Epoxy resins 39

나. Hardener 40

다. BPA 40

라. Toughening agent 41

2. HW-810 42

4) Conclusions 43

IV. Degree of achievement(achivement) and external contributions 44

V. Application plan of the research 45

VI. References[내용누락;p.78] 46

List of Table

Table 1. Classification of adhesive into MMA-A-132 47

Table 2. Classification of adhesive into DMS 2169D 48

Table 3-1. Lap-shear strength Requirements After Environmental Conditioning 49

Table 3-2. Lap-shear strength Requirements After Environmental Conditioning 50

Table 4. Lap-Shear Cyclic and Sustained Load Requirements During Environmental Exposure 51

Table 5. Qualified structural adhesive films 52

Table 6. 250℉ structural adhesive on commercial 53

Table 7. Specific character(charater) of FM73M-060 & EA9628NW-060 in catalogue 54

Table 8. Mechanical properties variations of DGEBA mixtures in CTBN addition 55

Table 9. Mechanical properties variations of adhesive for film thickness and temperature 56

Table 10. Mechanical properties variations of rubber toughened epoxy for Bisphenol-A addition 57

Table 11. Test conditions for Instron 58

Table 12. Test results of HW-810 mixture 59

Table 13. Objects and contents of the business years 60

List of Figure

Fig 1. Typical structural adhesives 61

Fig 2. Structural adhesives om commercial aircrafts 62

Fig 3. Bonded honeycomb sandwich 63

Fig 4. Fracture energy for initiation for (a):PBT, (b):Nylon 6, (c):CTBN, (d):PVDF 64

Fig 5. Specification for T-peel test 65

Fig 6. Specification for Lap-shear test 66

Fig 7. Specification for cimbing drum peel test 67

Fig 8. Pilot plant for continuos(cntinous) adhesive film 68

Fig 9. Chamber for Instron(low, room, hot temperature) 69

Fig 10. Autoclave 70

Fig 11. Climbing drum peel 71

Fig 12. Mixer 72

Fig 13. Effect of YD-128 content on bulk fracture(frature)(Lap-shear variation) 73

Fig 14. Effect of YD-011 content on bulk fracture(frature)(Lap-shear variation) 74

Fig 15. Change of epoxy mixture's viscosity with PBT-PTMG 75

Fig 16. Effect of hardener fractyre on bulk fracture(Lap-shear variation) 76

Fig 17. Effect of CTBN content on low temp. T-peel 77

Fig 18. Effect of CTBN content on low temp. Lap-shear 78

Fig 19. Effect of CTBN content on T-peel 79

Fig 20. Effect of CTBN content on Lap-shear 80

Fig 21. Effect of BPAcontent on T-peel 81

Fig 22. Effect of BPA content on Lap-shear 82

표목차

Table 1. MMA-A-132에 의한 접착제의 분류 47

Table 2. DMS 2169D에 의한 접착제의 분류 48

Table 3-1. Lap-Shear Strength Requirements After Environmental Conditioning 49

Table 3-2. Lap-Shear Strength Requirements After Environmental Conditioning 50

Table 4. Lap-Shear Cyclic and Sustained Load Requirements During Environmental Exposure 51

Table 5. 인증된 접착필름의 종류 52

Table 6. 상업 생산 판매 중인 250℉ 경화형 필름 53

Table 7. FM73M-060과 EA9628NW-060의 Catalogue상의 특성 54

Table 8. CTBN 첨가에 따른 DGEBA 혼합물의 물성치 변화 55

Table 9. 접착제의 접착두께 및 온도에 의한 영향(Effects of adhesive thickness and temperature) 56

Table 10. CTBN 변성 에폭시 접착제에서 Bisphenol-A의 혼입영향 57

Table 11. Instron 실험조건 58

Table 12. HW-810 접착력 test 59

Table 13. 연도별 목표 및 내용 60

Table 1. Recipe o f toughener-modified Epoxies 126

Table 2. Comparison of mechanical properties of PBT-PTMG modified epoxies 127

Table 3. Comparison of mechanical properties of rubber-modified epoxies 128

Table 4. The procedures for preparation of cured epoxy for TDCB test specimen 129

그림목차

Fig 1. 구조용 접착제의 일반 형태 61

Fig 2. 일반 상업용 항공기에서의 구조용 접착제의 응용 62

Fig 3. Honeycomb의 구조 및 접착 63

Fig 4. 여러 가지 강인화제와 에폭시 수지와의 혼합시 Fracture energy (a) : PBT, (b) : Nylon 6, (c) : CTBN, (d) : PVDF 64

Fig 5. T-peel용 시편 65

Fig 6. Lap-shear용 시편 66

Fig 7. Climbing drum peel용 시편 67

Fig 8. 연속식 접착필름 제조장치 68

Fig 9. Instron용 Chamber(저온,상온,고온용) 69

Fig 10. Autoclave(Autoclve) 70

Fig 11. Climbing drum peel 71

Fig 12. 혼련기(Mixer) 72

Fig 13. YD-128양 변화에 따른 Lap-shear 변화 73

Fig 14. YD-011 첨가에 따른 접착력의 변화 74

Fig 15. PBT-PTMG 첨가에 따른 점도 변화 75

Fig 16. 에폭시 수지 : 경화제 당량비 변화에 따른 Lap-shear의 변화 76

Fig 17. 저온 T-peel 접착력의 요인 분석 77

Fig 18. 저온 Lap-shear 접착력의 요인 분석 78

Fig 19. CTBN 사용량에 따른 T-peel 접착력 변화 79

Fig 20. CTBN 사용량에 따른 Lap-shear 접착력 변화 80

Fig 21. BPA사용량에 따른 T-peel 접착력 변화 81

Fig 22. BPA사용량에 따른 Lap-shear 접착력 변화 82

Fig.1. Geometry of test specimen (a) tapered double cantilever joint (b) lap shear joint 130

Fig.2. Effect of toughener content on crosslink molecular weight of toughener／epoxy blends 131

Fig.3. SEM micrographs of fracture surfaces of lap shear joint without toughener 132

Fig.4. Effect of toughener content on bulk fracture toughness of PBT-PTMG／epoxy blends 133

Fig.5. Optical micrographs of CTBN-epoxy blends under the crosspolarizer on hot stage: (A) 95-725 (b) 95-726 134

Fig.6. Coagulation of CTBN-epoxy blends at different time and temperature(a) 60°C,1min (b) 60°C,10min (c) 90°C, (d) 120°C 135

Fig.7. Optical micrographs of thin section of CTBN-epoxy blends under the crosspolarizer: (a)95-725 (b)95-726 136

Fig.8. SEM micrographs of fracture surfaces of CTBN-epoxy blends (a),(b):95-725, (c),(d):95-726 137

Fig.9. Effect of toughener content on bulk fracture toughness of CTBN／epoxy blends 138

Fig.10. Change in deformation zone size of deformed-epoxy with contents of CTBN (a) 5 phr (b) 20 phr 139

Fig.11. Comparison of ESCA profile of Al with different surface treatment 140

Fig.12. SEM micrographs of aluminium with different surface treatment (a) no treatment (b) aceton treatment (c),(d) chromic acid treatment 141

Fig.13. Effect of adhesive thickness on TDCB fracture toughness of toughened epoxy 142

Fig.14. SEM micrographs of microcrack in PBT-PTMG／epoxy blend 143

Fig.15. Three types of microcracks (a) Penny-shaped microrack (b) Annular-shaped microcrack (c) interface microrack 144

Fig.16. SEM micrographs of fracture surface in PBT-PTMG／epoxy blend 145

Fig.17. TOM micrographs of deformation zone in PBT-PTMG／epoxy blend (a) 120 ㎛ (b) 510 ㎛ 146

Fig.18. SEM micrographs of fracture surface in CTBN／epoxy blend 147

Fig.19. TOM micrographs of deformation zone in CTBN／epoxy blend (a) 120 ㎛ (b) 510 ㎛ 148

Fig.20. Effect of adhesive thickness on lap shear fracture toughness of toughened-epoxy blends 149

Fig.21. SEM micrographs of fracture surfaces of lap shear joint with different thickness of PBT-PTMG／epoxy blends (a) 40 ㎛ (b) 90 ㎛ (c) 730 ㎛ 150

Fig.22. TOM micrographs of fracture surfaces of lap shear joint with different thickness of PBT-PTMG／epoxy blends (a) 40 ㎛ (b) 90 ㎛ (c) 90 ㎛ (d) 730 ㎛ 151

Fig.23. Formation of secondary crack in PBT-PTMG／epoxy blend 153

Fig.24. Schematic diagram of secondary crack formation under shear loading (a) single secondary crack initiation (b) Development of multiple secondary crack with regular spacing 154

Fig.25. SEM micrographs of fracture surfaces of lap shear joint with different thickness of CTBN／epoxy blends (a) 45 ㎛ (b) 75 ㎛ (c) 540 ㎛ 155

Fig.26. TOM micrographs of fracture surfaces of lap shear joint with different thickness of CTBN／epoxy blends (a) 45 ㎛ (b) 75 ㎛ (c) 540㎛ 156

Fig.27. Formation of secondary crack in CTBN／epoxy 158

Fig.28. SEM micrographs of fracture surfaces of lap shear joint with different thickness of core-shell rubber／epoxy blends (a) 93㎛ (b) 700㎛ 159

Fig.29. Effect of epoxy equivalent weight on thermal property of toughened-epoxy 160

Fig.30. Effect of epoxy equivalent weight on TDCB fracture toughness of toughened-epoxy 161

Fig.31. SEM micrographs(mcrographs) of TDCB fracture surface of neat epoxy with different epoxy equivalent epoxy 162

Fig.32. SEM micrographs(mcrographs) of TDCB fracture surfaces of PBT-PTMG toughened-epoxy with different epoxy equivalent epoxy (a) YD128 (b) YD011 (c) YD014 163

Fig.33. TOM micrographs(mcrographs) of TDCB fracture surface of PBT-PTMG toughened epoxy with different epoxy equivalent weight (a) YD128 (b) YD011 (c) YD014 164

Fig.34. SEM micrographs(mcrographs) of TDCB fracture surfaces of CTBN toughened-epoxy with different epoxy equivalent weight (a) YD128 (b) YD011 (c) YD014 (d)YD014 166

Fig.35. TOM micrographs(mcrographs) of TDCB fracture surfaces of CTBN-toughened epoxy with different epoxy equivalent weight (a) YD128 (b) YD011 (c) YD014 (d)YD014 167

Fig.36. Effect of epoxy equivalent weight on lap shear fracture toughness of toughened epoxy[내용누락;p.78] 169

Fig.37. TOM micrographs(mcrographs) of fracture surface of toughened-epoxy with different fracture mode (a) PBT-PTMG bulk(mode I) (b) CTBN, bulk(mode I) (c) PBT-PTMG, lap shear (d) CTBN, lap shear 170

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