투명한 폴리이미드 축합 반응과 용제 증발 상대속도 연구 및 폴리이미드/그래핀 나노복합체 연구

국문 초록 (Abstract)

본 연구에서는 폴리아믹산(Polyamic acid, PAA)의 열처리 이미드화 반응에서 극성용매의 증발 속도에 따른 경화 속도의 관계를 연구하였다. 불소치환 모노머인 4,4’-(Hexafluoroisopropylidene)diphthalic anhydride (6FDA) 와 2,2-bis[4-(4-amino
-phenoxy)phenyl]hexafluropropane (BAPP) 의 조성으로 N,N-dimethylacetamide (DMAc) 용매에서 폴리아믹산을 합성 하였고, 폴리이미드(Polyimide, PI) 필름은 폴리아믹산을 80 ℃ ∼ 230 ℃사이에서 반응 시키면서 용매의 증발 속도에 따른 이미드화 반응 정도를 온도와 시간에 따라 측정한 결과 잔류용매의 양이 많고, 용매의 증발도가 높은 80 ℃ ∼ 200 ℃사이에서는 온도가 증가함에 따라서 이미드화도가 증가하나 그 이후의 온도에서는 잔류 용매와 용매의 증발도가 줄어들어 들기 때문에, 이미드화도는 일정하게 나타나는 것을 확인하였다.
또한 합성한 투명한 폴리 아믹산에 그래핀 함량을 0.01 wt%, 0.02 wt%, 0.05 wt%, 0.1 wt%, 0.2 wt% 으로 분산시켜 그래핀 함량에 따른 광학적, 열적, 기체투과도 특성을 분석을 실시하였다. 이에 광학적, 기체투과 특성은 함량이 증가 함에 따라 점차 특성 저하가 일어남을 확인하였고, 열적 특성은 그래핀 함량 0.01 wt% 에서 가장 우수한 특성을 보이는 것을 확인하였다.

다국어 초록 (Multilingual Abstract)

A poly(amic acid) (PAA) was prepared by reaction of 4,4’ - (hexafluoroisopropylidene) diphthalic anhydride (6FDA) and 2, 2 - bis [4 - (4 - aminophenoxy)phenyl]hexafluropropane(BAPP) in N,N - dimethylacetamide (DMAc). The cast films of PAA were thermally treated at different temperatures to create polyimide (PI) films. To prepare film, heat treatment was performed at 80 ℃ to 230 ℃ and to confirm degree of imidization depending on solvent evaporation. experimental results showed that the degree of imidization is very fast at the initial stage depending on solvent evaporation rate very fast and the degree of imidization was maintained steadily as time goes by. Because of the degree of solvent evaporation and amount of residual solvent were decreased.

목차 (Table of Contents)

• 제1장 서 론­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 1
• 제2장 이론적 배경­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 3
• 2.1. 폴리이미드 (PI) ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­3
• 2.2. 폴리이미드 수지의 제조 방법­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 4
• 2.3. CTC (Charge Trasfer Complex) 발생과 감소­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 7
• 2.4. 폴리이미드 합성 용매의 종류와 역할­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 11
• 2.5. 그래핀 (Graphene)­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 13
• 제3장 실 험 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­16
• 3.1. 시료 및 시약­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 16
• 3.2. 폴리아믹산 (PAA) 의 합성­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 16
• 3.3. 폴리아믹산의 열적 이미드화­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 17
• 3.4. Expanded 그래핀의 제조­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 21
• 3.5. 폴리이미드/그래핀 복합체 필름 제조­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 21
• 3.6. 분석 및 측정­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 23
• 3.6.1. 폴리이미드 열 축합 반응에서의 용매 증발 거동에 따른 이미드화 반응­­­ 23
• 3.6.2. 폴리이미드/그래핀 복합체 필름의 특성조사 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­24
• 제4장 결과 및 고찰­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 26
• 4.1. 폴리이미드 열축합 반응에서의 용매 증발 거동에 따른 이미드화 반응 ­­­­­­26
• 4.1.1. 이미드 반응 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­26
• 4.1.2. 용매증발과 이미드화 지수 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­35
• 4.2. 폴리이미드/그래핀 복합체 필름의 특성조사 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­41
• 4.2.1. 이미드 반응 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­41
• 4.2.2. 폴리이미드/그래핀 복합체 필름의 광학적 특성 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­43
• 4.2.3. 폴리이미드/그래핀 복합체 필름의 열적 특성­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 47
• 4.2.4. 폴리이미드/그래핀 복합체 필름의 기체투과도­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 52
• 제5장 결 론­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 54
• 참고문헌 ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­56
• Abstract­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­ 59