The Effect of Diamine and Solvent on The Synthesis of Polyimides and Their Film Properties

폴리이미드의 합성과 필름의 물성에 미치는 디아민과 용매의 효과

  • Choi, Hyeong-Ki (Department of Industrial Chemistry, College of Engineering, Hanyang University) ;
  • Lee, Ho-Sik (Department of Industrial Chemistry, College of Engineering, Hanyang University) ;
  • Chung, Chang-Nam (Department of Polymer Engineering, College of Engineering, Suncheon University) ;
  • Kim, Jum-Sik (Department of Industrial Chemistry, College of Engineering, Hanyang University)
  • 최형기 (한양대학교 공과대학 공업화학과) ;
  • 이호식 (한양대학교 공과대학 공업화학과) ;
  • 정창남 (순천대학교 공과대학 고분자공학과) ;
  • 김점식 (한양대학교 공과대학 공업화학과)
  • Received : 1991.06.13
  • Published : 1991.09.30

Abstract

Polyamic acids, precursor polymers of polyimides have been obtained by the solution polycondensation of benzophenone tetracarboxylic dianhydride (BTDA) with 4, 4'-diamino diphenyl methane (MDA) and/or 3, 3'-dimethyl benzidine (OTB). The reaction was carried in two solvent systems such as m-cresol and m-cresol/xylene mixture. The results of TGA analysis showed that the polyimide films had good thermal stability with the initial decomposition temperature ranging from $540^{\circ}$ to $590^{\circ}$. According to DSC analysis of polymers, the glass transition temperature was over $340^{\circ}$. Polyimide film samples, showed good mechanical and electrical properties, had over $16Kg/mm^2$ of tensile strength and about 200 KV/mm of dielectric breakdown voltage. The properties of the copolymer from MAD/OTB were better than those of the homopolymer from MDA. And the polymer synthesized in m-cresol had lower properties than that obtained in m-cresol/xylene.

폴리이미드의 전구체인 폴리아믹산을 benzophenone tetracarboxylic dianhydride (BTDA)와 4, 4'-diamino diphenyl methane (MDA) 혹은 MDA와 3, 3'-dimethyl benzidine (OTB)의 혼합디아민과 용액축중합반응에 의하여 합성하였다. 반응용매로는 m-cresol과 m-cresol/xylene의 혼합용매를 사용하였다. TGA 분석 결과 폴리이미드 필름은 초기분해 온도가 $540^{\circ}C-590^{\circ}C$의 범위로서 내열성이 우수하였다. DSC 분석으로 중합체의 유리전이온도는 $340^{\circ}$ 이상임을 확인하였다. 폴리이미드 필름은 양호한 기계적, 전기적 물성값을 갖는 시료에서 인장강도가 $16Kg/mm^2$ 이상이었고, 절연파괴전압이 200 KV/mm 정도였다. 대체로 MDA 만을 디아민으로 사용한 단일중합체보다 MDA/OTB 공중합체의 물성이 우수하였고, m-cresol에서 합성한 중합체보다 m-cresol/xylene 혼합용매계에서 합성한 중합체의 물성값이 우수하였다.

Keywords