화학공학소재연구정보센터
Polymer(Korea), Vol.41, No.1, 75-82, January, 2017
전기방사한 폴리아믹산 나노섬유 매트의 등온 열이미드화에 의한 나노섬유상 폴리이미드 부직포의 제조
Fabrication of Nanofibrous Polyimide Non-wovens by Isothermal Heat Treatment from Electrospun Poly(amic acid) Nanofiber Mats
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초록
전기방사공정에서 고분자용액의 구성은 나노섬유의 방사성 및 직경을 제어하는 중요한 요소이다. 전압, 방사거리, 토출속도 및 폴리아믹산(PAA)-디메틸아세트아미드(DMAc)/아세톤 용액농도의 변화에 따른 섬유형태를 고려하여 고효율 필터미디어소재로써 최적의 방사조건을 확립하였으며 제조된 나노섬유의 평균직경은 약 440 nm임을 확인하였다. PAA 나노섬유 매트는 200 °C의 오븐에서 각각 10, 30, 60, 90, 120, 150, 180, 210, 240분 동안 등온 열처리하여 이미드화시켰으며, 열이미드화 정도 및 열중량 특성은 ATR-FTIR과 TGA 측정을 통하여 확인하였다. ATR-FTIR을 이용하여 분석해 본 결과, 최소 30분 이상 열처리하였을 때 이미드화가 진행되었으며 그 이상 열처리시간이 증가하더라도 열이미드화의 현저한 변화는 없었다. 열처리한 폴리이미드 부직포를 200 °C 오븐에서 4주간 정치하였으나 중량감소는 보이지 않았다. 폴리아믹산 나노섬유의 최적화된 전기방사 및 등온열처리 이미드화 조건은 효율적인 내열성 폴리이미드 나노섬유 필터미디어 제조에 유용할 것으로 기대된다.
Composition of polymer solutions on electrospinning process is an important factor to control spinnability and diameter of nanofibers. The optimum electrospinning conditions on fiber morphology as a high-efficiency filter media were established by adjusting applied voltage, distance, feed rate and concentration of poly(amic acid) (PAA)-dimethylacetamide (DMAc)/acetone solutions. The average diameter of PAA nanofiber was 440 nm. Isothermal heat treatment of the PAA nanofiber mats was carried out using an electric oven (at 200 °C) for 10, 30, 60, 90, 120, 150, 180, 210, and 240 min, respectively. Imidization degree and the thermogravimetric property of PAA mats were confirmed by ATRFTIR and TGA measurement. Imidization of nanofiber mats occurred after 30 min of heat treatment. There was not significant variation of ATR-FTIR intensity after heat treatment longer than 30 min. Weight loss of the polyimide mats was negligible for 4 weeks incubation at 200 °C. Optimized conditions of electrospinning and isothermal heat treatment of nanofibrous poly(amic acid) mats might useful for fabrication of efficient polyimide non-wovens as a heat-resistance filter media.
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