• 专利标题:   Preparing polyimide/graphene composite carbon film comprises deoxygenating and polymerizing dianhydride and diamine, mixing polyamic acid and graphene oxide solutions, subjecting for imidization reaction, carbonization and graphitization.
  • 专利号:   CN110240150-A
  • 发明人:   GAO C, XU Z, WANG Y
  • 专利权人:   HANGZHOU GAOXI TECHNOLOGY CO LTD, UNIV ZHEJIANG
  • 国际专利分类:   C01B032/05, C01B032/184
  • 专利详细信息:   CN110240150-A 17 Sep 2019 C01B-032/184 201978 Pages: 10 Chinese
  • 申请详细信息:   CN110240150-A CN10614438 09 Jul 2019
  • 优先权号:   CN10614438

▎ 摘  要

NOVELTY - Preparing polyimide/graphene composite carbon film comprises (a) subjecting dianhydride and diamine for deoxygenation and polymerization in dimethylformamide to obtain polyamic acid solution, (b) mixing polyamic acid solution and aqueous graphene oxide solution to obtain composite solution, allowing to deposit and drying to obtain polyamic acid/graphene oxide composite film, (c) impregnating polyamic acid/graphene oxide composite film in mixed solution of hydroiodic acid solution and ethanol, subjecting for chemical reduction, washing and drying, placing in low temperature furnace, vacuuming, gradient heating, subjecting for imidization reaction and cooling to obtain imidized composite film, (d) carbonizing imidized composite film in medium temperature furnace and heating to obtain preliminary carbonized polyimide/graphene oxide composite film and (e) placing the preliminary carbonized polyimide/graphene oxide composite film in high temperature furnace, graphitizing and compacting. USE - The method is useful for preparing polyimide/graphene composite carbon film. ADVANTAGE - The carbon film has smooth surface and the interlayer peel strength of graphene composite carbon film is significantly higher than pure graphene film. DETAILED DESCRIPTION - Preparing polyimide/graphene composite carbon film comprises (a) subjecting dianhydride and diamine for deoxygenation and polymerization in a polar solvent of dimethylformamide in a molar ratio of 1.2:1 to obtain a polyamic acid solution, (b) uniformly mixing polyamic acid solution and aqueous graphene oxide solution based on 1-15 wt.% polyamic acid to obtain a composite solution, allowing to deposit and drying to obtain a polyamic acid/graphene oxide composite film. (c) impregnating the polyamic acid/graphene oxide composite film in a mixed solution of hydroiodic acid solution and ethanol in a volume ratio of 1:3; subjecting for chemical reduction at 95 degrees C for 12 hours, removing, washing and naturally drying, placing in a low temperature furnace, vacuuming, gradient heating at rate of 2 degrees C/minute, maintaining at 60 degrees C and 100 degrees C for 2 hours, 150 degrees C, 200 degrees C, 250 degrees C, 300 degrees C, 350 degrees C, 400 degrees C each for 1 hour, subjecting for imidization reaction and cooling to obtain an imidized composite film, where the hydriodic acid solution has 55-58 wt.% hydrogen iodide , (d) carbonizing the imidized composite film in a medium temperature furnace, heating to 800 degrees C at a heating rate of 5 degrees C/minute, heating 1000 degrees C at a heating rate of 3 degrees C/minute and then heating to 1200 degrees C at a heating rate of 2 degrees C/minute and maintaining for 1 hour to obtain a preliminary carbonized polyimide/graphene oxide composite film and (e) placing the preliminary carbonized polyimide/graphene oxide composite film in a high temperature furnace, heating to 2000 degrees C at a heating rate of 10 degrees C/minute and then graphitizing at 3000 degrees C at heating rate of 2 degrees C/minute and compacting.