• 专利标题:   Preparation of graphene/polyimide composite film involves adding polyamic acid solution to graphene oxide dispersion, imidization reacting and carbonizing composite film, graphitizing carbonized film and pressing crude composite film.
  • 专利号:   CN107337928-A
  • 发明人:   LI H, YANG J, DAI S, MIAO J, WU X
  • 专利权人:   UNIV SHANGHAI SCI TECHNOLOGY
  • 国际专利分类:   C08G073/10, C08K003/04, C08K009/00, C08L079/08, C09K005/14
  • 专利详细信息:   CN107337928-A 10 Nov 2017 C08L-079/08 201802 Pages: 17 Chinese
  • 申请详细信息:   CN107337928-A CN10656034 03 Aug 2017
  • 优先权号:   CN10656034

▎ 摘  要

NOVELTY - Polyamic acid solution is added to graphene oxide dispersion, evaporated and reacted, to obtain graphene oxide/polyamic acid composite film. The graphene oxide/polyamic acid composite film is put to hot-pressing sintering furnace, imidization reacted and carbonized, to obtain carbonized film. The carbonized film is put to graphitization furnace, graphitized and naturally cooled, to obtain crude graphene/polyimide composite film. The crude graphene/polyimide composite film is pressed, to obtain graphene/polyimide composite film product. USE - Preparation of graphene/polyimide composite film (claimed). ADVANTAGE - The method enables preparation of graphene/polyimide composite film with high yield by simple method. DETAILED DESCRIPTION - Graphene oxide is uniformly dispersed in N,N-dimethylformamide, to obtain graphene oxide dispersion. The mass ratio of graphene oxide and N,N-dimethylformamide is 1:10. 4,4'-Diaminodiphenyl ether and pyromellitic dianhydride are respectively dissolved in N,N-dimethylformamide, to obtain 4,4'-diaminodiphenyl ether solution with concentration of 0.2 g/ml and pyromellitic dianhydride solution with concentration of 0.2 g/ml, respectively. Pyromellitic dianhydride solution with dripping rate of 0.2 ml/minute is slowly dripped to 4,4'-diaminodiphenyl ether solution and reacted under normal temperature for 2 hours, to obtain polyamic acid solution. The molar ratio of 4,4'-diaminodiphenyl ether solution and pyromellitic dianhydride solution is 1:1. Polyamic acid solution is added to graphene oxide dispersion, evaporated and reacted at 50-80 degrees C for 4-8 hours, to obtain graphene oxide/polyamic acid composite film. The mass ratio of graphene oxide in graphene oxide dispersion and polyamic acid solution is 1-50:100. The graphene oxide/polyamic acid composite film is put to hot-pressing sintering furnace, reacted at 15 MPa, imidization reacted at 170-350 degrees C and heating rate of 0.5-2 degrees C/minute under nitrogen atmosphere for 1-4 hours and carbonized at 700-1000 degrees C and heating rate of 5-10 degrees C/minute for 1 hour, to obtain carbonized film. The carbonized film is put to graphitization furnace, graphitized at 2000-2800 degrees C, atmospheric pressure and heating rate of 20 degrees C/minute under protection of argon atmosphere for 40-120 minutes and naturally cooled to room temperature, to obtain crude graphene/polyimide composite film. The crude graphene/polyimide composite film is pressed with pressure of 30 MPa for 1-30 minutes by tableting machine, to obtain graphene/polyimide composite film product.