• 专利标题:   Manufacture of doped composite polymer electrolyte membrane used in polymer lithium ion battery, involves soaking doped graphene oxide-graft composite polymer film in organic liquid electrolyte and processing.
  • 专利号:   CN105244537-A, CN105244537-B
  • 发明人:   HUANG D, LI W, SHEN W, YANG G, WANG J, ZHU Z
  • 专利权人:   UNIV JIANGSU SCI TECHNOLOGY
  • 国际专利分类:   H01M010/0525, H01M010/0565
  • 专利详细信息:   CN105244537-A 13 Jan 2016 H01M-010/0565 201643 Pages: 13 English
  • 申请详细信息:   CN105244537-A CN10676059 16 Oct 2015
  • 优先权号:   CN10676059

▎ 摘  要

NOVELTY - To mixed solution containing N,N-dimethylformamide and glycerol, polyacrylic acid oxalate-lithium borate-grafted graphene oxide is added, ultrasonically dispersed, and polyvinylidene fluoride is added and stirred. Resultant mixture is uniformly mixed to obtain mixed solution having concentration of 0.05-0.15 g/ml. Obtained mixed solution is vacuum-deaerated, coated on glass plate, and dried hours to obtain doped graphene oxide-graft composite polymer film. Obtained film is soaked in organic liquid electrolyte, and processed to obtain doped composite polymer electrolyte membrane. USE - Manufacture of doped composite polymer electrolyte membrane used in polymer lithium ion battery. ADVANTAGE - The method efficiently provides doped composite polymer electrolyte membrane having excellent mechanical property and electrochemical property, and ionic conductivity of 3.91x 10-3 S.cm-1. DETAILED DESCRIPTION - Graphene oxide chloride is prepared using graphene oxide obtained by Hummer's method. The obtained graphene oxide chloride and synthetic polyacrylic boric acid ester are mixed in the mass ratio of 20:1-100:1, dispersed in N,N-dimethylformamide, and the obtained mixture having concentration of 0.1-5 g/ml is ultrasonically processed at 70 degrees C for 6-10 hours. Oxalic acid and lithium hydroxide are added to the resultant mixture, such that the molar ratio of oxalic acid, lithium hydroxide and polyacrylic boric acid ester is 0.9:0.9:2. The resultant mixture is heated at 60-80 degrees C for 6-12 hours, to obtain polyacrylic acid oxalate-lithium borate-grafted graphene oxide dispersion. The obtained dispersion is centrifuged at 10000-20000 rpm, washed using deionized water, baked at 80-100 degrees C under vacuum condition for 12-24 hours, to obtain polyacrylic acid oxalate-lithium borate grafted oxidized graphene. To mixed solution containing N,N-dimethylformamide and glycerol in the volume ratio 10:1-6:1, polyacrylic acid oxalate-lithium borate-grafted graphene oxide is added, ultrasonically dispersed at room temperature for 2-3 hours, and 0.5-5 wt.% polyvinylidene fluoride is added, and stirred for 5-12 hours at room temperature. The resultant mixture is uniformly mixed to obtain mixed solution having concentration of 0.05-0.15 g/ml. The obtained mixed solution is vacuum-deaerated, coated on a glass plate, placed in vacuum oven at 80-100 degrees C, and dried for 24-48 hours to obtain doped graphene oxide-graft composite polymer film by thermal induced phase separation method. The obtained composite polymer film is soaked in organic liquid electrolyte for 0.5-1 hour in glove box, and processed to obtain doped composite polymer electrolyte membrane having thickness of 40-70 mu m.