• 专利标题:   Preparation of polyimide-based high-heat-conductive graphite nanofiber film used for e.g. aerospace application, involves forming polyamic acid fiber film using dibasic anhydride, dibasic amine monomer, graphene and metal oxide, calendaring, carbonizing, and graphitizing.
  • 专利号:   CN114737318-A
  • 发明人:   ZHOU L, GONG M, LUO J, HUANG S, XU L, XU H, LI X, YIN C
  • 专利权人:   JIANGXI NCU HIGHTECH ENERGY MATERIAL
  • 国际专利分类:   D01F001/10, D01F009/24, D04H001/4326, D04H001/728, D06C007/04
  • 专利详细信息:   CN114737318-A 12 Jul 2022 D04H-001/728 202288 Chinese
  • 申请详细信息:   CN114737318-A CN10417775 18 Apr 2022
  • 优先权号:   CN10417775

▎ 摘  要

NOVELTY - Preparation of a polyimide-based high-heat-conductive graphite nanofiber film involves preparing a polyimide precursor-polyamic acid glue solution using a dibasic anhydride and a dibasic amine monomer as raw material by solution polycondensation in a solvent, adding graphene and metal oxide to the glue solution, and stirring well, electrospinning the polyamic acid glue solution containing graphene and metal oxide to form a polyamic acid fiber film, calendaring, subjecting to impregnation treatment, subjecting the partially-imidized fiber film to biaxial stretching chemical imidization treatment to obtain a polyimide fiber film with a three-dimensional crosslinked structure, carbonizing the three-dimensional crosslinked polyimide fiber membrane, cooling to room temperature to obtain a polyimide-based carbon fiber film, graphitizing the polyimide-based carbon fiber film in a graphitization furnace protected by flowing argon, and cooling to room temperature. USE - Preparation of polyimide-based high-heat-conductive graphite nanofiber film used for aerospace application, microelectronic application, separating film, and laser application. ADVANTAGE - The method produces polyimide-based high-heat-conductive graphite nanofiber film with high mechanical strength, flexibility, and thermal conductivity. DETAILED DESCRIPTION - Preparation of a polyimide-based high-heat-conductive graphite nanofiber film involves preparing a polyimide precursor-polyamic acid glue solution using a dibasic anhydride and a dibasic amine monomer as raw material by solution polycondensation in a solvent, adding graphene and metal oxide to the glue solution, and stirring well, electrospinning the polyamic acid glue solution containing graphene and metal oxide with a solid content of 5-25% to form a polyamic acid fiber film containing graphene and metal oxide, calendaring the polyamic acid fiber film containing graphene and metal oxide in a precision calendar, sending the calendered polyamic acid fiber film into a chemical imidization mixed solvent comprising a dehydrating agent, a catalyst, and a solvent, and soaking for 60-300 seconds for impregnation treatment, partial chemical imidizing the soaked calendered polyamic acid fiber film through three temperature sections of 40°C, 60°C and 80°C each for 1-10 minutes, subjecting the partially-imidized fiber film containing graphene and metal oxide to biaxial stretching chemical imidization treatment at 350-420°C for 0-1 hours to obtain a polyimide fiber film with a three-dimensional crosslinked structure, carbonizing the three-dimensional crosslinked polyimide fiber membrane in a carbonization furnace with an absolute pressure of 1-5 Pa according to following program temperature control: the heating rate of 1-6℃/min is increased to 480-500℃ and the temperature is maintained for 0.5-1 hour, the heating rate of 0.5-2℃/min is increased to 600-650℃ and the temperature is maintained for 0.5-1 hours, and the heating rate of 1-3℃/minute is increased to 1000-1400℃ and the temperature is kept for 0.5-1 hour, cooling to room temperature to obtain a polyimide-based carbon fiber film, graphitizing the polyimide-based carbon fiber film according to the following program temperature control in a graphitization furnace protected by flowing argon: the heating rate of 20°C/minute is increased to 1000°C, the heating rate of 4-6℃/minute is increased to 1800-2000℃ and the temperature is maintained for 0.5-1 hour, and the heating rate of 3-5℃/minute is increased to 2700-2850℃ and the temperature is maintained for 0.5-1 hours, and cooling to room temperature.