• 专利标题:   Preparation of three-dimensional graphene/polyaniline array composite material used as supercapacitor electrode material, involves dissolving nickel(II) chloride hexahydrate in deionized water, heating, etching, and removing metal nickel.
  • 专利号:   CN110223848-A
  • 发明人:   GAO X, YUE H, ZHANG T, WU P, WANG Z, WANG Y
  • 专利权人:   UNIV HARBIN SCI TECHNOLOGY
  • 国际专利分类:   H01G011/24, H01G011/30, H01G011/32, H01G011/48, H01G011/86
  • 专利详细信息:   CN110223848-A 10 Sep 2019 H01G-011/24 201976 Pages: 11 Chinese
  • 申请详细信息:   CN110223848-A CN10540404 21 Jun 2019
  • 优先权号:   CN10540404

▎ 摘  要

NOVELTY - Preparation of three-dimensional graphene/polyaniline array composite material involves (1) preparing nano-nickel powder by dissolving nickel(II) chloride hexahydrate in deionized water, and dispersing hydrazine monohydrate, stirring, adhering, adding sodium hydroxide solution to mixture, reacting, collecting precipitate, washing with deionized water and absolute ethanol, and vacuum-drying, (2) placing nano-nickel powder in ceramic mold, heating using argon gas and hydrogen as carrier gas, and introducing methane gas, cooling, and removing material, placing in hydrochloric acid solution, etching, removing metal nickel, cleaning and transferring into concentrated nitric acid solution to obtain three-dimensional graphene, (3) adding aniline monomer and ammonium persulfate to sulfuric acid solution, stirring, immersing in aniline solution, heating ammonium persulfate solution to aniline solution to obtain three-dimensional graphene/polyaniline array composite material, and vacuum-drying. USE - Preparation of three-dimensional graphene/polyaniline array composite material used as supercapacitor electrode material. ADVANTAGE - The three-dimensional graphene prepared has high strength, small pore size, uniform distribution of electric polyaniline array, and has improved electrochemical performance when compared to graphene. DETAILED DESCRIPTION - Preparation of three-dimensional graphene/polyaniline array composite material involves (1) preparing nano-nickel powder by dissolving 0.1-0.2 mol% nickel(II) chloride hexahydrate in 27.9 mL deionized water, and dispersing 0.2-0.8 mol% hydrazine monohydrate uniformly, stirring, washing the reactants, and adhering to inner wall of beaker with small amount of deionized water which shows color change of solution from light green to light purple with release of large amount of heat when temperature is lowered to room temperature, adding 8-32 mL sodium hydroxide solution having concentration of 25 mol/L to mixture, reacting for 12 hours, and stopping the reaction, collecting precipitate by filtration, washing with deionized water and absolute ethanol, and drying under vacuum at 80 degrees C for 6-12 hours, (2) preparing three-dimensional graphene by placing 0.5-2 g nano-nickel powder in ceramic mold having diameter of 20 mm, placing in tube furnace, using argon gas and hydrogen as carrier gas, heating to 800-1000 degrees C at room temperature for 30-60 minutes, and introducing 10-20 sccm methane gas into furnace at 800-1000 degrees C for 10-20 minutes, cooling the furnace to room temperature at 80-100 degrees C/minute, and removing material, placing in hydrochloric acid solution having concentration of 3 mol/L, etching at 90 degrees C for 10-24 hours, removing metal nickel, cleaning the material, and transferring cleaned three-dimensional graphene into concentrated nitric acid solution for 12-24 hours, (3) adding 0.25-1 mmol aniline monomer and ammonium persulfate separately to equal volume of sulfuric acid solution having concentration of 1 mol/L, stirring at room temperature for 30-60 minutes to completely dissolve, placing functionalized three-dimensional graphene on glass slide and immersing in aniline solution for 1-3 hours for complete contact of aniline monomer with three-dimensional graphene, heating ammonium persulfate solution to aniline solution under ice bath conditions for 0-24 hours to obtain three-dimensional graphene/polyaniline array composite material, cleaning with deionized water, and vacuum-drying in oven at 60 degrees C for 6-12 hours.