• 专利标题:   Preparation of vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material for oxygen evolution reaction, by using e.g. graphene oxide, L-cysteine, urea and vanadium chloride.
  • 专利号:   CN111155146-A
  • 发明人:   LIU Y, ZHAO R, YANG M, WANG H
  • 专利权人:   UNIV ZHEJIANG
  • 国际专利分类:   B01J027/24, B01J035/00, B01J037/28, C25B001/04, C25B011/06
  • 专利详细信息:   CN111155146-A 15 May 2020 C25B-011/06 202048 Pages: 8 Chinese
  • 申请详细信息:   CN111155146-A CN11367553 26 Dec 2019
  • 优先权号:   CN11367553

▎ 摘  要

NOVELTY - Preparing vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material involves: (1) grinding graphene oxide and L-cysteine in a mass ratio of 1:(5-15); (2) putting the grinded mixture in step (1) into a tubular furnace, heating at 600-800 degrees C in an inert atmosphere and heat preserving for 1-4 hours, cooling to room temperature, washing and drying to obtain nitrogen-sulfur doped-doped reduced graphene oxide; (3) dissolving nitrogen-sulfur double-doped reduced graphene oxide in deionized water, and ultrasonically treating for 4-10 hours to obtain a uniformly mixed nitrogen-sulfur double-doped reduced graphene oxide solution with concentration of 0.5-1 mg/ml; and (4) combining urea, ammonium fluoride, vanadium chloride and nickel salt, adding to the above nitrogen-sulfur double-doped reduced graphene oxide solution, and stirring until a homogeneous solution is formed. USE - The method is useful for preparing vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material, which is useful for oxygen evolution reaction. ADVANTAGE - The method enables simple and economical preparation of the vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material. DETAILED DESCRIPTION - Preparing vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material involves: (1) grinding graphene oxide and L-cysteine in a mass ratio of 1:(5-15); (2) putting the grinded mixture in step (1) into a tubular furnace, heating at 600-800 degrees C in an inert atmosphere and heat preserving for 1-4 hours, cooling to room temperature, washing and drying to obtain nitrogen-sulfur doped-doped reduced graphene oxide; (3) dissolving nitrogen-sulfur double-doped reduced graphene oxide in deionized water, and ultrasonically treating for 4-10 hours to obtain a uniformly mixed nitrogen-sulfur double-doped reduced graphene oxide solution with concentration of 0.5-1 mg/ml; (4) combining urea, ammonium fluoride, vanadium chloride and nickel salt, adding to the above nitrogen-sulfur double-doped reduced graphene oxide solution, where the mass ratio of urea to ammonium fluoride is (1-4):1, the mass ratio of nickel salt to vanadium chloride material is (3-9):1, and the total mass ratio of urea, ammonium fluoride, vanadium chloride and nickel salt to the mass of nitrogen-sulfur double-doped reduced graphene oxide is (22-50):1, and stirring until a homogeneous solution is formed; (5) transferring the solution in step (4) to a reactor, reacting at 100-150 degrees C for 8-18 hours, centrifuging to obtain a precipitate, washing with absolute ethanol and drying at 50-70 degrees C to obtain a precursor material of nickel-vanadium layered double hydroxide/nitrogen and sulfur co-doped graphene; and (6) placing the precursor material obtained in step (5) together with sodium hypophosphite in the tubular furnace, heating the sample at a heating rate of 2-5 degrees C/minute to 300-400 degrees C in an inert atmosphere, heat preserving for 1-5 hours, and cooling to room temperature.