• 专利标题:   Manufacturing zinc oxide nano-sheet spherical/foamy graphene composite material useful as working electrode, comprises reacting three-dimensional foam graphene/indium tin oxide glass with hydro-thermal reaction solution in a reactor.
  • 专利号:   CN103496734-A, CN103496734-B
  • 发明人:   CHANG J, GAO X, GUO E, HUANG S, YUE H, WANG L, ZHANG C, ZHANG H, YU Z, ZHANG J
  • 专利权人:   UNIV HARBIN SCI TECHNOLOGY
  • 国际专利分类:   B82Y030/00, C01B031/04, C01G009/02, G01N027/30
  • 专利详细信息:   CN103496734-A 08 Jan 2014 C01G-009/02 201430 Pages: 16 Chinese
  • 申请详细信息:   CN103496734-A CN10479300 15 Oct 2013
  • 优先权号:   CN10479300

▎ 摘  要

NOVELTY - Manufacturing zinc oxide nano-sheet spherical/foamy graphene composite material, comprises placing foam nickel having into quartz tube-type furnace and reacting under gas protection to obtain graphene coated foam nickel, adding polymethyl methacrylate-ethyl lactate into foam nickel and drying to obtain polymethyl methacrylate surface-coated foam graphene, cutting into cubes, soaking in hydrochloric acid, immersing in acetone, washing to obtain three-dimensional foam graphene/indium tin oxide glass, placing in reaction kettle containing hydro-thermal reaction solution and reacting. USE - The zinc oxide nano-sheet spherical/foamy graphene composite material is useful as a working electrode (claimed). DETAILED DESCRIPTION - Manufacturing zinc oxide nano-sheet spherical/foamy graphene composite material, comprises: (i) carrying out chemical vapor deposition method by (i.a) placing 420-440 g/m2 foam nickel having thickness of 1-6-2 mm into the center of quartz tube-type furnace and reacting under argon gas (flow rate of 480-500 cm3/minute) and hydrogen gas (flow rate of 180-200 cm3/minute) protection from room temperature to 1000-1100 degrees C for 30-60 minutes at a rate of 20-40 degrees C/minute, passing methane gas for 5-20 minutes with a rate of 5-10 cm3/minute at 1000-1100 degrees C, cooling the quartz tube-type furnace from 1000-1100 degrees C to room temperature at a rate of 80-100 degrees C/minute to obtain graphene coated foam nickel, (i.b) dissolving 4-5 wt.% polymethyl methacrylate in ethyl lactate at 80-120 degrees C for 1-2 hours by stirring to obtain mixed solution, drop-wisely adding mixed solution (100-200 mu l/cm2) into graphene coated foam nickel using a pipette, naturally drying at room temperature, incubating at 150-200 degrees C for 0.5-1 hour to obtain polymethyl methacrylate surface-coated foam graphene, (i.c) cutting the polymethyl methacrylate surface-coated foam graphene into 0.5-2 cm2 cubes, soaking in 3-4 mol/l hydrochloric acid solution at 80-90 degrees C for 4-6 hours to remove nickel and obtain a three-dimensional foam graphene, and (i.d) immersing the three-dimensional foam grapheme in acetone at 60-70 degrees C for 0.5-1.5 hours to remove polymethyl methacrylate from foam graphene, washing with distilled water, and transferring on a clean indium tin oxide glass to obtain three-dimensional foam graphene/indium tin oxide glass, where the clean indium tin oxide glass is cleaned ultrasonically with acetone for 15-20 minutes, with ethanol for 15-20 minutes and deionized water for 15-20 minutes, and naturally drying at room temperature; and (ii) carrying out hydrothermal synthesis method by (ii.a) dissolving 0.03-0.06 mol/l zinc nitrate, 0.03-0.06 mol/l hexamethylene tetramine and 0.18-0.36 mol/l sodium hydroxide in deionized water, stirring via magnetic stirrer at 450-550 rotations/minute for 3-5 minutes to obtain hydro-thermal reaction solution, and (ii.b) pouring hydro-thermal reaction solution into a reaction kettle, placing the three-dimensional foam graphene/indium tin oxide glass into the reaction solution in upright position, covering the reaction kettle with upper cover and reacting at 90-110 degrees C for 20-26 hours, taking out and naturally cooling to room temperature to obtain composite material, opening the reaction kettle, washing the composite material with distilled water, incubating at 400-450 degrees C for 1-1.5 hour and cooling to room temperature to obtain the product.