• 专利标题:   Synthesizing zinc sulfide nanosphere array/foamed graphene useful as working electrode of a biosensor for electrochemical detection of dopamine comprises e.g. performing chemical vapor deposition and hydrothermal synthesis.
  • 专利号:   CN110304650-A
  • 发明人:   YUE H, WU P, GAO X, GUO X, ZHANG T, CHEN H
  • 专利权人:   UNIV HARBIN SCI TECHNOLOGY
  • 国际专利分类:   C01B032/186, C01G009/08, G01N027/327, G01N027/48
  • 专利详细信息:   CN110304650-A 08 Oct 2019 C01G-009/08 201989 Pages: 9 Chinese
  • 申请详细信息:   CN110304650-A CN10519621 17 Jun 2019
  • 优先权号:   CN10519621

▎ 摘  要

NOVELTY - Synthesizing zinc sulfide nanosphere array/foamed graphene comprises e.g. performing chemical vapor deposition by placing foamed nickel in the center of the quartz tube furnace, heating from room temperature to 1000-200 degrees C at heating rate of 15-35 degrees C/minutes under protection of argon and hydrogen, maintaining temperature at 1000-1200 degrees C for 20-40 minutes, introducing methane gas into the tube furnace at temperature of 1000-1200 degrees C for 5-15 minutes at rate of 5-15 sccm, cooling quartz tube furnace to room temperature at cooling rate of 60-90 degrees C/minute to obtain graphene-encapsulated foamed nickel, where foamed nickel density is 410-450 g/m2, and thickness is 1.4-1.8 mm, the flow rate of the argon gas is 480-520 sccm, the flow rate of the hydrogen gas is 190-220 sccm, (ii) dissolving polymethyl methacrylate in ethyl lactate, heating mixture and stirring at 90-110 degrees C for 1.5-4 hours to obtain mixed solution, and adding mixed solution to the quilt. USE - The zinc sulfide nanosphere array/foamed graphene is useful as working electrode of a biosensor for electrochemical detection of dopamine (claimed). DETAILED DESCRIPTION - Synthesizing zinc sulfide nanosphere array/foamed graphene comprises (1) performing chemical vapor deposition by (i) placing foamed nickel in the center of the quartz tube furnace, heating from room temperature to 1000-200 degrees C at heating rate of 15-35 degrees C/minutes under protection of argon and hydrogen, maintaining temperature at 1000-1200 degrees C for 20-40 minutes, introducing methane gas into the tube furnace at temperature of 1000-1200 degrees C for 5-15 minutes at rate of 5-15 sccm, cooling quartz tube furnace to room temperature at cooling rate of 60-90 degrees C/minute to obtain graphene-encapsulated foamed nickel, where foamed nickel density is 410-450 g/m2, and thickness is 1.4-1.8 mm, the flow rate of the argon gas is 480-520 sccm, the flow rate of the hydrogen gas is 190-220 sccm, (ii) dissolving polymethyl methacrylate in ethyl lactate, heating mixture and stirring at 90-110 degrees C for 1.5-4 hours to obtain mixed solution, adding mixed solution to the quilt obtained in the step (i) using sample gun at usage amount of 100-150 mu l per square centimeter graphene-wrapped foamed nickel, naturally drying film at room temperature, heating at 180-220 degrees C for 0.5-1 hour to obtain surface coated polymethyl methacrylate foam graphene, where the amount of methyl methacrylate in the mixed solution is 4-5 wt.%, (iii) cutting surface-coated polymethyl methacrylate foamed graphene into cubes having surface area of 0.5-1.5 cm2, completely immersing in hydrochloric acid solution having temperature of 80-100 degrees C and concentration of 2-4 mol/l for 4-8 hours to obtain nickel-depleted three-dimensional foam graphene, (iv) immersing obtained nickel-depleted three-dimensional foamed graphene in acetone at 50-70 degrees C for 0.5-1.5 hours to obtain foamed graphene which removes polymethyl methacrylate, cleaning with distilled water to obtain cleaned polymethyl methacrylate-containing foamed graphene, cleaning indium tin oxide (ITO) glass ultrasonically in acetone for 15-20 minutes, ultrasonically cleaning in ethanol for 15-20 minutes, ultrasonically cleaning in deionized water for 15-20 minutes, and naturally drying at room temperature, and (2) performing hydrothermal synthesis by (a) placing three-dimensional foamed graphene in a beaker containing concentrated nitric acid for 12-16 hours, washing with acetone and deionized water, (b) adding 0.02-0.07 mol/l zinc sulfate and 0.04-0.09 mol/l thiourea to 40-70 ml deionized water, placing in magnetic stirrer, and stirring at 200-400 revolutions/minute for 20-30 minutes to obtain hydrothermal reaction solution, and (c) pouring hydrothermal reaction solution in reaction kettle, placing three-dimensional foamed graphene/ITO glass upside down in the mixed solution in the reaction vessel, covering reaction vessel lid, reacting at 160-200 degrees C for 10-14 hours, removing out, naturally cooling to room temperature in air to obtain composite material, opening reaction vessel, washing composite with distilled water, maintaining temperature at 400-500 degrees C for 0.5-1.5 hours, cooling furnace to room temperature to obtain zinc sulfide nanosphere array/foam graphene.