• 专利标题:   Preparation of zinc oxide nanorod-graphene nanosheet used for high sensitivity and high selectivity detection of uric acid, by mixing hexamethylenetetramine and sodium hydroxide solutions, ultrasonically treating and hydrothermally reacting.
  • 专利号:   CN106596674-A, CN106596674-B
  • 发明人:   YUE H, WANG Q, GAO X, WANG B, LIN X, YAO L, GUO E
  • 专利权人:   UNIV HARBIN SCI TECHNOLOGY
  • 国际专利分类:   B82Y030/00, B82Y040/00, G01N027/327
  • 专利详细信息:   CN106596674-A 26 Apr 2017 G01N-027/327 201742 Pages: 12 Chinese
  • 申请详细信息:   CN106596674-A CN11174173 19 Dec 2016
  • 优先权号:   CN11174173

▎ 摘  要

NOVELTY - A zinc oxide nanorod-graphene nanosheet is prepared by mixing zinc nitrate hexahydrate solution, hexamethylenetetramine solution and sodium hydroxide solution, moving into beaker, ultrasonically treating, pouring into PTFE lining reaction kettle for hydrothermal reaction, heating into vacuum drying box, taking out reaction kettle, naturally cooling, ultrasonically treating, standing product into large beaker, precipitating, washing, separating out deposit by centrifuge, and drying precipitate at into vacuum drying box to obtain zinc oxide nanorod. USE - Method for preparing zinc oxide nanorod-graphene nanosheet (claimed) used for high sensitivity and high selectivity detection of uric acid. ADVANTAGE - The nanosheet has high specific surface area and good conductivity and biological compatibility. DETAILED DESCRIPTION - A zinc oxide nanorod-graphene nanosheet is prepared by: (A) mixing 0.03-0.07 mol/L zinc nitrate hexahydrate solution, 0.03-0.07 mol/L hexamethylenetetramine solution and 0.36-1.2 mol/L sodium hydroxide solution for 3-5 minutes, moving into beaker, ultrasonically treating for 30 minutes, pouring into PTFE lining reaction kettle for hydrothermal reaction, heating into vacuum drying box at 100 degrees C, taking out reaction kettle, naturally cooling to room temperature, ultrasonically treating for 30 minutes, standing product into large beaker, precipitating, washing, separating out deposit by centrifuge, and drying precipitate at into vacuum drying box at 80 degrees C for 6 hours to obtain zinc oxide nanorod; (B) placing template foam nickel in the center of quartz tube furnace, heating under argon gas and hydrogen gas protection from room temperature to 1010 degrees C at rate of 20-40 degrees C/minute, insulating for 30-60 minutes, continuously introducing methane gas at rate of 10 sccm for 10 minutes, and rapid cooling to room temperature at rate of 80-100 degrees C/minute to obtain graphene coated foam nickel having density of 420-440 g/m2 and thickness of 1.6-2.0 mm; (C) cutting to sample of 1 cmasterisk1 cm, dropping 4 wt.% poly(methyl methacrylate) (PPMA) (4 g PMMA dissolved in 100 g ethyl lactate), curing at 180 degrees C for 30 minutes, protecting three-dimensional porous structure of the sample, putting into 3% hydrochloric acid solution at 90 degrees C for 5-10 hours, and removing nickel in the sample; (D) putting into 60 degrees C acetone solution for 1 hour to remove graphene surface of PMMA, transferring into indium tin oxide glass surface to obtain three-dimensional graphene foam, ultrasonically dispersing in deionized water, and ultrasonically dispersing at 540 W (maximal power of 600 W); (E) mixing 0.01 g zinc oxide, 3 mL graphene suspension and 17 mL water to obtain zinc oxide nanorod-graphene nanosheet mixed solution, ultrasonically dispersing to obtain uniform suspension, ultrasonically cleaning indium tin oxide conductive glass in acetone solution, ethanol solution and deionized water, naturally cooling and drying at room temperature, and fixing 6 indium tin oxide conductive glass on spraying device heating plate; and (F) automatically spraying uniform suspension at 10 psi (10 lb/in2), nozzle distance to indium tin oxide conductive glass of 10-15 cm and heating plate temperature of 110 degrees C, coating in quartz tube furnace under 400 sccm argon gas protection, heating at 700 degrees C at speed of 10 degrees C/minute, insulating for 2 hours, and cooling to room temperature. The flow rate of argon gas and hydrogen gas is 480-500 sccm and 180-200 sccm, respectively.