▎ 摘 要
NOVELTY - Preparing rose-shaped vanadium sulfide nanosphere-reduced graphene oxide material electrode comprises (1) adding thioacetamide and sodium metavanadate into deionized water, adding aqueous ammonia, gradually changing solution into light yellow, transferring into polytetrafluoroethylene lining, naturally cooling the product, filtering, drying, (2) adding graphene oxide, stirring, transferring into polytetrafluoroethylene lining, (3) mixing material in deionized water to obtain the suspension, cleaning the ITO conductive glass in acetone solution, ethanol solution and deionized water, naturally drying, spraying on ITO conductive glass by the automatic spraying device, preparing the vanadium sulfide nanosphere-graphene oxide/ITO electrode and (d) placing the obtained vanadium sulfide nanosphere-graphene oxide/ITO in a tubular furnace and heating under the protection of argon to obtain vanadium sulfide nanosphere-reduced graphene oxide/ITO electrode. USE - The material is useful as a working electrode of a biosensor and enzyme-free modified electrochemical detecting of the epinephrine (claimed). ADVANTAGE - The method: is simple and low in cost. The material: has good sensitivity; is uniformly distributed in the reduced graphene oxide nanosphere, providing a high specific surface area, rich active sites, and good conductivity of materials and has strong electrochemical signal response to epinephrine, when using. DETAILED DESCRIPTION - Preparing rose-shaped vanadium sulfide nanosphere-reduced graphene oxide material electrode comprises (1) preparing three-dimensional rose-shaped vanadium sulfide nanosphere by (1a) adding 1-2 g thioacetamide and 0.2-0.3 g sodium metavanadate into 60-80 ml deionized water, adding a certain amount of aqueous ammonia, placing in the magnetic stirrer to stir at 400-600 revolutions/minute, gradually changing the solution into light yellow, (1b) transferring the above mixed solution into 100 ml polytetrafluoroethylene lining, placing in stainless steel autoclave, screwing the stainless steel autoclave, heating for 6-9 hours at a certain temperature, (1c) naturally cooling the product obtained by the hydrothermal reaction to room temperature in the air, cleaning the obtained material with deionized water and ethanol, filtering, drying for 4-6 hours at 80 degrees C in the vacuum furnace to obtain the three-dimensional rose-shaped vanadium sulfide nanosphere, (2) adding a certain amount of graphene oxide to the above mixed solution, placing the magnetic stirrer to stir, stirring until the solution becomes dark black for 1-3 hours to obtain the hydrothermal reaction solution, transferring the mixed solution into 100 ml polytetrafluoroethylene lining, placing in the stainless steel autoclave, screwing the stainless steel autoclave, heating for 6-9 hours at 170 degrees C, naturally cooling the product obtained by the hydrothermal reaction to room temperature in the air, cleaning the obtained material with deionized water and ethanol, filtering, drying for 4-6 hours at 80 degrees C in the vacuum furnace, obtaining the rose-shaped vanadium sulfide nanosphere-graphene oxide material, (3) preparing the vanadium sulfide nanosphere-graphene oxide/indium tin oxide (ITO) electrode by automatic spraying method by (3a) using electronic balance to weigh 20-30 mg rose-shaped vanadium sulfide nanosphere-graphene oxide material, mixing in 40-50 ml deionized water to obtain the suspension, cleaning the ITO conductive glass for 10 minutes in the acetone solution, ethanol solution and deionized water, naturally drying at room temperature, fixing the six ITO conductive glass on the heating plate of the automatic spraying device, fixing the ITO conductive glass clamp electrode line on one side of the heating plate by the transparent adhesive tape, where the electrode line can be directly contact with the ITO conductive glass when detecting, placing the suspension in the spray gun, spraying on the ITO conductive glass by the automatic spraying device, preparing the vanadium sulfide nanosphere-graphene oxide/ITO electrode, where the whole spraying process is carried out at a pressure of 10 psi, the distance between the nozzle of the spray gun and the ITO conductive glass is 15 cm, the temperature of the heating plate is 120 degrees C, continuously stirring the suspension in thbime spraying process and (d) placing the obtained vanadium sulfide nanosphere-graphene oxide/ITO in a tubular furnace and heating at 400-600 degrees C under the protection of argon to obtain vanadium sulfide nanosphere-reduced graphene oxide/ITO electrode, where the flow speed of argon is 200-500 sccm and the heating time is 1-2 hours.