• 专利标题:   Preparing special shape zinc oxide thin film comprises e.g. using modified Hummers method preparing graphene oxide ice water bath and under strong stirring condition, adding potassium nitrate or sodium nitrate into the container.
  • 专利号:   CN106542744-A, CN106542744-B
  • 发明人:   QIN X, WANG L, ZHANG L, LU L, WANG X, SHAO G
  • 专利权人:   UNIV YANSHAN, UNIV YANSHAN
  • 国际专利分类:   C03C017/34, C08J007/06
  • 专利详细信息:   CN106542744-A 29 Mar 2017 C03C-017/34 201735 Pages: 10 Chinese
  • 申请详细信息:   CN106542744-A CN10959565 28 Oct 2016
  • 优先权号:   CN10959565

▎ 摘  要

NOVELTY - Preparing special shape zinc oxide thin film comprises e.g. using modified Hummers method preparing graphene oxide ice water bath and under strong stirring condition, adding potassium nitrate or sodium nitrate into the container, concentrated sulfuric acid and crystalline flake graphite, where the mass ratio of the potassium nitrate or sodium nitrate, concentrated sulfuric acid and crystalline flake graphite is 2-3:175-182:2, after 0.5-1 hours, slowly adding potassium permanganate, where potassium permanganate and potassium nitrate mass ratio is 16:1-3, and transferring to water bath. USE - The method is useful for preparing special shape zinc oxide thin film (claimed). ADVANTAGE - The method is simple, has good controllability, through adjusting performance of graphene oxide template, realizes the controllable growth of special shape zinc oxide transparent film, prepared zinc oxide film has multi-level structure shape, suitable for photo-catalysis, dye-sensitized solar battery, gas sensor fields. DETAILED DESCRIPTION - Preparing special shape zinc oxide thin film comprises (i) using modified Hummers method preparing graphene oxide ice water bath and under strong stirring condition, adding potassium nitrate or sodium nitrate into the container, concentrated sulfuric acid and crystalline flake graphite, where the mass ratio of the potassium nitrate or sodium nitrate, concentrated sulfuric acid and crystalline flake graphite is 2-3:175-182:2, after 0.5-1 hours, slowly adding potassium permanganate, where potassium permanganate and potassium nitrate mass ratio is 16:1-3, transferring to 30-40 degrees C stirring the water bath for 2-6 hours, with the speed of 1-3 drops/second mixture with de-ionized water by mass ratio of 1-1.2:2 adding deionized water to the mixture, transferring to 75-85 degrees C water bath, heating for 20-40 minutes, after finishing dropping, naturally cooling, adding 10-30% hydrogen peroxide to the mixed solution until the residual oxidant reduces, removing supernatant, using dilute hydrochloric acid and de-ionized water washing precipitate to neutral, removing unreacted graphite with low speed to obtain oxidized graphene, (ii) dispersing the step (i) oxidized graphene in dispersion liquid absolute ethyl alcohol solution to obtain 0.5-1.0 mg/ml graphene oxide, stirring uniformly, adding into ultrasonic oscillator, under 90-105 W oscillating for 10-20 minutes, after completely dispersing the graphene oxide, loading into centrifugal tube in the grading process, centrifuging at 1000 revolutions/minute for 4-6 minutes, taking supernatant, centrifuging at 4000 revolutions/minute for 4-6 minutes, taking precipitate, the constant volume to mass concentration is 0.5-1.0 mg/ml graphene oxide dispersion, (iii) pre-treating the substrate normal glass substrate after conventional cleaning program, using Piranha (man-eating fish) hydroxylating the substrate solution, or polyethylene terephthalate substrate cleaning, (iv) coating step (ii) graphene oxide dispersion film on the step (iii) glass substrate, maintaining pulling speed at 1-14 mm/minute, lifting layer 8-12, lifting the glass substrate, soaking in graphene oxide dispersion liquid for 1-2 minutes, does not need to soak, using drop-coating preparing graphene oxide film on the polyethylene terephthalate substrate, 0.2 ml the graphene oxide dispersion prepared in the step (ii), after four times dropping on the polyethylene terephthalate substrate, after the droplet is completely spread out on the substrate, drying by nitrogen to obtain the graphene oxide film, and (v) preparing zinc oxide film using de-ionized water as solvent, zinc nitrate hexahydrate as solute, adding hexamethylene tetramine quality e.g. nitric acid zinc, preparing into 0.05-0.07 mol/l zinc nitrate precursor, placing the step (iv) graphene oxide film coated glass substrate in a reaction kettle of polytetrafluoroethylene liner nitrate precursor at 80-90 degrees C constant temperature for 6-9 hours, cooling with the furnace, taking out the substrate, drying to obtain zinc oxide transparent film, taking absolute ethyl alcohol as solvent, zinc nitrate hexahydrate as solute, adding hexamethylene tetramine quality e.g. nitric acid zinc, preparing into 0.05-0.07 mol/l zinc nitrate precursor, placing the zinc precursor into polytetrafluoroethylene liner reaction kettle in the step (iv) polyethylene terephthalate substrate coated with graphene oxide film into the reaction kettle at 60-80 degrees C constant temperature for 3-5 hours, cooling to room temperature with the furnace, and taking out the substrate and drying to obtain zinc oxide film.