• 专利标题:   Quickly preparing graphene oxide film, useful e.g. in paper batteries, comprises agitating e.g. crystalline graphite powder, adding hydrogen peroxide, reacting to obtain graphite oxide, preparing graphene oxide layer, and pouring on glass.
  • 专利号:   CN102249220-A
  • 发明人:   CHANG D, HAN F, WANG X, WANG Y
  • 专利权人:   UNIV TAIYUAN TECHNOLOGY
  • 国际专利分类:   C01B031/04
  • 专利详细信息:   CN102249220-A 23 Nov 2011 C01B-031/04 201268 Chinese
  • 申请详细信息:   CN102249220-A CN10066634 18 Mar 2011
  • 优先权号:   CN10066634

▎ 摘  要

NOVELTY - Quickly preparing graphene oxide film comprises taking a flat glass, abrading, polishing, cleaning to form a mirror surface, taking four-neck flask, adding crystalline graphite powder, sodium nitrate and vitriol, agitating, adding potassium permanganate and deionized water, agitating, adding hydrogen peroxide and deionized water, reacting to obtain graphite oxide, ultrasonically processing to obtain a slurry, centrifuging, dissolving the pellet in deionized water, adding nitric acid solution, agitating, allowing to stand to obtain graphene oxide layer, pouring on flat glass, and drying. USE - The graphene oxide film is useful in paper battery materials and fuel cells catalyst carrier. ADVANTAGE - The film has high strength, strong toughness, and high crack resistance. The method is short, fast, easy, and suitable for large scale production. DETAILED DESCRIPTION - Quickly preparing graphene oxide film comprises: (a) selecting chemical materials comprising 0.016-0.032 mu m flat glass (solid) based on surface roughness Ra, 98% crystalline flake graphite powder (solid), 95% vitriol (liquid) based on mass consistency, 99.7% sodium nitrate (solid), 30% hydrogen peroxide (liquid) based on mass consistency, 99.9% deionized water (liquid), 95% oil bathing oil (liquid), 5 mol/l nitric acid (liquid), 99% nitrogen (gas), an abrasive paste (solid) containing silicon carbide (76%) and soft and flat deerskin (solid), controlling the mass purity, consistency and precision; (b) transferring the flat glass on a steel flat, abrading the plain through the abrasive paste, polishing via the deerskin, cleaning with deionized water for 60 minutes until the upper surface roughness is (Ra) 0.016-0.032 mu m, and forming a mirror surface; (c) transferring deionized water (500 ml) into a stainless steel container, storing the container into a refrigerator to freeze into ice at -15 degrees C, adding deionized water (1000 ml), agitating and mixing to obtain ice-water mixture, and allowing to stand; (d) taking four-neck flask, and placing on an oil bathing cylinder, mounting the oil bathing cylinder on an electric heating controller, mounting a nitrogen tube, a liquid adding funnel, an agitator and a water cycle condensation tube at the upper part of the four-neck flasks from left to right by: (d1) cleaning the inner side of the four-neck flask with deionized water (500 ml) until clean, and drying in air, (d2) weighing crystalline graphite powder (3 plus minus 0.01 g), sodium nitrate (1.5 plus minus 0.001) and vitriol (65 plus minus 0.1 ml), adding the materials into the four-neck flasks through the liquid adding funnel, (d3) transferring the four-neck flask on a beaker with the ice-water mixture, starting the agitator to agitate for 3 minutes to mix the solution, cooling from 25 degrees C to 10 degrees C, synchronously agitating and adding potassium permanganate (9 plus minus 0.01 g), continuously agitating for 10 minutes, allowing to stand, (d4) adding oil bathing oil (300 ml) to the oil bathing cylinder, transferring the four-neck flask into the oil bathing cylinder, covering 4/5 volume of the four-neck flask via the oil bathing oil, synchronously starting the nitrogen tube to supply nitrogen at a speed of 20 cm3/minute, and simultaneously starting the water cycle condensation tube, (d5) starting the electric heating controller to gradually rise the temperature in the four-neck flask to 35 degrees C, and continuously agitating for 30 minutes, (d6) adding deionized water (100 plus minus 1 ml) into the four-neck flask through the liquid adding funnel along with agitation until the color in the four-neck flask is bright yellow, (d7) continuously starting the electric heating controller to rise the temperature from 35 degrees C to 90 plus minus 2 degrees C, continuously agitating for 40 plus minus 2 minutes, (d8) synchronously agitating and adding hydrogen peroxide (50 plus minus 0.1 ml), adding deionized water (60 plus minus 1 ml) to dilute, (d9) chemically reacting the solution in the four-neck flask while cooling, heating, agitating and mixing, and (d10) closing the electric heating controller, the agitator, the water cycle condensation tube and the nitrogen tube to naturally cool the mixing solution in the four-neck flask to 25 degrees C along with the flask, cleaning and drying the material with deionized water to obtain graphite oxide; (e) preparing graphene oxide film by (e1) weighing graphite oxide (0.1 plus minus 0.0003 g) and adding into a beaker, adding deionized water (200 ml), ultrasonically processing the breaker into an ultrasonic cleaner at a power of 150 W for 60 minutes to obtain a slurry, (e2) pouring the slurry from the beaker into a centrifuge tube, centrifuging at 5000 revolutions per minute for 10 minutes, retaining graphite oxide at the bottom of the centrifuge tube, and dissolving in deionized water, (e3) collecting the solution containing dissolved graphene oxide in the breaker, adding 5 mol/l aqueous nitric acid solution (1 plus minus 0.01 ml), agitating, allowing to stand for 30 minutes until the flocculent separates out, where the liquid is divided into an upper layer which is the liquid and a lower layer which is offwhite graphene oxide after precipitating, removing the liquid at the upper layer, retaining the offwhite graphene oxide at the lower layer, (e4) pouring the precipitate at the lower layer on the flat glass to naturally flow in the liquid membrane, and naturally drying in air, (e5) transferring the liquid membrane flat glass into a vacuum dryer for 1440 minutes at 50 plus minus 2 degrees C and a vacuum degree of 5 Pa, (e6) generating the complete brownish-yellow graphene oxide film on the flat glass after drying to obtain the final product, and (e7) lifting the film through tweezers to transfer into a clean flat-bottom glass container to uniformly pave; (f) detecting, testing, analyzing and characterizing the appearance, color, thickness, components, physicochemical property and mechanical performance of the prepared graphene oxide film, analyzing the appearance through a scanning electron microscope and a transmission electron microscope, analyzing the component of the element through a X-ray photoelectron spectrometer, where the graphene oxide film layer is 1-2 mu m thick, and the components comprises single or multiple layers of graphene oxide films; and (g) uniformly paving the prepared graphene oxide sheet type film into a colorless transparent glass container, storing under dark, cool, clean, dry, waterproof, sunshine-proof, moisture-proof, alkali and sodium corrosion resistant conditions, and the storing at 20 plus minus 2 degrees C and a relative humidity of not greater than 10%.