• 专利标题:   Preparation of surface nickel nanoparticle-modified graphene nanomaterial by reacting graphite with hydrogen peroxide, peeling off graphite oxide layer to obtain graphene oxide, and reacting graphene oxide with nickel sulfate hexahydrate.
  • 专利号:   CN102583348-A, CN102583348-B
  • 发明人:   BAO T, DUAN Y, LI X, SUN J, WANG Y, ZHAO Y
  • 专利权人:   UNIV BEIJING AERONAUTICS ASTRONAUTICS
  • 国际专利分类:   B82Y040/00, C01B031/04, H01F001/12
  • 专利详细信息:   CN102583348-A 18 Jul 2012 C01B-031/04 201308 Pages: 13 Chinese
  • 申请详细信息:   CN102583348-A CN10039625 20 Feb 2012
  • 优先权号:   CN10039625

▎ 摘  要

NOVELTY - Surface nickel nanoparticle-modified graphene nanomaterial is prepared by mixing graphite, potassium nitrate and concentrated sulfuric acid, adding potassium permanganate and reacting for 6 hours, then dripping hydrogen peroxide into mixed solution, and drying to obtain graphite oxide solid; ultrasonically dispersing graphite oxide into water to fully peel off graphite oxide layer to obtain graphene oxide; reacting graphene oxide with tin(II) chloride and adding palladium(II) chloride to obtain modified graphene oxide; and reacting modified graphene oxide with nickel sulfate hexahydrate. USE - Method of preparing surface nickel nanoparticle-modified graphene nanomaterial (claimed). ADVANTAGE - The method can effectively control surface of nickel particles and crystal grain size and the oxidized graphene part. The deposition of nickel particles can prevent stacking of graphene sheet layer and provide the graphene layer with excellent soft magnetic material, where minimum external magnetic field can be magnetized. DETAILED DESCRIPTION - Preparation of surface nickel nanoparticle-modified graphene nanomaterial comprises: (A) mixing graphite, potassium nitrate and concentrated sulfuric acid, adding potassium permanganate at 35-40 degrees C, conducting magnetic stirring and reacting for 6 hours, then adding slowly adding deionized water to the mixture and regulating water bath temperature to 60-70 degrees C, reacting for 25-40 hours, adding deionized water, continuously reacting for 4-5 minutes, then dripping 30 mass% hydrogen peroxide into the mixed solution till the mixed solution is bright yellow, rinsing with deionized water to neutral and till the vacuum degree is - 0.1 MPa, and drying at 80-120 degrees C to obtain graphite oxide solid; (B) using ultrasonic dispersion method to peel graphite oxide to obtain graphene, where the operation comprises dissolving graphite oxide (500 mg) into deionized water (300 ml) and ultrasonically dispersing for two hours to fully peel off the graphite oxide layer to obtain graphene oxide aqueous solution; (C) adding tin(II) chloride (75 g) into 37 mass% concentrated hydrochloric acid (50 ml), dispersing graphene oxide aqueous solution (300 ml), then adding deionized water to prepare mixed liquid (500 ml) to obtain black flocculent solid, and ultrasonically scattering for 60 minutes at 60 degrees C in water bath; (D) adding palladium(II) chloride (1 g) into 37 mass% concentrated hydrochloric acid (50 ml), then adding into the black flocculent solid after filtering and adding water to prepare into mixed solution (500 ml), reacting for 60 minutes at 60 degrees C in water bath, ultrasonically dispersing, after the reaction is finished, adding the mixed liquid through a sand core and filtering, and cleaning till it is neutral with deionized water, then oven drying the product at 80 degrees C to obtain modified graphene oxide; (E) adding sodium citrate (41 g), nickel sulfate hexahydrate (10 g) and sodium hypophosphite (17 g) in deionized water (500 ml) to mix, after uniformly mixing, and adding ammonia water to adjust pH value to 10 to obtain reaction solution; and (F) taking reaction solution (500 ml), adding modified graphene oxide (200 mg), reacting at 60 degrees C till there is no bubble generated, stopping reaction, using sand core solvent filtering device to filter to obtain product, and drying product at 80 degrees C to obtain the surface nickel nanoparticle-modified graphene nanomaterial. An INDEPENDENT CLAIM is included for a surface nickel nanoparticle-modified graphene nanomaterial having a two-phase structure which is sheet-shaped carrier, where the nickel nanoparticle deposited on the surface is centered cubic crystal with nickel content of 17.27%.