CN102120186A - Preparation method of platinum nanoparticle loaded graphene - Google Patents
Preparation method of platinum nanoparticle loaded graphene Download PDFInfo
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- CN102120186A CN102120186A CN201010552955XA CN201010552955A CN102120186A CN 102120186 A CN102120186 A CN 102120186A CN 201010552955X A CN201010552955X A CN 201010552955XA CN 201010552955 A CN201010552955 A CN 201010552955A CN 102120186 A CN102120186 A CN 102120186A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention relates to a preparation method of platinum nanoparticle loaded graphene, comprising the following steps: (1), ultrasonically disperse restored graphene in a glycol solution, and adding the glycol solution of 1-pyrene methylamine, wherein the ratio (mg: ml: ml) of the graphene to the glycol to the glycol solution of the 1-pyrene methylamine is 1: (8-20): (1-1.5), and the concentration of the glycol solution of the 1-pyrene methylamine is 10<-3> M; stirring for 20-120 minutes to assemble the 1-pyrene methylamine on the surface of the graphene; and (2), adding Nml of a 0.048M chloroplatinic acid glycol solution, wherein the ratio (mg: ml) of the graphene to the Nml is 1: (0.8-1.5); adjusting the pH value of the glycol solution in the step (1) to be 8-9 with 0.1 M sodium hydroxide, continuing to stir, reacting for 2 hours in the oil bath at the temperature of 160 DEG C to obtain the high-density platinum nanoparticle loaded graphene, and cleaning and performing freeze-drying.
Description
Technical field:
The present invention be a kind of on Graphene the preparation method of high density supported platinum nano particle.
Technical background:
Graphene just has been subjected to extensive concern since 2004 are found by people such as Novoselov.This two-dimensional material has the electron mobility [1] of superelevation under the room temperature, higher mechanical strength [2], high specific area and good heat endurance [3], make it as the nano electron device material, sensor material, battery material, catalysis material fields such as [4] has application prospects.Recently, more and more paid close attention to as the carrier of catalysis material, and the work of having delivered has proved that the composite of this platinum/graphen has good catalytic performance [5,6], can well be applied in the methanol fuel cell by people with Graphene.But inertia and slickness because of the Graphene surface make that the Pt nanoparticle that directly reaches than steady load at Graphene surface acquisition higher density is very difficult, so the Graphene that electronation at present obtains often is used as the carrier of nano particle, because more not reduction group and defective, fixedly nano particle are contained in the Graphene surface that this method obtains.But the particulate load amount and the quality of the composite that the randomness of group and defect distribution of not reducing make to obtain also are restricted.The purpose of present patent application is by self-assembling method, the composite of high density supported platinum nano particle on the preparation electronation Graphene.The method not only can realize platinum high density, high load uniformly, because it is not with the not reduction group and the defective load platinum on surface, so can also be applied to composite synthetic of the Graphene that method of reducing non-chemically obtains.
Relating to Graphene area load method of metal nanoparticles can be referring to the open CN101797502A of Chinese patent, a kind of method for making of noble metal-graphene nanometer composite.Its key step is that noble metal precursor salt and electrolytic salt are joined in the aqueous solution that contains surfactant; Add the Graphene that water disperses in proportion, regulate the pH value, adopt the method for ultrasonic electrochemical, under constant current density and ultrasound intensity, react, make noble metal-graphene nanometer composite.The open CN101799444A of Chinese patent, graphene-Pt nano composite material synthesized by microwave method and application process thereof.Its method is that graphite oxide is dissolved in the hexylene glycol solution, handle through ultrasonic wave, chloroplatinic acid hexylene glycol drips of solution is added in the said mixture, stir the mixed solution that the back adds NaOH/hexylene glycol, put into microwave after stirring again and handle, obtain Graphene platinum nano composite material.These two kinds of methods all do not relate to carries out surperficial self-assembled modified load.
[1]K.I.Bolotin，K.J.Sikes，Z.Jiamg，M.Klima，G.Fudenberg，J.Hone，P.Kim?andStormer，Solid?State?Commun.2008，146，351.
[2]T.J.Booth，P.Blake，R.R.Nair，D.Jiang，E.W.Hill，U.Bangert，A.Bleloch，M.K.S.Novoselov，M.I.Katsnelson，A.K.Geim，Nano?Lett.2008，8，2442.
[3]H.M.A.Hassan，V.Abdelsayed，A.E.R.S.Khder，K.M.AbouZeid，J.Terner，]El-Shall，S.I.Al-Resayes，A.A.El-Azhary，J.Mater.Chem.2009，19，3832.
[4]A.K.Geim，K.S.Novoselov.Nat.Mater.2007，6，183.
[5]C.Xu，X.?Wang，J.W.Zhu，J.Phys.Chem.C?2008，112，19841.
[6]Y.J.Li，W.Gao，L.J.Ci，C.M.Wang，P.M.Ajayan，carbon?2010，48，1124.
Summary of the invention
The objective of the invention is to propose a kind of by self-assembled modified, the preparation method of the composite of high density supported platinum nano particle on the electronation Graphene
Technical scheme of the present invention is: the preparation method of supported platinum nano particle on Graphene, obtain the Graphene of reduction by the common chemical reduction, the interaction that utilizes π-π afterwards is at the self-assembled modified one deck 1-pyrene methylamine in Graphene surface, because the amino load that exists for nano particle provides nuclearing centre, so at last the Graphene of 1-pyrene methylamine modified is put into reduction of ethylene glycol chloroplatinic acid system, the composite of preparation supported platinum nano particle.
Concrete preparation method:
(1) gets ultrasonic being dispersed in the ethylene glycol solution of Graphene of reduction, add the ethylene glycol solution of 1-pyrene methylamine again, the ratio of the ethylene glycol solution of Graphene, ethylene glycol and 1-pyrene methylamine (mg: ml: be 1 ml): 8-20: 1-1.5; The concentration of the ethylene glycol solution of 1-pyrene methylamine is 10
-3M stirred 20-120 minute, made 1-pyrene methylamine self-assemble to the Graphene surface;
(2) the chloroplatinic acid ethylene glycol solution of the 0.048M of adding Nml, Graphene is than Nml (mg: be 1 ml): 0.8-1.5, regulating (1) middle ethylene glycol solution adjusting pH value with the NaOH of 0.1M is 8-9, continue to stir, reaction obtained high density supported platinum nano particle on the Graphene in 2 hours in 160 ℃ oil bath; Clean freeze-drying afterwards.
(3) interaction that utilizes π-π of 1-pyrene methylamine forms self-assembled film on the Graphene surface, and the lone pair electrons of nitrogen can interact with platinum in the amino, for the load of platinum provides nuclearing centre
(4) non-chemically the Graphene of reduction also can obtain the high load of platinum uniformly of high density by the method.
(5) Graphene that reduces by common chemical reduction acquisition: under 95 ℃, be equipped with graphite oxide, reacted a hour, clean freeze-drying, obtain the Graphene that reduces with hydrazine reduction Hummers legal system.
The present invention relates to the preparation of high density supported platinum nano particle on Graphene, the interaction of 4 phenyl ring by pyrene and the π-π on Graphene surface is at the self-assembled modified one deck 1-pyrene methylamine in Graphene surface, then owing to the lone pair electrons of nitrogen in the amino and the interaction of platinum, for the Pt nanoparticle load provides nuclearing centre, obtain the composite of supported platinum nano particle, the granular size of platinum is between 2-5nm, and height is evenly distributed on the Graphene, and high density has covered the Graphene surface.This composite can be applied in the methanol fuel cell because its good catalytic performance, and in other catalysis and field such as SERS good prospects for application is arranged.
The invention has the beneficial effects as follows: can obtain high density, the composite of high uniform load Pt nanoparticle, course of reaction is simple, and can be applicable to non-chemically to reduce the Graphene of preparation.
Description of drawings
Fig. 1: the finishing principle schematic of load platinum is again carried out in self assembly
Fig. 2: (a) electromicroscopic photograph of the Graphene of area load Pt nanoparticle, scale is 100nm; (b) Electronic Speculum enlarged photograph, scale 10nm.
Fig. 3:, carry out the characteristic element imaging for proving the self-assembled modified of certain realization 1-pyrene methylamine.Be respectively the SEM photo, the element imaging of C, the element imaging of N, the element imaging of Pt
The specific embodiment
The exemplary steps of the composite of high density supported platinum nano particle is as follows on the preparation electronation Graphene:
(1) hydrazine electronation graphite oxide: under 95 ℃, the graphite oxide with the preparation of hydrazine reduction Hummers method reacted one hour, cleaned freeze-drying, obtained the Graphene of reduction.
(2) at the self-assembled modified one deck 1-pyrene methylamine in Graphene surface, 1-pyrene methylamine utilizes the interaction of π-π to form self-assembled film on the Graphene surface: get in the ultrasonic 80ml of the being dispersed in ethylene glycol solution of Graphene of 8mg reduction, adding 12ml concentration is 10
-3The ethylene glycol solution of the 1-pyrene methylamine of M stirs 30 minutes (room temperature gets final product).Make 1-pyrene methylamine self-assemble to the Graphene surface
(3) ethylene glycol is in the pH8-9 interval, and 160 ℃ of following reduction chloroplatinic acids prepare Pt nanoparticle.Obtain the composite of high platinum load: add the chloroplatinic acid ethylene glycol solution of the 0.048M of 0.8ml, with the NaOH of 0.1M the ethylene glycol solution of step (2) being regulated the pH value is 8-9, continues to stir, and reaction is 2 hours in 160 ℃ oil bath.Clean freeze-drying afterwards, obtain sample.
(4) interaction that utilizes π-π of 1-pyrene methylamine forms self-assembled film on the Graphene surface, and the lone pair electrons of nitrogen can interact with platinum in the amino, for the load of platinum provides nuclearing centre
(5) non-chemically the Graphene of reduction also can obtain the high load of platinum uniformly of high density by the method.
Claims (1)
1. the preparation method of supported platinum nano particle on Graphene, it is characterized in that the step for preparing is as follows: (1) gets ultrasonic being dispersed in the ethylene glycol solution of Graphene of reduction, the ethylene glycol solution that adds 1-pyrene methylamine again, the ratio of the ethylene glycol solution of Graphene, ethylene glycol and 1-pyrene methylamine (mg: ml: be 1 ml): 8-20: 1-1.5; The concentration of the ethylene glycol solution of 1-pyrene methylamine is 10
-3M stirred 20-120 minute, made 1-pyrene methylamine self-assemble to the Graphene surface;
(2) the chloroplatinic acid ethylene glycol solution of the 0.048M of adding Nml, Graphene is than Nml (mg: be 1 ml): 0.8-1.5, regulating (1) middle ethylene glycol solution adjusting pH value with the NaOH of 0.1M is 8-9, continue to stir, reaction obtained high density supported platinum nano particle on the Graphene in 2 hours in 160 ℃ oil bath; Clean freeze-drying afterwards.2, according to claim 1 on Graphene the preparation method of high density supported platinum nano particle, it is characterized in that by under 95 ℃ be equipped with graphite oxide with hydrazine reduction Hummers legal system, the Graphene of this reduction is the supported platinum nano particle again.
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| CN102909005A (en) * | 2012-10-24 | 2013-02-06 | 中国科学院理化技术研究所 | Graphene-based composite material with surface coated by mesoporous silica and loaded with noble metal nanoparticles, as well as preparation method and application of graphene-based composite material |
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