CN102174702A - Preparation method for metallic nano-particle and graphene composite - Google Patents
Preparation method for metallic nano-particle and graphene composite Download PDFInfo
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- CN102174702A CN102174702A CN 201110004729 CN201110004729A CN102174702A CN 102174702 A CN102174702 A CN 102174702A CN 201110004729 CN201110004729 CN 201110004729 CN 201110004729 A CN201110004729 A CN 201110004729A CN 102174702 A CN102174702 A CN 102174702A
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Abstract
The invention relates to a preparation method for a metallic nano-particle and graphene composite. In the method, a conducting base is taken as a working electrode; the working electrode, a counter electrode and a reference electrode are placed into an aqueous dispersion containing graphene oxide and metallic compound; and graphene oxide and metallic compound are reduced and electro-deposited on the surface of the working electrode. The metallic nano-particle and graphene composite can be widely used in field of sensors, transparent electrodes, capacitors, batteries, catalysis and the like.
Description
Technical field:
The present invention relates to a kind of preparation method of metal nanoparticle-graphene complex.
Background technology:
Since finding Graphene, because machinery, electronics and the thermal stability of its excellence, Graphene and mixture thereof are subjected to people in application aspect electron device, electrode, battery, electrical condenser and the transmitter and extensively pay attention to, and become the popular research field in the current world.One is that mixture by chemistry or thermal reduction graphene oxide (or Graphene) metallizing thing obtains for metal current-graphene complex.These methods relate to highly toxic chemical reducing agent such as hydrazine hydrate etc., or require hot conditions, and often need multistep, and are more consuming time; In addition, Graphene and metallic particles all may be assembled in the mixture.
Summary of the invention:
The object of the invention is that by an one-step electrochemistry redox graphene and a metallic compound Graphene that electrochemical reduction produces and metal nanoparticle are deposited on electrode surface and form laminated film.
A kind of preparation method of metal nanoparticle-graphene complex, with conductive substrates as working electrode, working electrode, counter electrode and reference electrode are inserted in the aqueous dispersions that contains graphene oxide and metallic compound, graphene oxide and metallic compound are reduced also galvanic deposit to working electrode surface.
The mode of described galvanic deposit comprises cyclic voltammetric mode, constant potential mode, impulse current system or pulsed voltage mode.
The reduction of graphene oxide and metallic compound and the galvanic deposit step to working electrode surface is comprised: the reduction potential that earlier the scanning current potential in the electrodeposition process is reached nominal price metal in the metallic compound, at the earlier independent metal refining nanoparticle of working electrode surface, to scan the reduction potential that current potential reaches graphene oxide then, Graphene and metallics are deposited to working electrode surface simultaneously; Above-mentioned galvanic deposit scanning potential operations then circulates.
Metal in the metallic compound comprises Pt, Pd, Au or Ag.
Metallic compound can be HAuCl
4, NH
4AuCl
4, HPtCl
4, (NH
4)
2PtCl
6, HPdCl
4, H
2PdCl
4, (NH
4)
2PdCl
4Or Na
3[Ag (S
2O
3)
2].
Counter electrode is selected from Pt, inert metals such as Pd.
Reference electrode is selected from standard electrodes such as SCE, Ag/AgCl.
Detailed process of the present invention is as follows: conductive substrates as working electrode, is inserted working electrode, counter electrode and reference electrode in the aqueous dispersions that contains graphene oxide and metallic compound.In electrodeposition process, will scan the reduction potential that current potential reaches the nominal price metal of metallic compound earlier, at the earlier independent metal refining nanoparticle of electrode surface, scan the reduction potential (this current potential also satisfies the reduction of nominal price metal) that current potential reaches graphene oxide then, Graphene and metallics are deposited to electrode surface simultaneously; Above-mentioned galvanic deposit scanning potential operations then circulates.Promptly scan the current potential that current potential is recycled to independent metal refining nanoparticle, begin independent metal refining nanoparticle again, be recycled to Graphene and metallics codeposition current potential, require to determine cycle number according to the deposition number of plies.
Characteristics such as it is simple to operate, green, quick that present method has, metallic particles is evenly distributed between the Graphene lamella in the matrix material that this method obtains, prevented the gathering of Graphene, and, can interact with metal nanoparticle and also prevent the reunion of metal nanoparticle because remaining very difficult quilt thoroughly reduces oxy radical on the Graphene.Prepare laminated film by method of the present invention and can be widely used in transmitter, transistor, transparency electrode, electrical condenser, catalyzer and prepare composite.
Description of drawings
Fig. 1. embodiment 1 is deposited on the scanning electron microscope diagram of the gold-graphene complex on glass-carbon electrode surface.
Fig. 2. embodiment 2 is deposited on the scanning electron microscope diagram of the platinum-graphene complex on glass-carbon electrode surface.
Fig. 3. embodiment 3 is deposited on the platinum-graphene complex sem photograph of gold electrode surfaces.
Fig. 4. embodiment 4 is deposited on the silver-graphitic alkene mixture sem photograph of gold electrode surfaces.
Fig. 5. embodiment 5 is deposited on the gold-graphene complex sem photograph of copper-tungsten electrode surface.
Fig. 6. embodiment 6 is deposited on the scanning electron microscope diagram of the gold-graphene complex on glass-carbon electrode surface.
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1:
(1) working electrode: polish, clean up glass-carbon electrode standby;
(2) preparation graphene oxide aqueous dispersions: graphene oxide is scattered in ionogen HAuCl
4Solution in, ultrasonic 30 minutes are stand-by;
(3) preparation of metal nanoparticle-graphene complex: with the glass-carbon electrode is working electrode, and platinum electrode is a counter electrode, and saturated calomel electrode is a reference electrode, and above three electrodes are placed graphene oxide, and (concentration is 1.0mgmL
-1) and HAuCl
4In the aqueous dispersions of (concentration is 100 μ M), on electrochemical workstation, carry out cyclic voltammetry scan, the scanning potential region is-1.5 volts to 0.6 volt, at first sweep to-1.5 volts from 0 volt, be swept to 0.6 volt from-1.5 volts then, be swept to 0 volt from 0.6 volt again, finish a circulation, scanning speed is 25 millivolts of per seconds.Fig. 1 is the scanning electron microscope diagram that is deposited on the gold-graphene complex on glass-carbon electrode surface.
Embodiment 2:
With HAuCl among the embodiment 1
4Change HPtCl into
4, all the other are with embodiment 1.Fig. 2 is the platinum-graphene film sem photograph that is deposited on the glass-carbon electrode surface.
Embodiment 3
Change glass-carbon electrode among the embodiment 1 into gold electrode, HAuCl
4Change HPtCl into
4, all the other are with embodiment 1.Fig. 3 is the platinum-graphene film sem photograph that is deposited on gold electrode surfaces.
Embodiment 4
With HPtCl among the embodiment 3
4Change Na3[Ag (S into
2O
3)
2], all the other are with embodiment 3.Fig. 4 is the silver-graphitic alkene film scanning Electronic Speculum figure that is deposited on gold electrode surfaces.
Embodiment 5
Change glass-carbon electrode among the embodiment 1 into the copper-tungsten electrode, all the other are with embodiment 1.Fig. 5 is the gold-graphene film sem photograph that is deposited on the copper-tungsten electrode surface.
Embodiment 6
Change cyclic voltammetry among the embodiment 1 into the pulsed electrical platen press, on-state voltage is-1.3 volts, and the ON state time is 0.5 second, and OFF state voltage is-0.000001 volt, and the OFF state time is 1.0 seconds.Fig. 6 is the scanning electron microscope diagram of gold-Graphene laminated film of being deposited on the glass-carbon electrode surface.
Claims (7)
1. the preparation method of a metal nanoparticle-graphene complex, it is characterized in that, with conductive substrates as working electrode, working electrode, counter electrode and reference electrode are inserted in the aqueous dispersions that contains graphene oxide and metallic compound, graphene oxide and metallic compound are reduced also galvanic deposit to working electrode surface.
2. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 is characterized in that, the mode of described galvanic deposit comprises cyclic voltammetric mode, constant potential mode, impulse current system or pulsed voltage mode.
3. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 and 2, it is characterized in that, the reduction of graphene oxide and metallic compound and the galvanic deposit step to working electrode surface is comprised: the reduction potential that earlier the scanning current potential in the electrodeposition process is reached nominal price metal in the metallic compound, at the earlier independent metal refining nanoparticle of working electrode surface, to scan the reduction potential that current potential reaches graphene oxide then, Graphene and metallics are deposited to working electrode surface simultaneously; Above-mentioned galvanic deposit scanning potential operations then circulates.
4. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 and 2, it is characterized in that conductive substrates is selected from gold electrode, glass-carbon electrode, titanium electrode, copper electrode, platinum electrode, tungsten electrode, copper-tungsten electrode, silver tungsten electrode, cast iron electrode, cerium tungsten electrode, lanthanum-tungsten electrode, thorium tungsten electrode or zirconiated tungsten.
5. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 is characterized in that, the metal in the metallic compound comprises Pt, Pd, Au or Ag.
6. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 is characterized in that, the pH value of described aqueous dispersions is 2.6-9.9.
7. the preparation method of a kind of metal nanoparticle-graphene complex according to claim 1 is characterized in that, metallic compound is HAuCl
4, NH
4AuCl
4, HPtCl
4, (NH
4)
2PtCl
6, HPdCl
4, H
2PdCl
4, (NH
4)
2PdCl
4Or Na
3[Ag (S
2O
3)
2].
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Family
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Application publication date: 20110907 |