CN102061504A - Method for synthesizing graphene-containing composite thin film material - Google Patents
Method for synthesizing graphene-containing composite thin film material Download PDFInfo
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- CN102061504A CN102061504A CN2009101175924A CN200910117592A CN102061504A CN 102061504 A CN102061504 A CN 102061504A CN 2009101175924 A CN2009101175924 A CN 2009101175924A CN 200910117592 A CN200910117592 A CN 200910117592A CN 102061504 A CN102061504 A CN 102061504A
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Abstract
The invention discloses a method for synthesizing a graphene-containing composite thin film material. The method comprises: firstly, preparing a graphene oxide transparent thin film with uniform thickness by using graphene oxide colloidal suspension as a deposition medium; performing in-situ reduction on the graphene oxide thin film by an electrochemical process to obtain a graphene thin film; and finally, depositing uniformly-dispersed platinum nano particles on the surface of the obtained raphene thin film by a constant-potential depositing technique to obtain a platinum-graphene nano composite thin film. The catalytic behavior of the prepared composite thin film material on methanol is studied by using the prepared composite thin film material as an electrode. The experiment result proves that the composite thin film has remarkable catalytic effect on methanol.
Description
Technical field
The present invention relates to a kind of synthetic method that contains the Graphene composite film material, be specifically related to a kind of synthetic method that contains platinum and graphene composite material.
Background technology
Graphene, as a kind of novel carbon material, carbon atom intensive by one deck, that be wrapped on the honeycomb crystal lattice is formed, and is the thinnest in the world two-dimensional material, and its thickness only is 0.35nm.Graphene film has caused numerous investigators' concern with its excellent electricity, mechanical property and high characteristics such as aspect ratio.At present, this material discussed widely in the applied research in fields such as ultracapacitor, emission, nanoelectronics (referring to Science 2008,320,356.; Nano Lett.2008,8,1704.).In addition, because its good electrical conductivity and big specific surface area are estimated it also will be had broad application prospects as catalyst support material.Recently, document has been reported about Graphene as reduction (Electrochem.Commun.2009,11,954 of solid support material to oxygen and methyl alcohol; Nano Letters, 2009,9,2255), but experimentation relates to and uses some strong reductive agents, as sodium borohydride and hydrazine hydrate, they have produced great pollution to environment on every side, therefore how to obtain the Graphene solid support material by simple and free of contamination synthetic method and have become current very interested problem.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method that contains the Graphene composite film material.
We have prepared the Graphene composite film material that nano platinum particle is modified by eco-friendly electrochemical techniques.The present invention has prepared platinum and Graphene (platinum/graphene sheets, Pt-GS) nano composite film in conjunction with electrophoretic deposition technique, electrochemical in-situ reduction technique and permanent electromotive force deposition technique.
The present invention at first with the graphene oxide soliquid as deposition medium, the uniform graphene oxide of preparation thickness (graphene oxide, GO) transparent film, then utilize electrochemical process that graphene oxide film is carried out in-situ reducing and obtained graphene film, successfully deposit finely dispersed nano platinum particle by permanent electromotive force deposition technique on the graphene film surface that obtains subsequently, thereby obtained platinum-graphene nano laminated film.
Principle of work of the present invention is described below:
Graphene oxide is because there is a large amount of polarity oxygen-containing functional groups in its surface, for example carboxyl, epoxy group(ing), hydroxyl etc., the existence of these groups makes graphene oxide electrically charged under certain pH value, measure through Zetaplus analyzer, the Zeta potential of graphene oxide is about-64.7mV near pH=7.0 the aqueous-phase suspending medium, this value shows that the directional migration of anode direction can take place the graphene oxide colloidal solid under certain electrical potential conditions, this lays a good foundation for the enforcement of electrophoretic deposition process.In addition, the reduction of graphene oxide is everybody hot issue of all paying special attention to.Up to the present, graphene oxide being reduced into Graphene method relatively more commonly used is chemical reduction and thermal reduction.Chemical reduction relates to some strong original reagents of going back, and such as sodium borohydride, hydrazine hydrate etc., these reagent all have certain toxicity and danger; In addition, also there are some significant defectives in the Graphene that obtains by chemical reduction method, causes its electroconductibility poor.For the thermal reduction process, because required temperature is higher, correspondingly also improved requirement to base material, it is very unfavorable that this device to graphene film is used.The electrochemical reduction technology because its controllability is good, simple to operate, pollution-free, substrate is required characteristics such as low, has demonstrated good prospects for application as incipient a kind of new technology.For the deposition of nano platinum particle, we adopt relatively more classical potentiostatic electrodeposition method, in the graphene film surface preparation finely dispersed nano platinum particle, thereby obtained the platinum/graphen composite film material.
A kind of synthetic method that contains the Graphene composite film material is characterized in that this method may further comprise the steps:
A, electrophoretic deposition technique prepare graphene oxide film
Conductive glass sheet with cleaning is an anode, and the stainless steel substrates of same size is a negative electrode, is deposition medium with graphene oxide suspension, in 150-160V deposit 30-90 second;
B, electrochemical in-situ redox graphene film obtain graphene film
With graphene oxide film as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with the potassium chloride solution is electrolyte solution, by cyclic voltammetric or constant potential electrochemical reduction the graphene oxide reduction is obtained graphene film;
C, nano platinum particle are in the deposition on Graphene surface
The graphene film that obtains with reduction is a working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with H
2PtCl
6And H
2SO
4Mixing solutions be electrolyte solution, keep electromotive force in-0.25V deposit, prepare the graphene nano laminated film that metal platinum nano-particle is modified.
In the method for the present invention, the concentration of graphene oxide suspension is 0.4-0.6molL
-1
In the method for the present invention, potassium chloride solution concentration is 0.05-0.2molL
-1
We contain the Graphene composite film material as electrode to preparation, have studied its catalysis behavior to methyl alcohol, and experimental result confirms that this laminated film has good catalytic effect to methyl alcohol.This method technology is simple, easy handling, and preparation process has been avoided the pollution to environment to greatest extent, be a kind of green, eco-friendly technology of preparing, prepared laminated film will have broad application prospects in the nanoelectronic field as catalyst support material.
The present invention has following advantage:
1, by the electrochemical in-situ reduction technique graphene oxide is reduced to Graphene, has avoided in the past utilizing and gone back original reagent by force and high-temperature heat treatment method prepares defective and the deficiency that graphene film causes.
2, adopt permanent electromotive force deposition technique in the Graphene surface preparation platinum/graphene nano laminated film, this method is compared the former solution blending-method of restoring and is prepared relatively environmental friendliness of nano platinum particle.
3, the catalyzed reaction result to methyl alcohol shows, the platinum/graphene nano composite film electrode of the present invention's preparation is compared catalytic efficiency with business-like platinum/carbon black electrode and improved 3 times at least.
Description of drawings
Fig. 1 is that embodiment 2 platinum/graphene nano laminated films are as the cyclic voltammetry curve of working electrode to methanol oxidation.
Embodiment
For a better understanding of the present invention, describe by embodiment
1.1 the processing of conductive glass substrate
At first conductive glass is cut into 15mm * 25mm, use distilled water, ethanol ultrasonic cleaning 30 minutes successively, nitrogen dries up.
1.2 at conductive glass surface electrophoretic deposition graphene oxide film
With the conductive glass is anode, and the stainless steel substrates of same size is a negative electrode, is deposition medium with graphene oxide suspension, in 150-160V deposit 45-60 second.
1.3 the cyclic voltammetry redox graphene obtains graphene film
With graphene oxide film as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 0.1mo1L
-1The KCl aqueous solution is electrolyte solution, in the 0.0V-1.0V interval range with 10mVs
-1Sweep speed scanning 10 circles, obtain the graphene film of black.
1.4 nano platinum particle is in the deposition on graphene film surface
The graphene film that obtains with reduction is a working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 3mmolL
-1H
2PtCl
6+ 0.5molL
-1H
2SO
4Mixing solutions is an electrolyte solution, keeps electromotive force-0.25V deposit 1800 seconds.
1.5 catalyzed reaction to methyl alcohol
With the platinum/graphene nano composite film material as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 0.5M CH
3OH+0.5M H
2SO
4Mixing solutions be electrolyte solution, at 5mVs
-1The speed of sweeping studied down catalytic effect to methyl alcohol.
Embodiment 2
2.1 the processing of conductive glass substrate
At first conductive glass is cut into 15mm * 25mm, use distilled water, ethanol ultrasonic cleaning 30 minutes successively, nitrogen dries up.
2.2 at conductive glass surface electrophoretic deposition graphene oxide film
With the conductive glass is anode, and the stainless steel substrates of same size is a negative electrode, is deposition medium with graphene oxide suspension, in 150-160V deposit 45-60 second.
2.3 the potentiostatic method redox graphene obtains graphene film
With graphene oxide film as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 0.1molL
-1The KCl aqueous solution is electrolyte solution, and redox graphene film under-0.9V constant potential, obtains the graphene film of black at reaction times 3600-7200 second.
2.4 nano platinum particle is in the deposition on graphene film surface
The graphene film that obtains with reduction is a working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 3mmolL
-1H
2PtCl
6+ 0.5molL
-1H
2SO
4Mixing solutions is an electrolyte solution, keeps electromotive force-0.25V deposit 1800 seconds.
2.5 catalyzed reaction to methyl alcohol
With the platinum/graphene nano composite film material as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with 0.5M CH
3OH+0.5M H
2SO
4Mixing solutions be electrolyte solution, at 5mVs
-1The speed of sweeping studied down catalytic effect to methyl alcohol, see Fig. 1.
Claims (3)
1. synthetic method that contains the Graphene composite film material is characterized in that this method may further comprise the steps:
A, electrophoretic deposition technique prepare graphene oxide film
Conductive glass sheet with cleaning is an anode, and the stainless steel substrates of same size is a negative electrode, is deposition medium with graphene oxide suspension, in 150-160V deposit 30-90 second;
B, electrochemical in-situ redox graphene film obtain graphene film
With graphene oxide film as working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with the potassium chloride solution is electrolyte solution, by cyclic voltammetric or constant potential electrochemical reduction the graphene oxide reduction is obtained graphene film;
C, nano platinum particle are in the deposition on Graphene surface
The graphene film that obtains with reduction is a working electrode, with silver-silver chloride electrode and platinum wire electrode respectively as reference electrode and supporting electrode, with H
2PtCl
6And H
2SO
4Mixing solutions be electrolyte solution, keep electromotive force in-0.25V deposit, prepare the graphene nano laminated film that metal platinum nano-particle is modified.
2. the method for claim 1, the concentration that it is characterized in that graphene oxide suspension is 0.4-0.6molL
-1
3. the method for claim 1 is characterized in that potassium chloride solution concentration is 0.05-0.2molL
-1
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Application publication date: 20110518 |