CN103435037A - Method for preparing graphene/Pt nanocomposite material by liquid phase reduction method - Google Patents
Method for preparing graphene/Pt nanocomposite material by liquid phase reduction method Download PDFInfo
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- CN103435037A CN103435037A CN2013103712709A CN201310371270A CN103435037A CN 103435037 A CN103435037 A CN 103435037A CN 2013103712709 A CN2013103712709 A CN 2013103712709A CN 201310371270 A CN201310371270 A CN 201310371270A CN 103435037 A CN103435037 A CN 103435037A
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Abstract
The invention relates to a method for preparing a graphene/Pt nanocomposite material by a liquid phase reduction method. The method comprises the following steps of: under the condition of room temperature, dispersing graphite oxide and a dispersing agent into deionized water, adding a reducing agent after graphite oxide and the dispersing agent are completely dissolved, and carrying out heating with an oil bath and stirring to obtain a graphene solution, wherein the mass ratio of graphite oxide to the dispersing agent is (1:5)-(1:10); dissolving graphene and a platinum precursor in a solvent respectively, then mixing the solutions, and regulating the pH value to be 8-12 to obtain a reaction solution, wherein the mass ratio of graphite oxide to the platinum precursor is (1:1)-(10:1); heating the reaction solution with the oil bath for 0.5-4 hours to 110-120 DEG C, insulating the reaction solution for 2-8 hours, and then carrying out leaching and freeze drying, thus obtaining the graphene/Pt nanocomposite material. The preparation method is simple and has low requirements for production equipment. The Pt particles in the graphene/Pt composite material prepared by the method have small sizes, are not easy to agglomerate, are well composited with graphene and have good dispersibility in the graphene surface and layers.
Description
Technical field
The invention belongs to the preparation field of Graphene/Pt nano composite material, particularly a kind of liquid phase reduction prepares the method for Graphene/Pt nano composite material.
Background technology
Graphene is found a kind of New Two Dimensional plane carbon nanomaterial in 2004, the monoatomic layer structures shape that it is special it there is abundant and novel physicals.In the past few years, Graphene has become the study hotspot got most of the attention.Research shows, the characteristics such as Graphene has ultra-thin, super firm and superpower conductivity are expected to obtain widespread use at nano electron device, matrix material, stored energy and the field such as biomedical.
Recent study person finds, graphene-based matrix material can significantly improve the performances such as the hardness, specific conductivity of mixture.G.Williams etc. have reported that on ACS Nano 2 (2008) 1487-1491 the photocatalysis reduction-oxidation graphite that utilizes TiO2 prepares Graphene/TiO
2mixture, the TiO of 2.6～4nm
2particle is attached on the graphene film that about 2.2nm is thick.Y.J.Kin etc. have reported and have utilized vapour phase epitaxy method to make the ZnO nanorod vertical-growth on the Graphene surface on Applied Physics Letters 95 (2009) 213101-1-213101-3.Y.Fan etc. have reported the standby Graphene/Al that obtains of employing mechanical ball milling legal system on Carbon 48 (2010) 1743-1749
2o
3composite powder, by Al
2o
3specific conductivity improved 13～16 orders of magnitude.
In addition, due to the conductivity of platinum excellence and in the vital role of area of solar cell, the mixture of Graphene and platinum also receives much attention gradually.Y.Li etc. have reported with One-pot Reduction graphite oxide and Platinic chloride (H on Electrochem Commun 11 (2009) 846-849
2ptCl
6) prepared the method for the graphene nanometer sheet that the Pt nano-cluster decorates.
Mainly there is following defect in the method for preparing at present Graphene/Pt nano composite material: processing step is more, cost is higher, and prepared Pt nanoparticulate dispersed is bad.Therefore find the single stage method preparation size little, be difficult for the Graphene of reuniting, preparation process is easier/Pt nano composite material and become the focus of research.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that liquid phase reduction prepares Graphene/Pt nano composite material, and the method preparation method is simple, to production unit, requires low; In prepared Graphene/Pt matrix material, the Pt particle size is little, be difficult for to reunite, with Graphene compound good, in Graphene surface and layer good dispersity.
A kind of liquid phase reduction of the present invention prepares the method for Graphene/Pt nano composite material, comprising:
(1) at ambient temperature, graphite oxide, dispersion agent are distributed in deionized water, after dissolving fully, add reductive agent, oil bath heating, stirring, obtain graphene solution; Wherein the mass ratio of graphite oxide and reductive agent is 1:5～1:10, and the mass ratio of graphite oxide and dispersion agent is 1:5～1:10;
(2) precursor of above-mentioned Graphene and platinum is dissolved in respectively in solvent, then mixes, regulating the pH value is 8-12, obtains reaction solution; Wherein the mass ratio of the graphite oxide in step (1) and platinum precursor is 1:1～10:1;
(3) above-mentioned reaction solution is carried out to 0.5h-4h to 110-120 ℃ of oil bath heating, insulation 2h-8h, then suction filtration, lyophilize, obtain Graphene/Pt nano composite material.
In described step (1), dispersion agent is sodium polystyrene sulfonate PSS.
In described step (1), reductive agent is xitix VC, hydrazine hydrate or hydroiodic acid HI.
In described step (1), whipping temp is 30-40 ℃, and churning time is 12-24h.
In described step (2), the precursor of platinum is six hydration Platinic chloride H
2ptCl
66H
2o.
In described step (2), solvent is ethylene glycol, and concentration is 98wt%～99.5wt%.
In described step (2), the mass ratio of the solvent of Graphene and platinum precursor is 8:1.
In described step (2), the NaOH solution of 1M is regulated the pH value.
In described step (3), under the condition of insulation for condensing reflux, be incubated.
This preparation method, the graphene solution good dispersity that adopts PSS to make as reductive agent as dispersion agent, xitix, hydrazine hydrate or hydroiodic acid HI, the nano particle of platinum is more stable in organic solvent, regulates the extensive reunion that pH has also avoided platinum grain simultaneously.
beneficial effect
(1) preparation method of the present invention is simple, to production unit, requires low;
(2) in the prepared Graphene of the present invention/Pt matrix material the Pt particle size little, be difficult for reuniting, with Graphene compound good, in Graphene surface and layer good dispersity.
The accompanying drawing explanation
The transmission electron microscope photo that Fig. 1 is synthesizing graphite alkene/Pt matrix material;
The high-resolution-ration transmission electric-lens photo that Fig. 2 is synthesizing graphite alkene/Pt matrix material;
The high-resolution-ration transmission electric-lens photo that Fig. 3 is synthesizing graphite alkene/Pt matrix material;
The X-ray diffractogram that Fig. 4 is synthesizing graphite alkene/Pt matrix material.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for the present invention is described.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
80mg graphite oxide (GO) is joined in the 40mL deionized water, then add 800mg dispersion agent PSS, it was uniformly dispersed in ultrasonic 30 minutes in Ultrasonic Cleaners.Add reductive agent xitix (VC) 500mg, the constant temperature oil bath heating is stirred 24 hours under the condition of 40 ℃, obtains disperseing more uniform graphene aqueous solution.
Presoma (Platinic chloride H by graphene aqueous solution and 40mg platinum
2ptCl
66H
2o) join respectively in 53g and 6.67g ethylene glycol and mix, regulating the pH value with the 1M sodium hydroxide solution is 11, puts into 1h to 110 ℃ of oil bath pan heating, under the condition of condensing reflux, after insulation 4h, takes out, and obtains Graphene/Pt dispersion liquid.Again its suction filtration postlyophilization is obtained to graphite/Pt nano composite material.The transmission electron microscope photo that Fig. 1 is the present embodiment synthesizing graphite alkene/Pt matrix material, can find out: Pt nanoparticle singly is dispersed on graphene sheet layer equably, does not observe the platinum grain be free in outside Graphene.Fig. 2, the 3 high-resolution-ration transmission electric-lens photos that are the present embodiment synthesizing graphite alkene/Pt matrix material, can find out: the size of Pt nanoparticle is about 4nm, and spacing is about 0.22nm.The X-ray diffractogram that Fig. 4 is the present embodiment synthesizing graphite alkene/Pt matrix material, the diffraction peak in figure shows: the nano particle in this matrix material is platinum.
Embodiment 2
80mg graphite oxide (GO) is joined in the 40mL deionized water, then add 600mg dispersion agent PSS, it was uniformly dispersed in ultrasonic 30 minutes in Ultrasonic Cleaners.Add reductive agent xitix (VC) 400mg, the constant temperature oil bath heating is stirred 24 hours under the condition of 40 ℃, obtains disperseing more uniform graphene aqueous solution.
Presoma (Platinic chloride H by graphene aqueous solution and 40mg platinum
2ptCl
66H
2o) join respectively in 53g and 5.89g ethylene glycol and mix, regulating the pH value with the 1M sodium hydroxide solution is 10, puts into 2h to 110 ℃ of oil bath pan heating, under the condition of condensing reflux, after insulation 5h, takes out, and obtains Graphene/Pt dispersion liquid.Again its suction filtration postlyophilization is obtained to graphite/Pt nano composite material.Transmission electron microscope observing shows: Pt nanoparticle singly is dispersed on graphene sheet layer equably, does not observe the platinum grain be free in outside Graphene.High-resolution-ration transmission electric-lens is observed and shown: the size of Pt nanoparticle is about 4nm, and spacing is about 0.22nm.The XRD test result shows: the nano particle in this matrix material is platinum.
Embodiment 3
80mg graphite oxide (GO) is joined in the 40mL deionized water, then add 400mg dispersion agent PSS, it was uniformly dispersed in ultrasonic 30 minutes in Ultrasonic Cleaners.Add reductive agent xitix (VC) 600mg, the constant temperature oil bath heating is stirred 24 hours under the condition of 40 ℃, obtains disperseing more uniform graphene aqueous solution.
Presoma (Platinic chloride H by graphene aqueous solution and 40mg platinum
2ptCl
66H
2o) join respectively in 53g and 5.30g ethylene glycol and mix, regulating the pH value with the 1M sodium hydroxide solution is 12, puts into 3h to 110 ℃ of oil bath pan heating, under the condition of condensing reflux, after insulation 6h, takes out, and obtains Graphene/Pt dispersion liquid.Again its suction filtration postlyophilization is obtained to graphite/Pt nano composite material.Transmission electron microscope observing shows: Pt nanoparticle singly is dispersed on graphene sheet layer equably, does not observe the platinum grain be free in outside Graphene.High-resolution-ration transmission electric-lens is observed and shown: the size of Pt nanoparticle is about 4nm, and spacing is about 0.22nm.The XRD test result shows: the nano particle in this matrix material is platinum.
Claims (9)
1. a liquid phase reduction prepares the method for Graphene/Pt nano composite material, comprising:
(1) at ambient temperature, graphite oxide, dispersion agent are distributed in deionized water, after dissolving fully, add reductive agent, oil bath heating, stirring, obtain graphene solution; Wherein the mass ratio of graphite oxide and reductive agent is 1:5～1:10, and the mass ratio of graphite oxide and dispersion agent is 1:5～1:10;
(2) precursor of above-mentioned Graphene and platinum is dissolved in respectively in solvent, then mixes, regulating the pH value is 8-12, obtains reaction solution; Wherein the mass ratio of the graphite oxide in step (1) and platinum precursor is 1:1～10:1;
(3) above-mentioned reaction solution is carried out to 0.5h-4h to 110-120 ℃ of oil bath heating, insulation 2h-8h, then suction filtration, lyophilize, obtain Graphene/Pt nano composite material.
2. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (1), dispersion agent is sodium polystyrene sulfonate PSS.
3. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (1), reductive agent is xitix VC, hydrazine hydrate or hydroiodic acid HI.
4. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (1), whipping temp is 30-40 ℃, and churning time is 12-24h.
5. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (2), the precursor of platinum is six hydration Platinic chloride H2PtCl
66H
2o.
6. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (2), solvent is ethylene glycol, and concentration is 98wt%～99.5wt%.
7. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (2), the mass ratio of the solvent of Graphene and platinum precursor is 8:1.
8. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (2), the NaOH solution of 1M is regulated the pH value.
9. a kind of liquid phase reduction according to claim 1 prepares the method for Graphene/Pt nano composite material, it is characterized in that:
In described step (3), under the condition of insulation for condensing reflux, be incubated.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891477A (en) * | 2015-05-15 | 2015-09-09 | 北京交通大学 | Simple and environment-friendly graphene paper preparation method |
| CN105097298A (en) * | 2015-05-27 | 2015-11-25 | 北京交通大学 | Method for preparing graphene hydrogel electrode by graphene oxide solution |
| CN105542332A (en) * | 2015-12-15 | 2016-05-04 | 江南大学 | Preparation method of polystyrene/graphene/precious metal composite particle |
| TWI598295B (en) * | 2016-09-14 | 2017-09-11 | 國立臺灣科技大學 | Graphene nanoribbon composite and manufacturing method thereof |
| CN112169791A (en) * | 2020-10-22 | 2021-01-05 | 西安理工大学 | Preparation method of lamellar three-phase composite photocatalytic material |
| CN112642426A (en) * | 2020-12-23 | 2021-04-13 | 上海聚治新材料科技有限公司 | Preparation method of noble metal/graphene-supported manganese-zinc-based weak photocatalyst |
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| CN102430413A (en) * | 2011-10-08 | 2012-05-02 | 南京师范大学 | PtNi alloy/graphene combined nanometer catalyst with hollow structure and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104891477A (en) * | 2015-05-15 | 2015-09-09 | 北京交通大学 | Simple and environment-friendly graphene paper preparation method |
| CN104891477B (en) * | 2015-05-15 | 2016-11-09 | 北京交通大学 | A kind of simple and environmentally-friendly graphene paper preparation method |
| CN105097298A (en) * | 2015-05-27 | 2015-11-25 | 北京交通大学 | Method for preparing graphene hydrogel electrode by graphene oxide solution |
| CN105542332A (en) * | 2015-12-15 | 2016-05-04 | 江南大学 | Preparation method of polystyrene/graphene/precious metal composite particle |
| CN105542332B (en) * | 2015-12-15 | 2018-06-22 | 江南大学 | A kind of method for preparing polystyrene/graphene/noble metal compound particle |
| TWI598295B (en) * | 2016-09-14 | 2017-09-11 | 國立臺灣科技大學 | Graphene nanoribbon composite and manufacturing method thereof |
| CN112169791A (en) * | 2020-10-22 | 2021-01-05 | 西安理工大学 | Preparation method of lamellar three-phase composite photocatalytic material |
| CN112169791B (en) * | 2020-10-22 | 2022-09-02 | 西安理工大学 | Preparation method of lamellar three-phase composite photocatalytic material |
| CN112642426A (en) * | 2020-12-23 | 2021-04-13 | 上海聚治新材料科技有限公司 | Preparation method of noble metal/graphene-supported manganese-zinc-based weak photocatalyst |
| CN112642426B (en) * | 2020-12-23 | 2023-09-12 | 上海聚治新材料科技有限公司 | Preparation method of noble metal/graphene supported manganese-zinc-based weak photocatalyst |
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Application publication date: 20131211 |