CN102698741B - Method for preparing grapheme platinum nanocomposite material by using argon plasma - Google Patents
Method for preparing grapheme platinum nanocomposite material by using argon plasma Download PDFInfo
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- CN102698741B CN102698741B CN2012101114301A CN201210111430A CN102698741B CN 102698741 B CN102698741 B CN 102698741B CN 2012101114301 A CN2012101114301 A CN 2012101114301A CN 201210111430 A CN201210111430 A CN 201210111430A CN 102698741 B CN102698741 B CN 102698741B
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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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Abstract
The invention discloses a method for preparing grapheme platinum nanocomposite material by using argon plasma. The method comprises the steps of: putting graphene oxide into a beaker, then adding chloroplatinic acid, drying the obtained mixture, then putting the mixture into a sealed container, wherein the container is connected with a graphite electrode, the electrode is connected with alternating current power supply, and the power supply can generate an inductive coupling plasma source; introducing argon into the container, removing air, then opening a vacuum pump to vacuumize until the vacuum degree is about 3Pa; opening the alternating current power supply to generate the argon plasma, enabling the plasma flow directly to act on the surface of the dried powder for 28-32 minutes, fully washing, filtering and drying the reaction product by deionized water and proper organic solvent to prepare the grapheme platinum nanocomposite material. According to the method, not only can uniformly distributed grapheme platinum nanocomposite material be prepared effectively, but also the preparation time is shortened greatly, and the process is simplified.
Description
Technical field
The present invention relates to a kind of preparation method field of catalyst, relate in particular to a kind of method for preparing Graphene platinum nano composite material with argon plasma.
Background technology
Along with high speed development economic and science and technology, the energy problem of countries in the world facing, fuel problem and environmental problem are increasingly serious.Fuel cell is due to lightweight, simple in structure, the advantage such as energy conversion efficiency is high, environmentally safe, fuel source are rich and varied, and is called as 21st century environment-friendly and green energy, has development potentiality and application prospect.As everyone knows, the cost of Low-Temperature Fuel Cell Catalysts and performance have determined its development level and commercialization process.Its catalyst is still take the platinum group noble metal as main, and still, platinum metal exists expensive, resource-constrained, the problem such as anti-poisoning ability is poor.Therefore, find the catalyst of high usage, low consumption and strong anti methanol toxication ability, extensive use is of great significance for fuel cell.
Catalyst carrier should possess good electronic conduction ability, larger specific area, rational pore structure and excellent corrosion resistance, the discovery of Graphene, enriched material with carbon element family, formed the Graphene of CNT, two dimension of fullerene from zero dimension, one dimension to the integral framework of diamond and the graphite of three-dimensional, for the fields such as new material and Condensed Matter Physics provide new growth point.Recently, we have carried out the research of graphene-supported platinum as new catalyst.
At present, the method for preparing Graphene platinum composite is mainly chemical method, also has the people to use electrochemical method, high temperature method laser technology.Needing to use different chemical reagent in the chemical method preparation process assists metallic to be distributed to the material substrate surface, this has certain effect really for forming uniform and stable material, but also brought new pollution, especially on electronics industry, electric property for material requires very high, the chemical element of trace all can have a huge impact performance, inevitably can introduce some chemical elements so chemical method prepares in Graphene platinum composite material, this performance to material has a negative impact.The method such as electrochemical process and high temperature method, laser technology has reduced the pollution that chemical reagent brings, but harsher to the reaction condition requirement, and relatively power consumption.Plasma technique is lower temperature plasma technology particularly, has advantages of that additive method can not compare preparing aspect material, as fast, efficient, green, simple.This technology has boundless prospect in nano material aspect preparing.
Summary of the invention
, in order to overcome existing preparation method's process complexity, to be easy to introduce the deficiencies such as impurity, time consumption and energy consumption, the invention provides a kind of application of cold temperature plasma technique and prepare the method for Graphene platinum composite.The method can not only effectively prepare the graphene-based platinum nano composite material that is evenly distributed, and preparation time is shortened dramatically, and process is greatly simplified.
The present invention adopts following technical scheme to achieve these goals:
A kind of method for preparing Graphene platinum nano composite material with argon plasma is characterized in that: comprise the following steps:
A, the graphene oxide of 48-52mg is put into beaker, then add the 0.8-1.2 mol.L of 1.8-2.2ml
-1Chloroplatinic acid, the mixture of gained is placed in baking oven 58-62 ° of C oven dry, obtains the powder of oven dry;
B, the powder after drying are placed in a closed container, produce argon plasma stream in container, this argon plasma stream is acted directly on the surperficial 28-32 minute of the powder of oven dry, after discharge off, product is fully washed, filtered with deionized water or suitable organic solvent, drying, make Graphene platinum nano composite material.
A kind of described method for preparing Graphene platinum nano composite material with argon plasma is characterized in that: the described baking temperature of step B is 58-62 ° of C.
A kind of described method for preparing Graphene platinum nano composite material with argon plasma is characterized in that: described graphene oxide consumption is 50mg.
A kind of described method for preparing Graphene platinum nano composite material with argon plasma, it is characterized in that: be connected to graphite electrode in the described closed container of step b, electrode connects an AC power, this power supply can produce inductively-coupled plasma sources, first pass into argon gas again in container, drive air away, then open vavuum pump and be evacuated to the 3Pa left and right, open AC power this moment and can produce argon plasma stream.
Beneficial effect of the present invention:
1, the method can not only effectively prepare the graphene-based platinum nano composite material that is evenly distributed, and preparation time is shortened dramatically, and process is greatly simplified, and electro-chemical test shows, resulting materials has good electrocatalysis characteristic and anodic oxidation of methanol performance;
2, argon plasma has reproducibility, can the oxygen-containing functional group on graphene oxide surface be reduced, and can also make chloroplatinic acid (H simultaneously
2PtCl
6) in platinum reduction, so just, make platinum particles Direct precipitation after reduction on the surface of Graphene, this method is owing to avoiding carrying out the reduction of chloroplatinic acid and the reduction of graphene oxide with other chemical reagent, make preparation process by two to the three traditional steps, shorten to a step, also do not introduce unnecessary impurity element, reached efficient, fast, green, be a kind of very promising technology of preparing.
Description of drawings
Fig. 1 is the present invention auto levelizer figure used;
Fig. 2 is that the SEM of obtained material characterizes;
Fig. 3 is that the TEM of obtained material characterizes;
Fig. 4 is that the AFM of obtained material characterizes;
Fig. 5 is that the XPS of obtained material characterizes;
Fig. 6 is that the XRD of obtained material characterizes;
Fig. 7 is that effective electrochemical surface area of obtained material characterizes;
Fig. 8 is the electrochemical property test of obtained material to methanol catalytic oxidation.
The specific embodiment,
A kind of method for preparing Graphene platinum nano composite material with argon plasma comprises the following steps:
A, the graphene oxide of 50mg is put into beaker, then add 1 mol.L of 2ml
-1Chloroplatinic acid, the mixture of gained is placed in 60 ° of C of baking oven oven dry, obtains the powder of oven dry;
B, powder after oven dry is placed in a closed container (see figure 1), container is connected to graphite electrode, electrode connects an AC power, this power supply can produce inductively-coupled plasma sources, first pass into argon gas again in container, drive air away, then open vavuum pump and be evacuated to 3Pa, open AC power and produce argon plasma this moment, this plasma stream is acted directly on the surface 30 minutes of the powder of oven dry, after discharge off, product is fully washed with deionized water or suitable organic solvent, filter, 60 ° of C dryings, make Graphene platinum nano composite material.
The stereoscan photograph of made composite is seen Fig. 2, and transmission electron microscope photo is seen Fig. 3, and the atomic force microscopy electromicroscopic photograph is seen Fig. 4.Electronic Speculum shows, the evengranular surface that is dispersed in Graphene of Pt NPs.
Xps energy spectrum (Fig. 5) demonstration, composite contains the elements such as Pt, C, O.XRD analysis (Fig. 6) shows, Pt becomes face-centered cubic on the Graphene surface.What two kinds of X ray technology and electronic microscope photos had confirmed the method success has been deposited on Pt the Graphene surface.
The Pt/Graphene suspension of getting 5 μ L 0.1g/L is coated onto the glass-carbon electrode surface and dries.Use three-electrode system, 50 mV/s carry out cyclic voltammetry scan in the saturated 1.0M H2SO4 solution of nitrogen.Result shows, the electrochemical surface area of Pt/Graphene is 25.66 m2/g, has good electro catalytic activity (Fig. 7).This electrode 50 mV/s in 1 M CH3OH+0.5 M H2SO4 carry out cyclic voltammetry scan, and result shows, Pt/Graphene can effectively reduce the oxidation overpotential of methyl alcohol, and methanol oxidation is had good electro catalytic activity.
Claims (3)
1. method for preparing Graphene platinum nano composite material with argon plasma is characterized in that: comprise the following steps:
A, the graphene oxide of 48-52mg is put into beaker, then add the 0.8-1.2molL of 1.8-2.2ml
-1Chloroplatinic acid, the mixture of gained is placed in baking oven 58-62 ℃ oven dry, obtains the powder of oven dry;
B, the powder after drying are placed in a closed container, produce argon plasma stream in container, this argon plasma stream is acted directly on the surperficial 28-32 minute of the powder of oven dry, after discharge off, product is fully washed, filtered with deionized water or suitable organic solvent, drying, make Graphene platinum nano composite material; Be connected to graphite electrode in described closed container, electrode connects an AC power, and this power supply can produce inductively-coupled plasma sources, first pass into argon gas again in container, drive air away, then open vavuum pump and be evacuated to 3Pa, open AC power this moment and can produce argon plasma stream.
2. a kind of method for preparing Graphene platinum nano composite material with argon plasma according to claim 1, it is characterized in that: the described baking temperature of step B is 58-62 ℃.
3. a kind of method for preparing Graphene platinum nano composite material with argon plasma according to claim 1, it is characterized in that: described graphene oxide consumption is 50mg.
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| CN103563984B (en) * | 2013-04-27 | 2016-02-17 | 中国科学院等离子体物理研究所 | In a kind of use, air pressure jet flow plasma prepares the method for graphene oxide/silver-colored antibacterial composite material |
| CN107775014B (en) * | 2017-09-06 | 2020-05-22 | 深圳先进技术研究院 | Method for preparing noble metal/graphene composite nano material by using atmospheric pressure cold plasma |
| CN107686108B (en) * | 2017-09-20 | 2020-05-29 | 天津大学 | Method for preparing reduced graphene oxide by dielectric barrier discharge plasma |
| CN109904473B (en) * | 2019-02-26 | 2021-08-20 | 南京原磊纳米材料有限公司 | Atomic layer deposition equipment and method for preparing battery catalyst by using same |
| CN110655066A (en) * | 2019-09-30 | 2020-01-07 | 中科院合肥技术创新工程院 | Method for preparing platinum-graphene-molybdenum sulfide composite material by low-temperature plasma |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102324319A (en) * | 2011-07-12 | 2012-01-18 | 复旦大学 | Method for preparing graphene/platinum nano counter electrode material for dye sensitized solar cell |
| CN102350372A (en) * | 2011-07-12 | 2012-02-15 | 南昌大学 | Preparation method of polyaniline/graphene controllable load platinum nanoparticles |
| CN102361087A (en) * | 2011-10-27 | 2012-02-22 | 西北师范大学 | Graphene-polypyrrole/platinum nano modified glassy carbon electrode, preparation method for same and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102324319A (en) * | 2011-07-12 | 2012-01-18 | 复旦大学 | Method for preparing graphene/platinum nano counter electrode material for dye sensitized solar cell |
| CN102350372A (en) * | 2011-07-12 | 2012-02-15 | 南昌大学 | Preparation method of polyaniline/graphene controllable load platinum nanoparticles |
| CN102361087A (en) * | 2011-10-27 | 2012-02-22 | 西北师范大学 | Graphene-polypyrrole/platinum nano modified glassy carbon electrode, preparation method for same and application thereof |
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Address after: 230001 no.181 Gucheng Road, shiyangang Township, Hefei City, Anhui Province Patentee after: INSTITUTE OF PLASMA PHYSICS, CHINESE ACADEMY OF SCIENCES Address before: 230031 Shushan Lake Road, Shushan District, Anhui, China, No. 350, No. Patentee before: INSTITUTE OF PLASMA PHYSICS, CHINESE ACADEMY OF SCIENCES |