CN102698741A - 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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- CN102698741A CN102698741A CN2012101114301A CN201210111430A CN102698741A CN 102698741 A CN102698741 A CN 102698741A CN 2012101114301 A CN2012101114301 A CN 2012101114301A CN 201210111430 A CN201210111430 A CN 201210111430A CN 102698741 A CN102698741 A CN 102698741A
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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 of catalysts method field, relate in particular to a kind of method for preparing Graphene platinum nano composite material with argon plasma.
Background technology
Along with economy and high-speed development of science and technology, the energy problem that countries in the world face jointly, fuel problem and environmental problem are increasingly serious.Fuel cell is because in light weight, simple in structure, 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 catalyst and performance have determined its development level and commercialization process.It is main that its catalyst is still with the platinum group noble metal, and still, the platinum metal existence costs an arm and a leg resource-constrained, problems such as anti-poisoning ability difference.Therefore, seek the catalyst of high usage, low consumption and strong anti methanol toxication ability, extensive use has crucial meaning for fuel cell.
Catalyst carrier should possess good electron conducting power, bigger specific area, rational pore structure and excellent corrosion resistance; The discovery of Graphene; Enriched material with carbon element family; The Graphene of CNT, two dimension that has formed fullerene from zero dimension, one dimension is to the integral framework of the diamond and the graphite of three-dimensional, for 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 mainly is a chemical method, and human electrochemical method, high temperature method laser technology are also arranged.Chemical method prepares need be used different chemical reagent and assist metallic to be distributed to the material substrate surface in the process; This has certain effect really for forming uniform and stable material; But also brought new pollution; On electronics industry, very high for the electric property requirement of material, the chemical element of trace all can produce very big influence to performance especially; Inevitably can introduce some chemical elements so chemical method prepares in the Graphene platinum composite material, this performance to material has a negative impact.Method such as electrochemical process and high temperature method, laser technology has reduced the pollution that chemical reagent brings, but reaction condition is required relatively harshness, and relatively power consumption.Plasma technique is lower temperature plasma technology particularly, has the advantage that additive method can not be compared aspect the preparation material, as quick, efficient, green, simple.This technology has boundless prospect aspect nano material preparation.
Summary of the invention
In order to overcome prior preparation method process complicacy, to be easy to introduce deficiencies such as impurity, time consumption and energy consumption, the present invention provides a kind of application of cold temperature plasma technique to prepare the method for Graphene platinum composite.This 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 ofly prepare the method for Graphene platinum nano composite material, it is characterized in that: may further comprise the steps with argon plasma:
A, the graphene oxide of 48-52mg is put into beaker, add the 0.8-1.2 mol.L of 1.8-2.2ml then
-1Chloroplatinic acid, the mixture of gained places baking oven 58-62 ° of C oven dry, the powder that must dry;
B, the powder after will drying place a closed container; In container, produce argon plasma stream; This argon plasma stream is acted directly on surperficial 28-32 minute of powder of oven dry, behind the discharge off, with product with deionized water or suitably organic solvent fully wash, filter; Drying makes Graphene platinum nano composite material.
Describedly a kind ofly prepare the method for Graphene platinum nano composite material with argon plasma, it is characterized in that: the described baking temperature of step B is 58-62 ° of C.
Describedly a kind ofly prepare the method for Graphene platinum nano composite material with argon plasma, it is characterized in that: described graphene oxide consumption is 50mg.
Described a kind of 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, and this power supply can produce inductively-coupled plasma sources; In container, feed argon gas earlier again; Drive air away, open vavuum pump then and be evacuated to about 3Pa, open AC power this moment and can produce argon plasma stream.
Beneficial effect of the present invention:
1, this 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 that the gained material has good catalytic action 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 the platinum particles after the reduction directly be deposited on the surface of Graphene, this method is carried out the reduction of chloroplatinic acid and the reduction of graphene oxide owing to avoiding the use of other chemical reagent; Make the preparation process by two to the three traditional steps, shorten to a step, also do not introduce the redundant impurities element; Reached efficient; Fast, green is a kind of very promising technology of preparing.
Description of drawings
Fig. 1 is the used auto levelizer figure of the present invention;
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 electro-chemical activity area of obtained material characterizes;
Fig. 8 is the electrochemical property test of obtained material to methanol catalytic oxidation.
The specific embodiment,
A kind ofly prepare the method for Graphene platinum nano composite material, may further comprise the steps with argon plasma:
A, the graphene oxide of 50mg is put into beaker, add 1 mol.L of 2ml then
-1Chloroplatinic acid, the mixture of gained places 60 ° of C of baking oven oven dry, the powder that must dry;
B, the powder after will drying place a closed container (see figure 1), and container is connected to graphite electrode, and electrode connects an AC power; This power supply can produce inductively-coupled plasma sources, in container, feeds argon gas earlier again, drives air away; Open vavuum pump then and be evacuated to 3Pa, open AC power and produce argon plasma this moment, this plasma stream acted directly on the surface 30 minutes of the powder of oven dry; Behind the discharge off; Product is fully washed, filtered with deionized water or suitable organic solvent, and 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 micro-electromicroscopic photograph of atomic force is seen Fig. 4.Electronic Speculum shows, the evengranular surface that is dispersed in Graphene of Pt NPs.
Xps energy spectrum (Fig. 5) shows that composite contains elements such as Pt, C, O.XRD analysis (Fig. 6) shows that Pt becomes face-centered cubic on the Graphene surface.What two kinds of X ray technology and electronic microscope photos had confirmed this 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.The result shows that the electro-chemical activity 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 the result shows that Pt/Graphene can effectively reduce the oxidization of methanol overpotential, and methanol oxidation is had good electro catalytic activity.
Claims (4)
1. one kind prepares the method for Graphene platinum nano composite material with argon plasma, it is characterized in that: may further comprise the steps:
A, the graphene oxide of 48-52mg is put into beaker, add the 0.8-1.2 mol.L of 1.8-2.2ml then
-1Chloroplatinic acid, the mixture of gained places baking oven 58-62 ° of C oven dry, the powder that must dry;
B, the powder after will drying place a closed container; In container, produce argon plasma stream; This argon plasma stream is acted directly on surperficial 28-32 minute of powder of oven dry, behind the discharge off, with product with deionized water or suitably organic solvent fully wash, filter; Drying makes Graphene platinum nano composite material.
2. according to claim 1ly a kind ofly prepare the method for Graphene platinum nano composite material with argon plasma, it is characterized in that: the described baking temperature of step B is 58-62 ° of C.
3. according to claim 1ly a kind ofly prepare the method for Graphene platinum nano composite material with argon plasma, it is characterized in that: described graphene oxide consumption is 50mg.
4. a kind of method for preparing Graphene platinum nano composite material with argon plasma according to claim 1; It is characterized in that: be connected to graphite electrode in the described closed container of step b, electrode connects an AC power, and this power supply can produce inductively-coupled plasma sources; In container, feed argon gas earlier again; Drive air away, open vavuum pump then and be evacuated to about 3Pa, open AC power this moment and can produce argon plasma stream.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103563984A (en) * | 2013-04-27 | 2014-02-12 | 中国科学院等离子体物理研究所 | Method for preparing graphene oxide/ silver antibacterial composite material through intermediate pneumatic plasma jet |
| CN107686108A (en) * | 2017-09-20 | 2018-02-13 | 天津大学 | The method that dielectric barrier discharge plasma prepares redox graphene |
| CN107775014A (en) * | 2017-09-06 | 2018-03-09 | 深圳先进技术研究院 | A kind of method that atmosphere cold plasma prepares noble metal/graphene composite nano material |
| CN109904473A (en) * | 2019-02-26 | 2019-06-18 | 南京原磊纳米材料有限公司 | A kind of atomic layer deposition apparatus and its method for preparing cell catalyst |
| 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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| 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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| JP2010129385A (en) * | 2008-11-27 | 2010-06-10 | National Institute Of Advanced Industrial Science & Technology | Platinum cluster for electrode and method for producing the same |
| 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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103563984A (en) * | 2013-04-27 | 2014-02-12 | 中国科学院等离子体物理研究所 | Method for preparing graphene oxide/ silver antibacterial composite material through intermediate pneumatic plasma jet |
| 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 |
| CN107775014A (en) * | 2017-09-06 | 2018-03-09 | 深圳先进技术研究院 | A kind of method that atmosphere cold plasma prepares noble metal/graphene composite nano 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 |
| CN107686108A (en) * | 2017-09-20 | 2018-02-13 | 天津大学 | The method that dielectric barrier discharge plasma prepares redox graphene |
| CN109904473A (en) * | 2019-02-26 | 2019-06-18 | 南京原磊纳米材料有限公司 | A kind of atomic layer deposition apparatus and its method for preparing cell catalyst |
| 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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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 |