CN105655600A - Preparation method of Pt-Mn-graphene catalyst for fuel cell - Google Patents
Preparation method of Pt-Mn-graphene catalyst for fuel cell Download PDFInfo
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- CN105655600A CN105655600A CN201610168232.7A CN201610168232A CN105655600A CN 105655600 A CN105655600 A CN 105655600A CN 201610168232 A CN201610168232 A CN 201610168232A CN 105655600 A CN105655600 A CN 105655600A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a preparation method of a Pt-Mn-graphene catalyst for a fuel cell. The preparation method of the Pt-Mn-graphene catalyst for the fuel cell is used for catalyzing methanol oxidization in a direct methanol fuel cell, and is used for improving the performance of the direct methanol fuel cell. The Pt-Mn-graphene catalyst for the fuel cell, which is prepared by the preparation method has excellent catalytic performance on methanol; the performance is possibly related to the ratio of H2PtCl6.6H2O to MnCl2.4H20 in parts by weight; when the ratio of the H2PtCl6.6H2O to the MnCl2.4H20 in parts by weight is between (3 to 5): 1, the catalytic performance is the best. Compared with the prior art, the preparation method of the Pt-Mn-graphene catalyst for the fuel cell has outstanding substantive characteristics and obvious progress.
Description
Technical field
The invention belongs to energy field, it relates to graphene battery material, it is specifically related to preparation method and the application in the battery thereof of a kind of Pt-Mn-Graphene fuel-cell catalyst.
Background technology
Direct methanol fuel cell, owing to having the advantages such as easy to carry, structure is simple, theoretical specific energy height, fuel source are abundant, has broad application prospects in portable mobile power supply. So far, the anode catalyst of nearly all direct methanol fuel cell is all the matrix material adopting precious metals pt or platinum. The direct oxidation of methyl alcohol is had very high activity by Pt metal, but Pt is easy to tightly be adsorbed on by methanol oxidation intermediate product (such as CO) be difficult to carry out absorption and dissociate on the surface, so that anodic overpotential improves, Pt utilization ratio is caused to reduce, the scarcity of resources of Pt metal is expensive in addition, and this just greatly limit the commercial applications of direct methanol fuel cell.
The shape looks of nano Pt particles and the structures shape efficiency of catalyzer. The particle diameter of Pt catalyzer is more little, and dispersity is more high, and the efficiency of catalyzer catalytic oxidation methyl alcohol is also more high. Research finds, it is active that methyl alcohol is had good catalytic oxidation by the macroporous Pt of three-dimensional order. The Lv Gongxuan of the Lanzhou Chemistry and Physics Institute of the Chinese Academy of Sciences passes through in saturated IodineSodium Solution with Ag nano wire reduction H2PtCl6Method synthesized Pt nano tube catalyst. In addition, many carbon materials by people as support applications to direct methanol fuel cell field, such as gac, carbon nanotube, porous carbon, Graphene etc. In these carriers, Graphene is because having high-specific surface area, good electroconductibility and relatively high chemical stability, and obtains and study widely. Graphene is a kind of monolayer carbon atom material being stripped out from graphite, and carbon atom arrangement is cellular or positive hexagonal structure, is the two-dirnentional structure being made up of carbon atom. The thickness of this kind of graphite crystal film only hairline 200,000/. There is scholar to prepare Pt/ graphen catalyst, and have studied it to the oxidation susceptibility of methyl alcohol, it has been found that the anodic oxidation of methanol performance of Pt/ Graphene is 2 times of commercial catalyst, and stability is also better than commercial catalyst. There is investigator by Pt nanometer particle load on Graphene, obtain the Pt-FGS catalyzer that hydrogen reduction performance is far superior to commercial catalyst, and stability have also been obtained raising. Having scholar to adopt direct chemical reduction method, take sodium Metal 99.5 as reductive agent, zellon is Pt/ graphen catalyst prepared by carbon source, and exchange current density is 2.5 times of commercialization Pt/C electrode.
At present for mainly Pt metal and the Pt based composites of direct methanol fuel cell catalyzer, Pt consumption is big. Therefore, reducing Pt consumption, it is to increase composite catalyst catalytic activity, a kind of novel composite catalyst of synthesis is significant.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of Pt-Mn-Graphene fuel-cell catalyst, this Pt-Mn-grapheme material can as the composite catalyst of direct methanol dyestuff battery.
The above-mentioned purpose of the present invention is achieved by technical scheme below:
A preparation method for Pt-Mn-Graphene fuel-cell catalyst, comprises the steps:
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with graphene oxide solution;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 3��5:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-60��-40 DEG C of conditions, lyophilize 20��28h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 130��170 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
Further, in the preparation method of described Pt-Mn-Graphene fuel-cell catalyst, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 4:1.
Further, in the step S1 of the preparation method of described Pt-Mn-Graphene fuel-cell catalyst, the concentration of graphene oxide solution is 8g/L.
Further, the preparation method step S3 of described Pt-Mn-Graphene fuel-cell catalyst is: transferred to by biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely.
Further, the preparation method step S4 of described Pt-Mn-Graphene fuel-cell catalyst is: the sample removing moisture is put into moisture eliminator upper strata, pipette excessive hydrazine hydrate and inject moisture eliminator bottom, the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
Pt-Mn-Graphene fuel-cell catalyst prepared by the above-mentioned preparation method application in direct methanol fuel cell.
The advantage of the present invention:
Methyl alcohol is had excellent catalytic performance by Pt-Mn-Graphene fuel-cell catalyst provided by the invention, this kind of performance may with H in preparation method2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is relevant, works as H2PtCl6��6H2O and MnCl2��4H2When the weight ratio of O is between 3��5:1, catalytic performance is best.
Embodiment
The essentiality content of the present invention is described further below in conjunction with embodiment, but does not limit protection domain of the present invention with this. Although the present invention being explained in detail with reference to better embodiment, it will be understood by those within the art that, it is possible to the technical scheme of the present invention is modified or equivalent replacement, and do not depart from essence and the scope of technical solution of the present invention.
In the present invention, graphene oxide adopts the Hummers method preparation of improvement, see document Hummers, and W.S., Jr.; Offeman, R.E.J.Am.Chem.Soc.1958,80,1339.
The preparation of embodiment 1:Pt-Mn-Graphene fuel-cell catalyst
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with the graphene oxide solution that concentration is 8g/L;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 4:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
The preparation of embodiment 2:Pt-Mn-Graphene fuel-cell catalyst
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with the graphene oxide solution that concentration is 8g/L;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 3:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
The preparation of embodiment 3:Pt-Mn-Graphene fuel-cell catalyst
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with the graphene oxide solution that concentration is 8g/L;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 5:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
The preparation of embodiment 4:Pt-Mn-Graphene fuel-cell catalyst
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with the graphene oxide solution that concentration is 8g/L;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 2:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
The preparation of embodiment 5:Pt-Mn-Graphene fuel-cell catalyst
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with the graphene oxide solution that concentration is 8g/L;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 6:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
Embodiment 6: effect example, to the electrocatalytic oxidation property of methyl alcohol
The catalyst sample being carried out testing example 1��5 preparation by cyclic voltammetry (CV) is active to the catalytic oxidation of methyl alcohol. Taking the different sample of 0.002g respectively and be placed in 2ml ethanol, ultrasonic disperse is even; 10 �� l massfraction 5% perfluorinated sulfonic acid (Nafion117) solution are added, ultrasonic disperse 1min in scattered suspension; It is coated in pipetting the 30 above-mentioned uniform suspension of �� l on glass-carbon electrode that diameter is 3mm, at room temperature dries as working electrode; Reference electrode is as standard calomel electrode (SCE), and platinum electrode is as supporting electrode. At 0.5mol/L methyl alcohol and 0.5mol/LH2SO4The catalyzer of middle testing example 1��5 preparation is to the catalytic oxidation activity (the logical nitrogen 30min of electrolytic solution removes dissolved oxygen wherein) of methyl alcohol. The test of chemical property carries out all at ambient temperature, and sweep limit is-0.4��1.0V, and scanning speed is 50mV/s.
Under 50mV/s scanning speed scan 100 circulation CV, embodiment 1��3 prepare catalyst sample methyl alcohol is had good katalysis, embodiment 4��5 prepare catalyst sample to methyl alcohol without katalysis. Oxidation peak current potential, the peak current density of methyl alcohol are seen the following form by catalyst sample prepared by embodiment 1��3:
| Sample | Oxidation peak current potential (V) | Peak current density (A) |
| Embodiment 1 | 0.68 | 7.0��10-4 |
| Embodiment 2 | 0.57 | 0.8��10-4 |
| Embodiment 3 | 0.60 | 2.7��10-4 |
The peak current of catalyst sample prepared by embodiment 1 is the highest, and catalytic activity is best.
It thus is seen that methyl alcohol is had excellent catalytic performance by Pt-Mn-Graphene fuel-cell catalyst provided by the invention, this kind of performance may with H in preparation method2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is relevant, works as H2PtCl6��6H2O and MnCl2��4H2When the weight ratio of O is between 3��5:1, catalytic performance is best.
The effect of above-described embodiment is to illustrate the essentiality content of the present invention, but does not limit protection scope of the present invention with this. It will be understood by those within the art that, it is possible to the technical scheme of the present invention is modified or equivalent replacement, and do not depart from essence and the protection domain of technical solution of the present invention.
Claims (6)
1. the preparation method of a Pt-Mn-Graphene fuel-cell catalyst, it is characterised in that, comprise the steps:
Step S1, by the graphene oxide ultrasonic disperse of drying in water, is mixed with graphene oxide solution;
Step S2, by H2PtCl6��6H2O and MnCl2��4H2The mixture of O is scattered in graphene oxide solution, and mixing ultrasonic disperse is even obtains biased sample; H2PtCl6��6H2O and MnCl2��4H2The weight of the mixture of O is equal with the weight of dry graphene oxide, H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 3��5:1;
Step S3, transfers to biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, and freezing rear sample is placed in freeze drier, and under-60��-40 DEG C of conditions, lyophilize 20��28h is to removing moisture completely;
Step S4, puts into moisture eliminator upper strata by the sample removing moisture, pipettes excessive hydrazine hydrate and injects moisture eliminator bottom, and the baking oven insulation of 130��170 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
2. the preparation method of Pt-Mn-Graphene fuel-cell catalyst according to claim 1, it is characterised in that: H2PtCl6��6H2O and MnCl2��4H2The weight ratio of O is 4:1.
3. the preparation method of Pt-Mn-Graphene fuel-cell catalyst according to claim 2, it is characterised in that, in step S1, the concentration of graphene oxide solution is 8g/L.
4. the preparation method of Pt-Mn-Graphene fuel-cell catalyst according to claim 3, it is characterized in that, step S3 is: transferred to by biased sample after in dixie cup, dixie cup is placed in liquid nitrogen quick freeze, freezing rear sample is placed in freeze drier, and under-50 DEG C of conditions, lyophilize 24h is to removing moisture completely.
5. the preparation method of Pt-Mn-Graphene fuel-cell catalyst according to claim 3, it is characterized in that, step S4 is: the sample removing moisture is put into moisture eliminator upper strata, pipette excessive hydrazine hydrate and inject moisture eliminator bottom, the baking oven insulation of 150 DEG C put into by moisture eliminator after building, the hydrazine hydrate of bottom evaporates into steam makes sample fully be reduced.
6. the application of the Pt-Mn-Graphene fuel-cell catalyst that prepared by the arbitrary described preparation method of Claims 1 to 5 in direct methanol fuel cell.
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Citations (5)
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| CN103165916A (en) * | 2013-03-01 | 2013-06-19 | 北京化工大学常州先进材料研究院 | High-stability Pt-M/MOFs-graphene electro-catalytic agents and preparation method thereof |
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| CN103855411A (en) * | 2012-12-04 | 2014-06-11 | 中国科学院大连化学物理研究所 | Catalyst of fuel cell and application of catalyst |
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- 2016-03-22 CN CN201610168232.7A patent/CN105655600A/en active Pending
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| US20120094199A1 (en) * | 2009-06-02 | 2012-04-19 | Basf Se | Catalyst for electrochemical applications |
| CN102810677A (en) * | 2012-08-17 | 2012-12-05 | 中国东方电气集团有限公司 | Fuel cell catalyst and preparation method thereof |
| CN103855411A (en) * | 2012-12-04 | 2014-06-11 | 中国科学院大连化学物理研究所 | Catalyst of fuel cell and application of catalyst |
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