CN108615898B - Fe-S-N co-doped graphene Pt-loaded catalyst for direct methanol fuel cell and preparation method of catalyst - Google Patents
Fe-S-N co-doped graphene Pt-loaded catalyst for direct methanol fuel cell and preparation method of catalyst Download PDFInfo
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- CN108615898B CN108615898B CN201810334947.4A CN201810334947A CN108615898B CN 108615898 B CN108615898 B CN 108615898B CN 201810334947 A CN201810334947 A CN 201810334947A CN 108615898 B CN108615898 B CN 108615898B
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- H01M4/00—Electrodes
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- H—ELECTRICITY
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- 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
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- 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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- 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
Abstract
The invention discloses a preparation method of a Fe-S-N co-doped graphene Pt-loaded catalyst for a direct methanol fuel cell, which is characterized by comprising the following steps of: 1) carrying out heat treatment on the sodium iron phthalocyanine tetrasulfonate functionalized graphene GR to prepare the Fe-S-N co-doped GR composite material in one step; 2) and then depositing vermicular Pt nano particles by taking the composite material prepared in the step 1) as a carrier to obtain the Fe-S-N co-doped GR Pt-loaded catalyst. The method has the advantages of simple process, mild and controllable operation conditions and good application prospect, and the Pt catalyst prepared by the method can enhance the synergistic coupling effect between the catalytic nanoparticles and the Fe-S-N CO-doped GR carrier, can improve the electrocatalytic activity of the catalyst on methanol oxidation and oxygen reduction reactions, and shows excellent electrochemical stability and CO poisoning resistance.
Description
Technical Field
The invention relates to the field of electrocatalysis and fuel cells, in particular to a Fe-S-N co-doped graphene Pt-loaded catalyst for a direct methanol fuel cell and a preparation method thereof.
Background
At present, the higher cost and lower electrocatalytic performance of the anode and cathode electrocatalysts of the direct methanol fuel cell are still major factors hindering the large-scale commercial application of the electrocatalysts. Therefore, how to improve the utilization efficiency and the electrocatalytic performance of the noble metal Pt in the catalyst has been a hot issue of research in this field.
The size, dispersion and utilization efficiency of Pt nanoparticles in the electrocatalyst are closely related to the catalyst support used and its surface properties. Although the carbon-supported Pt-based electrocatalyst is widely used as an anode and cathode electrode material for a direct methanol fuel cell, the low Pt utilization efficiency and poor electrocatalytic performance of the catalyst are still to be improved due to the factors of small pore size in the carbon black of the support, poor electrochemical stability, etc. Graphene has excellent physical and chemical properties such as high specific surface area, outstanding electric and thermal conductivity, mechanical properties, extraordinary electron transfer performance and the like, and has attracted extensive attention in the field of preparation of fuel cell electrocatalysts. However, the graphene with a complete structure has high chemical stability, the surface of the graphene is in an inert state, and sufficient surface active sites are not available for fixing a catalyst precursor, so that the catalyst nanoparticles are unevenly dispersed and agglomerated, which obviously brings great difficulty to the construction of the graphene-based fuel cell catalyst. Therefore, activating the graphene surface to improve its surface properties and dispersion properties remains a big challenge.
Recent researches find that the introduction of foreign doping atoms (such as N, B, P, S and the like) on the surface of graphene is an effective way for enhancing the activity of metal nanoparticles deposited on the surface of graphene, wherein the electrocatalytic performance of a fuel cell catalyst can be further improved due to the synergistic coupling effect on the surface of graphene co-doped with two kinds of hetero atoms, and people pay attention to the invention. At present, the literature reports on the aspect mainly relate to S-N, Fe-N, B-N or I-N co-doped graphene-based composite materials, such as: (1) the research on the electrocatalytic performance of the nitrogen and sulfur co-doped graphene cobalt sulfide-loaded nano hollow sphere catalyst on the oxygen reduction and oxygen precipitation reaction is reported in Journal of Materials Chemistry A in 2017; (2) 2016, Small reports the research on the electrocatalytic performance of an iron and nitrogen co-doped graphene catalyst on an oxygen reduction reaction; (3) 2013, Angewandte Chemie International Edition reports a research on electrocatalysis performance of a boron and nitrogen two-step doped graphene composite catalyst on an oxygen reduction reaction; (4) research on electrocatalytic performance of an iodine and nitrogen doped graphene composite catalyst on an oxygen reduction reaction is reported in ChemSusChem 2015. However, the above co-doped graphene composite materials only contain two kinds of doping atoms, and studies on one-step preparation of Fe-S-N ternary co-doped graphene composite materials by heat treatment of iron phthalocyanine tetrasulfonate (TSFePc) functionalized graphene and application of the Fe-S-N ternary co-doped graphene composite materials to fuel cell anode and cathode electrocatalyst carriers have not been reported in documents and patents.
Disclosure of Invention
The invention aims to provide a Fe-S-N co-doped graphene Pt-loaded catalyst for a direct methanol fuel cell and a preparation method thereof, aiming at the defects of the prior art. The method has the advantages of simple process, mild and controllable operation conditions and good application prospect, and the Pt catalyst prepared by the method can enhance the synergistic coupling effect between the catalytic nanoparticles and the Fe-S-N CO-doped GR carrier, can improve the electrocatalytic activity of the catalyst on methanol oxidation and oxygen reduction reactions, and shows excellent electrochemical stability and CO poisoning resistance.
The technical scheme for realizing the purpose of the invention is as follows:
compared with the prior art, the preparation method of the Fe-S-N co-doped graphene Pt-loaded catalyst for the direct methanol fuel cell comprises the following steps:
1) adding 10mg of Graphene (GR) and 8-50mg of iron phthalocyanine tetrasulfonate (TSFePc) into a container filled with tertiary distilled water, ultrasonically dispersing for 6h at normal temperature, standing overnight, centrifuging, washing and vacuum drying the obtained product to obtain a TSFePc functionalized GR composite material, then weighing 20mg of a TSFePc functionalized GR sample, and placing the TSFePc functionalized GR sample in a quartz tube furnace to carry out heat treatment for 3h at the temperature of 300-1000 ℃ under the protection of argon to obtain the Fe-S-N co-doped GR composite material (Fe-S-N-GR);
2) 10mg of Fe-S-N-GR and 19.3mM of H were added to 20mL of ethylene glycol at a certain mass ratio (Pt/Fe-S-N-GR = 1/4)2PtCl6And (3) carrying out ultrasonic treatment on the solution for 2h, then transferring the solution into a 30mL reaction kettle, reacting for 24h at the temperature of 80-180 ℃, and centrifuging, washing and vacuum drying a reaction product to obtain the Fe-S-N co-doped GR Pt-loaded catalyst (Pt/Fe-S-N-GR).
The dosage of the phthalocyanine iron tetrasodium sulfonate in the step 1) is 20 mg.
The Fe-S-N co-doped graphene Pt-loaded catalyst prepared by the preparation method is used.
The Fe-S-N co-doped graphene Pt-loaded catalyst prepared by the preparation method is applied to a direct methanol fuel cell.
The morphology, the size and the utilization efficiency of Pt nanoparticles in the fuel cell electrocatalyst are closely related to a used catalyst carrier and surface properties of the catalyst carrier, and the Fe-S-N CO-doped GR composite material prepared by heat-treating iron phthalocyanine tetrasodium sulfonate (TSFePc) functionalized Graphene (GR) is used as the carrier to prepare vermicular Pt nanoparticles through deposition, so that the synergistic coupling effect between the catalytic nanoparticles and the Fe-S-N CO-doped GR carrier can be obviously improved.
The method has the advantages of simple process, mild and controllable operation conditions and good application prospect, the Pt catalyst prepared by the method enhances the synergistic coupling effect between the catalytic nanoparticles and the Fe-S-N CO-doped GR carrier, improves the electrocatalytic activity of the catalyst on methanol oxidation and oxygen reduction reactions, and shows excellent electrochemical stability and CO poisoning resistance.
Drawings
FIG. 1 is a schematic flow chart of the preparation of a Fe-S-N co-doped graphene Pt-supported catalyst in the example;
FIG. 2 is a TEM image of the Fe-S-N co-doped graphene Pt-supported catalyst prepared in example;
FIG. 3 shows Pt/Fe-S-N-GR, Pt/GO and commercial Pt/C catalysts prepared in the examples at 0.5M CH3OH+0.5M H2SO4Cyclic voltammograms in solution;
FIG. 4 is a graph of Pt/Fe-S-N-GR, Pt/GO and commercial Pt/C catalysts prepared in the examples at 0.5M H saturated with oxygen2SO4Linear sweep voltammogram in solution.
Detailed Description
The invention will be further illustrated, but not limited, by the following description of the embodiments with reference to the accompanying drawings.
Example (b):
referring to fig. 1, a preparation method of a direct methanol fuel cell Fe-S-N co-doped graphene supported Pt catalyst includes the following steps:
1) adding 10mg of Graphene (GR) and 8-50mg of iron phthalocyanine tetrasulfonate (TSFePc) into a container filled with tertiary distilled water, ultrasonically dispersing for 6h at normal temperature, standing overnight, centrifuging, washing and vacuum drying the obtained product to obtain a TSFePc functionalized GR composite material, then weighing 20mg of a TSFePc functionalized GR sample, and placing the TSFePc functionalized GR sample in a quartz tube furnace to carry out heat treatment for 3h at the temperature of 300-1000 ℃ under the protection of argon to obtain the Fe-S-N co-doped GR composite material (Fe-S-N-GR);
2) 10mg of Fe-S-N-GR and 19.3mM of H were added to 20mL of ethylene glycol at a certain mass ratio (Pt/Fe-S-N-GR = 1/4)2PtCl6And (3) carrying out ultrasonic treatment on the solution for 2h, then transferring the solution into a 30mL reaction kettle, reacting for 24h at the temperature of 80-180 ℃, and centrifuging, washing and vacuum drying a reaction product to obtain the Fe-S-N co-doped GR Pt-loaded catalyst (Pt/Fe-S-N-GR).
In this example, the amount of the sodium iron phthalocyanine tetrasulfonate in the step 1) is 20 mg.
The Fe-S-N co-doped graphene Pt-loaded catalyst prepared by the preparation method is used.
The Fe-S-N co-doped graphene Pt-loaded catalyst prepared by the preparation method is applied to a direct methanol fuel cell.
TEM results show that the vermicular Pt nanoparticles are uniformly dispersed on the surface of the Fe-S-N co-doped GR carrier, the average width of the vermicular Pt nanoparticles is 2.41nm, and as shown in FIG. 2, a TEM image of the Pt-loaded catalyst prepared in the example is given.
The electrocatalytic performance of the Pt/Fe-S-N-GR, graphene oxide supported Pt (noted as Pt/GO) and commercial Pt/C catalysts prepared in this example on methanol oxidation was compared by cyclic voltammetry and chronoamperometry. The results show that the electrocatalytic activity of the Pt/Fe-S-N-GR catalyst prepared in the example on methanol oxidation is 2.0 and 2.7 times that of the Pt/GO and commercial Pt/C catalysts respectively, and in addition, the Fe-S-N co-doped GR supported Pt catalyst also shows excellent electrochemical stability on methanol oxidation, as shown in FIG. 3, different catalysts are shown in 0.5M CH3OH+0.5M H2SO4Cyclic voltammogram in solution.
The performance of the Pt/Fe-S-N-GR, Pt/GO and commercial Pt/C catalysts prepared in the example against CO poisoning is compared by electrochemical CO stripping voltammetry, and the results indicate that the initial oxidation potential (0.40V) of CO on the Pt/Fe-S-N-GR catalyst is shifted by 70mV and 90mV respectively compared with that of the Pt/GO (0.47V) and the commercial Pt/C (0.49V) catalysts, which indicates that the Fe-S-N CO-doped GR Pt-loaded catalyst prepared in the example has excellent capability of resisting CO poisoning.
The electrocatalytic performance of the Pt/Fe-S-N-GR, Pt/GO and commercial Pt/C catalysts prepared in this example on oxygen reduction in acidic medium was compared by linear sweep voltammetry, and the results indicated that the limiting current density (4.11 mA cm) of the Pt/Fe-S-N-GR catalyst prepared in this example on oxygen reduction-2) Is obviously higher than Pt/GO (3.19 mA cm)-2) And commercial Pt/C (3.07 mA cm)-2) Catalyst, in addition, the half-wave potential (0.83V) of the oxygen reduction reaction on the Pt/Fe-S-N-GR prepared in this example was shifted by 10mV and 30mV more positively than the Pt/GO (0.82V) and commercial Pt/C (0.80V) catalysts, respectively, indicating that the Fe-S-N co-doped GR Pt-loaded catalyst prepared in this example has a higher electrocatalytic activity for the oxygen reduction reaction, as shown in FIG. 4, which gives 0.5M H for the different catalysts at oxygen saturation2SO4Linear sweep voltammograms in solution.
Claims (4)
1. A preparation method of a Fe-S-N co-doped graphene Pt-loaded catalyst for a direct methanol fuel cell is characterized by comprising the following steps:
1) adding 10mg of Graphene (GR) and 8-50mg of iron phthalocyanine tetrasulfonate (TSFePc) into a container filled with tertiary distilled water, ultrasonically dispersing for 6h at normal temperature, standing overnight, centrifuging, washing and vacuum drying the obtained product to obtain a TSFePc functionalized GR composite material, then weighing 20mg of a TSFePc functionalized GR sample, and placing the TSFePc functionalized GR sample in a quartz tube furnace to carry out heat treatment for 3h at the temperature of 300 plus materials and 1000 ℃ under the protection of argon to obtain Fe-S-N co-doped GR composite material Fe-S-N-GR;
2) 10mg of Fe-S-N-GR and 19.3mM of H were added to 20mL of ethylene glycol at a certain mass ratio, i.e., Pt/Fe-S-N-GR = 1/42PtCl6And (3) carrying out ultrasonic treatment on the solution for 2h, then transferring the solution into a 30mL reaction kettle, reacting for 24h at the temperature of 80-180 ℃, and centrifuging, washing and vacuum drying a reaction product to obtain the Fe-S-N co-doped GR Pt-loaded catalyst Pt/Fe-S-N-GR.
2. The preparation method of the Fe-S-N co-doped graphene Pt-supported catalyst for the direct methanol fuel cell as claimed in claim 1, wherein the amount of the sodium iron phthalocyanine tetrasulfonate in the step 1) is 20 mg.
3. The Fe-S-N co-doped graphene Pt-supported catalyst prepared by the preparation method of claim 1.
4. The application of the Fe-S-N co-doped graphene Pt-supported catalyst in the direct methanol fuel cell according to claim 3.
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| CN109560295A (en) * | 2018-12-28 | 2019-04-02 | 哈尔滨工业大学 | Composite catalyst and the preparation method and application thereof based on FeNC catalyst Yu Pt-C catalyst |
| CN110085880A (en) * | 2019-05-08 | 2019-08-02 | 广西师范大学 | A kind of Fe3O4The sulfur and nitrogen co-doped graphene of enhancing carries Pt catalyst and the preparation method and application thereof |
| CN111193035B (en) * | 2019-12-03 | 2021-06-11 | 青岛大学 | Preparation method of strong pi-pi conjugated defective graphene and iron phthalocyanine composite material |
| CN111477892B (en) * | 2020-05-27 | 2021-09-28 | 广西师范大学 | V, N co-doped graphene Pt-supported catalyst and preparation method and application thereof |
| CN111710877B (en) * | 2020-07-13 | 2021-05-28 | 广西师范大学 | N-F co-doped graphene Cu single-atom Pt-loaded catalyst and preparation method and application thereof |
| CN112436158B (en) * | 2020-11-06 | 2022-09-13 | 扬州大学 | Anode catalyst of alcohol fuel cell |
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| CN102935382A (en) * | 2012-11-15 | 2013-02-20 | 广西师范大学 | Method for preparing metal phthalocyanine functional grapheme Pt supported catalyst of direct methanol fuel cell |
| CN103990484A (en) * | 2014-05-26 | 2014-08-20 | 西北工业大学 | Preparation method of nitrogen doped and graphene loaded Cu-Cu2O nanocomposites |
| CN105322191A (en) * | 2015-11-06 | 2016-02-10 | 长春理工大学 | P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof |
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| CN102935382A (en) * | 2012-11-15 | 2013-02-20 | 广西师范大学 | Method for preparing metal phthalocyanine functional grapheme Pt supported catalyst of direct methanol fuel cell |
| CN103990484A (en) * | 2014-05-26 | 2014-08-20 | 西北工业大学 | Preparation method of nitrogen doped and graphene loaded Cu-Cu2O nanocomposites |
| CN105322191A (en) * | 2015-11-06 | 2016-02-10 | 长春理工大学 | P-phenyl di(3,4-dicyano phenyl) thioether polymeric iron phthalocyanine and preparation method and application thereof |
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