CN114361489A - PtC catalyst for fuel cell and preparation process thereof - Google Patents
PtC catalyst for fuel cell and preparation process thereof Download PDFInfo
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- CN114361489A CN114361489A CN202210000502.9A CN202210000502A CN114361489A CN 114361489 A CN114361489 A CN 114361489A CN 202210000502 A CN202210000502 A CN 202210000502A CN 114361489 A CN114361489 A CN 114361489A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- 239000000446 fuel Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 238000005580 one pot reaction Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 150000005846 sugar alcohols Polymers 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000002390 rotary evaporation Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical class 0.000 claims description 4
- VEJOYRPGKZZTJW-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;platinum Chemical compound [Pt].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O VEJOYRPGKZZTJW-FDGPNNRMSA-N 0.000 claims description 3
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 3
- 229910020437 K2PtCl6 Inorganic materials 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 150000003384 small molecules Chemical class 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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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 fuel cell PtC catalyst and a preparation process thereof, wherein a Pt/C catalyst with uniform appearance, concentrated nanoscale and high Pt loading capacity is prepared by a one-pot method through microwave reaction. The method has the advantages of simple process, good reproducibility, uniform distribution of the prepared Pt catalyst, high single-time yield and good catalytic activity and stability when being applied to the small-molecule fuel cell.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a fuel cell PtC catalyst and a preparation process thereof.
Background
The fuel cell is an electrochemical power generation device which directly converts chemical energy stored in fuel and oxidant into electric energy through an electrochemical reaction process, and is a new energy source with high efficiency and cleanness. Currently, while much progress has been made in its research, true commercialization faces many challenges. Among them, the catalyst is one of the key materials determining the performance, life and cost of the fuel cell, and is also one of the important factors hindering the commercialization of the fuel cell. The Pt/C catalyst is the most widely used and typical catalyst for fuel cells. The development of a Pt/C catalyst with high activity and low cost has very important significance for realizing large-scale commercialization. At present, few manufacturers for producing Pt/C catalysts at home and abroad have high price, complex preparation process and low single-time yield.
Disclosure of Invention
The present invention aims to provide a fuel cell PtC catalyst and a preparation process thereof, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a Pt catalyst for fuel cell is prepared from Pt/C catalyst with uniform shape, concentrated nano-scale and high Pt loading capacity by microwave reaction and one-pot method.
Preferably, the preparation process of the fuel cell Pt catalyst adopts microwave reaction and utilizes a polyol reduction method, and comprises the following specific steps:
A. adding a certain amount of Pt precursor and capping agent into the polyalcohol solution according to the proportion of the metal components of the catalyst;
B. introducing nitrogen to remove oxygen in the solution, and stirring and dissolving at 70-80 ℃;
C. after the precursor is dissolved, adding a carbon carrier, and continuously stirring for 10-30 minutes until the precursor is uniformly dispersed;
D. and adjusting the pH value, transferring the reactant into a microwave reactor for reaction, carrying out post-treatment on the reaction solution after the reaction is finished, cooling, washing and drying to obtain the Pt/C catalyst.
Preferably, the Pt mass fraction of the Pt catalyst is 20-60%
Preferably, the Pt precursor is K2PtCl6,H2PtCl6,Pt(acac)2 。
Preferably, the end-capping agent comprises citric acid, sodium citrate, PVP.
Preferably, the polyalcohol solution is a mixture of one or more polyalcohols such as isopropanol, ethylene glycol and pentaerythritol.
Preferably, the carbon carrier is conductive carbon black (XC-72R, EC-600 JD), graphene or carbon nanotubes.
Preferably, the pH adjusting range is 7-11, and the used adjusting agent is NaOH, KOH or Na2CO3Or ammonia.
Preferably, the microwave reaction conditions are as follows: the reaction temperature is 110-.
Preferably, before washing, high vacuum is adopted, part of solvent polyol is removed by rotary evaporation at a certain temperature, most of solvent is removed, when reactants become thick slurry, the temperature is reduced, deionized water is added, washing is carried out, suction filtration is carried out by using a microporous filter membrane, and drying conditions are vacuum drying at 60 ℃ or calcining in a tubular furnace under inert atmosphere.
Compared with the prior art, the invention has the beneficial effects that: the method has simple process, adopts microwave reaction, has short reaction time and good reproducibility, and can reach 3g of single output; in the invention, before the reaction liquid is washed by deionized water, most of the polyhydric alcohol is removed by high vacuum heating rotary evaporation, so that the reaction loss can be greatly reduced, and the yield can be improved. The polyalcohol is a good solvent of nano Pt, if the polyalcohol is not removed, part of Pt is always dispersed in the polyalcohol in the conventional washing process, and the Pt is lost in the washing process. And the ethylene glycol is removed by high vacuum rotary evaporation, and the Pt loading of the obtained catalyst is basically close to the theoretical yield.
Drawings
FIG. 1 is a comparison of cyclic voltammograms of the product of the invention and a JM Pt/C catalyst.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides the following technical solutions: a Pt catalyst for fuel cell is prepared from Pt/C catalyst with uniform shape, concentrated nano-scale and high Pt loading capacity by microwave reaction and one-pot method.
A preparation process of a fuel cell Pt catalyst adopts microwave reaction and utilizes a polyol reduction method, and comprises the following specific steps:
A. adding a certain amount of Pt precursor and capping agent into the polyalcohol solution according to the proportion of the metal components of the catalyst;
B. introducing nitrogen to remove oxygen in the solution, and stirring and dissolving at 70-80 ℃;
C. after the precursor is dissolved, adding a carbon carrier, and continuously stirring for 10-30 minutes until the precursor is uniformly dispersed;
D. and adjusting the pH value, transferring the reactant into a microwave reactor for reaction, carrying out post-treatment on the reaction solution after the reaction is finished, cooling, washing and drying to obtain the Pt/C catalyst.
In the invention, the Pt mass fraction of the Pt catalyst is 20-60%
In the invention, the Pt precursor is K2PtCl6,H2PtCl6,Pt(acac)2 。
In the invention, the end-capping reagent comprises citric acid, sodium citrate and PVP.
In the invention, the polyalcohol solution is one or a mixture of several polyalcohol such as isopropanol, ethylene glycol, pentaerythritol and the like.
In the invention, the carbon carrier is conductive carbon black (XC-72R, EC-600 JD), graphene and carbon nano tubes.
In the invention, the pH adjusting range is 7-11, and the used adjusting agents are NaOH, KOH and Na2CO3Or ammonia.
In the invention, the microwave reaction conditions are as follows: the reaction temperature is 110-.
In the invention, high vacuum is adopted before washing, partial solvent polyalcohol is removed by rotary evaporation at a certain temperature, most of solvent is removed, when reactants become thick slurry, the temperature is reduced, deionized water is added, washing is carried out, suction filtration is carried out by using a microporous filter membrane, and the drying condition is vacuum drying at 60 ℃ or calcining in a tubular furnace under inert atmosphere.
Example 1:
the preparation process of the Pt/C catalyst for the fuel cell with the 40 percent Pt loading comprises the following steps:
A. weighing 2.64g Pt (acac)22.6g of sodium citrate and 480g of ethylene glycol are put into a three-neck flask, nitrogen is introduced, the mixture is heated and stirred at 80 ℃ until the reagents are completely dissolved, the pH value is adjusted to 9 by adding saturated NaOH ethylene glycol solution, 2g of carbon black carrier is added, and the mixture is stirred uniformly;
B. the flask was placed in a microwave reactor, a thermocouple was inserted into the reaction solution to control the temperature, a magnetic stirrer was added, and the reaction was turned to 800 rpm. Setting the microwave reaction time to be 15 minutes, the temperature to be 140 ℃ and the microwave power to be 900W;
C. the reacted reaction solution was transferred to a eggplant-shaped bottle with a rotary evaporator vacuum of 30mbar and an oil bath temperature of 100 ℃. Removing most of ethylene glycol by using a rotary evaporator until the reactant is in a slurry state, stopping rotary evaporation, and cooling in an ice water bath;
D. adding deionized water into the reactant for washing, removing liquid by using a suction filtration device after washing, and obtaining the catalyst on a filter membrane. The catalyst was dried in a vacuum oven at 70 ℃. The catalyst was obtained with a mass fraction of Pt of 40%.
Example 2: preparation process of 50% Pt loaded Pt/C catalyst for fuel cell:
A. weighing 5gK2PtCl64g of sodium citrate and 480g of ethylene glycol are put into a three-neck flask, nitrogen is introduced, the mixture is heated and stirred at 80 ℃ until the reagent is completely dissolved, the pH value is adjusted to 7 (adjustment is not needed), 2g of carbon black carrier is added, and the mixture is stirred uniformly;
B. the flask was placed in a microwave reactor, a thermocouple was inserted into the reaction solution to control the temperature, a magnetic stirrer was added, and the reaction was turned to 1000 rpm. Setting the microwave temperature to be 120 ℃, the microwave power to be 800W, and the reaction procedure is as follows: the microwave reaction was stopped for 10 minutes after 5 minutes. Continuously repeating the steps for 2 times, and reacting for 15 minutes;
C. the reacted reaction solution was transferred to a eggplant-shaped bottle with a rotary evaporator vacuum of 50mbar and an oil bath temperature of 115 ℃. Removing most of ethylene glycol by using a rotary evaporator until the reactant is in a slurry state, stopping rotary evaporation, and cooling in an ice water bath;
D. and adding deionized water into the reactant for washing, standing until the reactant is completely precipitated after washing, pouring to remove supernatant, performing suction filtration by using a suction filtration device, and obtaining the catalyst on a filter membrane. And calcining the catalyst in a tubular furnace at 100 ℃ in a nitrogen atmosphere to obtain the catalyst, wherein the Pt loading capacity is 50%.
In conclusion, the method has simple process, adopts microwave reaction, has short reaction time and good reproducibility, and can reach 3g of single output; in the invention, before the reaction liquid is washed by deionized water, most of the polyhydric alcohol is removed by high vacuum heating rotary evaporation, so that the reaction loss can be greatly reduced, and the yield can be improved. The polyalcohol is a good solvent of nano Pt, if the polyalcohol is not removed, part of Pt is always dispersed in the polyalcohol in the conventional washing process, and the Pt is lost in the washing process. And the ethylene glycol is removed by high vacuum rotary evaporation, and the Pt loading of the obtained catalyst is basically close to the theoretical yield.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A fuel cell Pt catalyst, characterized by: the microwave reaction is utilized to prepare the Pt/C catalyst with uniform appearance, concentrated nanoscale and high Pt loading capacity by a one-pot method.
2. A preparation process of a fuel cell Pt catalyst is characterized by comprising the following steps: adopts microwave reaction and uses a polyol reduction method, and comprises the following specific steps:
A. adding a certain amount of Pt precursor and capping agent into the polyalcohol solution according to the proportion of the metal components of the catalyst;
B. introducing nitrogen to remove oxygen in the solution, and stirring and dissolving at 70-80 ℃;
C. after the precursor is dissolved, adding a carbon carrier, and continuously stirring for 10-30 minutes until the precursor is uniformly dispersed;
D. and adjusting the pH value, transferring the reactant into a microwave reactor for reaction, carrying out post-treatment on the reaction solution after the reaction is finished, cooling, washing and drying to obtain the Pt/C catalyst.
3. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the Pt mass fraction of the Pt catalyst is 20-60%.
4. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the Pt precursor is K2PtCl6,H2PtCl6,Pt(acac)2 。
5. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the end capping agent comprises citric acid, sodium citrate and PVP.
6. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the polyalcohol solution is one or more of isopropanol, ethylene glycol, pentaerythritol, etc.
7. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the carbon carrier is conductive carbon black (XC-72R, EC-600 JD), graphene and carbon nano tubes.
8. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the pH adjusting range is 7-11, and the used adjusting agents are NaOH, KOH and Na2CO3Or ammonia.
9. The fuel cell Pt catalyst preparation process according to claim 2, wherein: the microwave reaction conditions are as follows: the reaction temperature is 110-.
10. The fuel cell Pt catalyst preparation process according to claim 2, wherein: before washing, high vacuum is adopted, partial solvent polyalcohol is removed by rotary evaporation at a certain temperature, most of the solvent is removed, when the reactant becomes thick slurry, the temperature is reduced, deionized water is added, washing is carried out, suction filtration is carried out by using a microporous filter membrane, and the drying condition is vacuum drying at 60 ℃ or tubular furnace calcination under inert atmosphere.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN117080472A (en) * | 2023-07-26 | 2023-11-17 | 深圳大学 | Preparation method of small molecule modified platinum catalyst under microwave action |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN102327771A (en) * | 2011-07-14 | 2012-01-25 | 华南理工大学 | Method for preparing carbon-loaded platinum-based electro-catalyst by microwave organosol method |
CN103730668A (en) * | 2013-12-21 | 2014-04-16 | 南京大学昆山创新研究院 | Pt/C catalyst of fuel cell and preparation technology thereof |
CN106532075A (en) * | 2016-11-14 | 2017-03-22 | 南京大学 | Preparation method of Pt/C catalyst for fuel cell with high Pt carrying capacity |
CN110931815A (en) * | 2019-12-05 | 2020-03-27 | 中船重工黄冈贵金属有限公司 | Preparation method of fuel cell carbon-supported platinum-based catalyst |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102327771A (en) * | 2011-07-14 | 2012-01-25 | 华南理工大学 | Method for preparing carbon-loaded platinum-based electro-catalyst by microwave organosol method |
CN103730668A (en) * | 2013-12-21 | 2014-04-16 | 南京大学昆山创新研究院 | Pt/C catalyst of fuel cell and preparation technology thereof |
CN106532075A (en) * | 2016-11-14 | 2017-03-22 | 南京大学 | Preparation method of Pt/C catalyst for fuel cell with high Pt carrying capacity |
CN110931815A (en) * | 2019-12-05 | 2020-03-27 | 中船重工黄冈贵金属有限公司 | Preparation method of fuel cell carbon-supported platinum-based catalyst |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN117080472A (en) * | 2023-07-26 | 2023-11-17 | 深圳大学 | Preparation method of small molecule modified platinum catalyst under microwave action |
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Application publication date: 20220415 |