CN113629258A - Platinum-cobalt alloy catalyst with platinum-rich surface and preparation method and application thereof - Google Patents
Platinum-cobalt alloy catalyst with platinum-rich surface and preparation method and application thereof Download PDFInfo
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- CN113629258A CN113629258A CN202110955317.0A CN202110955317A CN113629258A CN 113629258 A CN113629258 A CN 113629258A CN 202110955317 A CN202110955317 A CN 202110955317A CN 113629258 A CN113629258 A CN 113629258A
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- 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
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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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
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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 belongs to the technical field of fuel cell catalysts, and particularly relates to a platinum-cobalt alloy catalyst with a platinum-rich surface, and a preparation method and application thereof. The preparation method of the platinum-cobalt alloy catalyst with platinum-rich surface comprises the following steps: dispersing a carbon material in water, adding a cobalt raw material liquid, shearing and dispersing to form a uniform suspension, removing oxygen in the slurry, adjusting the pH value of the solution to 8-13, adding a platinum raw material liquid, and performing ultrasonic treatment to form special carbon slurry; carrying out filter pressing and washing on the obtained carbon slurry, drying to obtain solid powder, and roasting the dried powder to obtain solid powder; and finally, carrying out surface platinum enrichment treatment: and adding the treatment liquid into the obtained solid powder, stirring, performing ultrasonic treatment, washing until the pH value of the filtrate is 2-7, and drying to obtain the platinum-cobalt alloy catalyst. The platinum-rich surface platinum-containing platinum-cobalt alloy catalyst prepared by the method has excellent oxygen reduction performance due to the platinum-rich surface treatment, and the performance of the catalyst applied to a fuel cell is obviously improved.
Description
Technical Field
The invention belongs to the technical field of fuel cell catalysts, and particularly relates to a platinum-cobalt alloy catalyst with a platinum-rich surface, and a preparation method and application thereof.
Background
In recent years, the demand for environmental protection has been increasing along with the economic development. For technologists in the energy field, the fuel cell is a very good direction because the technology should aim to reduce the pollution to the environment as much as possible in the process of fully utilizing energy. The fuel cell can directly convert chemical energy into electric energy, in particular to a proton exchange membrane fuel cell, and the reaction product is water without any pollution to the environment. The "most core" material of a fuel cell is the catalyst, the performance of which directly affects the performance of the fuel cell.
Among fuel cell catalysts, platinum alloy catalysts and catalysts with special morphology are hot spots of current research, and the catalysts with special morphology are more suitable for scale production due to higher preparation difficulty and difficult control of scale production morphology. Among the alloy catalysts, the platinum-cobalt alloy catalyst exhibits excellent oxygen reduction performance, and the power density applied to the fuel cell is also higher than that of the conventional catalyst. In the reports of the existing preparation methods, most methods use complex raw materials in the preparation process, have multiple steps and are not easy to realize large-scale production.
Disclosure of Invention
The invention aims to provide a platinum-cobalt alloy catalyst with a platinum-rich surface, and a preparation method and application thereof, aiming at the defects of the prior art. The platinum-rich surface platinum-containing platinum-cobalt alloy catalyst prepared by the method has excellent oxygen reduction performance due to the platinum-rich surface treatment, and the performance of the catalyst applied to a fuel cell is obviously improved.
In a first aspect, an embodiment of the present invention provides a preparation method of a platinum-cobalt alloy catalyst with a platinum-rich surface, including the following steps:
(1) preparing special carbon slurry: dispersing a carbon material in water with the mass of 0.1-100 times of that of the carbon material, adding a cobalt raw material liquid, and shearing and dispersing for 5-480min to form a uniform suspension; introducing inert gas to remove oxygen in the slurry, adding an additive to adjust the pH value of the solution to 8-13, adding a platinum raw material solution, performing ultrasonic treatment for 5-720min, and stirring at 20-90 ℃ for 0.5-120 h to form special carbon slurry;
(2) alloying process: filter-pressing and washing the carbon slurry obtained in the step (1), drying for 0.5-24 h at 20-85 ℃ to obtain solid powder, roasting the dried powder for 10-240min at 150-350 ℃ in a protective atmosphere, and roasting for 0.5-24 h at 400-900 ℃ to obtain solid powder;
(3) surface platinum enrichment treatment: and (3) adding 0.1-80L of treatment liquid with the concentration of 0.01-10mol/L into the solid powder obtained in the step (2), stirring and treating for 0.5-120 h at the temperature of 0-80 ℃, then carrying out ultrasonic treatment for 0.1-48 h, washing until the pH value of the filtrate is 2-7, and drying at the temperature of 20-85 ℃ to obtain the platinum-cobalt alloy catalyst.
Further, the carbon material in the step (1) is one or more of partially graphitized carbon black, XC-72R carbon black, Ketjen black, acetylene black or carbon nano-tubes, and the nitrogen adsorption specific surface area of the carbon material is 60-1200 m2The carbon material has a microscopic size of 5 to 90 nm.
Further, the cobalt raw material liquid is a solution of cobalt nitrate, cobalt acetate, cobalt chloride or cobalt sulfate, wherein the concentration of cobalt element is 0.01-300 g/L.
Further, the additive is a mixture of an alkaline substance and a reducing substance, the alkaline substance is one or more of sodium hydroxide, ammonia water or sodium carbonate, and the reducing substance is one or more of sodium formate, ethanol, ethylene glycol, ascorbic acid, oxalic acid and sodium sulfite.
Further, the platinum raw material liquid is an ethylene glycol solution or an aqueous solution of a platinum-containing compound including dinitroso diammine platinum, platinum dichloride, platinum tetrachloride, chloroplatinic acid, and potassium chloroplatinate, and the concentration is 5 to 800 g/L.
Further, the inert gas in the step (1) is nitrogen and/or argon;
and (3) in the roasting process of the step (2), the protective atmosphere is nitrogen, argon, hydrogen-nitrogen mixed gas or hydrogen-argon mixed gas.
Further, the treatment solution in the step (3) is one or more aqueous solutions of acetic acid, hydrochloric acid, nitric acid, sulfuric acid, citric acid, hydrogen peroxide, salicylic acid, low molecular weight hyaluronic acid, trimethylglycine, tartaric acid, ethanol and ethylene glycol or a mixed solution thereof, and the concentration range is 0.02-4mol/L, wherein the molecular weight of the low molecular weight hyaluronic acid is 10000-500000.
Further, the mass fraction of cobalt element in the platinum-cobalt alloy catalyst is 1% -20%, and the mass fraction of platinum element is 2% -50%.
In a second aspect, the embodiment of the invention provides a platinum-cobalt alloy catalyst with a platinum-rich surface, which is prepared by adopting the preparation method.
In a third aspect, the embodiment of the invention provides an application of the platinum-cobalt alloy catalyst with a platinum-rich surface in a fuel cell.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
1. the platinum-cobalt alloy catalyst with the platinum-rich surface uses a preparation process of firstly loading cobalt and then reducing platinum, the used raw materials are green and environment-friendly, and the preparation steps are favorable for large-scale production.
2. The platinum-cobalt alloy catalyst with the platinum-rich surface can further reduce the consumption of noble metals, further optimize the cost and strengthen the stability of the catalyst.
3. According to the surface platinization treatment method in the preparation method of the platinum-cobalt alloy catalyst with the platinum-rich surface, the cobalt element on the surface of the alloy catalyst is removed, so that the platinum element is rich on the surface of the alloy, the utilization rate of noble metal platinum in the catalyst is improved, and the catalytic efficiency can be effectively improved.
4. The platinum-cobalt alloy catalyst with the platinum-rich surface has better performance when being applied to a fuel cell after the platinum-rich treatment.
Drawings
Fig. 1 is a transmission electron microscope image of a platinum-cobalt alloy carbon catalyst prepared in example 1 according to the present invention.
FIG. 2 is a graph comparing X-ray powder diffraction curves of catalysts prepared in examples 2 and 4 of the present invention.
FIG. 3 shows example 2 of the present invention and comparative example2 polarization curves of the fuel cell unit cells made of the prepared catalyst. The test conditions in the figure are as follows: the area of the single cell is 20cm2The anode inlet pressure is 1.1bar, the cathode inlet pressure is 1.0bar, the testing temperature is 80 ℃, the anode dew point is 64 ℃, and the cathode dew point is 64 ℃.
Fig. 4 is a graph of the power density of the platinum-cobalt alloy catalyst with a platinum-rich surface prepared in example 5.
Description of reference numerals: 1-carbon powder; 2-platinum cobalt alloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a platinum-cobalt alloy catalyst with platinum-rich surface comprises the following steps:
(1) dispersing 5g of XC-72R carbon black in 100mL of water, adding 5mL of cobalt sulfate aqueous solution with the concentration of 100g/L, and shearing and dispersing for 10min to obtain uniform suspension; introducing nitrogen to remove oxygen in the slurry, adding 1g of sodium carbonate, 1g of sodium formate and a proper amount of sodium hydroxide solution with the concentration of 10g/L to adjust the pH value of the suspension to 11, adding 22 mL of ethylene glycol solution with the concentration of 200g/L dinitrosoproplatin, performing ultrasonic treatment for 240min, and stirring at 80 ℃ for 120 h to form special carbon slurry;
(2) filter-pressing and washing the carbon slurry obtained in the step (1), drying at 60 ℃ for 6h to obtain powder, roasting the dried powder in hydrogen-nitrogen mixed gas (wherein the volume fraction of hydrogen is 5%) at 200 ℃ for 30min, switching to nitrogen atmosphere, roasting at 550 ℃ for 2h to obtain solid powder;
(3) and (3) adding 100mL of nitric acid with the concentration of 0.5mol/L, 5g of citric acid and 1g of salicylic acid into the solid powder obtained in the step (2), stirring at 35 ℃ for 24 hours, performing ultrasonic treatment for 2 hours, washing until the pH value of the filtrate is 6, and drying at 70 ℃ for 8 hours to obtain the platinum-cobalt alloy catalyst.
(4) Manufacturing a single fuel cell: accurately weighing 200mg of the prepared platinum-cobalt alloy catalyst; measuring 20mL of pure water, 15mL of isopropanol and 1.5mL of perfluorosulfonic acid resin solution (the mass fraction is 5%), adding the pure water, the isopropanol and the perfluorosulfonic acid resin solution into a catalyst, crushing cells for 30min to form uniform catalyst ink, and uniformly coating the ink on a cut proton exchange membrane to be marked as a cathode; weighing 200mg of platinum-carbon catalyst (adopting 60% platinum-carbon catalyst of Manchu-Xin-Wanfeng company), weighing 20mL of pure water, 15mL of isopropanol and 1.5mL of perfluorinated sulfonic acid resin solution, adding the pure water, the isopropanol and the perfluorosulfonic acid resin solution into the catalyst, crushing cells for 30min to form uniform catalyst ink, coating the catalyst ink on the other surface of the membrane, and marking as an anode to form CCM; the gas diffusion layer adopts SGL 28BC model GDL. The baltcFuelCells QCF25 fast assembly test fixture is disassembled, the thickness limiting sheet, the first GDL, the CCM and the second GDL are sequentially placed in the test fixture, the pneumatic button is rotated after the test fixture is fixed, and clamping is finished. And after the gas pipeline is connected, performing single cell test after the gas tightness is detected to be qualified.
Single cell test conditions: the area of the single cell is 20cm2The anode and cathode stoichiometric ratio is 1.5:2.5, the anode dew point is set to 64 ℃, the cathode dew point is 64 ℃, the anode pile entering pressure is 1.1bar, the cathode pile entering pressure is 1.0bar, and the cell test temperature is 80 ℃.
Example 2
A preparation method of a platinum-cobalt alloy catalyst with platinum-rich surface comprises the following steps:
(1) dispersing 0.5g of Ketjen black in 20mL of water, adding 7.5 mL of aqueous solution of cobalt chloride with the concentration of 10g/L, and dispersing for 10min to form uniform suspension; introducing nitrogen to remove oxygen in the slurry, adding a proper amount of ammonia water (the mass fraction is 26%), 0.2g of sodium hydroxide and 5mL of ethanol to adjust the pH value of the solution to be 10.5, adding 40 mL of 10g/L ethylene glycol solution of chloroplatinic acid, performing ultrasonic treatment for 30min, and stirring at 90 ℃ for 48h to form special carbon slurry;
(2) filter-pressing and washing the carbon slurry obtained in the step (1), drying at 80 ℃ for 6h to obtain powder, roasting the dried powder at 250 ℃ for 30min under argon atmosphere, and roasting at 650 ℃ for 12h to obtain solid powder;
(3) and (3) adding 100mL of mixed aqueous solution of sulfuric acid and acetic acid with the concentration of 0.5mol/L and 0.5g of low molecular weight hyaluronic acid (adopting low molecular weight hyaluronic acid with the Fowler-Nordheim molecular weight of 20-40 ten thousand) into the solid powder obtained in the step (2), stirring at the temperature of 70 ℃ for 2 hours, carrying out ultrasonic treatment for 30 minutes, washing until the pH value of the filtrate is 5, and drying at the temperature of 60 ℃ for 8 hours to obtain the platinum-cobalt alloy catalyst.
(4) The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
Example 3
The difference between this example and example 1 is that 3 g of carbon nanotubes are weighed, and the specific surface area of the carbon nanotubes is 800 m2The diameter of the particles is 5-20 nm. The other conditions were the same as in example 1.
The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
Example 4
The present example differs from example 2 in that the dried powder in step (2) is calcined at 300 ℃ for 30min under a nitrogen atmosphere, and 100mL of an aqueous solution of acetic acid and nitric acid having a concentration of 0.5mol/L, and 2g of fruit acid are added to the solid powder obtained in step (2) in step (3), and the other conditions are the same as in example 2.
The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
Example 5
The difference between the preparation method of the platinum-cobalt alloy catalyst with rich platinum on the surface and the embodiment 1 is that 10g/L sodium hydroxide, 1g sodium carbonate and 4g ascorbic acid are added in the step (1) to adjust the pH value of the solution to be 10, the pH value of the filtrate in the step (3) is 4, and the other conditions are the same as the embodiment 1.
The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
Comparative example 1
The present comparative example provides a method for preparing a platinum-cobalt alloy catalyst, and is different from example 1 in that the platinization-enriching treatment process of step (3) is not performed, and the other conditions are the same as example 1.
The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
Comparative example 2
This comparative example provides a platinum-cobalt alloy catalyst, and differs from example 2 in that the platinization-enriching treatment process of step (3) is not performed, and the other conditions are the same as example 2.
The platinum-cobalt alloy catalyst with platinum-rich surface prepared in this example was used as a single cell according to the method for manufacturing a single cell in example 1, and the performance of the single cell was tested under the same conditions as in example 1.
A transmission electron microscope scanning is performed on the platinum-cobalt alloy catalyst sample prepared in the embodiment 1 of the present invention to obtain a transmission electron microscope image, as shown in fig. 1, it can be seen from fig. 1 that the platinum-cobalt alloy catalyst with a platinum-rich surface prepared in the present invention has a relatively uniform distribution of alloy particles.
Fig. 2 is a graph comparing X-ray powder diffraction curves of the catalysts prepared in examples 2 and 4 of the present invention, and it can be seen from fig. 2 that characteristic diffraction peak angles of platinum all have a certain degree of right shift, which shows that the platinum cobalt element alloying degree of the catalyst prepared in the present invention is good.
FIG. 3 is a comparative plot of polarization curves for fuel cell single cells made with catalysts prepared in example 2 of the present invention, comparative example 2; it can be seen from fig. 3 that the current density of the platinum-cobalt alloy catalyst prepared in application example 2 is higher than that of comparative example 2 under the same voltage, which shows that the single cell performance of the platinum-cobalt alloy catalyst subjected to the rich platinum treatment of the present invention is obviously improved compared with the performance of the untreated catalyst.
FIG. 4 is a graph of the power density of a platinum-cobalt alloy catalyst with a platinum-rich surface prepared in example 5 of the present invention; as can be seen from FIG. 4, the current density of the single fuel cell test made of the platinum-cobalt alloy carbon catalyst prepared by the method can reach 1.68A/cm2@0.65V, high power density and good performance.
The platinum-cobalt alloy catalyst with the platinum-rich surface is simple and easily available in raw materials in the preparation process, few in preparation steps and easy for large-scale production, so that the production cost can be reduced.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a platinum-cobalt alloy catalyst with platinum-rich surface is characterized by comprising the following steps:
(1) preparing special carbon slurry: dispersing a carbon material in water with the mass of 0.1-100 times of that of the carbon material, adding a cobalt raw material liquid, and shearing and dispersing for 5-480min to form a uniform suspension; introducing inert gas to remove oxygen in the slurry, adding an additive to adjust the pH value of the solution to 8-13, adding a platinum raw material solution, performing ultrasonic treatment for 5-720min, and stirring at 20-90 ℃ for 0.5-120 h to form special carbon slurry;
(2) alloying process: filter-pressing and washing the carbon slurry obtained in the step (1), drying for 0.5-24 h at 20-85 ℃ to obtain solid powder, roasting the dried powder for 10-240min at 150-350 ℃ in a protective atmosphere, and roasting for 0.5-24 h at 400-900 ℃ to obtain solid powder;
(3) surface platinum enrichment treatment: and (3) adding 0.1-80L of treatment liquid with the concentration of 0.01-10mol/L into the solid powder obtained in the step (2), stirring and treating for 0.5-120 h at the temperature of 0-80 ℃, then carrying out ultrasonic treatment for 0.1-48 h, washing until the pH value of the filtrate is 2-7, and drying at the temperature of 20-85 ℃ to obtain the platinum-cobalt alloy catalyst.
2. The method for preparing the platinum-cobalt alloy catalyst with rich platinum on the surface according to claim 1, wherein the carbon material in the step (1) is one or more of partially graphitized carbon black, XC-72R carbon black, Ketjen black, acetylene black or carbon nanotubes, and the nitrogen adsorption specific surface area of the carbon material is 60-1200 m2The carbon material has a microscopic size of 5 to 90 nm.
3. The method for preparing a platinum-cobalt alloy catalyst with platinum-rich surface according to claim 1, wherein the cobalt raw material solution is a solution of cobalt nitrate, cobalt acetate, cobalt chloride or cobalt sulfate, and the concentration of cobalt element is 0.01-300 g/L.
4. The method for preparing the platinum-cobalt alloy catalyst with rich platinum on the surface according to claim 1, wherein the additive is a mixture of an alkaline substance and a reducing substance, the alkaline substance is one or more of sodium hydroxide, ammonia water or sodium carbonate, and the reducing substance is one or more of sodium formate, ethanol, ethylene glycol, ascorbic acid, oxalic acid and sodium sulfite.
5. The method of claim 1, wherein the platinum raw material solution is an ethylene glycol solution or an aqueous solution containing platinum compounds including dinitroso diammine platinum, platinum dichloride, platinum tetrachloride, chloroplatinic acid, and potassium chloroplatinate, and has a concentration of 5 to 800 g/L.
6. The method for preparing a platinum-cobalt alloy catalyst with platinum rich on the surface according to claim 1, wherein the inert gas in the step (1) is nitrogen and/or argon;
and (3) in the roasting process of the step (2), the protective atmosphere is nitrogen, argon, hydrogen-nitrogen mixed gas or hydrogen-argon mixed gas.
7. The method for preparing a platinum-cobalt alloy catalyst with rich platinum on the surface as claimed in claim 1, wherein the treating fluid in step (3) is one or more aqueous solutions of acetic acid, hydrochloric acid, nitric acid, sulfuric acid, citric acid, hydrogen peroxide, salicylic acid, low molecular weight hyaluronic acid, trimethylglycine, fruit acid, ethanol, ethylene glycol or a mixed solution thereof, and the concentration range is 0.02-4mol/L, wherein the molecular weight of the low molecular weight hyaluronic acid is 10000-500000.
8. The method for preparing a platinum-cobalt alloy catalyst with platinum-rich surface according to claim 1, wherein the mass fraction of cobalt element in the platinum-cobalt alloy catalyst is 1-20%, and the mass fraction of platinum element is 2-50%.
9. A platinum-cobalt alloy catalyst with a platinum-rich surface, characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. Use of the platinum-cobalt alloy catalyst having a platinum-rich surface according to claim 9 in a fuel cell.
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