CN116979076A - Catalyst preparation method, catalyst and fuel cell - Google Patents

Catalyst preparation method, catalyst and fuel cell Download PDF

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Publication number
CN116979076A
CN116979076A CN202310925963.1A CN202310925963A CN116979076A CN 116979076 A CN116979076 A CN 116979076A CN 202310925963 A CN202310925963 A CN 202310925963A CN 116979076 A CN116979076 A CN 116979076A
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catalyst
precursor
liquid
mixed solution
preparing
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王智捷
黄磊
陈实
唐雪君
周江峰
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Dongfeng Motor Group Co Ltd
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Dongfeng Motor Group Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • 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
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)

Abstract

The application relates to a preparation method of a catalyst, which comprises the following steps: providing ethylene glycol dissolved with chloroiridium acid and sodium hydroxide as a precursor solution; performing first heat treatment on the precursor solution at a first temperature and in an inert gas atmosphere to obtain a prefabricated liquid; providing a dispersion of Pt/C catalyst; mixing the prefabricated liquid with the dispersion liquid to obtain a mixed liquid; adjusting the pH value of the mixed solution until the mixed solution is strongly acidic; carrying out solid-liquid separation on the mixed solution to obtain a catalyst precursor, and drying the catalyst precursor after cleaning; and performing second heat treatment on the catalyst precursor at a second temperature to obtain the catalyst. The application enables iridium dioxide to form a nano-network structure on the surface of the Pt/C catalyst, has the characteristics of smaller particle size and high specific surface area, not only can protect the carbon carrier from corrosion in an omnibearing manner, but also has more active sites for water electrolysis reaction, and can show better water electrolysis activity.

Description

Catalyst preparation method, catalyst and fuel cell
Technical Field
The application relates to the field of fuel cells, in particular to a fuel cell anode catalyst.
Background
The proton exchange membrane fuel cell mainly comprises a membrane electrode (comprising a diffusion layer, a catalytic layer and a proton exchange membrane), a bipolar plate and a sealing material. The reaction gas is guided by the polar plate to reach the three-phase junction through the gas diffusion layer to react. In the operation process of the electric pile, insufficient air supply can be caused due to flooding or air supply faults, and the phenomenon of starvation of reaction gas is generated. In particular, this phenomenon occurs for battery anodes, which can lead to more severe effects.
When hydrogen starvation occurs at the anode of the cell, the single-chip cell, which should originally generate current, cannot effectively perform a Hydrogen Oxidation Reaction (HOR) due to insufficient hydrogen supply, and the voltage of the single-chip cell is negative at this time, so that the voltage of the single-chip cell is reversed. When the counter electrode occurs, the anode potential of the single-chip battery will rise under the influence of the whole galvanic pile, and the abnormal anode potential can promote the water electrolysis and carbon corrosion reactions in the single-chip battery. The occurrence of carbon corrosion reaction (COR) will lead to irreversible destruction of Pt particle agglomeration, surface deformation, etc. in the anode catalytic layer, and at the same time, the GDL and flow field plate will also be corroded to cause thinning and perforation. The phenomenon of counter electrode is also accompanied by the water electrolysis reaction (OER). The water electrolysis reaction rate is larger than that of the carbon corrosion reaction, and the continuous progress of the water electrolysis reaction can inhibit the counter-electrode voltage, generate a water electrolysis platform and reduce the intensity of the carbon corrosion reaction. In order to increase the rate of the water electrolysis reaction and inhibit the carbon corrosion reaction, a water electrolysis catalyst is often added to the anode catalyst. The conventional method is to directly add the water electrolysis catalyst into the Pt/C catalyst slurry, so that the dispersion effect is poor, the specific surface area is low, and the phenomenon that part of the carbon carrier is not in good contact with the water electrolysis catalyst exists. Carbon supports that do not have good contact with the water electrolysis catalyst are not protected during the occurrence of counter-electrodes and can be directly corroded.
Disclosure of Invention
The embodiment of the application provides a preparation method of a catalyst, the catalyst and a fuel cell, which are used for solving the technical problem that a water electrolysis catalyst has poor dispersion effect in a Pt/C catalyst.
In a first aspect, an embodiment of the present application provides a method for preparing a catalyst, the method for preparing a catalyst including the steps of:
providing ethylene glycol dissolved with chloroiridium acid and sodium hydroxide as a precursor solution;
performing first heat treatment on the precursor solution at a first temperature and in an inert gas atmosphere to obtain a prefabricated liquid;
providing a dispersion of Pt/C catalyst;
mixing the prefabricated liquid with the dispersion liquid to obtain a mixed liquid;
adjusting the pH value of the mixed solution until the mixed solution is strongly acidic;
carrying out solid-liquid separation on the mixed solution to obtain a catalyst precursor, and drying the catalyst precursor after cleaning;
and performing second heat treatment on the catalyst precursor at a second temperature to obtain the catalyst.
In some embodiments of the application, sodium acetate is also dissolved in the precursor solution.
In some embodiments of the present application, the mass ratio of chloroiridium acid, sodium hydroxide, sodium acetate and ethylene glycol in the precursor solution is 1-3:10:1:2.
in some embodiments of the application, the first temperature is 150-170 ℃.
In some embodiments of the application, the first heat treatment has a duration of 2-4 hours.
In some embodiments of the present application, the adjusting the pH value of the mixed solution until the mixed solution is strongly acidic is specifically:
and adjusting the pH value of the mixed solution to 0.5-0.7.
In some embodiments of the application, the second temperature is 200-280 ℃.
In some embodiments of the application, the second heat treatment is for a duration of 1.5-3 hours.
In a second aspect, embodiments of the present application provide a catalyst, where the catalyst is prepared by a method for preparing the catalyst according to any one of the embodiments of the first aspect.
In a third aspect, embodiments of the present application provide a fuel cell comprising the catalyst according to any one of the embodiments of the second aspect.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the preparation method of the catalyst provided by the embodiment of the application, the prefabricated liquid in which the iridium dioxide nano particles are dispersed is prepared, the dispersion liquid of the Pt/C catalyst is mixed with the prefabricated liquid to obtain the mixed liquid, the pH value of the mixed liquid is adjusted to 0.5-0.7, so that the iridium dioxide nano particles are uniformly distributed in the Pt/C catalyst, after further heat treatment, the iridium dioxide forms a nano net structure on the surface of the Pt/C catalyst, and the catalyst has the characteristics of smaller particle size and high specific surface area, so that the carbon carrier is fully contacted with the iridium dioxide with a water electrolysis catalysis function, and the carbon carrier can be comprehensively protected from degradation phenomena such as corrosion after the reverse electrode phenomenon occurs. Meanwhile, due to the high dispersion characteristic of the reticular structure, the membrane electrode has more active sites for water electrolysis reaction, can show better water electrolysis activity, and further enhances the anti-counter electrode performance of the membrane electrode.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the application or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic flow chart of a method for preparing a catalyst according to an embodiment of the present application;
fig. 2 is a graph showing polarization curves of the membrane electrode provided in example 1 and comparative example of the present application.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Unless specifically stated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or may be prepared by existing methods.
The existing water electrolysis catalyst has the technical problem of poor dispersing effect in the Pt/C catalyst.
The technical scheme provided by the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
in a first aspect, an embodiment of the present application provides a method for preparing a catalyst, the method for preparing a catalyst including the steps of:
s1: providing ethylene glycol dissolved with chloroiridium acid and sodium hydroxide as a precursor solution;
s2: performing first heat treatment on the precursor solution at a first temperature and in an inert gas atmosphere to obtain a prefabricated liquid;
s3: providing a dispersion of Pt/C catalyst;
s4: mixing the prefabricated liquid with the dispersion liquid to obtain a mixed liquid;
s5: adjusting the pH value of the mixed solution until the mixed solution is strongly acidic;
s6: carrying out solid-liquid separation on the mixed solution to obtain a catalyst precursor, and drying the catalyst precursor after cleaning;
s7: and performing second heat treatment on the catalyst precursor at a second temperature to obtain the catalyst.
The Pt/C catalyst is a platinum-carbon catalyst.
As will be appreciated by those skilled in the art, inert gases are conventional materials in the art. As an example, the inert gas in the present application may be at least one of nitrogen and rare gas.
It will be appreciated by those skilled in the art that step S2 is for converting chloroiridic acid into iridium dioxide nanoparticles, and that a suitable first temperature value may be selected by those skilled in the art for this technical purpose.
In the step S5, the pH value of the mixed solution is regulated to be strong acid, so that the chargeability of the surfaces of the nano particles can be increased, and the agglomeration and sedimentation of the metal nano particles are avoided; it is also possible to suppress the formation of complexes such as hydroxides and hydrates. This is advantageous in controlling the particle size of the iridium dioxide nanoparticles to be small. In order to enable the iridium dioxide nanoparticles to be uniformly distributed in the Pt/C catalyst.
In step S6, after the catalyst precursor is washed and dried, iridium dioxide nano particles are loaded on the surface of the Pt/C catalyst. After the second heat treatment in step S7, the load becomes more firm, forming a uniform nano-network structure macroscopically; and removes a portion of the unstable impurities, increasing the performance of the resulting catalyst.
According to the application, the prefabricated liquid in which the iridium dioxide nano particles are dispersed is prepared, then the dispersion liquid of the Pt/C catalyst is mixed with the prefabricated liquid to obtain the mixed liquid, the pH value of the mixed liquid is regulated to be 0.5-0.7, so that the iridium dioxide nano particles are uniformly distributed in the Pt/C catalyst, after further heat treatment, the iridium dioxide forms a nano network structure on the surface of the Pt/C catalyst, and the carbon carrier has the characteristics of smaller particle size and high specific surface area, so that the carbon carrier is fully contacted with the iridium dioxide with a water electrolysis catalysis function, and the carbon carrier can be comprehensively protected from degradation phenomena such as corrosion after the counter electrode phenomenon occurs. Meanwhile, due to the high dispersion characteristic of the reticular structure, the membrane electrode has more active sites for water electrolysis reaction, can show better water electrolysis activity, and further enhances the anti-counter electrode performance of the membrane electrode.
In some embodiments of the application, sodium acetate is also dissolved in the precursor solution.
The sodium acetate can play a role of a surfactant, so that the reaction rate of chloroiridic acid is regulated, the crystal nucleus formation and the crystal growth rate of iridium dioxide nano-particles are further controlled, and the particle size and morphology are controlled; meanwhile, the pH value of the precursor solution can be controlled more accurately by fine adjustment of the pH value of the sodium acetate.
In some embodiments of the present application, the mass ratio of chloroiridium acid, sodium hydroxide, sodium acetate and ethylene glycol in the precursor solution is 1-3:9-11:0.9-1.1:2.
the concentration of chloroiridic acid in ethylene glycol can affect the size and quality of the iridium dioxide nanoparticles formed. Too low a concentration of chloroiridium can result in difficult formation of iridium dioxide nanoparticles, and too high a concentration can result in too large a particle size of iridium dioxide nanoparticles for uniform distribution into the Pt/C catalyst.
In some embodiments of the application, the first temperature is 150-170 ℃.
Too low a first temperature may result in a slow or non-productive rate of iridium dioxide nanoparticles; too high a first temperature may result in too large a particle size of iridium dioxide nanoparticles.
In some embodiments of the application, the first heat treatment has a duration of 2-4 hours.
The duration of the first heat treatment is too short, the reaction is easy to be incomplete, and raw material waste is caused; too long a time for the first heat treatment may result in too large a particle size of iridium dioxide nanoparticles.
In some embodiments of the present application, the adjusting the pH value of the mixed solution until the mixed solution is strongly acidic is specifically:
and adjusting the pH value of the mixed solution to 0.5-0.7.
In some embodiments of the application, the providing a dispersion of Pt/C catalyst comprises the steps of:
dispersing the Pt/C catalyst into an acid solution.
Dispersing the Pt/C catalyst into the acid solution can lead the surface of the Pt/C catalyst to be acidic in advance, and is favorable for uniformly distributing iridium dioxide nano particles into the Pt/C catalyst.
The acid in the acid solution is preferably a volatile acid, as will be appreciated by those skilled in the art. The volatile acid, if present, may be removed during the second heat treatment. The volatile acid may preferably be hydrochloric acid.
In some embodiments of the application, the adjusting the mixed liquor to a predetermined pH value is achieved by adding hydrochloric acid to the mixed liquor.
In some embodiments of the application, the second temperature is 200-280 ℃.
Too low a second temperature may result in the inability of the nanoweb structure to form. The second temperature is too high to easily cause agglomeration of the nano particles, thereby damaging the nano network structure.
In some embodiments of the application, the second heat treatment is for a duration of 1.5-3 hours.
Too short a time for the second heat treatment may result in the inability of the nanoweb structure to form. Too long a second heat treatment can easily cause agglomeration of the nanoparticles, thereby destroying the nano-network structure.
In a second aspect, embodiments of the present application provide a catalyst, where the catalyst is prepared by a method for preparing the catalyst according to any one of the embodiments of the first aspect. Since the catalyst is prepared by the embodiment of the first aspect, the specific embodiment of the catalyst can refer to the technical scheme of the first aspect. Because the catalyst adopts some or all of the technical solutions of the embodiments of the first aspect, at least the catalyst has all the beneficial effects brought by the technical solutions of the first aspect, which are not described in detail herein.
In a third aspect, embodiments of the present application provide a fuel cell comprising the catalyst according to any one of the embodiments of the second aspect. Since the fuel cell is prepared by the embodiment of the second aspect, the specific embodiment of the fuel cell can be referred to the conventional knowledge in the field of fuel cells and the technical solution of the second aspect. Since the fuel cell adopts some or all of the embodiments of the second aspect, at least all of the advantages brought by the technical aspects of the second aspect are provided, and will not be described in detail herein.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
The present example first provides a catalyst prepared by the following method:
dissolving chloroiridium acid, sodium hydroxide and sodium acetate in ethylene glycol to obtain a precursor solution, wherein the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 1:10:1:2;
putting the precursor solution into argon atmosphere, and heating at 170 ℃ for 3 hours to obtain a prefabricated solution;
providing a commercial Pt/C catalyst with Pt content of 50%, adding the commercial Pt/C catalyst into hydrochloric acid, and uniformly mixing by adopting an ultrasonic dispersion mode to obtain a dispersion liquid;
mixing the prefabricated solution with the dispersion liquid, regulating the pH value of the obtained mixed solution to 0.6 by using hydrochloric acid, uniformly stirring, standing for 3 hours, filtering, washing filter residues by using deionized water, collecting the filter residues, and drying to obtain a catalyst precursor;
and (3) carrying out heat treatment on the catalyst precursor for 2 hours in an air atmosphere at 250 ℃ to obtain the catalyst.
The present embodiment also provides a fuel cell prepared by the following method:
providing a proton exchange membrane;
preparing an anode catalyst: the catalyst provided by the embodiment is taken, deionized water is added for wetting, then a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol are added, and the catalyst ink is obtained after uniform mixing, and the solid content of the catalyst ink is controlled to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode.
Preparing a cathode catalyst: taking a commercial Pt/C catalyst with the Pt content of 50%, adding deionized water for wetting, adding a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol, uniformly mixing to obtain catalyst ink, and controlling the solid content of the catalyst ink to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode to obtain the membrane electrode.
And assembling the obtained membrane electrode, the gas exchange layer and a shell component of the fuel cell to obtain the fuel cell.
Example 2
This embodiment differs from embodiment 1 only in that:
the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 3:11:0.9:2. the method comprises the following steps:
the present example first provides a catalyst prepared by the following method:
dissolving chloroiridium acid, sodium hydroxide and sodium acetate in ethylene glycol to obtain a precursor solution, wherein the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 3:11:0.9:2;
putting the precursor solution into argon atmosphere, and heating at 170 ℃ for 3 hours to obtain a prefabricated solution;
providing a commercial Pt/C catalyst with Pt content of 50%, adding the commercial Pt/C catalyst into hydrochloric acid, and uniformly mixing by adopting an ultrasonic dispersion mode to obtain a dispersion liquid;
mixing the prefabricated solution with the dispersion liquid, regulating the pH value of the obtained mixed solution to 0.6 by using hydrochloric acid, uniformly stirring, standing for 3 hours, filtering, washing filter residues by using deionized water, collecting the filter residues, and drying to obtain a catalyst precursor;
and (3) carrying out heat treatment on the catalyst precursor for 2 hours in an air atmosphere at 250 ℃ to obtain the catalyst.
The present embodiment also provides a fuel cell prepared by the following method:
providing a proton exchange membrane;
preparing an anode catalyst: the catalyst provided by the embodiment is taken, deionized water is added for wetting, then a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol are added, and the catalyst ink is obtained after uniform mixing, and the solid content of the catalyst ink is controlled to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode.
Preparing a cathode catalyst: taking a commercial Pt/C catalyst with the Pt content of 50%, adding deionized water for wetting, adding a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol, uniformly mixing to obtain catalyst ink, and controlling the solid content of the catalyst ink to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode to obtain the membrane electrode.
And assembling the obtained membrane electrode, the gas exchange layer and a shell component of the fuel cell to obtain the fuel cell.
Example 3
This embodiment differs from embodiment 1 only in that:
the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 2:9:1.1:2. the method comprises the following steps:
the present example first provides a catalyst prepared by the following method:
dissolving chloroiridium acid, sodium hydroxide and sodium acetate in ethylene glycol to obtain a precursor solution, wherein the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 2:9:1.1:2;
putting the precursor solution into argon atmosphere, and heating at 170 ℃ for 3 hours to obtain a prefabricated solution;
providing a commercial Pt/C catalyst with Pt content of 50%, adding the commercial Pt/C catalyst into hydrochloric acid, and uniformly mixing by adopting an ultrasonic dispersion mode to obtain a dispersion liquid;
mixing the prefabricated solution with the dispersion liquid, regulating the pH value of the obtained mixed solution to 0.6 by using hydrochloric acid, uniformly stirring, standing for 3 hours, filtering, washing filter residues by using deionized water, collecting the filter residues, and drying to obtain a catalyst precursor;
and (3) carrying out heat treatment on the catalyst precursor for 2 hours in an air atmosphere at 250 ℃ to obtain the catalyst.
The present embodiment also provides a fuel cell prepared by the following method:
providing a proton exchange membrane;
preparing an anode catalyst: the catalyst provided by the embodiment is taken, deionized water is added for wetting, then a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol are added, and the catalyst ink is obtained after uniform mixing, and the solid content of the catalyst ink is controlled to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode.
Preparing a cathode catalyst: taking a commercial Pt/C catalyst with the Pt content of 50%, adding deionized water for wetting, adding a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol, uniformly mixing to obtain catalyst ink, and controlling the solid content of the catalyst ink to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode to obtain the membrane electrode.
And assembling the obtained membrane electrode, the gas exchange layer and a shell component of the fuel cell to obtain the fuel cell.
Comparative example
This comparative example differs from example 1 in that after iridium dioxide nanoparticles were prepared, they were directly added to Pt/C catalyst slurry to prepare a fuel cell. The method comprises the following steps:
first, the preparation of iridium dioxide nanoparticles was performed in this comparative example, specifically as follows:
dissolving chloroiridium acid, sodium hydroxide and sodium acetate in ethylene glycol to obtain a precursor solution, wherein the mass ratio of chloroiridium acid to sodium hydroxide to sodium acetate to ethylene glycol is 1:10:1:2;
and (3) putting the precursor solution into an argon atmosphere, and heating at 170 ℃ for 3 hours to obtain the prefabricated liquid containing iridium dioxide nano particles.
This comparative example provides a fuel cell prepared by the following method:
providing a proton exchange membrane;
preparing an anode catalyst: the catalyst provided by the embodiment is taken, deionized water is added for wetting, then a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol are added, and the catalyst ink is obtained after uniform mixing, and the solid content of the catalyst ink is controlled to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode.
Preparing a cathode catalyst: taking a commercial Pt/C catalyst with the Pt content of 50%, adding deionized water for wetting, adding a certain amount of Nafion emulsion with the mass fraction of 5% and isopropanol, uniformly mixing to obtain catalyst ink, and controlling the solid content of the catalyst ink to be 2%; and (3) carrying out ultrasonic treatment on the catalyst ink for 30min in an ice water bath, and then carrying out ultrasonic spraying on the surface of the proton exchange membrane anode to obtain the membrane electrode.
And assembling the obtained membrane electrode, the gas exchange layer and a shell component of the fuel cell to obtain the fuel cell.
Related experiment and effect data:
the membrane electrodes prepared in example 1 and comparative example were tested for their anti-counter electrode capability. Since the single cell does not have the counter electrode, the counter electrode condition is simulated by the next 850e fuel cell test system. The resulting polarization curve is shown in figure 2.
As shown in fig. 2, example 1 has higher performance and smaller loss than comparative example after the counter electrode, and in ohmic polarization and mass transfer polarization areas, the example has better proton transmission channel and shows more excellent performance because more water electrolysis catalytic reaction active sites are provided, corrosion of carbon carrier and collapse of catalytic layer structure are avoided when the counter electrode occurs. This demonstrates that the membrane electrode obtained in example 1 has better anti-counter electrode properties than the comparative example.
Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In the present application, unless otherwise specified, terms such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present specification, the terms "include", "comprising" and the like mean "including but not limited to". Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other like elements in a process, method, article or apparatus that comprises the element. Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. For the association relation of more than three association objects described by the "and/or", it means that any one of the three association objects may exist alone or any at least two of the three association objects exist simultaneously, for example, for a, and/or B, and/or C, any one of the A, B, C items may exist alone or any two of the A, B, C items exist simultaneously or three of the three items exist simultaneously. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A method for preparing a catalyst, comprising the steps of:
providing ethylene glycol dissolved with chloroiridium acid and sodium hydroxide as a precursor solution;
performing first heat treatment on the precursor solution at a first temperature and in an inert gas atmosphere to obtain a prefabricated liquid;
providing a dispersion of Pt/C catalyst;
mixing the prefabricated liquid with the dispersion liquid to obtain a mixed liquid;
adjusting the pH value of the mixed solution until the mixed solution is strongly acidic;
carrying out solid-liquid separation on the mixed solution to obtain a catalyst precursor, and drying the catalyst precursor after cleaning;
and performing second heat treatment on the catalyst precursor at a second temperature to obtain the catalyst.
2. The method for preparing a catalyst according to claim 1, wherein sodium acetate is further dissolved in the precursor solution.
3. The method for preparing the catalyst according to claim 2, wherein the mass ratio of chloroiridic acid, sodium hydroxide, sodium acetate and ethylene glycol in the precursor solution is 1-3:10:1:2.
4. the method for preparing a catalyst according to claim 1, wherein the first temperature is 150-170 ℃.
5. The method for preparing a catalyst according to claim 1, wherein the duration of the first heat treatment is 2 to 4 hours.
6. The method for preparing the catalyst according to claim 1, wherein the adjusting the pH value of the mixed solution to the mixed solution is strongly acidic is specifically:
and adjusting the pH value of the mixed solution to 0.5-0.7.
7. The method for preparing a catalyst according to claim 1, wherein the second temperature is 200-280 ℃.
8. The method for preparing a catalyst according to claim 1, wherein the duration of the second heat treatment is 1.5 to 3 hours.
9. A catalyst prepared by the method of any one of claims 1-8.
10. A fuel cell, characterized in that it comprises the catalyst of claim 9.
CN202310925963.1A 2023-07-26 2023-07-26 Catalyst preparation method, catalyst and fuel cell Pending CN116979076A (en)

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