CN115000427A - Fuel cell electrode preparation method and electrode - Google Patents
Fuel cell electrode preparation method and electrode Download PDFInfo
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- CN115000427A CN115000427A CN202210870730.1A CN202210870730A CN115000427A CN 115000427 A CN115000427 A CN 115000427A CN 202210870730 A CN202210870730 A CN 202210870730A CN 115000427 A CN115000427 A CN 115000427A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- H01M4/8605—Porous electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8817—Treatment of supports before application of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
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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 provides a preparation method of a fuel cell electrode and the electrode, wherein the preparation method of the fuel cell electrode comprises the following steps: doping with copper atoms to form an inorganic material containing copper atoms; disposing an inorganic substance containing copper atoms on both sides of the inorganic film; replacing copper atoms with platinum atoms, thereby forming a porous catalytic layer structure on the surface layer; and sintering the surface layer of the porous catalytic layer structure and the inorganic film to form the electrode. The porous catalyst layer structure is formed on the surface layer, so that the contact area of the catalyst and reaction substances is increased, the number of active sites is increased, the high-efficiency gas transmission is ensured, and the purpose of improving the performance of the membrane electrode of the fuel cell is achieved.
Description
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a preparation method of a fuel cell electrode and the electrode.
Background
At present, the working temperature of the proton exchange membrane fuel cell is below 90 ℃, heat dissipation is needed to keep proper temperature, the heat dissipation requirement of a high-power heavy truck is a challenge, hydrothermal management is difficult at high temperature, flooding, membrane drying and other conditions are easy to occur, and on the other hand, impurities such as carbon monoxide in hydrogen can cause cell poisoning, which is not beneficial to prolonging the service life of the fuel cell. The high-temperature proton exchange membrane fuel cell has the advantages of reducing the heat dissipation requirement, using the fuel containing impurities and the like. However, the main technical difficulty of high temperature fuel cells is the high temperature resistance of the membrane, and compared with an organic membrane with a lower glass transition temperature, an inorganic membrane is more stable at high temperature and can resist higher temperature.
In the existing high-temperature proton exchange membrane, a phosphoric acid doped Polybenzimidazole (PBI) membrane is suitable for being used in the temperature range of 120-200 ℃, but the phosphoric acid loss problem exists, so that the service life is short. The high-temperature inorganic membrane, such as pyrophosphate, dihydrogen phosphate, etc., has a simple preparation method and can resist the high temperature of 200-300 ℃. Although the high-temperature inorganic membrane has better tolerance to temperature and humidity, the problems that the proton transmission resistance of the catalytic layer is larger, the utilization rate of the catalyst is lower, and the contact with the inorganic membrane is not tight enough to cause shedding exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for at least partially solving the problem of high proton transmission resistance in the prior art.
In a first aspect, an embodiment of the present disclosure provides a fuel cell electrode preparation method, including:
doping with copper atoms to form an inorganic material containing copper atoms;
disposing an inorganic substance containing copper atoms on both sides of the inorganic film;
replacing copper atoms with platinum atoms, thereby forming a porous catalytic layer structure on the surface layer;
and sintering the surface layer of the porous catalytic layer structure and the inorganic film to form the electrode.
Optionally, the doping with copper atoms to form an inorganic substance containing copper atoms includes:
through copper atom doping, a pyrophosphate-copper atom surface layer is formed.
Optionally, before the step of forming the inorganic substance containing copper atoms by doping with copper atoms, the method further comprises:
mixing zirconium pyrophosphate, H3PO4 and ethanol to obtain a mixture;
fully mixing the mixture and then drying to obtain dry powder;
and heating the dried powder at a first set temperature for a set time, and cooling the heated powder to obtain precursor powder.
Optionally, heating the dry powder at a first set temperature for a set time, and cooling the heated powder to obtain a precursor powder, including:
heating the dried powder at 800 deg.C for 5 hr, and cooling to room temperature.
Optionally, the preparation method of the inorganic membrane comprises:
and preparing an ethanol solution of polyvinyl butyral to be used as a binder, and mixing the binder and the precursor powder to obtain inorganic film powder.
Optionally, doping with copper atoms is used to form an inorganic containing copper atoms, including:
and fully mixing the precursor powder and CuCl2 & 2H2O in ethanol, drying the mixed substance, introducing hydrogen, heating to a second set temperature, adding a binder, and mixing to obtain the inorganic powder containing copper atoms.
Optionally, the inorganic substance containing copper atoms is disposed on both sides of the inorganic film, and includes:
the inorganic substance containing copper atoms, the inorganic film powder and the inorganic substance containing copper atoms are sequentially added and spread, and pressing is performed under a set pressure.
Optionally, the replacing copper atoms with platinum atoms to form a porous catalytic layer structure on the surface layer comprises:
the substitution reaction is carried out by using H2PtCl6 & 6H2O aqueous solution in an ultrasonic environment, and platinum atoms are used for replacing copper atoms.
Optionally, the sintering the porous surface layer of the catalytic layer structure and the inorganic film to form an electrode includes:
heating at 1000 deg.C for 10 hr.
In a second aspect, embodiments of the present disclosure also provide a fuel cell electrode using the preparation method of any one of the first aspects.
According to the fuel cell electrode preparation method and the electrode, the porous catalyst layer structure is formed on the surface layer, so that the contact area of a catalyst and a reaction substance is increased, the number of active sites is increased, high-efficiency gas transmission is guaranteed, and the purpose of improving the performance of a fuel cell membrane electrode is achieved. The electrode does not use a carbon carrier, so that the cost of the catalyst is reduced, and the problem of carbon corrosion is avoided.
Drawings
The foregoing and other objects, features and advantages of the disclosure will be apparent from the following more particular descriptions of exemplary embodiments of the disclosure as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the disclosure.
Fig. 1 is a flow chart of a method for preparing a fuel cell electrode according to an embodiment of the present disclosure;
fig. 2 is a schematic structural diagram of an electrode provided in an embodiment of the present disclosure.
Detailed Description
The embodiments of the present disclosure are described in detail below with reference to the accompanying drawings.
It is to be understood that the embodiments of the present disclosure are described below by specific examples, and other advantages and effects of the present disclosure will be readily apparent to those skilled in the art from the disclosure herein. It is to be understood that the described embodiments are merely illustrative of some, and not restrictive, of the embodiments of the disclosure. The disclosure may be embodied or carried out in various other specific embodiments, and various modifications and changes may be made in the details within the description without departing from the spirit of the disclosure. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the appended claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the disclosure, one skilled in the art should appreciate that one aspect described herein may be implemented independently of any other aspects and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. Additionally, such an apparatus may be implemented and/or such a method may be practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present disclosure, and the drawings only show the components related to the present disclosure rather than the number, shape and size of the components in actual implementation, and the type, amount and ratio of the components in actual implementation may be changed arbitrarily, and the layout of the components may be more complicated.
In addition, in the following description, specific details are provided to facilitate a thorough understanding of the examples. However, it will be understood by those skilled in the art that the aspects may be practiced without these specific details.
An electrode: refers to a CCM in which a proton exchange membrane is combined with a catalyst, excluding a gas diffusion layer.
The embodiment discloses a preparation method of a fuel cell electrode, which comprises the following steps:
doping with copper atoms to form an inorganic material containing copper atoms;
optionally, the doping with copper atoms to form an inorganic substance containing copper atoms includes:
through copper atom doping, a pyrophosphate-copper atom surface layer is formed.
Optionally, doping with copper atoms is used to form an inorganic containing copper atoms, including:
and fully mixing the precursor powder and CuCl2 & 2H2O in ethanol, drying the mixed substance, introducing hydrogen, heating to a second set temperature, adding a binder, and mixing to obtain the inorganic powder containing copper atoms.
Disposing an inorganic substance containing copper atoms on both sides of the inorganic film;
optionally, the inorganic substance containing copper atoms is disposed on both sides of the inorganic film, and includes:
the inorganic substance containing copper atoms, the inorganic film powder and the inorganic substance containing copper atoms are sequentially added and spread, and pressing is performed under a set pressure.
Replacing copper atoms with platinum atoms, thereby forming a porous catalytic layer structure on the surface layer;
optionally, the replacing copper atoms with platinum atoms to form a porous catalytic layer structure on the surface layer comprises:
the substitution reaction was carried out using an aqueous solution of H2PtCl6 & 6H2O in an ultrasonic environment to substitute the copper atom with a platinum atom.
And sintering the surface layer of the porous catalytic layer structure and the inorganic film to form the electrode.
Optionally, the sintering the surface layer of the porous catalytic layer structure and the inorganic film to form the electrode includes:
heating at 1000 deg.C for 10 hr.
Optionally, before the step of forming the inorganic substance containing copper atoms by doping with copper atoms, the method further comprises:
mixing zirconium pyrophosphate, H3PO4 and ethanol to obtain a mixture;
fully mixing the mixture and then drying to obtain dry powder;
and heating the dried powder at a first set temperature for a set time, and cooling the heated powder to obtain precursor powder.
Optionally, the heating the dry powder for a set time at a first set temperature, and cooling the heated powder to obtain a precursor powder, includes:
heating the dried powder at 800 deg.C for 5 hr, and cooling to room temperature.
Optionally, the preparation method of the inorganic membrane comprises:
and preparing an ethanol solution of polyvinyl butyral to be used as a binder, and mixing the binder and the precursor powder to obtain inorganic film powder.
In one particular example, the preparation method is shown in fig. 1, and comprises:
in step (1), precursor powder is prepared: weighing 15 g of zirconium pyrophosphate-Zr (HPO4) 2. H2O, weighing 1 ml of H3PO4, adding 30 ml of ethanol, mixing, fully mixing the components by using an ultrasonic crusher, and drying in an oven after 10 minutes. And (3) placing the dried powder in a muffle furnace, heating to 800 ℃, keeping for 5 hours, and cooling to room temperature after heating for later use.
In the step (2), 0.05g/ml of polyvinyl butyral ethanol solution is prepared to be used as a binder, 5g of the precursor powder prepared in the step (1) is added with 1 ml of the binder and mixed in a mortar, and the mixture is marked as first powder; weighing 40 mg of CuCl from 2 g of the powder prepared in the step (1) 2 ·2H 2 And O, fully mixing the powder in 10 ml of ethanol by using an ultrasonic crusher, drying the powder in an oven, putting the powder in a tubular furnace, introducing hydrogen, heating the powder to 300 ℃, reducing copper ions into copper atoms, adding 0.5 ml of binder, mixing the powder in a mortar, and marking the mixture as second powder.
In step (3), the green inorganic film: adding and spreading 1.5g of second powder, 5g of first powder and 0.5g of second powder in a grinding tool in sequence, pressing under 15MPa, placing the pressed green body into a flat-bottom culture dish, and adding 20 mL of H2PtCl 6.6H 2O aqueous solution (2 mg mL of H2PtCl 6.6H 2O -1 ) Performing displacement reaction in an ultrasonic environment, replacing copper atoms on the surface of a green body with platinum atoms, taking out after 30 minutes, and naturally airingAnd (5) drying.
In step (4), an inorganic film is prepared: and (4) placing the green body obtained in the step (3) in a muffle furnace, heating to 1000 ℃, keeping for 10 hours, cooling, and taking out to obtain the final inorganic film product.
As shown in fig. 2, a fuel cell electrode includes an anode 1, a cathode 3, and a proton membrane 2, and the anode and the cathode have a porous catalytic layer structure.
The foregoing describes the general principles of the present disclosure in conjunction with specific embodiments, however, it is noted that the advantages, effects, etc. mentioned in the present disclosure are merely examples and are not limiting, and they should not be considered essential to the various embodiments of the present disclosure. Furthermore, the foregoing disclosure of specific details is for the purpose of illustration and description and is not intended to be limiting, since the disclosure is not intended to be limited to the specific details so described.
In this disclosure, 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, and words such as "comprising," "including," "having," and the like are open-ended words of art, meaning "including, but not limited to," and may be used interchangeably therewith. The words "or" and "as used herein mean, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
Also, as used herein, "or" as used in a list of items beginning with "at least one" indicates a separate list, such that, for example, a list of "A, B or at least one of C" means A or B or C, or AB or AC or BC, or ABC (i.e., A and B and C). Furthermore, the phrase "exemplary" does not mean that the described example is preferred or better than other examples.
It should also be noted that, in the systems and methods of the present disclosure, various components or steps may be decomposed and/or recombined. These decompositions and/or recombinations are to be considered equivalents of the present disclosure.
Various changes, substitutions and alterations to the techniques described herein may be made without departing from the techniques of the teachings as defined by the appended claims. Moreover, the scope of the claims of the present disclosure is not limited to the particular aspects of the process, machine, manufacture, composition of matter, means, methods and acts described above. Processes, machines, manufacture, compositions of matter, means, methods, or acts, presently existing or later to be developed that perform substantially the same function or achieve substantially the same result as the corresponding aspects described herein may be utilized. Accordingly, the appended claims are intended to include within their scope such processes, machines, manufacture, compositions of matter, means, methods, or acts.
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present disclosure. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the disclosure. Thus, the present disclosure is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, this description is not intended to limit embodiments of the disclosure to the form disclosed herein. While a number of example aspects and embodiments have been discussed above, those of skill in the art will recognize certain variations, modifications, alterations, additions and sub-combinations thereof.
Claims (10)
1. A method of making a fuel cell electrode, comprising:
doping with copper atoms to form an inorganic material containing copper atoms;
disposing an inorganic substance containing copper atoms on both sides of the inorganic film;
replacing copper atoms with platinum atoms, thereby forming a porous catalytic layer structure on the surface layer;
and sintering the surface layer of the porous catalytic layer structure and the inorganic film to form the electrode.
2. The fuel cell electrode preparation method of claim 1, wherein the doping with copper atoms to form an inorganic substance containing copper atoms comprises:
through copper atom doping, a pyrophosphate-copper atom surface layer is formed.
3. The method of manufacturing a fuel cell electrode according to claim 1, wherein the step of forming an inorganic substance containing copper atoms using copper atom doping is preceded by the step of:
mixing zirconium pyrophosphate, H3PO4 and ethanol to obtain a mixture;
fully mixing the mixture and then drying to obtain dry powder;
and heating the dry powder at a first set temperature for a set time, and cooling the heated powder to obtain precursor powder.
4. The method for preparing a fuel cell electrode according to claim 3, wherein the step of heating the dry powder at a first set temperature for a set time and cooling the heated powder to obtain a precursor powder comprises:
heating the dried powder at 800 deg.C for 5 hr, and cooling to room temperature.
5. The method for producing a fuel cell electrode according to claim 3, characterized in that the method for producing an inorganic membrane comprises:
and preparing an ethanol solution of polyvinyl butyral to be used as a binder, and mixing the binder and the precursor powder to obtain the inorganic film.
6. The fuel cell electrode preparation method of claim 3, wherein the forming of the inorganic substance containing copper atoms using copper atom doping comprises:
and fully mixing the precursor powder and CuCl2 & 2H2O in ethanol, drying the mixed substance, introducing hydrogen, heating to a second set temperature, adding a binder, and mixing to obtain the inorganic powder containing copper atoms.
7. The fuel cell electrode production method according to claim 1, wherein the disposing inorganic substances containing copper atoms on both sides of the inorganic film comprises:
an inorganic substance containing copper atoms, an inorganic film, and an inorganic substance containing copper atoms are sequentially added and laid flat, and pressing is performed under a set pressure.
8. The fuel cell electrode production method according to claim 1, wherein the replacing of copper atoms with platinum atoms to form a porous catalytic layer structure on the surface layer comprises:
the substitution reaction was carried out using an aqueous solution of H2PtCl6 & 6H2O in an ultrasonic environment to substitute the copper atom with a platinum atom.
9. The method for preparing an electrode for a fuel cell according to claim 1, wherein the sintering the porous catalytic layer structure surface layer and the inorganic film to form the electrode comprises:
heating at 1000 deg.C for 10 hr.
10. A fuel cell electrode, characterized by using the production method according to any one of claims 1 to 9.
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| CN202210870730.1A CN115000427B (en) | 2022-07-23 | 2022-07-23 | Fuel cell electrode preparation method and electrode |
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| CN202210870730.1A CN115000427B (en) | 2022-07-23 | 2022-07-23 | Fuel cell electrode preparation method and electrode |
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Cited By (1)
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| CN115566207A (en) * | 2022-10-12 | 2023-01-03 | 北京科技大学 | Transition metal pyrophosphate ORR catalyst anchored on MOFs derived carbon skeleton and preparation method and application thereof |
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