CN115000427B - Fuel cell electrode preparation method and electrode - Google Patents

Fuel cell electrode preparation method and electrode Download PDF

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Publication number
CN115000427B
CN115000427B CN202210870730.1A CN202210870730A CN115000427B CN 115000427 B CN115000427 B CN 115000427B CN 202210870730 A CN202210870730 A CN 202210870730A CN 115000427 B CN115000427 B CN 115000427B
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copper atoms
inorganic
substance containing
electrode
fuel cell
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CN115000427A (en
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曹季冬
李飞强
方川
徐云飞
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Beijing Sinohytec 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
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • 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
    • 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
    • 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]
    • 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
    • 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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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Composite Materials (AREA)
  • Inert Electrodes (AREA)
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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 substance 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 with the inorganic film to form the electrode. By forming a porous catalytic layer structure on the surface layer, the contact area of the catalyst and the reaction substance is increased, the number of active sites is increased, and meanwhile, the efficient gas transmission is ensured, so that the purpose of improving the performance of the fuel cell membrane electrode is achieved.

Description

Fuel cell electrode preparation method and electrode
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 a proton exchange membrane fuel cell is below 90 ℃, heat dissipation is required to be carried out in order to keep a proper temperature, the heat dissipation requirement for a high-power heavy truck is a challenge, water heat management is difficult at high temperature, water flooding, membrane drying and other conditions are easy to occur, on the other hand, carbon monoxide and other impurities in hydrogen can cause a cell poisoning phenomenon, and the service life of the fuel cell is not facilitated to be prolonged. The high-temperature proton exchange membrane fuel cell has the advantages of reducing heat dissipation requirements, using fuel containing impurities and the like. However, the main technical difficulty of the high temperature fuel cell is that the high temperature resistance of the membrane is that the inorganic membrane is more stable at high temperature and can withstand higher temperatures than the organic membrane having a lower glass transition temperature.
In the existing high-temperature proton exchange membrane, the phosphate doped polystyrene imidazole (PBI) membrane is suitable for the temperature range of 120-200 ℃, but has the problem of phosphate loss, so that the service life is relatively short. The high-temperature inorganic membrane, such as pyrophosphate, dihydrogen phosphate and the like, has 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 proton transmission resistance of the catalytic layer is larger, the catalyst utilization rate is lower, and the inorganic membrane is not tightly contacted, so that the problem of falling off exists.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for at least partially solving the problem of larger proton transmission resistance in the prior art.
In a first aspect, an embodiment of the present disclosure provides a method for preparing an electrode of a fuel cell, including:
doping with copper atoms to form an inorganic substance 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 with the inorganic film to form the electrode.
Optionally, the doping with copper atoms forms an inorganic substance containing copper atoms, including:
by copper atom doping, a pyrophosphate-copper atom surface layer is formed.
Optionally, before the step of forming the inorganic substance containing copper atoms, doping with copper atoms further comprises:
zirconium pyrophosphate, H 3 PO 4 Mixing with ethanol to obtain a mixture;
fully mixing the mixture and drying to obtain dry powder;
heating the dry 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 at a first set temperature for a set time, cooling the heated powder to obtain precursor powder, including:
the dried powder was heated at 800℃for 5 hours and cooled to room temperature after the completion of heating.
Optionally, the preparation method of the inorganic film comprises the following steps:
preparing an ethanol solution of polyvinyl butyral as a binder, and mixing the binder with the precursor powder to obtain the inorganic film powder.
Optionally, doping with copper atoms to form an inorganic substance containing copper atoms includes:
the precursor powder and CuCl 2 ·2H 2 And (3) fully mixing O in ethanol, drying the mixed substances, introducing hydrogen, heating to a second set temperature, adding a binder, and mixing to obtain the inorganic powder containing copper atoms.
Optionally, the disposing the inorganic substance containing copper atoms on both sides of the inorganic film includes:
sequentially adding and paving inorganic matters containing copper atoms, inorganic film powder and inorganic matters containing copper atoms, and pressing under a set pressure.
Optionally, the replacing copper atoms with platinum atoms, thereby forming the surface layer into a porous catalytic layer structure, includes:
using H 2 PtCl 6 ·6H 2 O aqueous solution, substitution reaction is carried out in ultrasonic environment, and platinum atoms are used for replacing copper atoms.
Optionally, the sintering the surface layer of the porous catalytic layer structure with the inorganic film to form an electrode includes:
heating at 1000℃for 10 hours.
In a second aspect, embodiments of the present disclosure also provide a fuel cell electrode using any of the methods of preparation of the first aspect.
According to the preparation method of the fuel cell electrode and the electrode, provided by the invention, the porous catalytic layer structure is formed on the surface layer, so that the contact area of the catalyst and the reactant is increased, the number of active sites is increased, and meanwhile, the efficient gas transmission is ensured, so that the purpose of improving the performance of the fuel cell membrane electrode is achieved. The electrode does not use a carbon carrier, reduces the cost of the catalyst and avoids the problem of carbon corrosion.
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 according to an embodiment of the present disclosure.
Detailed Description
Embodiments of the present disclosure are described in detail below with reference to the accompanying drawings.
It should be appreciated that the following specific embodiments of the disclosure are described in order to provide a better understanding of the present disclosure, and that other advantages and effects will be apparent to those skilled in the art from the present disclosure. It will be apparent that the described embodiments are merely some, but not all embodiments of the present disclosure. The disclosure may be embodied or practiced in other different specific embodiments, and details within the subject specification may be modified or changed from various points of view and applications without departing from the spirit of the disclosure. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict. All other embodiments, which can be made by one of ordinary skill in the art without inventive effort, based on the embodiments in this disclosure are intended to be within the scope of this disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the following 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 present disclosure, one skilled in the art will appreciate that one aspect described herein may be implemented independently of any other aspect, 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. In addition, such apparatus may be implemented and/or such methods practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
It should also be noted that the illustrations provided in the following embodiments merely illustrate the basic concepts of the disclosure by way of illustration, and only the components related to the disclosure are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of the components in actual implementation may be arbitrarily changed, and the layout of the components may be more complicated.
In addition, in the following description, specific details are provided in order to provide 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 proton exchange membrane-catalyst combined CCM that does not include 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 substance containing copper atoms;
optionally, the doping with copper atoms forms an inorganic substance containing copper atoms, including:
by copper atom doping, a pyrophosphate-copper atom surface layer is formed.
Optionally, doping with copper atoms to form an inorganic substance containing copper atoms includes:
the precursor powder and CuCl 2 ·2H 2 And (3) fully mixing O in ethanol, drying the mixed substances, 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 disposing the inorganic substance containing copper atoms on both sides of the inorganic film includes:
sequentially adding and paving inorganic matters containing copper atoms, inorganic film powder and inorganic matters containing copper atoms, and pressing 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, thereby forming the surface layer into a porous catalytic layer structure, includes:
using H 2 PtCl 6 ·6H 2 O aqueous solution, substitution reaction is carried out in ultrasonic environment, and platinum atoms are used for replacing copper atoms.
And sintering the surface layer of the porous catalytic layer structure with the inorganic film to form the electrode.
Optionally, the sintering the surface layer of the porous catalytic layer structure with the inorganic film to form an electrode includes:
heating at 1000℃for 10 hours.
Optionally, before the step of forming the inorganic substance containing copper atoms, doping with copper atoms further comprises:
zirconium pyrophosphate, H 3 PO 4 Mixing with ethanol to obtain a mixture;
fully mixing the mixture and drying to obtain dry powder;
heating the dry 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 at a first set temperature for a set time, cooling the heated powder to obtain precursor powder, including:
the dried powder was heated at 800℃for 5 hours and cooled to room temperature after the completion of heating.
Optionally, the preparation method of the inorganic film comprises the following steps:
preparing an ethanol solution of polyvinyl butyral as a binder, and mixing the binder with the precursor powder to obtain the inorganic film powder.
In a specific example, the preparation method is as shown in fig. 1, and includes:
in step (1), a precursor powder is prepared: 15 g of zirconium pyrophosphate-Zr (HPO) was weighed out 4 ) 2 ·H 2 O, 1 ml of H is measured 3 PO 4 After adding 30 ml of ethanol for mixing, the components are fully mixed by an ultrasonic crusher, and are dried in an oven after 10 minutes. And (3) placing the dried powder in a muffle furnace, heating to 800 ℃ and keeping for 5 hours, and cooling to room temperature for later use after heating.
In the step (2), preparing 0.05g/ml ethanol solution of polyvinyl butyral as a binder, taking 5g of the precursor powder prepared in the step (1), adding 1 ml of binder, mixing in a mortar, and marking as first powder; weighing 2 g of the powder prepared in the step (1), and weighing 40mg of CuCl 2 ·2H 2 O, fully mixing in 10 ml of ethanol by using an ultrasonic crusher, placing the powder in a tubular furnace after drying in an oven, introducing hydrogen, heating to 300 ℃, reducing copper ions into copper atoms, adding 0.5 ml of binder, mixing in a mortar, and marking as second powder.
In step (3), an inorganic film green body: sequentially adding and paving 1.5g of second powder, 5g of first powder and 0.5g of second powder into a grinding tool, pressing under 15MPa, placing the pressed green body into a flat-bottom culture dish, and adding 20mL of H 2 PtCl 6 ·6H 2 O aqueous solution (2 mgmL) -1 ) And (3) carrying out displacement reaction in an ultrasonic environment, replacing copper atoms on the surface of the green body with platinum atoms, taking out after 30 minutes, and naturally airing.
In step (4), the inorganic film is prepared: and (3) placing the green body obtained in the step (3) in a muffle furnace, heating to 1000 ℃ and keeping for 10 hours, and taking out after cooling to obtain the inorganic film final product.
As shown in fig. 2, a fuel cell electrode comprises an anode 1, a cathode 3 and a proton membrane 2, wherein the anode and the cathode are porous catalytic layer structures.
The basic principles of the present disclosure have been described above in connection with specific embodiments, however, it should be noted that the advantages, benefits, effects, etc. mentioned in the present disclosure are merely examples and not limiting, and these advantages, benefits, effects, etc. are not to be considered as necessarily possessed by the various embodiments of the present disclosure. Furthermore, the specific details disclosed herein are for purposes of illustration and understanding only, and are not intended to be limiting, since the disclosure is not necessarily limited to practice with the specific details described.
In this disclosure, relational terms such as first and second, and the like are 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, such as "comprising," "including," "having," and the like are open ended terms that include, but are not limited to, and are used interchangeably therewith. The terms "or" and "as used herein refer to and are used interchangeably with the term" and/or "unless the context clearly indicates otherwise. The term "such as" as used herein refers to, and is used interchangeably with, the phrase "such as, but not limited to.
In addition, as used herein, the use of "or" in the recitation of items beginning with "at least one" indicates a separate recitation, such that recitation of "at least one of A, B or C" for example means a or B or C, or AB or AC or BC, or ABC (i.e., a and B and C). Furthermore, the term "exemplary" does not mean that the described example is preferred or better than other examples.
It is also noted that in the systems and methods of the present disclosure, components or steps may be disassembled and/or assembled. Such decomposition and/or recombination should be considered equivalent to the present disclosure.
Various changes, substitutions, and alterations are possible to the techniques described herein without departing from the teachings of the techniques defined by the appended claims. Furthermore, 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. The 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 the embodiments of the disclosure to the form disclosed herein. Although a number of example aspects and embodiments have been discussed above, a person of ordinary skill in the art will recognize certain variations, modifications, alterations, additions, and subcombinations thereof.

Claims (3)

1. A method of manufacturing a fuel cell electrode, comprising:
doping with copper atoms to form an inorganic substance containing copper atoms;
disposing an inorganic substance containing copper atoms on both sides of the inorganic film;
using H 2 PtCl 6 ·6H 2 O aqueous solution, carrying out displacement reaction with copper atoms in an ultrasonic environment, so that a porous catalytic layer structure is formed on the surface layer;
sintering the surface layer of the porous catalytic layer structure and the inorganic film to form an electrode;
the preparation method of the inorganic film comprises the following steps:
preparing an ethanol solution of polyvinyl butyral as a binder, and mixing the binder with precursor powder to obtain an inorganic film;
the step of forming an inorganic substance containing copper atoms, prior to the step of doping with copper atoms, further comprises:
zirconium pyrophosphate, H 3 PO 4 Mixing with ethanol to obtain a mixture;
fully mixing the mixture and drying to obtain dry powder;
heating the dry powder at 800 ℃ for 5 hours, and cooling the heated powder to obtain precursor powder;
using copper atom doping to form an inorganic substance containing copper atoms, comprising:
the precursor powder and CuCl 2 ·2H 2 Fully mixing O in ethanol, drying the mixed substances, introducing hydrogen, heating to a second set temperature, reducing copper ions into copper atoms, adding a binder, and mixing to obtain inorganic powder containing the copper atoms;
the method for disposing an inorganic substance containing copper atoms on both sides of an inorganic film comprises:
sequentially adding and paving the inorganic substance containing copper atoms, the inorganic film and the inorganic substance containing copper atoms, and pressing under a set pressure.
2. The method of manufacturing a fuel cell electrode according to claim 1, wherein sintering the surface layer of the porous catalytic layer structure with the inorganic film to form the electrode comprises:
heating at 1000℃for 10 hours.
3. A fuel cell electrode characterized by using the production method according to any one of claims 1 to 2.
CN202210870730.1A 2022-07-23 2022-07-23 Fuel cell electrode preparation method and electrode Active CN115000427B (en)

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CN115566207B (en) * 2022-10-12 2023-07-07 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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