CN110676466A - Air electrode, preparation method thereof and metal-air battery comprising air electrode - Google Patents
Air electrode, preparation method thereof and metal-air battery comprising air electrode Download PDFInfo
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- CN110676466A CN110676466A CN201910832868.0A CN201910832868A CN110676466A CN 110676466 A CN110676466 A CN 110676466A CN 201910832868 A CN201910832868 A CN 201910832868A CN 110676466 A CN110676466 A CN 110676466A
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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
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8892—Impregnation or coating of the catalyst layer, e.g. by an ionomer
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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Abstract
The invention discloses an air electrode, a preparation method thereof and a metal-air battery comprising the air electrode. This air electrode is the direct growth catalyst on the mass flow body, easily changes the catalytic layer thickness simultaneously, can save the adhesive, is connected catalyst and mass flow body are firm, slows down the catalyst loss in the metal-air battery working process, reduces air electrode internal resistance simultaneously. Compared with the traditional air electrode of the metal-air battery, the preparation method of the air electrode is suitable for regulating and controlling the hydrophilic and hydrophobic degrees of the catalyst layer and the contact site density of the three-phase reaction in the electrode reaction area, and the preparation method is simple and is easy for batch production. The metal-air battery assembled by the air electrode has higher power density and longer charge-discharge cycle life.
Description
Technical Field
The invention relates to the technical field of metal-air batteries, in particular to an air electrode, a preparation method thereof and a metal-air battery comprising the air electrode.
Background
The metal-air battery is an electrochemical reaction device which takes metal as an anode and oxygen in air as a cathode. The metal air battery has high energy density, simple and light structure, abundant reserves of zinc, aluminum, magnesium and other metals which are usually used as anode materials of the metal air battery, low price and certain application in the fields of field emergency, reserve power supply, communication power supply and the like. Compared with widely used lead-acid batteries and lithium ion batteries, metal air batteries such as zinc air batteries and the like are safer and more environment-friendly, the problems of flammability, easy explosion, heavy metal pollution and the like of electrolyte solution are avoided, and the metal air batteries are hopefully applied to more fields of production and life of people.
The main problems of the existing metal-air battery are that the power density is not high, the charge-discharge cycle life is short, and the charge-discharge voltage difference is large, so that the application of the metal-air battery as an energy storage device is limited by the characteristics. The performance of the metal-air battery is not only related to the catalytic activity of the catalyst, but also related to the structure and preparation process of the air electrode.
As shown in fig. 1, a conventional air electrode structure includes a hydrophobic diffusion layer 101, a current collector 102, and a catalyst layer 103, where the catalyst layer is a composite layer containing catalyst powder, a conductive material, a hydrophilic material, and a hydrophobic material, and is easy to fall off during long-time discharge or cyclic charge and discharge, and at the same time, when the catalyst layer is too thick, the internal resistance is large, the electron transfer rate is slow, and the performance of the metal-air battery is not improved. Therefore, the development of an air electrode which has a simple preparation process and is beneficial to the exertion of catalytic activity of a catalyst becomes a key topic for the development and application of a metal-air battery.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
Therefore, a first object of the present invention is to provide an air electrode, which is easy to change the thickness of a catalyst layer, and can reduce the catalyst loss during the operation of a metal-air battery and simultaneously reduce the internal resistance of the air electrode.
The second purpose of the invention is to provide a preparation method of the air electrode.
A third object of the present invention is to provide a metal-air battery.
In order to achieve the above object, an embodiment of a first aspect of the present invention provides an air electrode including: a hydrophobic diffusion layer; the catalytic conductive composite layer comprises at least one current collector on which a catalyst grows and a hydrophobic material.
According to the air electrode disclosed by the embodiment of the invention, the catalyst directly grows on the current collector, the thickness of the catalytic layer is easy to change, an adhesive can be omitted, the catalyst is stably connected with the current collector, the loss of the catalyst in the working process of the metal-air battery is reduced, and the internal resistance of the air electrode is reduced.
In addition, the air electrode according to the above embodiment of the present invention may also have the following additional technical features:
further, in one embodiment of the present invention, the current collector includes one or more of nickel metal, nickel alloy, and carbon fiber cloth.
Further, in one embodiment of the invention, the catalyst is a combination of one or more of a carbon material, a metal oxide, a metal nitride, a metal sulfide, a metal phosphide, and a defect-containing or hetero-atom-containing dopant compound thereof.
Further, in one embodiment of the present invention, the catalyst is grown on the current collector by hydrothermal reaction or electrodeposition.
Further, in one embodiment of the invention, the number of said at least one current collector is in the interval [1, 10 ].
Further, in one embodiment of the present invention, the hydrophobic material is one or a combination of PTFE and Nafion.
In order to achieve the above object, a second embodiment of the present invention provides a method for manufacturing an air electrode according to the above embodiment, including the following steps: pretreating the current collector; growing the catalyst on the pretreated current collector; hot-pressing at least one current collector with the catalyst at a first preset hot-pressing temperature and pressure to generate the catalytic conductive composite layer; placing the catalytic conductive composite layer in a hydrophobic material solution with a preset concentration, soaking for a preset time, repeating the drying operation and the soaking operation for a preset number of times, and calcining in air at a preset temperature for a preset time; and hot-pressing the treated catalytic conductive composite layer and the hydrophobic diffusion layer at a second preset hot-pressing temperature and pressure to form a whole as a catalytic layer.
Compared with the traditional air electrode of the metal-air battery, the preparation method of the air electrode is suitable for regulating and controlling the hydrophilic and hydrophobic degrees of the catalyst layer and the contact site density of the three-phase reaction in the electrode reaction area, and the preparation method is simple in preparation process and easy for batch production.
In order to achieve the above object, a metal-air battery is provided in an embodiment of a third aspect of the present invention, which includes the air electrode of the above embodiment. The metal-air battery assembled by the air electrode has higher power density and longer charge-discharge cycle life.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic structural diagram of a conventional air electrode according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an air electrode according to an embodiment of the present invention;
FIG. 3 is a flow chart of a method of making an air electrode according to an embodiment of the present invention;
FIG. 4 is a schematic structural view of an air electrode according to embodiment 1 of the present invention;
FIG. 5 is a schematic structural view of an air electrode according to embodiment 2 of the present invention;
fig. 6 is a polarization curve of a zinc-air cell with an air electrode assembly according to example 1 of the present invention;
fig. 7 is a polarization curve of a zinc-air battery with an air electrode assembly according to example 2 of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
An air electrode proposed according to an embodiment of the present invention, a method of manufacturing the same, and a metal-air battery including the air electrode will be described below with reference to the accompanying drawings, in which the air electrode proposed according to an embodiment of the present invention will be described first.
Fig. 2 is a schematic structural view of an air electrode according to an embodiment of the present invention.
As shown in fig. 2, the air electrode includes: a hydrophobic diffusion layer 201 and a catalytically conductive composite layer 202.
Wherein, the catalytic conductive composite layer comprises at least one current collector on which a catalyst grows and a hydrophobic material.
It is understood that the catalytic conductive composite layer 202 is composed of a certain amount of a current collector on which a catalyst is grown, and a certain amount of hydrophobic material contained therein.
Further, in one embodiment of the present invention, the current collector includes one or more of nickel metal, nickel alloy, and carbon fiber cloth.
Further, in one embodiment of the present invention, the catalyst may be a combination of one or more of a carbon material, a metal oxide, a metal nitride, a metal sulfide, a metal phosphide, and defect-containing or hetero-atom-containing dopant compounds thereof.
Further, in one embodiment of the present invention, the catalyst is grown on the current collector by hydrothermal reaction or electrodeposition.
Further, in one embodiment of the present invention, the number of the current collectors on which the catalyst is grown is 1 to 10.
Further, in one embodiment of the present invention, the hydrophobic material may be one or a combination of PTFE, Nafion.
According to the air electrode disclosed by the embodiment of the invention, the catalyst directly grows on the current collector, the thickness of the catalytic layer is easy to change, an adhesive can be omitted, the catalyst is stably connected with the current collector, the loss of the catalyst in the working process of the metal-air battery is reduced, and the internal resistance of the air electrode is reduced.
Next, a method of manufacturing the air electrode according to the above embodiment, which is proposed according to an embodiment of the present invention, will be described with reference to the accompanying drawings.
Fig. 3 is a flow chart of a method of manufacturing an air electrode according to an embodiment of the present invention.
As shown in fig. 3, the preparation method of the air electrode includes the steps of:
in step S301, a current collector is pretreated.
The current collector can be nickel metal, nickel alloy or carbon fiber cloth, and the pretreatment method comprises the steps of soaking the current collector in 1-6mol/L hydrochloric acid solution, carrying out ultrasonic treatment for 3-20min, and finally cleaning the current collector with deionized water for 3-10 times.
In step S302, a catalyst is grown on the pretreated current collector.
The catalyst can be one or more of carbon material, metal oxide, metal nitride, metal sulfide, metal phosphide and doped compound containing defects or hetero atoms, and is grown on the current collector through hydrothermal reaction or electrodeposition.
In step S303, at least one current collector on which a catalyst is grown is hot-pressed at a first preset hot-pressing temperature and pressure to generate a catalytic conductive composite layer.
Wherein, the number of the current collectors with the catalyst is 1-10, the hot pressing temperature is 50-100 ℃, and the hot pressing pressure is 0.1-1.0 MPa.
In step S304, the catalytic conductive composite layer is soaked in the hydrophobic material solution with a preset concentration for a preset time, and the drying operation and the soaking operation are repeated for a preset number of times, and calcined in the air at a preset temperature for a preset time.
Wherein the hydrophobic material is one or the combination of PTFE and Nafion, the solution concentration is 1-10%, the soaking time is 30-120min, the calcining temperature is 150-.
In step S305, the treated catalytic conductive composite layer and the hydrophobic diffusion layer are hot-pressed at a second preset hot-pressing temperature and pressure to form a whole as a catalytic layer.
Wherein the hot pressing temperature is 50-100 ℃, and the hot pressing pressure is 0.1-1.0 MPa.
Compared with the traditional air electrode of the metal-air battery, the preparation method of the air electrode provided by the embodiment of the invention is suitable for regulating and controlling the hydrophilic and hydrophobic degrees of the catalyst layer and the contact site density of the three-phase reaction in the electrode reaction area, and is simple in preparation process and easy for batch production.
The air electrode and the method for producing the same will be further described below by way of examples.
Embodiment 1, wherein, the structure of the air electrode of embodiment 1 is shown in fig. 4, and embodiment 1 specifically includes:
s1, cutting a 15 mm-40 mm foamed nickel sheet;
s2, soaking the foamed nickel in a 3mol/L hydrochloric acid solution for ultrasonic treatment for 10 min;
s3, washing the foamed nickel with deionized water for three times and drying in air at 60 ℃ for later use;
s4, dissolving 0.25g of potassium permanganate powder in 25mL of deionized water to prepare a precursor solution;
s5, completely soaking the foamed nickel in the precursor solution, transferring the foamed nickel into a polytetrafluoroethylene liner of a 50mL hydrothermal reaction kettle, and screwing the hydrothermal reaction kettle tightly;
s6, placing the hydrothermal reaction kettle in an environment of 180 ℃ for 8 hours, and then cooling to room temperature;
s7, taking the foamed nickel growing with manganese dioxide from the hydrothermal reaction kettle, washing the foamed nickel with deionized water for 3 times, and drying the foamed nickel in air at 60 ℃ for later use;
s8, repeating the steps, and continuously hot-pressing two layers of foamed nickel with manganese dioxide at the temperature of 80 ℃ and the pressure of 0.5MPa for three times to form a catalytic conductive composite layer;
s9, completely soaking the catalytic conductive composite layer in 10% PTFE emulsion for 1min, then quickly taking out and placing in air at 60 ℃ for drying;
s10, repeating the soaking and drying steps for four catalytic conductive layers for a certain number of times according to the table 1; wherein, table 1 is a table of the number of the four soaking and drying steps;
TABLE 1
| Numbering | Number 1 | |
No. 3 | Number 4 |
| Number of |
0 time | 1 time of | 2 times (one time) | 3 times of |
| PTFE content | 0mg·cm-2 | 0.2mg·cm-2 | 0.4mg·cm-2 | 0.6mg·cm-2 |
S11, continuously hot-pressing the catalytic conductive layer and the hydrophobic diffusion layer at the temperature of 80 ℃ and the pressure of 0.5MPa for three times to form an air electrode.
s1, cutting a 15 mm-40 mm foamed nickel sheet;
s2, soaking the foamed nickel in a 3mol/L hydrochloric acid solution for ultrasonic treatment for 10 min;
s3, washing the foamed nickel with deionized water for three times and drying in air at 60 ℃ for later use;
s4, dissolving 0.25g of potassium permanganate powder in 25mL of deionized water to prepare a precursor solution;
s5, completely soaking the foamed nickel in the precursor solution, transferring the foamed nickel into a polytetrafluoroethylene liner of a 50mL hydrothermal reaction kettle, and screwing the hydrothermal reaction kettle tightly;
s6, placing the hydrothermal reaction kettle in an environment of 180 ℃ for 8 hours, and then cooling to room temperature;
s7, taking the foamed nickel growing with manganese dioxide from the hydrothermal reaction kettle, washing the foamed nickel with deionized water for 3 times, and drying the foamed nickel in air at 60 ℃ for later use;
s8, repeating the steps and carrying out continuous hot pressing on a certain number of layers of foamed nickel with manganese dioxide grown according to the table 2 at the temperature of 80 ℃ and the pressure of 0.5MPa for three times to form four catalytic conductive composite layers with different thicknesses; wherein, table 2 is a table of thicknesses of four catalytic conductive composite layers;
TABLE 2
S9, completely soaking the catalytic conductive composite layer in 10% PTFE emulsion for 1min, then quickly taking out and placing in air at 60 ℃ for drying;
s10, repeating the soaking and drying steps for the four catalytic conductive layers twice according to the table 1;
s11, continuously hot-pressing the catalytic conductive layer and the hydrophobic diffusion layer at the temperature of 80 ℃ and the pressure of 0.5MPa for three times to form an air electrode.
Further, the air electrode fabricated in example was assembled with a zinc-air battery using a 6mol/L KOH solution as an electrolyte and a 0.2mm zinc plate as an anode, and tested using an electrochemical workstation. Discharge polarization curve test conditions were linearly swept from open circuit voltage to 0.4V at a rate of 0.01V/s.
In summary, the test results of the discharge polarization curve of example 1 are shown in fig. 6, and the test results of the discharge polarization curve of example 2 are shown in fig. 7. The embodiment 1 shows that the air electrode preparation method is beneficial to adjusting the content of the hydrophobic material, the embodiment 2 shows that the air electrode preparation method is beneficial to adjusting the thickness of the catalytic conductive composite layer, and the two embodiments show that the air electrode and the air electrode preparation method are applied to a zinc-air battery and have obvious effects on improving the performance of the battery.
It should be noted that the foregoing explanation of the embodiment of the air electrode also applies to the method for manufacturing the air electrode of this embodiment, and details are not repeated here.
In addition, the embodiment of the invention provides a metal-air battery, which comprises the air electrode of the embodiment. The metal-air battery assembled by the air electrode has higher power density and longer charge-discharge cycle life.
In the description of the present specification, the terms "first", "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (8)
1. An air electrode, comprising:
a hydrophobic diffusion layer;
the catalytic conductive composite layer comprises at least one current collector on which a catalyst grows and a hydrophobic material.
2. The air electrode of claim 1, wherein the current collector comprises one or more of nickel metal, nickel alloy, and carbon fiber cloth.
3. The air electrode of claim 1, wherein the catalyst is a combination of one or more of a carbon material, a metal oxide, a metal nitride, a metal sulfide, a metal phosphide, and a defect-containing or hetero-atom-containing dopant compound thereof.
4. The air electrode of claim 1, wherein the catalyst is grown on the current collector by hydrothermal reaction or electrodeposition.
5. The air electrode according to claim 1, wherein the number of the at least one current collector is in the interval [1, 10 ].
6. The air electrode of claim 1, wherein the hydrophobic material is one or a combination of PTFE, Nafion.
7. A method of manufacturing an air electrode according to any of claims 1 to 6, comprising the steps of:
pretreating the current collector;
growing the catalyst on the pretreated current collector;
hot-pressing at least one current collector with the catalyst at a first preset hot-pressing temperature and pressure to generate the catalytic conductive composite layer;
placing the catalytic conductive composite layer in a hydrophobic material solution with a preset concentration, soaking for a preset time, repeating the drying operation and the soaking operation for a preset number of times, and calcining in air at a preset temperature for a preset time;
and hot-pressing the treated catalytic conductive composite layer and the hydrophobic diffusion layer at a second preset hot-pressing temperature and pressure to form a whole as a catalytic layer.
8. A metal-air battery comprising the air electrode according to any one of claims 1 to 6.
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| US20180212254A1 (en) * | 2017-01-25 | 2018-07-26 | Korea Advanced Institute Of Science And Technology | Catalyst electrode for oxygen evolution and method for preparing the same |
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Application publication date: 20200110 |