CN106611858B - carbon-free air electrode and preparation method thereof - Google Patents
carbon-free air electrode and preparation method thereof Download PDFInfo
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- CN106611858B CN106611858B CN201611184300.5A CN201611184300A CN106611858B CN 106611858 B CN106611858 B CN 106611858B CN 201611184300 A CN201611184300 A CN 201611184300A CN 106611858 B CN106611858 B CN 106611858B
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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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- 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
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
- H01M4/662—Alloys
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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
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
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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
- H01M4/9041—Metals or alloys
-
- 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
- H01M4/921—Alloys or mixtures with metallic elements
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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
- Y02E60/10—Energy storage using batteries
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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
Abstract
The invention discloses a carbon-free air electrode and a preparation method thereof. Wherein, this carbon-free air electrode includes: a foam metal layer; a catalytic layer covering at least a portion of a surface of the metal foam; and the waterproof layer covers the catalytic layer and the surface of the foam metal, and is provided with a ventilation pore passage. The carbon-free air electrode avoids the problem of carbon in the catalyst layer of the existing air electrode, solves the problem of carbonization of the air electrode, prolongs the service life and improves the discharge effect.
Description
Technical Field
The present invention relates to the field of metal fuel cells, and in particular, to carbon-free air electrodes, and methods of making carbon-free air electrodes.
background
The existing air electrode preparation process is to press a catalytic membrane and a waterproof membrane together with a conductive current collector into an air electrode after the catalytic membrane and the waterproof membrane are pressed separately, the catalyst preparation, the catalytic membrane and the waterproof membrane pressing process are complicated, the yield is low, and the consistency of the prepared air electrode is poor; the use of the conductive carbon causes serious carbonization problem in the use process of the air electrode, and influences the service life of the air electrode.
Thus, the existing air electrode is yet to be improved.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, an object of the present invention is to provide a carbon-free air electrode which solves the carbonization problem and has a long service life.
According to one aspect of the present invention, a carbon-free air electrode is provided. According to an embodiment of the present invention, the carbon-free air electrode includes: a foam metal layer; a catalytic layer covering at least a portion of the surface of the metal foam layer; and the waterproof layer covers the surfaces of the catalyst layer and the foam metal layer and is provided with a ventilation pore passage.
According to the carbon-free air electrode disclosed by the embodiment of the invention, the problem of carbon contained in a catalyst layer of the conventional air electrode is avoided, the problem of carbonization of the air electrode is solved, the service life is prolonged, and the discharge effect is improved; the catalyst layer is tightly combined with the current collector, so that the polarization of the air electrode is reduced.
in addition, the carbon-free air electrode according to the above embodiment of the present invention may also have the following additional technical features:
according to an embodiment of the invention, the catalytic layer is composed of nickel cobaltate nanoparticles.
According to an embodiment of the present invention, the metal foam layer is composed of at least one selected from the group consisting of copper, nickel, nichrome, zinc-copper alloy, nickel-chromium-tungsten alloy, and nickel-iron alloy.
according to the embodiment of the invention, the mass ratio of the catalytic layer to the foam metal layer is 0.1-10: 100.
According to another aspect of the present invention, there is provided a method of manufacturing the aforementioned air electrode. According to an embodiment of the invention, the method comprises: forming a catalytic layer on at least part of the surface of the foam metal; carrying out pressing treatment on the foam metal with the catalytic layer formed on the surface and the waterproof breathable film, and forming a waterproof layer on the catalytic layer and the surface of the foam metal so as to obtain an air electrode intermediate; and roasting the air electrode intermediate to obtain the air electrode.
According to the method provided by the embodiment of the invention, the prepared air electrode does not contain carbon, so that the problem of carbon contained in a catalyst layer of the conventional air electrode is avoided, the problem of carbonization of the air electrode is solved, the service life is prolonged, and the discharge effect is improved.
In addition, the method for preparing the air electrode according to the above embodiment of the present invention may further have the following additional technical features:
According to the embodiment of the invention, the catalytic layer is formed on at least part of the surface of the foam metal by using a hydrothermal synthesis method.
According to an embodiment of the present invention, the step of forming the catalytic layer on at least a part of the surface of the metal foam comprises:
Preparing a hydrothermal reaction solution; cleaning the foam metal to obtain cleaned foam metal; and placing the hydrothermal reaction liquid and the cleaned foam metal in a hydrothermal reaction kettle for hydrothermal reaction so as to form the catalytic layer on at least part of the surface of the foam metal.
According to the embodiment of the invention, the hydrothermal reaction liquid contains cobalt nitrate, nickel nitrate, urea, ethanol and a dispersing agent.
According to the embodiment of the invention, the concentration of the cobalt nitrate is 5-20g/L, and the concentration of the nickel nitrate is 30-60 g/L. The concentration of the urea is 5-20g/L, the concentration of the ethanol is 5-10g/L, and the concentration of the dispersing agent is 1-10 g/L.
according to the embodiment of the invention, the reaction temperature of the hydrothermal reaction is 90-300 ℃, and the reaction time is 2-24 hours.
according to the embodiment of the invention, the pressure of the pressing treatment is 10-20MPa, and the dwell time is 0.5-5 minutes.
According to the embodiment of the invention, the temperature of the roasting treatment is 200-350 ℃, and the time is 1-4 hours.
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 above 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 shows a schematic structural diagram of a carbon-free air electrode according to one embodiment of the present invention;
Fig. 2 shows a schematic flow diagram of a method of preparing an air electrode according to an embodiment 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 accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are for convenience of description of the present invention only and do not require that the present invention must be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
it should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Further, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
according to one aspect of the present invention, a carbon-free air electrode is provided. Referring to fig. 1, the carbon-free air electrode is explained according to an embodiment of the present invention. The carbon-free air electrode includes: foam metal layer 2, catalysis layer 3 and waterproof layer 1. The following explains the components of the carbon-free air electrode one by one, specifically as follows:
Foam metal layer 2: according to an embodiment of the invention, the metal foam layer acts as a current collector to conduct the current. The foam metal has the advantages of small density, large specific surface area and good conductivity, so that the performance of the current collector is better.
According to an embodiment of the present invention, the metal foam layer 2 is composed of at least one selected from the group consisting of copper, nickel, nichrome, zinc-copper alloy, nickel-chromium-tungsten alloy, and nickel-iron alloy. The foam metal with large specific surface area can provide enough attachment surface for the silver particle catalyst to ensure that the silver particles can be uniformly and lowly deposited on the surface of the foam metal to obtain better catalytic activity, and can transmit current generated by discharge.
Catalytic layer 3: according to the embodiment of the invention, the catalytic layer 3 covers at least part of the surface of the foam metal layer 2, and the chemical polarization of the air electrode oxidation reduction is reduced by using the catalytic layer.
According to the embodiment of the invention, the mass ratio of the catalytic layer 3 to the foam metal layer 2 is 0.1-10: 100. therefore, the catalytic layer is uniformly distributed on the surface of the foam metal, and the current generated by the catalytic reaction is conducted through the foam metal.
According to an embodiment of the invention, the catalytic layer is composed of nickel cobaltate nanoparticles. Therefore, the catalytic particles are uniformly distributed, the specific surface area is large, the catalytic activity is good, the combination with the foam metal is tight, the electronic conduction speed is high, and the corrosion resistance is strong.
The inventors found that the smaller the particle size of the nickel cobaltate nanoparticles, the larger the specific surface area, and the better the catalytic activity. However, if the particle size of the nickel cobaltate nanoparticles is too small, the preparation process is difficult and the cost is high, and when the particle size of the nickel cobaltate nanoparticles is 100-1000nm, the preparation process is relatively simple, the specific surface area is large, the catalytic activity is good, the conductivity of the air electrode is large, and the economic benefit is high.
Waterproof layer 1: according to the embodiment of the invention, the waterproof layer 1 covers the surfaces of the catalyst layer 2 and the foam metal layer 2, and the waterproof layer 1 is provided with the air-permeable pore passages 4, so that air enters the electrolyte through the air-permeable pore passages 4 and the electrolyte in the battery is prevented from leaking out.
According to some embodiments of the invention, the diameter of the gas-permeable channels 4 is between 5 and 30 nm. Therefore, air can enter the electrolyte from the pore channel, and water with larger particle size cannot leak out through the air-permeable pore channel.
According to another aspect of the present invention, there is provided a method of manufacturing the aforementioned air electrode. Referring to fig. 2, a method of manufacturing the aforementioned air electrode, according to an embodiment of the present invention, is explained, the method including:
S100 Forming the catalyst layer
According to an embodiment of the invention, a catalytic layer is formed on at least part of the surface of the metal foam. The catalyst layer is directly formed on the surface of the foam metal through a one-step method without independently pressing the catalyst layer and then coating the catalyst layer on the surface of the foam metal, and the method is simple in step and easy for industrial production.
According to an embodiment of the present invention, a catalytic layer is formed on at least a portion of the surface of the metal foam using hydrothermal synthesis. Therefore, the catalyst directly grows on the matrix of the foam metal by adopting a hydrothermal synthesis method, and the catalyst layer does not need to be pressed separately and then coated on the surface of the foam metal, so that the method has simple steps, is easy for industrial production, has good product consistency, and has fine granularity, large specific surface area and high catalytic activity of the catalyst particles formed on the surface.
according to an embodiment of the present invention, the step of forming a catalytic layer on at least a part of the surface of the metal foam comprises: preparing a hydrothermal reaction solution; cleaning the foam metal to remove dirt and grease on the surface of the foam metal to obtain the cleaned foam metal; and then placing the hydrothermal reaction liquid and the cleaned foam metal into a hydrothermal reaction kettle for hydrothermal reaction to form a catalytic layer on at least part of the surface of the foam metal. Therefore, the catalyst can be directly grown on the foam metal substrate by one step by using a hydrothermal synthesis method, the steps are simple, the industrial production is easy, the product consistency is good, and the catalyst particles formed on the surface have fine granularity, large specific surface area and high catalytic activity.
according to the embodiment of the invention, the hydrothermal reaction solution contains cobalt nitrate, nickel nitrate, urea, ethanol and a dispersing agent. Therefore, the hydrothermal reaction liquid is used for carrying out hydrothermal reaction, a nickel cobaltate catalyst layer can be formed on the surface of the foam metal, the hydrothermal reaction liquid is a cyanide-free hydrothermal reaction liquid, the hydrothermal reaction liquid is safe and pollution-free, the cost is low, the obtained catalyst layer is tightly combined with the matrix, the compactness is good, and the catalytic activity is high.
According to some embodiments of the invention, the hydrothermal reaction solution has a cobalt nitrate concentration of 5-20g/L, a nickel nitrate concentration of 30-60g/L, a urea concentration of 5-20g/L, an ethanol concentration of 5-10g/L, and a dispersant concentration of 1-10 g/L. Therefore, the catalyst layer is uniform in thickness, and the formed nickel cobaltate nanoparticles are small in particle size, large in specific surface area, good in compactness and high in catalytic activity.
According to the embodiment of the invention, the reaction temperature of the hydrothermal reaction is 90-300 ℃, and the reaction time is 2-24 hours. Therefore, the catalyst produced by the reaction has complete shape growth and good crystallization form.
s200 roasting treatment
According to the embodiment of the present invention, the metal foam having the catalyst layer formed on the surface thereof is subjected to the baking treatment, whereby the catalyst layer can be tightly bonded to the metal foam and is less likely to fall off.
According to the embodiment of the invention, the temperature of the roasting treatment is 200-350 ℃, and the time is 1-4 hours. Therefore, the catalytic layer has good curing effect.
S300 forming an air electrode
According to the embodiment of the invention, the electrode intermediate and the waterproof breathable film are subjected to pressing treatment, and a waterproof layer is formed on the catalyst layer and the surface of the foam metal, so that the air electrode is obtained.
according to the embodiment of the invention, the pressure of the pressing treatment is 10-20MPa, and the dwell time is 0.5-5 min. From this, waterproof ventilated membrane is laminated on the surface of foam metal closely, and the waterproof ventilative layer on air electrode surface can effectively prevent the electrolyte seepage in the battery and can allow the air to pass through simultaneously.
The present invention is described below with reference to specific examples, which are intended to be illustrative only and are not to be construed as limiting the invention.
Example 1
The method for preparing the air electrode comprises the following specific steps:
(1) Preparing a hydrothermal reaction solution with the following components: 15g/L of cobalt nitrate, 40g/L of nickel nitrate, 10g/L of urea, 8g/L of ethanol and 5g/L of dispersing agent.
(2) And (3) removing oil from the foam metal by using alcohol, and then ultrasonically cleaning the foam metal to obtain clean foam metal.
(3) Adding clean foam metal into a hydrothermal reaction kettle, and then soaking the clean foam metal into hydrothermal reaction liquid, wherein the upper part of the foam metal is exposed out of the liquid surface.
(4) and sealing and heating the hydrothermal reaction kettle, and carrying out hydrothermal reaction at the reaction temperature of 200 ℃ for 5 hours.
(5) After the reaction is finished, cooling the reaction kettle to room temperature, opening the reaction kettle, taking out the foam metal, washing the reaction kettle with clear water, and then putting the reaction kettle into a furnace for roasting at the roasting temperature of 200-350 ℃ for 1-4 h.
(6) And taking out the roasted foam metal, pressing the foam metal with the waterproof breathable film under the pressure of 10-20MPa, and maintaining the pressure for 0.5-5min to obtain the air electrode.
(7) And (3) performing a discharge test on the air electrode, wherein the discharge current density reaches 300mA/cm2, and the service life reaches more than 3000 h.
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 do not necessarily 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.
while embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (8)
1. A carbon-free air electrode, comprising:
A foam metal layer;
A catalytic layer covering at least a portion of the surface of the metal foam layer; and
A waterproof layer covering the catalytic layer and the surface of the foam metal layer and having a ventilation pore passage,
The diameter of the air-permeable pore passage is 5-30nm, the catalytic layer is composed of nickel cobaltate nanoparticles, the particle size of the nickel cobaltate nanoparticles is 100-1000nm, and the mass ratio of the catalytic layer to the foamed metal layer is 0.1-10: 100.
2. The air electrode of claim 1, wherein the foam metal layer is composed of at least one selected from the group consisting of copper, nickel, nichrome, zinc-copper alloy, nickel-copper alloy, nichrome-tungsten alloy, and nickel-iron alloy.
3. A method of producing the air electrode of claim 1 or 2, comprising:
Forming a catalytic layer on at least part of the surface of the foam metal;
Roasting the foam metal with the catalytic layer formed on the surface so as to obtain an electrode intermediate; and
And carrying out pressing treatment on the electrode intermediate and the waterproof breathable film to form a waterproof layer on the catalyst layer and the surface of the foam metal so as to obtain the air electrode.
4. The method of claim 3, wherein the catalytic layer is formed on at least a portion of the surface of the metal foam using hydrothermal synthesis.
5. The method of claim 4, wherein the step of forming the catalytic layer on at least a portion of the surface of the metal foam comprises:
Preparing a hydrothermal reaction solution;
cleaning the foam metal to obtain cleaned foam metal; and
Placing the hydrothermal reaction liquid and the cleaned foam metal in a hydrothermal reaction kettle for hydrothermal reaction so as to form the catalytic layer on at least part of the surface of the foam metal,
Optionally, the hydrothermal reaction liquid contains cobalt nitrate, nickel nitrate, urea, ethanol and a dispersing agent,
optionally, the concentration of the cobalt nitrate is 5-20g/L, the concentration of the nickel nitrate is 30-60g/L, the concentration of the urea is 5-20g/L, the concentration of the ethanol is 5-10g/L, and the concentration of the dispersing agent is 1-10 g/L.
6. The method according to claim 5, wherein the hydrothermal reaction is carried out at a reaction temperature of 90 to 300 ℃ for 2 to 24 hours.
7. the method according to claim 3, wherein the pressure of the press-bonding process is 10 to 20MPa, and the dwell time is 0.5 to 5 minutes.
8. The method as claimed in claim 3, wherein the temperature of the roasting treatment is 200-350 ℃ and the time is 1-4 hours.
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| CN108736019A (en) * | 2018-04-10 | 2018-11-02 | 云南铝业股份有限公司 | Metal fuel battery air electrode and preparation method thereof |
| CN108598494B (en) * | 2018-06-21 | 2020-09-22 | 西安科技大学 | Fuel cell anode and fuel cell using same |
| JP7112268B2 (en) * | 2018-07-03 | 2022-08-03 | シャープ株式会社 | Method for manufacturing air electrode and method for manufacturing metal-air battery |
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Effective date of registration: 20190507 Address after: 650000 Yunnan Province Kunming Yangzonghai Scenic Spot Yunnan Aluminum Co., Ltd. Applicant after: Yunnan Chuangneng Feiyuan Metal Fuel Cell Co., Ltd. Address before: 650502 Qidian Township, Chenggong County, Kunming City, Yunnan Province Applicant before: Yunnan Aluminium Co., Ltd. |
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