CN111640953A - Air electrode catalyst of aluminum-air battery and preparation method thereof - Google Patents
Air electrode catalyst of aluminum-air battery and preparation method thereof Download PDFInfo
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- CN111640953A CN111640953A CN202010539263.5A CN202010539263A CN111640953A CN 111640953 A CN111640953 A CN 111640953A CN 202010539263 A CN202010539263 A CN 202010539263A CN 111640953 A CN111640953 A CN 111640953A
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
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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
- H01M4/8882—Heat treatment, e.g. drying, baking
Abstract
The invention discloses a nano perovskite air electrode catalyst of an aluminum-air battery and a preparation method thereof. The invention belongs to the technical field of preparation of aluminum-air batteries, and aims at the perovskite catalyst with larger particle size, small specific surface area and less morphological characteristics prepared by the conventional preparation method, and the perovskite catalyst La prepared by the conventional preparation method is synthesized by a sol-gel method0.4Sr0.6Co0.7Fe0.2Nb0.1O3The catalyst has the advantages of small particle size, uniform size, large specific surface area, good repeatability, high catalytic activity, stable physical and chemical properties, cheap and easily-obtained medicines and the like, and the temperature required by material preparation is low, the time is short, the raw material cost is low, the preparation process is environment-friendly, and the industrial production is easy to realize. La0.4Sr0.6Co0.7Fe0.2Nb0.1O3Can be used as an air electrode catalyst of an aluminum-air battery. The aluminum-air battery prepared by the method has the advantages of high discharge voltage, good stability and the like. The preparation process provided by the invention is simple and easy to control, and is favorable for large-scale batch production.
Description
Technical Field
The invention belongs to the technical field of aluminum-air battery preparation, and particularly relates to an air electrode catalyst of an aluminum-air battery and a preparation method thereof.
Background
Modern society is currently in the transition from fossil fuel based economies to clean energy sources needed to reduce environmental pollution. Therefore, some renewable energy sources are being developed, such as solar energy, wind energy, and hydroelectric power. Among these new energy storage systems, metal-air batteries are receiving attention because of their advantages of high energy density, large capacity, low cost (depending on the metal anode), constant discharge voltage, etc. However, the kinetics of oxygen reduction reactions are slow, which requires additional energy (overpotential) to overcome the kinetic barriers of these reactions, and the energy efficiency of these devices is greatly reduced, thereby limiting the commercialization of these energy devices. Therefore, there is a need to develop electrocatalysts to promote such reactions, thereby reducing the additional energy required to drive these reactions in these devices.
At present, the noble metal platinum (Pt) is considered to be a better oxygen reduction reaction electrocatalyst in alkaline oxygen electrocatalysis, but the commercial application development of the noble metal is severely limited due to the defects of expensive price, single catalytic performance and the like of the noble metal. The development of non-noble metal catalysts has become a focus of metal-air batteries. To date, many types of non-noble metal catalysts, such as metal macrocycles and carbonaceous materials that have been reported, transition metal oxides in the form of perovskites, spinels, and dopants thereof. Among the various bifunctional catalysts, perovskite-based oxides are used as oxygen catalysts because of their good catalytic activity and stability in alkaline solutions. Due to the great flexibility of perovskites in composition and crystal structure, resulting in perovskite oxides having tunable electronic structures, their physicochemical properties can be widely varied, which can further tune their catalytic activity. Giving it a variety of physical and chemical properties. In addition, perovskites have great potential for catalyzing oxygen reduction reaction, oxygen evolution reaction and hydrogen evolution reaction, and are expected to become high-efficiency electrocatalysts for various energy related applications due to the advantages of easy synthesis, relatively low cost, flexible structure, high intrinsic catalytic activity and the like.
Conventional methods for synthesizing perovskite catalysts (e.g., solid phase synthesis, molten salt method, and coprecipitation method) generally can only obtain perovskite catalysts with large particle size, small specific surface area, and few morphological features, and have limited catalytic activity, limiting their large-scale practical applications (e.g., metal air batteries, electrolyzed water, solid oxide fuel cells). The synthesis of the nano perovskite is an effective way for improving the catalytic performance, which is closely related to the nano size effect, and the surface area and the catalytic active sites of the nano perovskite are increased along with the reduction of the particle size of the nano perovskite, so that the catalytic performance is improved.
Disclosure of Invention
The invention aims to provide an aluminum-air battery air electrode catalyst with low raw material price, high catalytic activity and good chemical stability aiming at the problems of the existing aluminum-air battery, wherein the aluminum-air battery air electrode catalyst has the molecular formula of La0.4Sr0.6Co0.7Fe0.2Nb0.1O3The perovskite structure particles with the average particle size of 100nm are aggregated to form a loose porous shape.
The invention also aims to provide a preparation method of the aluminum-air battery air electrode catalyst, which adopts a sol-gel method to prepare metal oxide powder with fine particles and larger specific surface area.
The object of the present invention is achieved by a method for preparing an air electrode catalyst for an aluminum-air battery, comprising the steps of:
(a) respectively weighing 0.85-0.87 g of lanthanum nitrate hexahydrate, 0.63-0.64 g of strontium nitrate, 1.00-1.02 g of cobalt nitrate hexahydrate, 0.40-0.41 g of ferric nitrate nonahydrate and 0.26-0.27 g of niobium oxalate, and adding 200ml of deionized water to form a metal salt solution, and marking as solution A;
(b) weighing 1.55-1.58 g of citric acid powder, adding the citric acid powder into the solution A, stirring until the citric acid powder is dissolved, and marking as a solution B;
(c) weighing 0.29-0.30 g of ethylenediamine tetraacetic acid, adding the ethylenediamine tetraacetic acid into the solution B, adding ammonia water to adjust the pH value of the solution to 4, and stirring for 0.5-1 hour;
(d) continuously stirring the solution obtained in the step (c) in a water bath at 80 ℃ until gel is formed, and then placing the gel in a drying oven at 90 ℃ for drying for 12h to form a gel precursor;
(e) heating the precursor to 650 ℃ at the speed of 3 ℃/min, carrying out heat preservation and calcination for 1 hour, then continuously heating to 700 ℃ at the speed of 1 ℃/min, carrying out heat preservation and calcination for 3 hours, and then naturally cooling to obtain the aluminum-air battery air electrode catalyst.
Preferably, in the step (a), 0.866g of lanthanum nitrate hexahydrate, 0.635g of strontium nitrate, 1.019g of cobalt nitrate hexahydrate, 0.404g of ferric nitrate nonahydrate and 0.269g of niobium oxalate are weighed;
1.576g of citric acid in step (b);
in step (c), ethylenediaminetetraacetic acid was 0.292 g.
The preparation method of the air electrode of the aluminum-air battery comprises the following steps: respectively weighing 0.240g of air electrode catalyst, 0.030g of acetylene black and 0.030g of vinylidene fluoride, uniformly mixing, dropwise adding 4-6 drops of N-methylpyrrolidone to mix into slurry, coating the slurry on a nickel screen, wherein the thickness of the coating catalyst layer is 1.2mm, then placing the nickel screen in a blast drying oven, and heating for 1 hour at 60 ℃ to obtain the air electrode of the aluminum-air battery.
Further defined, the conductive carbon is acetylene black and the binder is polyvinylidene fluoride (PVDF).
Further limiting, the coating process is completed by adopting a full-automatic coating machine.
Compared with the prior art, the invention has the beneficial effects that:
1. the raw materials used in the invention are all cheap and easily available products, the process is simple, and the manufacturing cost and the production period of the catalyst and the air electrode of the aluminum air battery are greatly reduced.
2. The metal oxide catalyst prepared by the invention has the advantages of fine granularity, uniform particles, large specific surface area, high catalytic activity, stable chemical property and the like.
3. The air electrode of the aluminum-air battery prepared by the invention has the advantages of higher discharge voltage, good stability, long service life and the like.
Drawings
Fig. 1 is an XRD pattern of the catalyst obtained in example 1.
FIG. 2 is an SEM photograph of the catalyst obtained in example 1.
FIG. 3 is a BET plot of the catalyst obtained in example 1.
Fig. 4 is a graph of the discharge voltage of the catalyst obtained in example 1 at different current densities in an aluminum-air battery.
FIG. 5 shows the catalyst obtained in example 1 in an aluminum-air cell at 40mA cm-2Degradation curve at current density of (a).
Detailed Description
Example 1 an air electrode catalyst for an aluminum-air battery and a method for preparing the same according to the present example were performed as follows:
(a) 0.866g of lanthanum nitrate hexahydrate, 0.635g of strontium nitrate, 1.019g of cobalt nitrate hexahydrate, 0.404g of ferric nitrate nonahydrate and 0.269g of niobium oxalate were weighed, and 200ml of deionized water was added to form a metal salt solution, which was denoted as solution A.
(b) 1.576g of citric acid was weighed into solution A and stirred until dissolved, and the mark was given as solution B.
(c) And 0.292g of ethylenediamine tetraacetic acid is weighed and added into the solution B, then ammonia water is added to adjust the pH value of the solution to 4, and the solution is stirred for 0.5 to 1 hour.
(d) And (c) continuously stirring the solution obtained in the step (c) in a water bath at 80 ℃ until gel is formed, and then placing the gel in an oven at 90 ℃ for drying for 12h to form a gel-like precursor.
(e) Heating the precursor to 650 ℃ at the speed of 3 ℃/min, carrying out heat preservation and calcination for 1 hour, then continuously heating to 700 ℃ at the speed of 1 ℃/min, carrying out heat preservation and calcination for 3 hours, and then naturally cooling to obtain the nano perovskite material La0.4Sr0.6Co0.7Fe0.2Nb0.1O3。
Figure 1 is the XRD pattern of the catalyst obtained in example 1: from figure 1 it can be seen that the XRD results confirm that a well-crystallized catalyst was obtained in this work.
FIG. 2 is an SEM photograph of the catalyst obtained in example 1, and it can be seen from FIG. 2 that the catalyst has a small and uniform particle size, an average particle size of about 100nm, and a loose and porous structure.
FIG. 3 is a BET plot of the catalyst obtained in example 1, which shows a large specific surface area. The larger the specific surface area, the stronger the adsorption capacity as the contact area between the catalyst and oxygen increases. This allows the catalyst to have more active sites and increases the rate and capacity of oxygen catalysis.
The preparation method of the air electrode of the embodiment is carried out according to the following steps:
respectively weighing 0.240g of air electrode catalyst, 0.030g of acetylene black and 0.030g of vinylidene fluoride, uniformly mixing, dropwise adding 4-6 drops of N-methylpyrrolidone to mix into slurry, adjusting the thickness of a catalyst layer to 1.2mm by using an automatic coating machine, coating the catalyst layer on a nickel screen, then placing the nickel screen in a blast drying oven, and heating for 1 hour at 60 ℃ to obtain the air electrode of the aluminum-air battery.
And assembling the air cathode and the aluminum metal anode into a single cell, and testing the discharge performance of the aluminum-air battery in 4M potassium hydroxide electrolyte.
FIG. 4 is a graph showing the discharge voltage of the catalyst obtained in example 1 at different current densities in an aluminum-air battery, and it can be seen from FIG. 4 that the catalyst is at 10mA cm-2、20mA cm-2、40mA cm-2、60mA cm-2、80mA cm-2The discharge voltage under the current density is 1.520V, 1.257V, 1.146V, 0.974V and 0.832V respectively, and the catalyst enables the aluminum-air battery to have higher discharge voltage.
FIG. 5 shows the catalyst obtained in example 2 in an aluminum-air cell at 40mA cm-2As can be seen from fig. 5, the voltage of the battery was almost constant after passing the 175-hour stability test, indicating that the catalyst provides the aluminum-air battery with excellent stability.
While the foregoing shows and describes the principles of the present invention, together with the general features and advantages thereof, the foregoing embodiments and description merely illustrate the principles of the invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is further defined in the appended claims. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. The air electrode catalyst of the aluminum-air battery is characterized in that the molecular formula of the catalyst is La0.4Sr0.6Co0.7Fe0.2Nb0.1O3The perovskite structure particles with the average particle size of 100nm are aggregated to form a loose porous shape.
2. A method for preparing the air electrode catalyst of the aluminum-air battery according to claim 1, comprising the steps of:
(a) respectively weighing 0.85-0.87 g of lanthanum nitrate hexahydrate, 0.63-0.64 g of strontium nitrate, 1.00-1.02 g of cobalt nitrate hexahydrate, 0.40-0.41 g of ferric nitrate nonahydrate and 0.26-0.27 g of niobium oxalate, and adding 200ml of deionized water to form a metal salt solution, and marking as solution A;
(b) weighing 1.55-1.58 g of citric acid powder, adding the citric acid powder into the solution A, stirring until the citric acid powder is dissolved, and marking as a solution B;
(c) weighing 0.29-0.30 g of ethylenediamine tetraacetic acid, adding the ethylenediamine tetraacetic acid into the solution B, adding ammonia water to adjust the pH value of the solution to 4, and stirring for 0.5-1 hour;
(d) continuously stirring the solution obtained in the step (c) in a water bath at 80 ℃ until gel is formed, and then placing the gel in a drying oven at 90 ℃ for drying for 12h to form a gel precursor;
(e) heating the precursor to 650 ℃ at the speed of 3 ℃/min, carrying out heat preservation and calcination for 1 hour, then continuously heating to 700 ℃ at the speed of 1 ℃/min, carrying out heat preservation and calcination for 3 hours, and then naturally cooling to obtain the aluminum-air battery air electrode catalyst.
3. The method for preparing the air electrode catalyst of the aluminum-air battery as recited in claim 1, wherein in the step (a), 0.866g of lanthanum nitrate hexahydrate, 0.635g of strontium nitrate, 1.019g of cobalt nitrate hexahydrate, 0.404g of iron nitrate nonahydrate, and 0.269g of niobium oxalate are weighed.
4. The method for preparing an air electrode catalyst for an aluminum-air battery according to claim 1, wherein the citric acid in the step (b) is 1.576 g.
5. The method of preparing an air electrode catalyst for an aluminum-air battery according to claim 1, wherein the amount of ethylenediaminetetraacetic acid in step (c) is 0.292 g.
6. Use of the aluminum-air battery air electrode catalyst of claim 1 for the preparation of an air electrode in an aluminum-air battery.
7. The use of the air electrode catalyst of the aluminum-air battery according to claim 6, wherein 0.240g of the air electrode catalyst, 0.030g of acetylene black and 0.030g of vinylidene fluoride are respectively weighed, uniformly mixed, 4-6 drops of N-methylpyrrolidone are added dropwise to mix into slurry, the slurry is coated on a nickel screen, the thickness of the coating catalyst layer is 1.2mm, and then the aluminum-air battery is placed in a blast drying oven and heated at 60 ℃ for 1 hour to obtain the air electrode of the aluminum-air battery.
8. Use of the aluminum-air battery air electrode catalyst according to claim 7, characterized in that the conductive carbon is acetylene black and the binder is polyvinylidene fluoride.
9. Use of the aluminum-air battery air electrode catalyst according to claim 7, characterized in that the coating process is done with a fully automatic coating machine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115000430A (en) * | 2022-05-08 | 2022-09-02 | 上海交通大学 | Magnesium metal air battery anode catalytic material and preparation method thereof |
| CN115074747A (en) * | 2021-03-12 | 2022-09-20 | 中国科学院物理研究所 | Quadruple perovskite oxide, preparation method and application thereof, and method for electrolyzing water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115074747A (en) * | 2021-03-12 | 2022-09-20 | 中国科学院物理研究所 | Quadruple perovskite oxide, preparation method and application thereof, and method for electrolyzing water |
| CN115074747B (en) * | 2021-03-12 | 2023-08-08 | 中国科学院物理研究所 | Quadruple perovskite oxide, preparation method and application thereof, and method for electrolyzing water |
| CN115000430A (en) * | 2022-05-08 | 2022-09-02 | 上海交通大学 | Magnesium metal air battery anode catalytic material and preparation method thereof |
| CN115000430B (en) * | 2022-05-08 | 2024-03-12 | 上海交通大学 | Magnesium metal air battery anode catalytic material and preparation method thereof |
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