CN111180720A - Aluminum air battery anode and preparation method thereof - Google Patents
Aluminum air battery anode and preparation method thereof Download PDFInfo
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- CN111180720A CN111180720A CN201911006194.5A CN201911006194A CN111180720A CN 111180720 A CN111180720 A CN 111180720A CN 201911006194 A CN201911006194 A CN 201911006194A CN 111180720 A CN111180720 A CN 111180720A
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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/46—Alloys based on magnesium or aluminium
- H01M4/463—Aluminium based
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- H—ELECTRICITY
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- 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
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Abstract
The invention relates to the technical field of aluminum-air batteries, and discloses an aluminum-air battery anode and a preparation method thereof, aiming at the problems of complex preparation process and poor corrosion resistance of the aluminum-air battery anode in the prior art, wherein the aluminum-air battery anode comprises the following components in parts by mass (100): 0.01-0.05% of Ga, 0.2-0.6% of Mn, 1-5% of Mg, 0.1-0.6% of Pb and the balance of Al. The method comprises the following steps: (1) melting aluminum; (2) adding Mn; (3) adding Ga and Pb; (4) adding Mg; (5) removing slag; (6) and (5) casting. The battery anode alloy prepared by the invention has good electrochemical performance, the addition of each alloy element reduces the anisotropy of anode material crystal grains, improves the corrosion uniformity of the alloy, has low overpotential, low self-discharge rate and higher hydrogen evolution overpotential, can eliminate the harmful influence of Fe element on the electrode, and has simple preparation process, short synthesis period and high synthesis efficiency.
Description
Technical Field
The invention relates to the technical field of aluminum-air batteries, in particular to an aluminum-air battery anode and a preparation method thereof.
Background
The battery technology is widely applied to different green energy fields at present, different batteries have unique advantages, and the aluminum-air battery has the advantages of high specific energy, rich and cheap raw materials, recyclability, environmental friendliness and the like, and has great research value. The cathode of the aluminum-air battery is aluminum alloy, which is continuously consumed and generates Al (OH) when the battery is discharged3. The aluminum has rich sources, is the metal element with the highest content in the earth crust, is convenient to process, has soft texture and can be processed into various shapes; environmental protection recyclableAnd most of discharge products of the aluminum cathode can be electrolyzed, reduced and recycled.
The industrial pure aluminum contains impurities such as iron, copper and the like, self-corrosion and hydrogen evolution corrosion of an aluminum anode are easily caused in an electrolyte (especially in a strong alkaline electrolyte), and the aluminum anode is suitable for being used as an aluminum air battery anode only when the purity of the aluminum reaches more than 99.999 percent, but the requirement on an aluminum electrolysis process is high, and the cost of the battery is increased. In addition, a dense oxide film is formed on the surface of pure aluminum, which can cause passivation of an anode and cause reduction of current density, and generally, pure aluminum or high-purity aluminum is not directly adopted for an aluminum electrode, and is usually subjected to alloying treatment, and other elements are added into an aluminum matrix, so that the self-corrosion and hydrogen evolution corrosion of the aluminum electrode are reduced.
The invention discloses an aluminum air battery anode material and a preparation method thereof, and the aluminum air battery anode material comprises the following components in percentage by mass: 0.10-0.15% of bismuth, 0.10-0.15% of lead, 0.015-0.035% of gallium and the balance of aluminum; the anode material is prepared by adopting the processing technologies of batching, smelting, rolling and heat treatment.
The method has the disadvantages of complex preparation process, long preparation process time and poor corrosion resistance of the obtained anode material.
Disclosure of Invention
The invention aims to overcome the problems of complex preparation process and poor corrosion resistance of the aluminum air battery anode in the prior art, and provides the aluminum air battery anode and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an aluminum air battery anode comprising, by 100 parts by mass: 0.01-0.05% of Ga, 0.2-0.6% of Mn, 1-5% of Mg, 0.1-0.6% of Pb and the balance of Al.
The anisotropy of crystal grains is reduced by the alloy element Ga in the alloy dissolving process, the corrosion uniformity of the alloy is improved, eutectic can be formed by the Ga and the eutectic element Pb, and the dissolving activity of the aluminum alloy material is improved; the alloy element Mg also has the function of changing the microstructure of the aluminum alloy anode material, so that the uniformity of alloy corrosion is improved; the alloy element Mn can reduce the corrosion of the aluminum alloy anode under the load condition, and can form an intermetallic compound with the impurity Fe element, eliminate the harmful effect of the Fe element on the electrode, and prepare the aluminum air battery anode with excellent electrical property.
A preparation method of the aluminum-air battery anode comprises the following preparation steps:
(1) melting aluminum: heating the container, spraying a release agent on the container, adding Al into the container, heating to melt, heating and preserving heat to obtain aluminum liquid;
(2) and adding Mn: adding an alloy element Mn into the high-temperature aluminum liquid, heating and preserving heat to obtain a molten metal A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the molten metal A, and stirring to obtain molten metal B;
(4) and adding Mg: adding an alloy element Mg into the molten metal B, and stirring to obtain molten metal C;
(5) and deslagging: heating, pressing a deslagging agent into a movable fixing piece at the bottom of the container by using the fixing piece, horizontally rotating, moving, standing, and then starting slagging off;
(6) and casting: heating the mold, spraying a release agent on the surface in contact with the molten metal C, and casting into ingots to obtain the finished product.
Preferably, the Mg in the step (4) is wrapped by aluminum foil and pressed into the bottom of the container by a fixing member.
The melting point of Mg is low, and the aluminum foil is wrapped to prevent the Mg with too high temperature from being burnt when being close to aluminum molten metal.
Preferably, the container is a graphite crucible, and the fixing member is a bell jar.
Preferably, before spraying the release agent in the step (1), the container is heated to 200-210 ℃, heated to 770-790 ℃ and kept for 1-1.5 h.
Preferably, the high temperature of the aluminum liquid in the step (2) is 730-740 ℃, the temperature is raised to 750-780 ℃, and the temperature is kept for 10-15 min.
The melting point of Mn is high, so that Mn can be molten in molten metal aluminum, Mn metal elements are uniformly distributed, and the performance of the anode material is optimal.
Preferably, the temperature of the molten metal A in the step (3) and the temperature of the molten metal B in the step (4) are both 730-740 ℃, and the stirring time is 10-15 min.
Preferably, the temperature of the molten metal C in the step (5) is 760-820 ℃, and the standing time is 15-20 min.
Preferably, the casting process in the step (6) is one-time continuous casting molding.
The continuous casting ensures the integrity and uniformity of the aluminum-air battery anode, avoids the attribute defects caused by the discontinuity and stress concentration of the anode material, and improves the mechanical property of the anode material.
Preferably, the heating temperature of the mold in the step (6) is 200-210 ℃.
The grinding tool is preheated in advance, so that the phenomenon that the forming quality of the aluminum-air battery anode is influenced due to stress concentration of the metal silver in the cooling forming process is avoided.
Therefore, the invention has the following beneficial effects:
(1) the prepared battery anode alloy has good electrochemical performance, low overpotential, low self-discharge rate, higher hydrogen evolution overpotential and good corrosion resistance;
(2) the anisotropy of crystal grains is reduced by the alloy element Ga in the alloy dissolving process, the corrosion uniformity of the alloy is improved, eutectic can be formed by the Ga and the eutectic element Pb, and the dissolving activity of the aluminum alloy material is improved;
(3) the alloy element Mg also has the function of changing the microstructure of the aluminum alloy anode material, so that the uniformity of alloy corrosion is improved;
(4) the alloy element Mn can reduce the self-corrosion of the aluminum alloy anode under the load condition, and can form an intermetallic compound with the impurity Fe element, thereby eliminating the harmful effect of the Fe element on the electrode;
(5) the preparation process is simple, the synthesis period is short, the controllability of the process steps is good, the synthesis cost is low, and the synthesis efficiency is high.
Detailed Description
The invention is further described with reference to specific embodiments.
Example 1
An aluminum air battery anode comprising, by 100 parts by mass: 0.03% Ga, 0.45% Mn, 2.5% Mg, 0.3% Pb, and the balance Al.
A preparation method of an aluminum-air battery anode, wherein aluminum alloy is smelted by adopting a crucible, and smelting and heating processes are carried out in a crucible smelting furnace, comprises the following preparation steps:
(1) heating the crucible to 205 ℃, spraying a release agent on the crucible, adding pure aluminum, heating to 780 ℃ for melting, and preserving heat for 1.3 h;
(2) and adding Mn: adding an alloy element Mn into 735 ℃ high-temperature aluminum liquid, heating to 765 ℃, and then preserving heat for 13min to obtain metal liquid A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the metal liquid A at 735 ℃, and stirring for 13min to obtain metal liquid B;
(4) and adding Mg: adding an alloy element Mg into the metal liquid B at 735 ℃, stirring for 8min, wrapping the Mg by using an aluminum foil, and pressing the Mg into the bottom of the crucible by using a bell jar to obtain metal liquid C;
(5) heating to 790 deg.C, pressing slag-removing agent into the pan bottom by bell jar, horizontally rotating, standing for 18min, and removing slag;
(6) heating the mould to 205 ℃, spraying a release agent on the surface contacting with the molten metal C, and continuously casting into ingots at one time.
Example 2
The difference from example 1 is that an aluminum air battery anode comprises the following components by 100 mass percent: 0.02% Ga, 0.3% Mn, 2% Mg, 0.2% Pb, and the balance Al.
A preparation method of an aluminum-air battery anode, wherein aluminum alloy is smelted by adopting a crucible, and smelting and heating processes are carried out in a crucible smelting furnace, comprises the following preparation steps:
(1) heating the crucible to 202 ℃, spraying a release agent on the crucible, adding pure aluminum, heating to 775 ℃, melting, and keeping the temperature for 1.2 h;
(2) and adding Mn: adding an alloy element Mn into the high-temperature aluminum liquid at 733 ℃, heating to 755 ℃, and then preserving the heat for 11min to obtain a molten metal A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the metal liquid A at 732 ℃, and stirring for 11min to obtain metal liquid B;
(4) and adding Mg: adding an alloy element Mg into the metal liquid B at 733 ℃, stirring for 6min, wrapping the Mg with aluminum foil, and pressing the Mg into the bottom of the crucible by using a bell jar to obtain metal liquid C;
(5) heating to 770 ℃, pressing a deslagging agent into the pot bottom by using a bell jar to move the bell jar, horizontally rotating, standing for 16min, and deslagging;
(6) the mould is heated to 202 ℃, and the surface of the mould contacted with the molten metal C is sprayed with a release agent, and the mould is continuously cast into ingots at one time.
Example 3
The difference from example 1 is that an aluminum air battery anode comprises the following components by 100 mass percent: 0.04% Ga, 0.5% Mn, 4% Mg, 0.5% Pb, and the balance Al.
A preparation method of an aluminum-air battery anode, wherein aluminum alloy is smelted by adopting a crucible, and smelting and heating processes are carried out in a crucible smelting furnace, comprises the following preparation steps:
(1) heating the crucible to 208 ℃, spraying a release agent on the crucible, adding pure aluminum, heating to 785 ℃ for melting, and keeping the temperature for 1.4 h;
(2) and adding Mn: adding an alloy element Mn into 738 ℃ high-temperature aluminum liquid, heating to 775 ℃, and then preserving heat for 14min to obtain molten metal A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the molten metal A at 738 ℃, and stirring for 14min to obtain molten metal B;
(4) and adding Mg: adding an alloy element Mg into the molten metal B at 738 ℃, stirring for 9min, wrapping the Mg by using an aluminum foil, and pressing the Mg into the bottom of the crucible by using a bell jar to obtain molten metal C;
(5) heating to 810 deg.C, pressing slag-removing agent into the pot bottom by using bell jar, moving the bell jar horizontally, standing for 19min, and removing slag;
(6) heating the mould to 208 ℃, spraying a release agent on the contact surface of the mould and the molten metal C, and continuously casting into ingots at one time.
Example 4
The difference from example 1 is that an aluminum air battery anode comprises the following components by 100 mass percent: 0.01% Ga, 0.2% Mn, 1% Mg, 0.1% Pb, and the balance Al.
A preparation method of an aluminum-air battery anode, wherein aluminum alloy is smelted by adopting a crucible, and smelting and heating processes are carried out in a crucible smelting furnace, comprises the following preparation steps:
(1) heating the crucible to 200 ℃, spraying a release agent on the crucible, adding pure aluminum, heating to 770 ℃ for melting, and keeping the temperature for 1 h;
(2) and adding Mn: adding an alloy element Mn into 730 ℃ high-temperature aluminum liquid, heating to 750 ℃, and then preserving heat for 10min to obtain a metal liquid A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the metal liquid A at 730 ℃, and stirring for 10min to obtain metal liquid B;
(4) and adding Mg: adding an alloy element Mg into the metal liquid B at 730 ℃, and stirring for 5min to obtain metal liquid C;
(5) heating to 760 deg.C, pressing slag-removing agent into the pot bottom by using bell jar, moving the bell jar horizontally, standing for 15min, and removing slag;
(6) heating the mould to 200 ℃, spraying a release agent on the surface contacting with the molten metal C, and continuously casting into ingots at one time.
Example 5
The difference from example 1 is that an aluminum air battery anode comprises the following components by 100 mass percent: 0.05% Ga, 0.6% Mn, 5% Mg, 0.6% Pb, and the balance Al.
A preparation method of an aluminum-air battery anode, wherein aluminum alloy is smelted by adopting a crucible, and smelting and heating processes are carried out in a crucible smelting furnace, comprises the following preparation steps:
(1) heating the crucible to 210 ℃, spraying a release agent on the crucible, adding pure aluminum, heating to 790 ℃ for melting, and keeping the temperature for 1.5 hours;
(2) and adding Mn: adding an alloy element Mn into 740 ℃ high-temperature aluminum liquid, heating to 780 ℃, and then preserving heat for 15min to obtain a metal liquid A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the metal liquid A at 740 ℃, and stirring for 15min to obtain metal liquid B;
(4) and adding Mg: adding an alloy element Mg into the metal liquid B at 740 ℃, stirring for 10min, wrapping the Mg by using an aluminum foil, and pressing the Mg into the bottom of the crucible by using a bell jar to obtain metal liquid C;
(5) heating to 820 deg.C, pressing slag-removing agent into the pot bottom by using bell jar, moving bell jar, horizontally rotating, standing for 20min, and removing slag;
(6) heating the mould to 210 ℃, spraying a release agent on the surface contacting with the molten metal C, and continuously casting into ingots at one time.
Comparative example 1
The difference from example 1 is that the Ga content is 0.005%.
Comparative example 2
The difference from example 1 is that the mass content of Mg is 0.
Comparative example 3
The difference from example 1 is that the order of Mg, Mn, Ga, Pb addition is adjusted to precede step (2) in step (4).
The resulting data are shown in table 1:
TABLE 1 electrolyte temperature 50 ℃ and current density 200mA cm-2Electrode potential of the conditioned material
And (4) conclusion: in the embodiments 1-5, the degree of negative displacement of the electrode potential of the anode material prepared within the parameter range of the invention is far larger than that in the comparative example, the more negative the anode electrode potential is, the better the performance is, the degree of negative displacement of the electrode potential is large, the corrosion of the electrode surface is uniform, the overpotential of hydrogen evolution is high, and the utilization rate of the aluminum alloy anode is high.
The negative electrode potential shift degrees in the comparative examples 1-3 are all reduced, and for the comparative example 1, the anode alloy material has larger polarization, the surface is easy to passivate, the electrode reaction is hindered, and the anode utilization rate is reduced; for the comparative example 2, the anode alloy material has poor corrosion resistance, uneven surface corrosion and a block falling phenomenon, so that the utilization rate of the anode is greatly reduced; for comparative example 3, because magnesium is added too early and heated for too long time, burning loss is easy to occur, so that the mass content is reduced, the surface corrosion of the anode alloy material is still not uniform, the phenomenon of block falling occurs, and the utilization rate of the anode is not high.
It can be seen from the data of examples 1-5 and comparative examples 1-3 that the above requirements can be satisfied in all aspects only by the solution within the scope of the claims of the present invention, resulting in an optimized solution and an aluminum air cell anode with optimal performance. The change of the mixture ratio, the replacement/addition/subtraction of raw materials or the change of the feeding sequence can bring corresponding negative effects.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. An aluminum-air battery anode is characterized by comprising the following components by 100 mass percent: 0.01-0.05% of Ga, 0.2-0.6% of Mn, 1-5% of Mg, 0.1-0.6% of Pb and the balance of Al.
2. A method for preparing an aluminum-air battery anode according to claim 1, comprising the steps of:
(1) melting aluminum: heating the container, spraying a release agent on the container, adding Al into the container, heating to melt, heating and preserving heat to obtain aluminum liquid;
(2) and adding Mn: adding an alloy element Mn into the high-temperature aluminum liquid, heating and preserving heat to obtain a molten metal A;
(3) and adding Ga and Pb: adding alloy elements Ga and Pb into the molten metal A, and stirring to obtain molten metal B;
(4) and adding Mg: adding an alloy element Mg into the molten metal B, and stirring to obtain molten metal C;
(5) and deslagging: heating, pressing a deslagging agent into a movable fixing piece at the bottom of the container by using the fixing piece, horizontally rotating, moving, standing, and then starting slagging off;
(6) and casting: heating the mold, spraying a release agent on the surface in contact with the molten metal C, and casting into ingots to obtain the finished product.
3. The method for preparing an anode of an aluminum-air battery according to claim 2, wherein the Mg in the step (4) is wrapped by aluminum foil and pressed into the bottom of the container by a fixing member.
4. The method for preparing an aluminum-air battery anode according to claim 2 or 3, wherein the container is a graphite crucible, and the fixing member is a bell jar.
5. The method for preparing the anode of the aluminum-air battery according to claim 2, wherein the container is heated to 200-210 ℃ before spraying the release agent in the step (1), the temperature is raised to 770-790 ℃, and the temperature is kept for 1-1.5 hours.
6. The method for preparing the anode of the aluminum-air battery as claimed in claim 2, wherein the high temperature of the aluminum liquid in the step (2) is 730-740 ℃, the temperature is raised to 750-780 ℃ and the temperature is kept for 10-15 min.
7. The method for preparing the anode of the aluminum-air battery according to claim 2, wherein the temperature of the molten metal A in the step (3) and the temperature of the molten metal B in the step (4) are both 730-740 ℃, and the stirring time is 10-15 min.
8. The method for preparing an anode of an aluminum-air battery according to claim 2, wherein the temperature of the molten metal C in the step (5) is 760 to 820 ℃ and the standing time is 15 to 20 min.
9. The method for preparing the anode of the aluminum-air battery according to claim 2, wherein the casting process in the step (6) is one-time continuous casting molding.
10. The method for preparing an aluminum-air battery anode according to claim 2, wherein the heating temperature of the mold in the step (6) is 200-210 ℃.
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| CN111668454A (en) * | 2020-05-27 | 2020-09-15 | 超威电源集团有限公司 | Aluminum electrode structure of aluminum-air battery |
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