CN112921201B - Ceramic particle composite anode material of aluminum-air battery and preparation method thereof - Google Patents

Ceramic particle composite anode material of aluminum-air battery and preparation method thereof Download PDF

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CN112921201B
CN112921201B CN202110087515.XA CN202110087515A CN112921201B CN 112921201 B CN112921201 B CN 112921201B CN 202110087515 A CN202110087515 A CN 202110087515A CN 112921201 B CN112921201 B CN 112921201B
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aluminum
particle composite
air battery
anode material
preparation
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CN112921201A (en
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胡正飞
俞佳晟
莫凡
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Tongji University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/36—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
    • 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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  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Composite Materials (AREA)
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Abstract

The invention relates to an aluminum-air battery ceramic particle composite anode material and a preparation method thereof, belonging to the field of metal materials. The preparation method provided by the invention comprises the following steps: preheating ceramic particles, mixing the ceramic particles with heated and melted pure aluminum or aluminum alloy, obtaining a particle composite anode material with uniformly dispersed particles by adopting a common aluminum melting furnace and mechanical stirring or vacuum semi-solid stirring technology, and directly cutting the cast particle composite material or further processing the particle composite material by pressure to prepare the aluminum-air battery composite anode. The preparation method provided by the invention is simple and low in cost, and the obtained composite anode material has good electrochemical activity in alkaline electrolyte, low self-corrosion rate and high utilization rate of the battery anode, so that the preparation method provided by the invention is suitable for large-scale production and processing.

Description

Ceramic particle composite anode material of aluminum-air battery and preparation method thereof
Technical Field
The invention relates to the field of metal materials, in particular to an aluminum-air battery ceramic particle composite anode material and a preparation method thereof.
Background
The aluminum-air battery has the characteristics of high energy density, low price of electrode materials, simple and convenient use, environmental friendliness and the like. And thus has great commercial potential in applications such as electric vehicles and portable power supplies. However, the aluminum-air battery also has the following problems: the surface of the aluminum is easy to generate a passive film, so that the reaction activity of the aluminum in the electrolyte is reduced, the potential of the aluminum is shifted positively, and the anode polarization is caused and the anode electrochemistry is reduced; in addition, in alkaline solutions, strong hydrogen evolution reactions occur between aluminum and the alkaline solution, and this self-corrosion leads to a considerable reduction in the service life of aluminum and in the utilization of the anode.
In order to solve the problems, the currently adopted aluminum anode material is a high-purity aluminum material, the high-purity aluminum reduces the adverse effect of impurity elements on the performance of the anode, the commercialized aluminum anode material is further alloyed, elements such as Bi, Sn, Mg, Ga, In and the like are added into an ultrapure aluminum matrix to play a role In activating the anode, the hydrogen evolution overpotential of the whole aluminum alloy is improved, and the self-corrosion is inhibited, however, the ultrapure aluminum is expensive compared with the common industrial pure aluminum, and even if the improvement of the electrochemical performance of the anode by alloying is limited, the commercial demand of the aluminum-air battery is limited by the high-cost aluminum anode. Therefore, it is necessary to introduce some new methods to reduce the cost of the anode and improve the performance of the aluminum anode.
Disclosure of Invention
The present invention is made to solve the above problems, and an object of the present invention is to provide a ceramic particle composite anode material for an aluminum air battery and a method for preparing the same.
The invention provides a preparation method of a ceramic particle composite anode material of an aluminum-air battery, which is characterized by comprising the following steps of: step 1, cleaning, drying and preheating ceramic particles to obtain preheated ceramic particles; step 2, heating and melting pure aluminum or aluminum alloy, stirring and casting the pure aluminum or aluminum alloy and preheated ceramic particles in a vacuum environment to obtain a particle composite material; and step 3, cutting the particle composite material to obtain the ceramic particle composite anode material of the aluminum-air battery.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein the aluminum alloy is any one of magnesium aluminum alloy, calcium aluminum alloy and tin aluminum alloy.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein, the pure aluminum is industrial pure aluminum containing more than 99.9 mass percent of aluminum.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein the mass of the ceramic particles is 0.5-3.0 wt.% of the composite material.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein the ceramic particles are any one of silicon carbide particles, magnesium oxide particles, aluminum nitride particles or titanium carbide particles.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein the ceramic particles have a particle size of 10 to 100 μm.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: wherein, the stirring in the step 2 is carried out in an aluminum melting furnace, and mechanical stirring or semi-solid stirring is adopted.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: the semi-solid stirring method comprises the following steps: heating pure aluminum or alloy to 750 ℃ at 720-.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: the cutting method in the step 3 comprises mechanical cutting or cutting after the plate is processed by pressure.
The preparation method of the ceramic particle composite anode material for the aluminum-air battery provided by the invention is also characterized in that: the method for cutting the plate after the plate is processed by pressure comprises the following steps: the particulate composite material is rolled into a sheet of predetermined thickness and further cut to the desired anode size.
The invention provides an aluminum-air battery ceramic particle composite anode material which has the characteristics that the aluminum-air battery ceramic particle composite anode material is prepared by the preparation method of the aluminum-air battery ceramic particle composite anode material.
Action and Effect of the invention
The preparation method of the ceramic particle composite anode material for the aluminum-air battery comprises the following steps: mixing the preheated ceramic particles with the heated and melted pure aluminum or aluminum alloy, obtaining the composite anode material with uniformly dispersed particles by adopting a common aluminum melting furnace and mechanical stirring or vacuum semi-solid stirring technology, and further rolling the composite anode material into a plate after casting, and cutting the plate into the required anode size. The preparation method provided by the invention is simple and low in cost, and the obtained composite anode has good electrochemical activity in alkaline electrolyte, low self-corrosion rate and high utilization rate of the battery anode, so that the preparation method provided by the invention is suitable for large-scale production and processing.
Drawings
FIG. 1 is a graph showing the amount of hydrogen evolution in an alkaline solution in test example 1 of the present invention using the anode materials of examples 1 to 3 and comparative example 1;
FIG. 2 is a graph showing a discharge curve of an aluminum-air battery prepared in test example 2 of the present invention using examples 1-2 and comparative example 1; and
fig. 3 is a graph showing the dynamic polarization of the anode material according to example 8, comparative example 1 and comparative example 3 in test example 3 of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is specifically described below by combining the embodiment and the attached drawings.
< example 1>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method specifically comprises the following steps:
step 1, fully cleaning and drying magnesium oxide particles with the particle size of 50 microns, fully preheating at 300 ℃, and preserving heat for 1.5 hours to obtain preheated magnesium oxide particles;
step 2, heating industrial pure aluminum 4N6 (the mass fraction of aluminum is more than 99.9%) to 710 ℃ in a vacuum environment to completely melt the pure aluminum, mixing and stirring the pure aluminum and preheated magnesium oxide particles with the mass fraction of 0.5 wt.%, reducing the temperature to be a semi-solid temperature of 640 ℃, continuously stirring and heating to 690 ℃, stopping heating and stirring, and casting and molding to obtain the Al-MgO composite material;
and 3, cutting the cast ingot of the Al-MgO composite material to obtain the composite anode of the aluminum-air battery, or rolling the cast ingot into a plate with the thickness of 5mm, and cutting the plate into the anode plate with the required size.
< example 2>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method was the same as in example 1 except that the preheated magnesium oxide particles having a mass fraction of 0.5 wt.% in step 2 were changed to preheated magnesium oxide particles having a mass fraction of 1 wt.%.
< example 3>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method was the same as in example 1 except that the preheated magnesium oxide particles having a mass fraction of 0.5 wt.% in step 2 were changed to preheated magnesium oxide particles having a mass fraction of 1.5 wt.%.
< comparative example 1>
Preparation method of aluminum-air battery anode material
The preparation method is the same as that of the embodiment 1, and only the difference is that the industrial pure aluminum 4N6 (the mass fraction of the aluminum is more than 99.9%) is directly adopted as the anode material, and no ceramic particles are added.
< example 4>
Aluminum-air battery
Negative pole piece: the anode material prepared in example 1 was used.
Positive pole piece: an air electrode membrane containing an oxygen reduction catalyst.
Assembling the aluminum-air battery: the anode material prepared in example 1, a negative electrode plate, and an electrolyte (an alkaline solution or a salt solution) were assembled into an aluminum anode air battery containing 0.5 wt.% of magnesium oxide particles.
< example 5>
Aluminum-air battery
The assembly method was the same as in example 4, except that the negative electrode sheet was changed to the anode material prepared in example 2.
< example 6>
Aluminum-air battery
The assembly method was the same as in example 4, except that the negative electrode sheet was changed to the anode material prepared in example 3.
< comparative example 2>
Preparation method of aluminum-air battery
The assembly method was the same as example 4 except that the negative electrode sheet was changed to the anode material prepared in comparative example 1.
< example 7>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method comprises the following steps:
step 1, fully cleaning and drying 100 mu m silicon carbide particles, fully preheating at 900 ℃, and preserving heat for 1.5 hours to obtain preheated silicon carbide particles;
step 2, heating industrial pure aluminum 4N6 (the mass fraction of aluminum is more than 99.9%) to 730 ℃ in a vacuum environment to completely melt the pure aluminum, mixing the pure aluminum with preheated silicon carbide particles with the mass fraction of 1.0 wt.%, stirring, reducing the temperature to 645 ℃ of semi-solid temperature, continuously stirring, heating to 700 ℃, stopping heating and stirring, and casting and molding to obtain the Al-SiC composite material;
and 3, carrying out ingot casting cutting on the cast Al-SiC composite material to prepare the aluminum-air battery composite anode, or rolling the ingot casting into a plate with the thickness of 5mm, and cutting into the anode plate with the required size.
< example 8>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method comprises the following steps:
step 1, fully cleaning and drying 100 mu m silicon carbide particles, fully preheating at 900 ℃, and preserving heat for more than 1 hour to obtain preheated silicon carbide particles;
step 2, heating industrial pure aluminum 4N6 (the mass fraction of aluminum is more than 99.9%) to 730 ℃ in a vacuum environment to completely melt the pure aluminum, firstly adding 1.0 wt.% of pure magnesium, then mixing with preheated silicon carbide particles with the mass fraction of 1.0 wt.%, stirring, reducing the temperature to 645 ℃ of a semi-solid state, continuously stirring, heating to 690 ℃, stopping heating and stirring, and casting and molding to obtain the Al-Mg-SiC composite material;
and 3, carrying out ingot casting and cutting on the cast Al-Mg-SiC composite material to prepare the aluminum-air battery composite anode, or rolling the ingot casting into a plate with the thickness of 5mm, and cutting into the anode plate with the required size.
< comparative example 3>
Preparation method of aluminum-air battery anode material
The preparation method is the same as that of the embodiment 1, and the difference is that the magnesium-aluminum alloy is directly used as the anode material, and no ceramic particles are added. Wherein the aluminum is industrial pure aluminum 4N6 (the mass fraction of aluminum is more than 99.9%), the magnesium is pure magnesium, and the addition amount is 1.0 wt.%.
< example 9>
Preparation method of ceramic particle composite anode material of aluminum-air battery
The preparation method comprises the following steps:
step 1, fully cleaning and drying 80 mu m aluminum oxide particles, fully preheating at 500 ℃, and preserving heat for more than 1 hour to obtain preheated aluminum oxide particles;
step 2, heating industrial pure aluminum 4N6 (the mass fraction of aluminum is more than 99%) to 730 ℃ in a vacuum environment to completely melt the pure aluminum, mixing and stirring the pure aluminum and preheated aluminum oxide particles with the mass fraction of 0.5 wt.%, reducing the temperature to 645 ℃ of a semi-solid state temperature, continuously stirring the mixture, heating the mixture to 700 ℃, stopping heating and stirring, and casting and molding to obtain the Al-Al alloy2O3A composite material;
step 3, carrying out casting on the obtained Al-Al2O3And (3) cutting the composite material into a cast ingot and preparing the aluminum-air battery composite anode, or rolling the cast ingot into a plate with the thickness of 4mm and cutting the plate into an anode plate with the required size.
< test example 1>
Hydrogen evolution test of aluminum air cell anode materials
Electrochemical tests were performed on the anode materials of the aluminum air batteries of examples 1 to 3 and comparative example 1, respectively, using the test system.
The test results are shown in fig. 1. FIG. 1 shows the amount of hydrogen evolved in the alkaline solution in this test example 1 using the anode materials of examples 1 to 3 and comparative example 1.
As can be seen from FIG. 1, compared with a pure aluminum anode, the hydrogen evolution amount of the MgO particle composite anode in the alkaline solution is reduced along with the increase of the content of the magnesium oxide, and the magnesium oxide particles can obviously reduce the self-corrosion of the anode.
< test example 2>
Electrochemical performance testing of aluminum air cells
The electrochemical performance of the aluminum-air cells of examples 1-2 and comparative example 1 was respectively tested using the test system.
The test results are shown in fig. 2. Fig. 2 is a discharge curve diagram of the aluminum-air battery prepared in this test example 2 using examples 1-2 and comparative example 1.
As can be seen from fig. 2, compared with a pure aluminum anode, the open circuit potential of the MgO particle composite anode in the alkali solution increases with the increase of the content of the magnesium oxide, and the open circuit potential of the composite anode can be significantly increased by the magnesium oxide particles.
< test example 3>
Dynamic polarization test of aluminum air battery anode material
The dynamic polarization test was performed on the anode materials of the aluminum air batteries of example 8, comparative example 1 and comparative example 3 using the test system, respectively.
The test results are shown in fig. 3. Fig. 3 is a graph showing the dynamic polarization of the anode material of example 8, comparative example 1 and comparative example 3 used in this test example 3.
As can be seen from fig. 3, the corrosion potential of the Al — Mg alloy anode added with 1 wt.% Mg relative to the pure aluminum anode in the alkaline solution is significantly shifted negatively, and the corrosion potential of the Al — Mg — SiC composite anode further compounded with silicon carbide in the alkaline solution is further shifted negatively. The electrochemical activity of the Al-Mg alloy anode in the alkaline solution is improved, and the electrochemical activity of the Al-Mg-SiC composite anode in the alkaline solution is higher.
Effects and effects of the embodiments
The preparation method of the ceramic particle composite anode material for the aluminum-air battery according to the embodiment comprises the following steps: mixing the preheated ceramic particles with the heated and melted pure aluminum or aluminum alloy, obtaining the composite anode material with uniformly dispersed particles by adopting a common aluminum melting furnace and mechanical stirring or vacuum semi-solid stirring technology, and further rolling the composite anode material into a plate after casting, and cutting the plate into the required anode size. The preparation method provided by the embodiment is simple, the components of the composite anode material are adjustable, the cost is low, and the obtained composite anode has the advantages of high electrochemical activity, low self-corrosion rate and high utilization rate of the battery anode in the alkaline electrolyte, so that the preparation method provided by the embodiment is suitable for large-scale production and processing.
Further, in the aluminum-based composite material provided by the embodiment, the metal ceramic particles are proved to be capable of destroying the integrity of the pure aluminum surface passivation film, reducing anode polarization, facilitating the proceeding of electrochemical reaction and improving the electrochemical activity of the anode. In addition, the ceramic particles do not react with the alkaline solution, can provide attachment points for corrosion products in the reaction process, plays a certain role in protecting the self-corrosion of the aluminum matrix, simultaneously reduces the self-corrosion rate, reduces the hydrogen release, and obviously improves the discharge performance and the electrode efficiency of the anode material of the alkaline aluminum-air battery.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.

Claims (5)

1. A preparation method of a ceramic particle composite anode material of an aluminum-air battery is characterized by comprising the following steps:
step 1, cleaning, drying and preheating ceramic particles to obtain preheated ceramic particles;
step 2, heating and melting pure aluminum or aluminum alloy, and stirring and casting the pure aluminum or aluminum alloy and the preheated ceramic particles in a vacuum environment to obtain a particle composite material; and
step 3, cutting the particle composite material to obtain the ceramic particle composite anode material of the aluminum-air battery,
wherein the ceramic particles are any one of alumina particles, aluminum nitride particles or titanium carbide particles, the particle size is 10-100 μm,
the mass of the ceramic particles is 0.5-3.0 wt.% of the composite material,
the stirring in the step 2 is carried out in an aluminum melting furnace, semi-solid stirring is adopted,
the semi-solid stirring method comprises the following steps:
heating the pure aluminum or the alloy to the temperature of 720-750 ℃ until the pure aluminum or the alloy is completely melted, adding the preheated ceramic particles, stirring and cooling to the semi-solid temperature of 630-650 ℃, stirring for 10-20min, heating to the temperature of 680-720 ℃, stopping heating and stirring, and casting and molding to obtain the particle composite material.
2. The method for preparing the ceramic particle composite anode material for the aluminum-air battery according to claim 1, wherein the method comprises the following steps:
wherein the pure aluminum is industrial pure aluminum containing aluminum with the mass fraction of more than 99.9%.
3. The method for preparing the ceramic particle composite anode material for the aluminum-air battery according to claim 1, wherein the method comprises the following steps:
the cutting method in the step 3 comprises mechanical cutting or cutting after the plate is processed by pressure.
4. The method for preparing the ceramic particle composite anode material for the aluminum-air battery according to claim 3, wherein the method comprises the following steps:
the method for cutting the plate after the plate is processed by pressure comprises the following steps:
the particulate composite material is rolled into a sheet of predetermined thickness and further cut to the desired anode size.
5. An aluminum-air battery ceramic particle composite anode material, which is characterized by being prepared by the preparation method of the aluminum-air battery ceramic particle composite anode material as claimed in any one of claims 1 to 4.
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