CN115490251A - Lithium metaaluminate powder and preparation method and application thereof - Google Patents
Lithium metaaluminate powder and preparation method and application thereof Download PDFInfo
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- CN115490251A CN115490251A CN202211337427.1A CN202211337427A CN115490251A CN 115490251 A CN115490251 A CN 115490251A CN 202211337427 A CN202211337427 A CN 202211337427A CN 115490251 A CN115490251 A CN 115490251A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/043—Lithium aluminates
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0236—Glass; Ceramics; Cermets
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/14—Fuel cells with fused electrolytes
- H01M8/144—Fuel cells with fused electrolytes characterised by the electrolyte material
- H01M8/145—Fuel cells with fused electrolytes characterised by the electrolyte material comprising carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/14—Fuel cells with fused electrolytes
- H01M2008/147—Fuel cells with molten carbonates
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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
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Fuel Cell (AREA)
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Abstract
The invention relates to the technical field of battery materials, in particular to lithium metaaluminate powder, a preparation method and application thereof. The preparation method of the lithium metaaluminate powder comprises the following steps: and co-grinding the lithium carbonate, the alumina and the aluminum powder, and performing heat treatment at a temperature above the melting point of the aluminum powder. The lithium metaaluminate powder prepared by the method not only can improve the strength of the electrolyte diaphragm, but also has simple and convenient method and low cost.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to lithium metaaluminate powder, a preparation method and application thereof.
Background
The Molten Carbonate Fuel Cell (MCFC) is a pollution-free and efficient power generation device, which is composed of a cathode, an anode, an electrolyte and a diaphragm of the cell, wherein the diaphragm is a core component of the cell, and the diaphragm is required to have high heat resistance and high resistance to corrosion of high-temperature molten salt, and the quality of the diaphragm directly affects the quality of the cell. MgO was originally used as a separator material for MCFCs, but it is easily dissolved in high-temperature molten salts to affect the battery life. LiAlO 2 Has strong capability of resisting corrosion of molten carbonate, so that LiAlO is generally adopted at present 2 As a battery separator material.
LiAlO 2 The preparation method of the powder mainly comprises three main categories of a solid-phase reaction sintering method, a molten salt hydrolysis method and a solution method, wherein the solid-phase reaction sintering method is used for preparing LiAlO 2 The raw material of the powder is mainly Li 2 CO 3 Or Li 2 O 2 Mixing it with an equimolar amount of Al 2 O 3 After mixing, ball milling and mixing by adopting a dry method or a wet method and calcining at a certain temperature to prepare the LiAlO 2 Powder, however, liAlO prepared by the prior art 2 The powder has the problem that the strength of the prepared electrolyte diaphragm is not high when the powder is prepared into the electrolyte diaphragm.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the LiAlO in the prior art 2 The powder prepared electrolyte diaphragm has the defect of low strength, thereby providing the lithium metaaluminate powder and the preparation method and the application thereof for solving the problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing lithium metaaluminate powder comprises the following steps: and co-grinding the lithium carbonate, the alumina and the aluminum powder, and performing heat treatment at a temperature above the melting point of the aluminum powder.
Preferably, the molar ratio of the lithium carbonate, the alumina and the aluminum powder is (5.6-6): (5.6-5.8): (0.8-1.2);
and/or the alumina is alkaline alumina.
Preferably, the heat treatment temperature is above 700 ℃, and the heat treatment time is above 12 h.
Preferably, the heat treatment process is as follows: heating to 420-460 ℃, and preserving heat for 3h; then raising the temperature to 650-710 ℃, and preserving the temperature for 15h; then heating to 720-760 ℃, and preserving the heat for 12h; and finally, cooling along with the furnace.
Preferably, the temperature rise speed is 0.5-4 ℃/min.
Preferably, the heat treatment is performed in an air atmosphere.
Preferably, the way of co-grinding is ball milling; the rotation speed of the ball milling is 320r/min-400r/min; the ball milling time is 36h; the ball milling adopts distilled water as a dispersing agent.
Preferably, the method specifically comprises the following steps:
1) Co-grinding the aluminum powder, lithium carbonate and aluminum oxide to obtain a mixed powder material;
2) Carrying out heat treatment on the mixed powder material obtained in the step 1) to obtain the lithium metaaluminate material.
Preferably, drying treatment is carried out after the co-grinding treatment; and/or, carrying out crushing and grinding treatment after the heat treatment; preferably, the average particle size of the lithium metaaluminate powder obtained after the crushing and grinding treatment is 2-15 μm.
Preferably, the crushing and grinding treatment equipment is a planetary ball mill.
The invention also provides lithium metaaluminate powder which is prepared by the preparation method of the lithium metaaluminate powder.
The invention also provides application of the lithium metaaluminate powder in preparing the diaphragm of the molten carbonate fuel cell.
The technical scheme of the invention has the following advantages:
1. the invention provides a preparation method of lithium metaaluminate powder, which comprises the following steps: and co-grinding the lithium carbonate, the alumina and the aluminum powder, and performing heat treatment at a temperature above the melting point of the aluminum powder. The aluminum powder is melted in the temperature rising process and oxidized by oxygen in the air, and then reacts with lithium carbonate to generate lithium metaaluminate, the lithium metaaluminate generated by taking the aluminum powder as an aluminum source is in a fibrous state, the surface of the lithium metaaluminate is coarsened, and the fibrous lithium metaaluminate with the coarsened surface is interwoven in the electrolyte diaphragm, so that the unidirectional compression strength of the electrolyte diaphragm is improved.
2. According to the preparation method of the lithium metaaluminate powder, air is introduced to provide oxygen to participate in the reaction of the aluminum powder and the lithium carbonate, and meanwhile, carbon dioxide generated by the reaction can be taken away, so that the reaction is promoted to move towards the direction of a product, and the generation of lithium metaaluminate is further promoted.
3. The preparation method of the lithium metaaluminate powder provided by the invention has the advantages of cheap raw materials and simple and convenient process.
Detailed Description
The following examples are provided to better understand the present invention, not to limit the best mode, and not to limit the content and protection scope of the present invention, and any product that is the same or similar to the present invention and is obtained by combining the present invention with other features of the prior art and the present invention falls within the protection scope of the present invention.
The examples do not indicate specific experimental procedures or conditions, and can be performed according to the procedures or conditions of the conventional experimental procedures described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
Lithium carbonate with the particle size of 25 mu m, alkaline alumina with the particle size of 30 mu m and Al powder with the particle size of 50 mu m are mixed according to the mol ratio of 5.8:5.7:1, ball-milling for 36 hours in a ball mill at the rotating speed of 350r/min by taking water as a medium, drying, then placing in a muffle furnace, and introducing air for heat treatment, wherein the specific temperature rise program is from room temperature to 450 ℃ for 2 hours; keeping the temperature at 450 ℃ for 3h; 450-700 ℃ for 3h; keeping the temperature at 700 ℃ for 15h;700 ℃ to 750 ℃ for 1h; keeping the temperature at 750 ℃ for 12h; furnace cooling is carried out from 750 ℃ to room temperature, and then crushing and grinding are carried out in a planet ball mill for 6 hours, so as to prepare the lithium metaaluminate powder.
The average grain diameter of the lithium metaaluminate powder is 2.4 mu m through inspection; the electrolyte diaphragm is prepared by adopting lithium metaaluminate powder as a raw material, polyvinyl alcohol as a binder, distilled water as a solvent, lactic acid as a dispersing agent, glycerol and glycerol triacetate as plasticizers, and polyether as a defoaming agent through ball milling, vacuumizing and tape casting. The electrolyte diaphragm prepared by the lithium metaaluminate powder provided by the embodiment of the invention is placed between pressure heads of a tester by using a unidirectional compression tester, and is loaded until the diaphragm is cracked, so that the unidirectional compression strength of the electrolyte diaphragm prepared by the lithium metaaluminate powder provided by the embodiment of the invention is measured to be 3.5MPa.
Example 2
Lithium carbonate with the particle size of 25 mu m, alkaline alumina with the particle size of 30 mu m and Al powder with the particle size of 50 mu m are mixed according to the molar ratio of 6:5.8:1.2, ball-milling for 36 hours in a ball mill at the rotating speed of 400r/min by using distilled water as a medium, drying, then placing in a muffle furnace and introducing air for heat treatment, wherein the specific temperature rise procedure is from room temperature to 460 ℃ for 2 hours; keeping the temperature at 460 ℃ for 3h; 460-710 ℃ for 3h; keeping the temperature at 710 ℃ for 15h;710 ℃ to 760 ℃ for 1h; keeping the temperature at 760 ℃ for 12h; cooling the mixture to room temperature along with the furnace from 760 ℃, and then crushing and grinding the mixture in a planet ball mill for 6 hours to prepare the lithium metaaluminate powder.
The lithium metaaluminate powder is checked to have the average grain diameter of 2.9 mu m, the electrolyte diaphragm is prepared by adopting the method the same as the embodiment 1, and the unidirectional compression strength of the electrolyte diaphragm prepared by the lithium metaaluminate powder provided by the embodiment of the invention is 3.1MPa.
Example 3
Lithium carbonate with the particle size of 25 mu m, alkaline alumina with the particle size of 30 mu m and Al powder with the particle size of 50 mu m are mixed according to the mol ratio of 5.6:5.6:0.8, taking distilled water as a medium in a ball mill, carrying out ball milling for 36 hours at the rotating speed of 320r/min, drying, then placing in a muffle furnace, and introducing air for heat treatment, wherein the specific temperature rise program is from room temperature to 420 ℃ for 2 hours; keeping the temperature at 420 ℃ for 3h; the temperature is 420 ℃ to 650 ℃, and the time is 3 hours; keeping the temperature at 650 ℃ for 15h; 650-720 ℃ for 1h; keeping the temperature at 720 ℃ for 12h; cooling the mixture from 720 ℃ to room temperature along with the furnace, and then crushing and grinding the mixture in a planet ball mill for 6 hours to prepare the lithium metaaluminate powder.
The lithium metaaluminate powder has an average particle size of 3.2 μm, and is tested to be prepared into the electrolyte diaphragm by the same method as the embodiment 1, and the unidirectional compression strength of the electrolyte diaphragm prepared from the lithium metaaluminate powder provided by the embodiment of the invention is 2.9MPa.
Comparative example 1
This comparative example differs from example 1 in that no aluminum powder was added, and the other examples are the same as example 1.
Mixing alkaline alumina powder with the grain diameter of 30 mu m and lithium carbonate with the grain diameter of 25 mu m according to a molar ratio of 1:1, ball-milling for 36 hours in a ball mill at the rotating speed of 350r/min by using distilled water as a medium, drying, then placing in a muffle furnace and introducing air for heat treatment, wherein the specific temperature rise procedure is from room temperature to 450 ℃ for 2 hours; keeping the temperature at 450 ℃ for 3h; 450-700 ℃ for 3h; keeping the temperature at 700 ℃ for 15h;700 ℃ to 750 ℃ for 1h; keeping the temperature at 750 ℃ for 12h; furnace cooling is carried out from 750 ℃ to room temperature, and then crushing and grinding are carried out in a planet ball mill for 6 hours, so as to prepare the lithium metaaluminate powder.
It was examined that the lithium metaaluminate powder had an average particle size of 3.1 μm, and an electrolyte membrane was prepared in the same manner as in example 1, and the electrolyte membrane prepared from the lithium metaaluminate powder provided in this comparative example had a unidirectional compressive strength of 1.8MPa.
Comparative example 2
This comparative example differs from example 1 in that only aluminum powder was used as an aluminum source and the heat treatment temperature was adjusted to 600 ℃.
Aluminum powder with the particle size of 50 microns and lithium carbonate with the particle size of 25 microns are mixed according to a molar ratio of 1:1, ball-milling for 36 hours in a ball mill at the rotating speed of 350r/min by using distilled water as a medium, drying, then placing in a muffle furnace, and introducing air for heat treatment, wherein the specific temperature rise program is from room temperature to 450 ℃ for 2 hours; keeping the temperature at 450 ℃ for 3h; the temperature is 450-600 ℃ and the time is 3h; keeping the temperature at 600 ℃ for 15h, cooling the mixture to room temperature from 600 ℃ along with the furnace, and crushing and grinding the mixture in a planet ball mill device for 6h to prepare the lithium metaaluminate powder.
It was examined that the lithium metaaluminate powder had an average particle size of 4 μm and an electrolyte membrane was prepared in the same manner as in example 1, and the electrolyte membrane prepared from the lithium metaaluminate powder provided in this comparative example had a unidirectional compressive strength of 1.6MPa.
TABLE 1
According to the data analysis of examples 1 to 3 and comparative examples 1 to 2 in table 1, the analysis results are as follows:
comparative example 1 when no powdered aluminum was added, the prepared lithium metaaluminate powder had a defect that the unidirectional compressive strength of the electrolyte membrane prepared therefrom was low, although the average particle diameter was good; comparative example 2 when only aluminum powder was used as the aluminum source, not only was the particle size of the lithium metaaluminate powder poor but also the electrolyte membrane prepared therefrom was low in strength; the lithium metaaluminate powder prepared by the method has smaller particle size, and the strength of the electrolyte diaphragm prepared by the lithium metaaluminate powder is obviously improved.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for preparing lithium metaaluminate powder is characterized by comprising the following steps: and co-grinding the lithium carbonate, the alumina and the aluminum powder, and performing heat treatment at a temperature above the melting point of the aluminum powder.
2. The production method according to claim 1, characterized in that the molar ratio of lithium carbonate, alumina and aluminum powder is (5.6-6): (5.6-5.8): (0.8-1.2);
and/or the alumina is alkaline alumina.
3. The method according to claim 1 or 2, wherein the heat treatment temperature is 700 ℃ or more, and the heat treatment time is 12 hours or more.
4. The method according to claim 3, wherein the heat treatment is carried out by: heating to 420-460 ℃, and preserving heat for 3h; then heating to 650-710 ℃, and preserving heat for 15h; then heating to 720-760 ℃, and preserving the heat for 12h; and finally, cooling along with the furnace.
5. The production method according to claim 4, wherein the temperature increase rate is 0.5 to 4 ℃/min.
6. The production method according to any one of claims 1 to 5, wherein the heat treatment is performed in an air atmosphere.
7. The production method according to any one of claims 1 to 6, wherein the co-milling is performed by ball milling; the rotation speed of the ball milling is 320r/min-400r/min; the ball milling time is 36h; the ball milling adopts distilled water as a dispersing agent.
8. The method according to any one of claims 1 to 7, wherein a drying treatment is further performed after the co-grinding treatment; and/or, carrying out crushing and grinding treatment after the heat treatment; preferably, the average particle size of the lithium metaaluminate powder obtained after the crushing and grinding treatment is 2-15 μm.
9. A lithium metaaluminate powder prepared by the method of any one of claims 1 to 8.
10. The use of the lithium metaaluminate powder of claim 9 in the preparation of a membrane for a molten carbonate fuel cell.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116444261A (en) * | 2023-03-23 | 2023-07-18 | 宜春国轩电池有限公司 | Lithium metaaluminate material and preparation method and application thereof |
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