CN115028214A - Method for preparing manganese-based sodium ion composite oxide positive electrode material - Google Patents
Method for preparing manganese-based sodium ion composite oxide positive electrode material Download PDFInfo
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- CN115028214A CN115028214A CN202210760284.9A CN202210760284A CN115028214A CN 115028214 A CN115028214 A CN 115028214A CN 202210760284 A CN202210760284 A CN 202210760284A CN 115028214 A CN115028214 A CN 115028214A
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- sodium ion
- manganese
- composite oxide
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- positive electrode
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing manganese-based sodium ion composite oxide anode material, which comprises three metal oxides, wherein the three metal oxides are subjected to ball milling and crushing treatment according to different proportions, sieving treatment is carried out after ball milling, sodium salt is added into a treated raw material mixture and is mixed in a ball milling tank, the mixed raw material is put in a sagger and is put in a tunnel kiln for presintering, the presintering raw material is briquetted, the briquetted raw material is put in the sagger again for three times of roasting, magnetic substances are removed from the roasted raw material, and the raw material is vibrated and sieved, so that the used raw material is low in cost, the whole process is pure solid phase reaction, no wastewater and no pollution are generated, the process route is simple, the industrial production is easy, the crystal structure of the sodium ion battery anode material produced by using the metal oxides is of a layered structure, the electronic conductivity is better, the crystal structure is stable, and the large-scale electric energy storage is more facilitated.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a method for preparing a manganese-based sodium ion composite oxide positive electrode material.
Background
In recent years, the shortage of lithium source and the sharp rise of lithium price limit the further development of lithium ion batteries, and as sodium in the same family with lithium has electrochemical characteristics similar to lithium, so that the sodium ion batteries are more regarded as "substitutes" for lithium ion batteries, and the positive electrode materials of the currently commonly used sodium ion batteries comprise transition metal oxides with a layered structure, polyanion compounds and prussian blue compounds. The layered structure NaxFeMO2 and the open framework structure Na2MFe (CN)6(M is transition metal such as Fe, Co, Ni, Mn and the like) materials based on variable-valence iron are hot spots developed at present. The preparation processes (such as coprecipitation, precipitation, crystallization, high-temperature sintering and the like) and process parameters thereof have great influence on the structure and performance of the cathode material, the current preparation method is complex, a large amount of wastewater is generated, and the wastewater needs to be properly treated so as to be discharged, or the preparation process is divided into two steps: firstly synthesizing a precursor, and then mixing and calcining the precursor and a sodium source, wherein the synthesis route is complex.
Therefore, a method for preparing the manganese-based sodium ion composite oxide cathode material is provided to solve the problems.
Disclosure of Invention
The invention aims to provide a method for preparing a manganese-based sodium ion composite oxide positive electrode material, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a manganese-based sodium ion composite oxide cathode material, which comprises three metal oxides, comprises the following preparation steps:
step one, performing ball milling and crushing treatment according to different proportions;
step two, sieving treatment is carried out after crushing;
step three, adding sodium salt based on the raw material mixture obtained in the step two, and mixing in a ball milling tank;
step four, loading the raw materials based on the step three into a sagger, and putting the sagger into a tunnel kiln for pre-burning;
step five, briquetting the presintered raw materials, so as to increase the contact degree between material particles and ensure that the high-temperature solid-phase reaction is more sufficient;
sixthly, putting the briquetted raw materials into the saggar again for three times of roasting;
and seventhly, removing magnetic substances from the roasted raw materials, and vibrating and sieving the raw materials.
In further embodiments, the three metal oxides manganese oxide, nickel oxide, and iron oxide.
In a further embodiment, the ratio of the three metal oxides is 3: 3: 4. 4: 2: 4 and 5: 2: 3, or a pharmaceutically acceptable salt thereof.
In a further embodiment, in the step one, the ball-to-material ratio is 4:1, the ball milling time is more than 5 hours, the ball milling and crushing of the materials are carried out, and the reaction between different materials is more sufficient when the particle size of the material particles is reduced.
In a further embodiment, in the third step, the sodium salt may be sodium carbonate, but is not limited to this.
In a further embodiment, in the fourth step, the pre-burning temperature is 400 ℃, the time is 15 hours, and the low-temperature pre-burning treatment is carried out on the material, so that the discharge of the crystallized water and some harmful substances in the material is ensured.
In a further embodiment, in the sixth step, the first temperature is constant at 600 ℃ for 15 hours, the second temperature is constant at 850 ℃ for 15 hours, the third roasting temperature is constant at 700 ℃ for 15 hours, three times of roasting are carried out on the material at different temperatures, and crushing and mixing are added in the middle, so that the uniformity and the sufficiency of roasting are ensured.
In a further embodiment, in step six, a crushing and mixing process is performed between each firing.
In a further embodiment, in the seventh step, the magnetic substances are removed by a professional iron attracting device, and the magnetic substances are sieved by an ultrasonic oscillation screen with 200 meshes to obtain a finished product.
Compared with the prior art, the invention has the beneficial effects that:
the used raw materials have low cost, the whole process is pure solid phase reaction, no wastewater and no pollution, the process route is simple, the industrial production is easy, the crystal structure of the sodium ion battery anode material produced by using the metal oxide is a layered structure, the electronic conductivity is better, the crystal structure is stable, and the large-scale electric energy storage is more facilitated.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a manganese-based sodium ion composite oxide positive electrode material according to the present invention;
Detailed Description
In the description of the present invention, "a plurality" means two or more unless otherwise specified.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a method for preparing a manganese-based sodium ion composite oxide positive electrode material includes ball-milling and crushing three metal oxides according to different proportions, sieving after ball-milling, adding sodium salt into a treated raw material mixture, mixing in a ball-milling tank, loading the mixed raw material into a sagger, placing the sagger into a tunnel kiln for pre-sintering, briquetting the pre-sintered raw material, placing the briquetted raw material into the sagger again for three times of roasting, removing magnetic substances from the roasted raw material, and vibrating and sieving.
Example 1
The three oxides are manganese oxide, nickel oxide and iron oxide, and the proportion is 3: 3: 4, ball milling and crushing treatment is carried out, the ball-material ratio is 4:1, the ball milling time is not less than 5 hours, the ball milling is carried out and then the ball milling is carried out for standby application, sodium carbonate (or other sodium salts) is added into the treated raw material mixture, fully mixing the raw materials in a ball milling tank for 5 hours, putting the mixed raw materials in a sagger, putting the sagger in a tunnel kiln for presintering, wherein the presintering temperature is 400 ℃ and the presintering time is 15 hours, briquetting the pre-sintered material to form round or square material cake, placing into a sagger for three times of roasting, keeping the temperature at 600 ℃ for 15 hours for the first time, the second time temperature is 850 ℃ for 15 hours, the third time roasting temperature is 700 ℃ for 15 hours, wherein, crushing and mixing treatment are carried out between each roasting, after the roasting for three times, the crushing treatment is carried out, magnetic substances are simultaneously removed through professional iron absorption equipment, and the magnetic substances are sieved through a 200-mesh screen by ultrasonic oscillation to obtain a finished product.
Example 2
The three oxides are manganese oxide, nickel oxide and iron oxide, and the ratio of manganese oxide to nickel oxide to iron oxide is 4: 2: 4, ball milling and crushing treatment is carried out, the ball-material ratio is 4:1, the ball milling time is not less than 5 hours, the ball milling is carried out and then the ball milling is carried out for standby application, sodium carbonate (or other sodium salts) is added into the treated raw material mixture, fully mixing the raw materials in a ball milling tank for 5 hours, putting the mixed raw materials into a sagger, putting the sagger into a tunnel kiln for presintering, wherein the presintering temperature is 400 ℃, the presintering time is 15 hours, briquetting the pre-sintered material to form round or square material cake, placing into a sagger for three times of roasting, keeping the temperature at 600 ℃ for 15 hours for the first time, the second time temperature is 850 ℃ for 15 hours, the third time roasting temperature is 700 ℃ for 15 hours, wherein, crushing and mixing treatment are carried out between each roasting, after the roasting for three times, the crushing treatment is carried out, magnetic substances are simultaneously removed through professional iron absorption equipment, and the magnetic substances are sieved through a 200-mesh screen by ultrasonic oscillation to obtain a finished product.
Example 3
The three oxides are manganese oxide, nickel oxide and iron oxide, and the proportion is as follows: 2: 3, ball milling and crushing treatment, wherein the ball-material ratio is 4:1, the ball milling time is not less than 5 hours, the ball milling is carried out and then sieving is carried out for standby application, sodium carbonate (or other sodium salts) is added into the treated raw material mixture, fully mixing the raw materials in a ball milling tank for 5 hours, putting the mixed raw materials into a sagger, putting the sagger into a tunnel kiln for presintering, wherein the presintering temperature is 400 ℃, the presintering time is 15 hours, briquetting the pre-sintered material to form round or square material cake, placing into a sagger for three times of roasting, keeping the temperature at 600 ℃ for 15 hours for the first time, the second time temperature is 850 ℃ for 15 hours, the third time roasting temperature is 700 ℃ for 15 hours, wherein, crushing and mixing treatment are carried out between each roasting, after the roasting for three times, the crushing treatment is carried out, magnetic substances are simultaneously removed through professional iron absorption equipment, and the magnetic substances are sieved through a 200-mesh screen by ultrasonic oscillation to obtain a finished product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. A method for preparing a manganese-based sodium ion composite oxide cathode material is characterized by comprising the following steps: the material comprises three metal oxides, and the preparation steps are as follows:
step one, performing ball milling and crushing treatment according to different proportions;
step two, sieving treatment is carried out after crushing;
step three, adding sodium salt based on the raw material mixture obtained in the step two, and mixing in a ball milling tank;
step four, loading the raw materials based on the step three into a sagger, and putting the sagger into a tunnel kiln for pre-burning;
step five, briquetting the presintered raw materials;
sixthly, putting the briquetted raw materials into the saggar again for three times of roasting;
and seventhly, removing magnetic substances from the roasted raw materials, and vibrating and sieving the raw materials.
2. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: the three metal oxides are manganese oxide, nickel oxide and iron oxide.
3. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: the ratio of the three metal oxides is 3: 3: 4. 4: 2: 4 and 5: 2: 3, or a pharmaceutically acceptable salt thereof.
4. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: in the first step, the ball-material ratio is 4:1, and the ball milling time is more than 5 hours.
5. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: in the third step, the sodium salt may be sodium carbonate, but is not limited to this.
6. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, wherein: in the fourth step, the presintering temperature is 400 ℃, and the time is 15 hours.
7. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: in the sixth step, the first temperature is kept constant at 600 ℃ for 15 hours, the second temperature is kept constant at 850 ℃ for 15 hours, and the third roasting temperature is kept constant at 700 ℃ for 15 hours.
8. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, wherein: in the sixth step, crushing and mixing treatment is carried out between each roasting.
9. The method for preparing a manganese-based sodium ion composite oxide positive electrode material according to claim 1, characterized in that: and seventhly, removing magnetic substances by a professional iron absorption device, and screening the magnetic substances by a 200-mesh screen through ultrasonic oscillation to obtain a finished product.
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Citations (8)
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| CN111186861A (en) * | 2020-01-09 | 2020-05-22 | 南京大学 | Layered chromium-based positive electrode material of sodium ion battery and preparation method thereof |
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| CN111952579A (en) * | 2020-08-25 | 2020-11-17 | 东华理工大学 | High-energy-density sodium ion battery iron-manganese-based positive electrode material and preparation method thereof |
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2022
- 2022-06-30 CN CN202210760284.9A patent/CN115028214A/en active Pending
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