CN114976013A - Preparation method of battery negative electrode material - Google Patents
Preparation method of battery negative electrode material Download PDFInfo
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- CN114976013A CN114976013A CN202210706958.7A CN202210706958A CN114976013A CN 114976013 A CN114976013 A CN 114976013A CN 202210706958 A CN202210706958 A CN 202210706958A CN 114976013 A CN114976013 A CN 114976013A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/027—Negative 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 belongs to the technical field of batteries, and particularly relates to a preparation method of a battery cathode material, which comprises the following steps of 1, mixing graphite raw materials, crushing, grinding and grading to obtain aggregate; step 2, mixing the aggregate and the adhesive according to a preset proportion, and then carrying out low-temperature heat treatment; step 3, screening the material subjected to low-temperature heat treatment, and graphitizing; step 4, carrying out liquid phase coating on the graphitized material and a liquid phase coating agent; and 5, carbonizing the product obtained in the step 4, and screening and demagnetizing to obtain the graphite cathode material. According to the invention, by optimizing the preparation process, the quick charging capacity and the high-temperature cycle performance of the battery can be considered, and the quality of the battery is improved.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a battery cathode material.
Background
Lithium ion batteries have been widely used in 3C consumer and power batteries due to their high energy density, long cycle life, no memory effect, and the like. Graphite has a low lithium intercalation potential and a stable layered structure, and is a mainstream negative electrode material of a lithium ion battery. With the increasing demand of consumers on the quick charge performance, the graphite cathode as a material for accommodating lithium ions cannot meet the high-rate quick charge capability.
The existing graphite material cannot give consideration to quick charging performance, high-temperature cycle performance and storage performance.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the preparation method of the battery cathode material is provided, the preparation process is optimized, the quick charge capacity and the high-temperature cycle performance of the battery can be considered, and the quality of the battery is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a battery negative electrode material comprises the following steps:
step 1, mixing graphite raw materials, crushing, grinding and grading to obtain aggregate;
step 2, mixing the aggregate and the adhesive according to a preset proportion, and then carrying out low-temperature heat treatment;
step 3, screening the material subjected to low-temperature heat treatment, and graphitizing;
step 4, carrying out liquid phase coating on the graphitized material and a liquid phase coating agent;
and 5, carbonizing the product obtained in the step 4, and screening and demagnetizing to obtain the graphite cathode material.
Preferably, the graphite raw material is at least one of isotropic petroleum green coke or equirectangular coke, and the true density of the graphite raw material is 1.28-1.52 g/cm 3 The aggregate contains 5-8% of volatile components and less than 1% of sulfur components, and the Dv50 of the aggregate is 4-10 um.
Preferably, the adhesive is asphalt or resin, the adhesive is ground into 3-7 um by powder Dv50, and the coking value is 13-60%.
Preferably, in the step 2, the preset ratio is 100: 8-15, the stirring speed is 5-35 Hz, the temperature rise range is 25-560 ℃, and the temperature rise speed is 2-5 ℃/min.
Preferably, in the step 3, the graphitization temperature is 2700-3200 ℃, the graphitization degree is more than 92%, and the graphitization time is 40-60 h.
Preferably, in the step 4, the liquid phase coating agent is formed by mixing aluminum fluoride solid powder and a liquid phase solvent, the liquid phase solvent is at least one of anthracene oil, castor oil and liquid phase resin, and the density of the liquid phase solvent is 0.7-1.7 g/cm 3 The coking value is 10-40%.
Preferably, in the step 5, the carbonization temperature is 1200 ℃.
Preferably, in the step 4, the graphitized material and the liquid-phase coating agent are added into a fusion machine according to a proportion of 10-30% for normal-temperature fusion, the rotation speed of the fusion machine is 20-50 Hz, and the fusion time is 3-6 min.
Preferably, in the step 2, the weight ratio of the adhesive is 5% -20%, the aggregate and the adhesive are placed in a horizontal kettle to be stirred, and inert gas is introduced.
Preferably, in the step 3, the product obtained in the step 4 is loaded into a graphite crucible and then sent into a roller kiln for carbonization.
The method has the beneficial effects that the method is simple in process and easy to realize industrialization, the steps are fewer, two substances can be coated on the surface of the graphite, the process is mature, large-scale mass production is facilitated, the aluminum fluoride coating layer prevents the graphite from being in direct contact with electrolyte, the first irreversible reaction is avoided, the first efficiency and the circulation stability are improved, meanwhile, the aluminum fluoride is introduced, the impedance of the composite material is reduced, the reaction power of the material in the circulation process is improved, lithium ions can be rapidly inserted and removed under a large multiplying power, and the quick charge performance and the high temperature performance of the graphite material can be effectively improved.
Drawings
Features, advantages and technical effects of exemplary embodiments of the present invention will be described below with reference to the accompanying drawings.
FIG. 1 is an SEM photograph of example 1 of the present invention.
FIG. 2 is an SEM photograph of example 2 of the present invention.
FIG. 3 is an SEM photograph of comparative example 1 of the present invention.
Detailed Description
As used in the specification and in the claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect.
Furthermore, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The present invention will be described in further detail with reference to fig. 1 to 3, but the present invention is not limited thereto.
The preparation method of the battery negative electrode material comprises the following steps:
step 1, mixing graphite raw materials, crushing, grinding and grading to obtain aggregate;
step 2, mixing the aggregate and the adhesive according to a preset proportion, and then carrying out low-temperature heat treatment;
step 3, screening the material subjected to low-temperature heat treatment, and graphitizing;
step 4, carrying out liquid phase coating on the graphitized material and a liquid phase coating agent;
and 5, carbonizing the product obtained in the step 4, and screening and demagnetizing to obtain the graphite cathode material.
It should be noted that: the liquid phase coating agent comprises aluminum fluoride solid powder and a liquid phase solvent, the aluminum fluoride is a common inorganic substance in the market, the liquid phase solvent is a common anthracene oil, cheap organic substances such as coal tar and the like, the material cost is reduced, the process is simple and easy to realize industrialization, the steps are fewer, two substances can be coated on the surface of the graphite, the process is mature, the large-scale mass production is facilitated, the aluminum fluoride coating layer prevents the graphite from being in direct contact with electrolyte, the first irreversible reaction is avoided, the first efficiency and the circulation stability are improved, meanwhile, the aluminum fluoride is introduced, the impedance of the composite material is reduced, the reaction power of the material in the circulation process is improved, lithium ions can be rapidly embedded and detached under a large multiplying power, and the quick charging performance and the high temperature performance of the graphite material can be effectively improved.
In the preparation method of the battery negative electrode material, the graphite raw material is at least one of isotropic petroleum green coke or isosbotto, and the true density of the graphite raw material is 1.28-1.52 g/cm 3 The volatile component is 5-8%, the sulfur content is less than 1%, and the Dv50 of the aggregate formed by grinding the graphite raw material is 4-10 um.
In the preparation method of the battery cathode material, the adhesive is asphalt or resin, the adhesive is ground into 3-7 um Dv50, and the coking value is 13-60%. The adhesive is common medium-medium temperature asphalt, resin and the like, the uniformly mixed materials are subjected to low-temperature heat treatment in a coating kettle, and the treatment temperature is according to a temperature rise curve.
In the preparation method of the battery anode material, in the step 2, the preset ratio is 100: 8-15 Hz, the stirring speed is 5-35 Hz, the temperature rising range is 25-560 ℃, the temperature rising speed is 2-5 ℃/min, wherein the temperature is preserved when the temperature reaches 370 ℃, the temperature preservation time is 70-120 min, the temperature is preserved when the temperature reaches 560 ℃, and the temperature preservation time is 60-90 min.
In the preparation method of the battery cathode material, in the step 3, the material after low-temperature heat treatment is simply screened and then graphitized, wherein the graphitization temperature is 2700-3200 ℃, the graphitization degree is more than 92%, and the graphitization time is 40-60 h.
In the preparation method of the battery negative electrode material, in the step 4, the liquid phase coating agent is formed by mixing aluminum fluoride solid powder and a liquid phase solvent, the liquid phase solvent is at least one of anthracene oil, castor oil and liquid phase resin, and the density of the liquid phase solvent is 0.7-1.7 g/cm 3 And the coking value is 10-40%, wherein the aluminum fluoride is dispersed in the liquid phase coating agent, and the aluminum fluoride can be added into a fusion machine to be coated with graphite after being uniformly dispersed.
In the preparation method of the battery cathode material, in the step 5, the highest temperature of carbonization is 1200 ℃, the cathode graphite material with good charging performance and good high-temperature performance can be obtained after carbonization, the furnace temperature in the carbonization process is increased from room temperature to 1200 ℃ and is higher than the melting point 1040 ℃ of aluminum fluoride, the molten material is infiltrated into amorphous carbon gaps, and the amorphous carbon gaps are solidified in a coating layer after cooling.
In the preparation method of the battery cathode material, in the step 4, the graphitized material and the liquid-phase coating agent are added into a fusion machine according to the proportion of 10-30% for normal-temperature fusion, the rotation speed of the fusion machine is 20-50 Hz, and the fusion time is 3-6 min, so that the co-coating of the organic solvent and the aluminum fluoride can be completed.
In the preparation method of the battery cathode material, in the step 2, the weight ratio of the adhesive is 5-20%, the aggregate and the adhesive are placed in a horizontal kettle to be stirred, and inert gas is introduced.
In the preparation method of the battery cathode material, in the step 3, the product obtained in the step 4 is put into a graphite crucible and then sent into a roller kiln for carbonization.
Example 1
1) Crushing, grinding and grading petroleum green coke to obtain aggregates with Dv50 of 4-10 respectively;
2) adding 8% of medium-temperature asphalt, stirring and dynamically granulating in a horizontal kettle, introducing inert gas into the reaction kettle, and controlling the stirring speed of heat treatment to be 15Hz, the temperature rise range to be 25-560 ℃ and the temperature rise speed to be 2-4 ℃/min, wherein the heat preservation time at 350 ℃ is 70-110 min, and the heat preservation time at 560 ℃ is 60-90 min;
3) screening, putting into a graphite crucible, and graphitizing under the protection of inert gas at the graphitization temperature of 3000 ℃ for 48 h;
4) adding a 10% aluminum fluoride liquid phase solvent into a fusion machine for normal-temperature fusion, wherein the rotation speed is 20-50 Hz, and the fusion time is 3-6 min, so that the organic solvent and aluminum fluoride can be coated together;
5) and (3) putting the fused material into a graphite crucible, then sending the fused material into a roller kiln for carbonization, wherein the highest carbonization temperature is 1200 ℃, and directly screening and demagnetizing the fused material after carbonization to obtain a final product.
Example 2
1) Crushing, grinding and grading petroleum green coke to obtain aggregates with Dv50 of 4-10 respectively;
2) adding 8% medium temperature asphalt, stirring and dynamically granulating in a horizontal kettle, and introducing inert gas into the reaction kettle. The stirring speed of the heat treatment is 15Hz, the temperature rise range is 25-560 ℃, the temperature rise speed is controlled to be 2-4 ℃/min, wherein the heat preservation time at 350 ℃ is 70-110 min, and the heat preservation time at 560 ℃ is 60-90 min;
3) screening, putting into a graphite crucible, and graphitizing under the protection of inert gas at the graphitization temperature of 3000 ℃ for 48 h;
4) adding a fluorinated aluminum liquid phase solvent with the mass ratio of 5% into a fusion machine for normal-temperature fusion, wherein the rotating speed is 20-50 Hz, and the fusion time is 3-6 min, so that the organic solvent and aluminum fluoride can be coated together;
5) and (3) putting the fused material into a graphite crucible, then sending the fused material into a roller kiln for carbonization, wherein the highest carbonization temperature is 1200 ℃, and directly screening and demagnetizing the fused material after carbonization to obtain a final product.
Comparative example 1
1) Crushing, grinding and grading petroleum green coke to obtain aggregates with Dv50 of 4-10 respectively;
2) adding 8% of medium temperature asphalt, stirring and dynamically granulating in a horizontal kettle, and introducing inert gas into the reaction kettle. The stirring speed of the heat treatment is 15Hz, the temperature rise range is 25-560 ℃, the temperature rise speed is controlled to be 2-4 ℃/min, wherein the heat preservation time at 350 ℃ is 70-110 min, and the heat preservation time at 560 ℃ is 60-90 min;
3) screening, putting into a graphite crucible, and graphitizing under the protection of inert gas at the graphitization temperature of 3000 ℃ for 48 h;
4) only adding a liquid phase solvent into a fusion machine for normal temperature fusion, wherein the rotating speed is 20-50 Hz, and the fusion time is 3-6 min;
5) and (3) putting the fused material into a graphite crucible, then sending the fused material into a roller kiln for carbonization, wherein the highest carbonization temperature is 1200 ℃, and directly screening and demagnetizing the fused material after carbonization to obtain a final product.
Manufacturing a lithium ion half battery: the materials of examples 1-2 and comparative example 1 were used as electrode materials, and assembled together with a separator and an electrolyte into a button-type lithium ion half cell in a glove box filled with argon, and gram capacity was tested.
Preparing a lithium ion soft package battery:
1) preparing a positive electrode into a sheet: uniformly mixing lithium cobaltate, conductive carbon and an adhesive (polyvinylidene fluoride) in an N-methyl pyrrolidone solvent according to a mass ratio of 97.6:1.1:1.3 to prepare anode slurry, then coating the anode slurry on an aluminum foil, drying the aluminum foil, and performing cold pressing and sheet cutting to prepare an anode sheet;
2) and (3) preparing a negative electrode: graphite, CMC and SBR prepared in examples 1 and 2 and comparative example 1 are mixed according to a mass ratio of 98: 0.8:1.2, uniformly mixing in deionized water to prepare negative electrode slurry, then coating the negative electrode slurry on a copper foil, drying, and then carrying out cold pressing and cutting to prepare a negative electrode sheet;
3) manufacturing an electric core: the positive plate, the conventional diaphragm and the negative plate are superposed to prepare a laminated battery core, the positive electrode is led out by aluminum tab spot welding, the negative electrode is led out by nickel tab spot welding, then the battery core is placed in an aluminum plastic packaging bag, high-voltage electrolyte is injected, and the battery is prepared by the processes of packaging, formation and capacity grading.
TABLE 1 graphite BET, gram Capacity, and 45 ℃ Cyclic test results for the batteries of examples and comparative examples
As can be seen from table 1, the specific surface areas of the graphite of the batteries prepared in examples 1-2 are larger than those of comparative example 1, i.e., the specific surface area of the graphite is increased with the increase of the amount of the coated aluminum fluoride, because the small particles of aluminum fluoride are attached to the surface of the graphite, the high-temperature cycle performance at 45 ℃ is improved with the increase of the coating amount, the contact between the electrolyte and the graphite can be reduced by the coating layer, the side reaction is reduced, and the high-temperature cycle performance is improved.
TABLE 2 results of the lithium evolution window test on charging at room temperature for the batteries of examples and comparative examples
As can be seen from Table 2, the battery prepared in example 1 has no lithium precipitation, which is superior to that of comparative example 1, namely, the resistance of the composite material coated with aluminum fluoride is reduced, the migration speed of lithium ions is increased, and the charging window is improved.
Table 3, results of hot box test of the batteries of examples and comparative examples
As can be seen from Table 3, the batteries prepared in examples 1-2 have better pass rate in hot box test than that of comparative example 1, namely the SEI structure of the material coated with aluminum fluoride has better stability, and the thermal shock performance is improved
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A preparation method of a battery negative electrode material is characterized by comprising the following steps:
step 1, mixing graphite raw materials, crushing, grinding and grading to obtain aggregate;
step 2, mixing the aggregate and the adhesive according to a preset proportion, and then carrying out low-temperature heat treatment;
step 3, screening the material subjected to low-temperature heat treatment, and graphitizing;
step 4, carrying out liquid phase coating on the graphitized material and a liquid phase coating agent;
and 5, carbonizing the product obtained in the step 4, and screening and demagnetizing to obtain the graphite cathode material.
2. The method for preparing a negative electrode material for a battery according to claim 1, wherein: the graphite raw material is at least one of isotropic petroleum green coke or isotropic petroleum green coke, and the true density of the graphite raw material is 1.28-1.52 g/cm 3 The aggregate contains 5-8% of volatile components and less than 1% of sulfur components, and the Dv50 of the aggregate is 4-10 um.
3. The method for preparing a negative electrode material for a battery according to claim 1, wherein: the adhesive is asphalt or resin, the adhesive is ground into 3-7 um Dv50, and the coking value is 13-60%.
4. The method for preparing a negative electrode material for a battery according to claim 1, wherein: in the step 2, the preset proportion is 100: 8-15, the stirring speed is 5-35 Hz, the temperature rise range is 25-560 ℃, and the temperature rise speed is 2-5 ℃/min.
5. The method for preparing a negative electrode material for a battery according to claim 1, wherein: in the step 3, the graphitization temperature is 2700-3200 ℃, the graphitization degree is more than 92%, and the graphitization time is 40-60 h.
6. The method for preparing the battery negative electrode material according to claim 1, wherein in the step 4, the liquid phase coating agent is formed by mixing aluminum fluoride solid powder and a liquid phase solvent, the liquid phase solvent is at least one of anthracene oil, castor oil and liquid phase resin, and the density of the liquid phase solvent is 0.7-1.7 g/cm 3 The coking value is 10-40%.
7. The method for preparing a negative electrode material for a battery according to claim 1, wherein: in the step 5, the carbonization temperature is 1200 ℃.
8. The method for preparing a battery negative electrode material according to claim 1, wherein in the step 4, the graphitized material and the liquid phase coating agent are added into a fusion machine according to a proportion of 10-30% for normal temperature fusion, the rotation speed of the fusion machine is 20-50 Hz, and the fusion time is 3-6 min.
9. The method for preparing a negative electrode material for a battery according to claim 1, wherein: in the step 2, the weight ratio of the adhesive is 5-20%, the aggregate and the adhesive are placed in a horizontal kettle to be stirred, and inert gas is introduced.
10. The method for preparing a battery negative electrode material according to claim 9, characterized in that: and in the step 3, the product obtained in the step 4 is put into a graphite crucible and then sent into a roller kiln for carbonization.
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