CN112366315A - Production method of lithium battery negative electrode material - Google Patents
Production method of lithium battery negative electrode material Download PDFInfo
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- CN112366315A CN112366315A CN202011372858.2A CN202011372858A CN112366315A CN 112366315 A CN112366315 A CN 112366315A CN 202011372858 A CN202011372858 A CN 202011372858A CN 112366315 A CN112366315 A CN 112366315A
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- negative electrode
- lithium battery
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- electrode material
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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 discloses a method for producing a lithium battery cathode material, which comprises the following steps: s1, grading finished graphite produced by needle coke raw materials or petroleum coke raw materials, and screening out fine artificial graphite powder with the average particle size of 5-40 mu m; s2, adding the screened artificial graphite and the screened asphalt into a powder mixer according to the mass ratio of 2.5: 1-15: 1, and fully mixing for 30-150min under a vacuum condition; s3, taking out the mixed materials, putting the mixed materials into an isostatic press, pressing the materials into a cylinder with the diameter of 5-20cm, and wrapping a layer of resin A on the surface of the cylinder after isostatic pressing; s4, putting the cylinder into a vacuum atmosphere furnace, heating to 550-650 ℃ under the protection of N2, and preserving heat for 0.5-5h for carbonization; s5, placing the carbonized sample beside a high-temperature heat radiation source for carrying out firing tracing graphitization; s6, cleaning impurities on the outer surface of the graphitized sample, scattering and screening to obtain the graphite cathode material of the lithium ion battery. The method is simple, convenient, quick and easy to operate, and can be used for large-scale preparation.
Description
Technical Field
The invention relates to the technical field of lithium battery production, in particular to a production method of a lithium battery negative electrode material.
Background
The cathode material is the key to realizing miniaturization and high capacity of the lithium ion battery. At present, most of the negative electrode materials are carbon materials, and the graphite negative electrode materials have the advantages of high specific capacity, good cycle performance, high intercalation and deintercalation lithium platform voltage, low cost and the like, so that the graphite negative electrode materials become the negative electrode materials of the power lithium ion battery with the most commercial value.
The graphite negative electrode materials are divided into natural graphite and artificial graphite, the artificial graphite is mostly used at present, but the artificial graphite has poor compatibility with electrolyte, and irreversible decomposition of an organic solvent on a carbon negative electrode can generate negative effects on electrode behaviors, so that a graphite layer expands and contracts to cause fracture and peeling of the graphite layer, thereby reducing the cycle efficiency; in the traditional process, the powder obtained by mixing the asphalt powder and the graphite powder is directly put into a graphite crucible for sample carbonization and then graphitized. The process needs to be filled into a specific container to isolate impurities, but wastes a large amount of volume in the mass production process, the container absorbs a large amount of heat in the carbonization and graphitization processes, and a specific graphitization furnace needs to be designed, so that the one-time investment cost is high, and the energy consumption in the graphitization process is high.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a production method of a lithium battery negative electrode material.
The invention provides a production method of a lithium battery cathode material, which comprises the following steps:
s1, grading finished graphite produced by needle coke raw materials or petroleum coke raw materials, and screening out fine artificial graphite powder with the average particle size of 5-40 mu m;
s2, adding the screened artificial graphite and the screened asphalt into a powder mixer according to the mass ratio of 2.5: 1-15: 1, and fully mixing for 30-150min under a vacuum condition;
s3, taking out the mixed materials, putting the mixed materials into an isostatic press, pressing the materials into a cylinder with the diameter of 5-20cm, and wrapping a layer of resin A on the surface of the cylinder after isostatic pressing;
s4, putting the cylinder into a vacuum atmosphere furnace, heating to 550-650 ℃ under the protection of N2, and preserving heat for 0.5-5h for carbonization;
s5, placing the carbonized sample beside a high-temperature heat radiation source for carrying out firing tracing graphitization;
s6, cleaning impurities on the outer surface of the graphitized sample, scattering and screening to obtain the graphite cathode material of the lithium ion battery.
In the step S2, the mass ratio of the artificial graphite to the asphalt is preferably 4: 1-12: 1; the mixing time is 90-150 min.
Preferably, the bulk density of the cylindrical sample pressed in the step S3 is 0.5-2.0g/cm 3.
Preferably, the resin a used in step S3 is one or more of phenolic resin, furan resin, epoxy resin, polyester resin, polyvinyl chloride resin, and the like.
Preferably, the thickness of the surface layer coating resin A of the sample of the step S3 is 0.1mm-8mm, and more preferably, the thickness is 1-3 mm.
Preferably, the temperature raising rate of the step S4 is 5-15 ℃/min to 550-650 ℃, more preferably, the temperature range is 580-620 ℃, and the heat preservation time is 0.5-1.5 h.
Preferably, the high-temperature thermal radiation source of step S5 can provide a burning graphitization temperature of 2600-.
Preferably, the coal tar pitch of step S2 has an average particle diameter of 5 to 8 μm and a softening point of 100 to 300 ℃.
The invention has the technical effects that:
the method presses the powdery raw materials into a column shape, eliminates a crucible container, is convenient to carry and place, fully utilizes a high-temperature heat radiation source, saves a large amount of energy, has the characteristics of simplicity, convenience, quickness and easy operation, and can be used for large-scale preparation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A preparation method of a lithium battery negative electrode material comprises the following steps: adding 5 parts of asphalt and 30 parts of artificial graphite into a powder mixer, fully mixing for 90min under a vacuum condition, taking out the mixed material, putting the mixed material into an isostatic press, pressing the mixed material into a column with the diameter of 10cm, wrapping a layer of phenolic resin on the surface of a pressed sample, putting the sample into a vacuum atmosphere furnace, protecting the furnace by N2, heating to 600 ℃, keeping the temperature for 1h, cooling the sample, putting the cooled sample into an inner series graphitization furnace for co-firing, taking out the sample after the graphitization is finished, cleaning impurities on the outer surface, crushing by using a crusher, grinding by using a grinding machine, and sieving the material by using a 200-mesh sieve to obtain the graphite; the raw materials are in parts by weight.
Example 2
A preparation method of a lithium battery negative electrode material comprises the following steps: adding 4 parts of asphalt and 36 parts of artificial graphite into a powder mixer, fully mixing for 90min under a vacuum condition, taking out the mixed material, putting the mixed material into an isostatic press, pressing the mixed material into a column with the diameter of 10cm, wrapping a layer of phenolic resin on the surface of a pressed sample, putting the sample into a vacuum atmosphere furnace, protecting the furnace by N2, heating to 600 ℃, keeping the temperature for 1h, cooling the sample, putting the cooled sample into an inner series graphitization furnace for co-firing, taking out the sample after the graphitization is finished, cleaning impurities on the outer surface, crushing by using a crusher, grinding by using a grinding machine, and sieving the material by using a 200-mesh sieve to obtain the graphite; the raw materials are in parts by weight.
Example 3
A preparation method of a lithium battery negative electrode material comprises the following steps: adding 4 parts of asphalt and 36 parts of artificial graphite into a powder mixer, fully mixing for 120min under a vacuum condition, taking out the mixed material, putting the mixed material into an isostatic press, pressing the mixed material into a column with the diameter of 10cm, wrapping a layer of phenolic resin on the surface of a pressed sample, putting the sample into a vacuum atmosphere furnace, protecting the furnace by N2, heating to 600 ℃, keeping the temperature for 1h, cooling the sample, putting the cooled sample into an inner series graphitization furnace for co-firing, taking out the sample after the graphitization is finished, cleaning impurities on the outer surface, crushing by using a crusher, grinding by using a grinding machine, and sieving the material by using a 200-mesh sieve to obtain the graphite; the raw materials are in parts by weight.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A method for producing a negative electrode material of a lithium battery is characterized by comprising the following steps:
s1, grading finished graphite produced by needle coke raw materials or petroleum coke raw materials, and screening out fine artificial graphite powder with the average particle size of 5-40 mu m;
s2, adding the screened artificial graphite and the screened asphalt into a powder mixer according to the mass ratio of 2.5: 1-15: 1, and fully mixing for 30-150min under a vacuum condition;
s3, taking out the mixed materials, putting the mixed materials into an isostatic press, pressing the materials into a cylinder with the diameter of 5-20cm, and wrapping a layer of resin A on the surface of the cylinder after isostatic pressing;
s4, putting the cylinder into a vacuum atmosphere furnace, heating to 550-650 ℃ under the protection of N2, and preserving heat for 0.5-5h for carbonization;
s5, placing the carbonized sample beside a high-temperature heat radiation source for carrying out firing tracing graphitization;
s6, cleaning impurities on the outer surface of the graphitized sample, scattering and screening to obtain the graphite cathode material of the lithium ion battery.
2. The method for producing the negative electrode material of the lithium battery as claimed in claim 1, wherein in the step S2, the mass ratio of the artificial graphite to the asphalt is preferably 4: 1-12: 1; the mixing time is 90-150 min.
3. The method for producing a negative electrode material for a lithium battery as claimed in claim 1, wherein the bulk density of the cylindrical sample pressed in step S3 is 0.5-2.0g/cm 3.
4. The method for producing a negative electrode material for a lithium battery as claimed in claim 1, wherein the resin a used in step S3 is one or more of phenolic resin, furan resin, epoxy resin, polyester resin, polyvinyl chloride resin, and the like.
5. The method for producing a negative electrode material for a lithium battery as claimed in claim 1, wherein the thickness of the coating resin A on the surface of the sample obtained in step S3 is 0.1mm to 8mm, preferably 1mm to 3 mm.
6. The method as claimed in claim 1, wherein the temperature rise rate of step S4 is 5-15 ℃/min to 550-650 ℃, preferably 580-620 ℃, and the temperature holding time is 0.5-1.5 h.
7. The method as claimed in claim 1, wherein the high temperature thermal radiation source of step S5 is capable of providing a burning graphitization temperature of 2600 ℃ 3200 ℃.
8. The method for producing a negative electrode material for a lithium battery as claimed in claim 1, wherein the coal pitch of step S2 has an average particle size of 5 to 8 μm and a softening point of 100 to 300 ℃.
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| CN202011372858.2A CN112366315A (en) | 2020-11-30 | 2020-11-30 | Production method of lithium battery negative electrode material |
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| CN202011372858.2A CN112366315A (en) | 2020-11-30 | 2020-11-30 | Production method of lithium battery negative electrode material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113437321A (en) * | 2021-06-28 | 2021-09-24 | 开封平煤新型炭材料科技有限公司 | Method for preparing graphite composite bipolar plate by continuous molding |
| CN115849363A (en) * | 2022-12-01 | 2023-03-28 | 青岛瀚博电子科技有限公司 | Method for processing cathode material by using inner-string graphitization furnace |
| CN116835579A (en) * | 2023-06-17 | 2023-10-03 | 江苏宏基高新材料股份有限公司 | Large-specification isostatic pressing graphite production process |
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| CN115849363A (en) * | 2022-12-01 | 2023-03-28 | 青岛瀚博电子科技有限公司 | Method for processing cathode material by using inner-string graphitization furnace |
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Effective date of registration: 20210803 Address after: 475000 Dong Jiao Bian Cun, Shunhe District, Kaifeng City, Henan Province Applicant after: Kaifeng Pingmei new carbon material technology Co.,Ltd. Address before: 475000 Dongjiao Xiangbian village, Shunhe District, Kaifeng City, Henan Province Applicant before: Henan Kaitan new material design and Research Institute Co.,Ltd. |
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