CN112952070A - Graphite lithium battery negative electrode material and preparation method thereof - Google Patents
Graphite lithium battery negative electrode material and preparation method thereof Download PDFInfo
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- CN112952070A CN112952070A CN202110378107.XA CN202110378107A CN112952070A CN 112952070 A CN112952070 A CN 112952070A CN 202110378107 A CN202110378107 A CN 202110378107A CN 112952070 A CN112952070 A CN 112952070A
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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
- 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
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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
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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
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Abstract
The invention relates to the technical field of processing of negative electrode materials, and discloses a preparation method of a negative electrode material of a graphite lithium battery, which comprises the following steps: carrying out spheroidization on natural graphite to obtain spherical graphite; uniformly coating a compound containing a metal element on the surface of the spherical graphite, and carrying out heat treatment to obtain porous spherical graphite; adding porous spherical graphite and a binder into a stirring kettle, mixing and stirring, adding the obtained mixture into a carbonization furnace, introducing inert gas and carrying out carbonization treatment; scattering, screening and demagnetizing the carbonized product to obtain a graphite negative electrode material; the natural graphite material prepared by the invention has a complete coating shell, can effectively protect the internal graphite from being eroded by external electrolyte, and meanwhile, the heat treatment pore-forming work is carried out before coating, so that more pores are formed on the surface of the spherical graphite, the capacitance of the graphite cathode is improved, the process flow is simple, the condition is controllable, the production cost is effectively reduced, and the industrial production is more facilitated.
Description
Technical Field
The invention relates to the technical field of lithium battery negative electrode material processing, in particular to a graphite lithium battery negative electrode material and a preparation method thereof.
Background
The lithium ion battery has the advantages of high working voltage, high energy density, high charging and discharging efficiency, no memory effect, small self-discharge, greenness, no pollution and the like, and is considered as the most ideal energy source in the 21 st century;
the preparation method mainly comprises the steps of fully mixing graphite and a coating material, carrying out heat treatment under the protection of inert atmosphere, carrying out heat preservation for 0.5-6 hours, cooling, and carrying out secondary high-temperature graphitization treatment under the protection of inert atmosphere;
according to the preparation method, after the mixing and graphitization treatment are finished, the crushing and screening are carried out, so that the surface coating of the negative electrode material is incomplete, the subsequent use effect is influenced, and the use is inconvenient.
Disclosure of Invention
In order to meet the edible requirement of consumers at any time and any place, the invention provides a graphite lithium battery cathode material and a preparation method thereof, and solves the problems of incomplete coating and low later-stage use performance of the existing preparation process.
In order to meet the requirements, the invention adopts the following technical scheme: a preparation method of a negative electrode material of a graphite lithium battery comprises the following steps:
s1, shaping: carrying out spheroidization on natural graphite to obtain spherical graphite;
s2, pore forming: uniformly coating a compound containing a metal element on the surface of the spherical graphite to obtain a compound, and carrying out heat treatment on the compound in an oxygen-containing atmosphere to obtain porous spherical graphite;
s3, mixing: adding the porous spherical graphite obtained in the step S2 and a binder into a stirring kettle, and mixing and stirring to obtain a mixture;
s4, carbonization: adding the mixture obtained in the step S3 into a carbonization furnace, introducing inert gas and carrying out carbonization treatment to obtain a carbonized product;
s5: finishing: and scattering, screening and demagnetizing the carbonized product obtained in the step S4 to obtain the graphite negative electrode material.
Preferably, the binder is any one of asphalt, phenolic resin and epoxy resin.
Preferably, the heat treatment temperature in step S2 is 450-480 ℃, and the heat treatment time is 5-40 h.
Preferably, the weight ratio of the porous spherical graphite to the binder in the step S3 is 1: 0.06-0.25.
Preferably, the stirring time in step S3 is 60 to 80 min.
Preferably, the carbonization roasting temperature in the step S4 is 900-1200 ℃.
Preferably, the inert gas in step S4 is any one of nitrogen, argon, neon and helium.
Preferably, the oxygen-containing atmosphere in step S2 is composed of a mixed gas containing oxygen, and the oxygen-containing atmosphere may be air.
The negative electrode material of the graphite lithium battery is prepared by the preparation method of the negative electrode material of the graphite lithium battery.
Preferably, the average particle size of the graphite negative electrode material is 15-45 mu m, and the compaction density is 0.9-1.1 g/cm3。
The invention has the beneficial effects that:
the natural graphite material prepared by the invention has a complete coating shell, is uniformly coated, can effectively protect the internal graphite from being eroded by external electrolyte, and meanwhile, the heat treatment pore-forming work is carried out before coating, so that more pores are formed on the surface of the spherical graphite, the entry passing rate of lithium ions is increased, and the electric capacity of the graphite cathode is improved.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention is further described below with reference to specific embodiments:
example 1
A preparation method of a negative electrode material of a graphite lithium battery comprises the following steps:
s1, shaping: carrying out spheroidization on natural graphite to obtain spherical graphite;
s2, pore forming: uniformly coating a compound containing a metal element on the surface of the spherical graphite to obtain a compound, and carrying out heat treatment on the compound in an oxygen-containing atmosphere, wherein the heat treatment temperature is 450 ℃ and the heat treatment time is 5 hours to obtain porous spherical graphite;
s3, mixing: adding the porous spherical graphite obtained in the step S2 and asphalt into a stirring kettle, and mixing and stirring the mixture, wherein the weight ratio of the porous spherical graphite to the binder is 1:0.06, and the stirring time is 60min to obtain a mixture;
s4, carbonization: adding the mixture obtained in the step S3 into a carbonization furnace, introducing nitrogen and carrying out carbonization treatment, wherein the carbonization roasting temperature is 900 ℃, and obtaining a carbonized product;
s5: finishing: and scattering, screening and demagnetizing the carbonized product obtained in the step S4 to obtain the graphite negative electrode material.
The graphite negative electrode material had an average particle diameter of 15 μm and a compacted density of 0.9g/cm3。
Example 2
A preparation method of a negative electrode material of a graphite lithium battery comprises the following steps:
s1, shaping: carrying out spheroidization on natural graphite to obtain spherical graphite;
s2, pore forming: uniformly coating a compound containing a metal element on the surface of the spherical graphite to obtain a compound, and carrying out heat treatment on the compound in an oxygen-containing atmosphere, wherein the heat treatment temperature is 465 ℃, and the heat treatment time is 20 hours to obtain porous spherical graphite;
s3, mixing: adding the porous spherical graphite obtained in the step S2 and asphalt into a stirring kettle, and mixing and stirring the mixture, wherein the weight ratio of the porous spherical graphite to the binder is 1:0.15, and the stirring time is 70min to obtain a mixture;
s4, carbonization: adding the mixture obtained in the step S3 into a carbonization furnace, introducing nitrogen and carrying out carbonization treatment, wherein the carbonization roasting temperature is 1100 ℃, and obtaining a carbonized product;
s5: finishing: and scattering, screening and demagnetizing the carbonized product obtained in the step S4 to obtain the graphite negative electrode material.
The graphite negative electrode material had an average particle diameter of 30 μm and a compacted density of 1g/cm3。
Example 3
A preparation method of a negative electrode material of a graphite lithium battery comprises the following steps:
s1, shaping: carrying out spheroidization on natural graphite to obtain spherical graphite;
s2, pore forming: uniformly coating a compound containing a metal element on the surface of the spherical graphite to obtain a compound, and carrying out heat treatment on the compound in an oxygen-containing atmosphere, wherein the heat treatment temperature is 480 ℃, and the heat treatment time is 40 hours to obtain porous spherical graphite;
s3, mixing: adding the porous spherical graphite obtained in the step S2 and asphalt into a stirring kettle, and mixing and stirring the mixture, wherein the weight ratio of the porous spherical graphite to the binder is 1:0.25, and the stirring time is 80min to obtain a mixture;
s4, carbonization: adding the mixture obtained in the step S3 into a carbonization furnace, introducing nitrogen and carrying out carbonization treatment, wherein the carbonization roasting temperature is 1200 ℃, and obtaining a carbonized product;
s5: finishing: and scattering, screening and demagnetizing the carbonized product obtained in the step S4 to obtain the graphite negative electrode material.
The graphite negative electrode material had an average particle diameter of 45 μm and a compacted density of 1.1g/cm3。
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A preparation method of a negative electrode material of a graphite lithium battery is characterized by comprising the following steps:
s1, shaping: carrying out spheroidization on natural graphite to obtain spherical graphite;
s2, pore forming: uniformly coating a compound containing a metal element on the surface of the spherical graphite to obtain a compound, and carrying out heat treatment on the compound in an oxygen-containing atmosphere to obtain porous spherical graphite;
s3, mixing: adding the porous spherical graphite obtained in the step S2 and a binder into a stirring kettle, and mixing and stirring to obtain a mixture;
s4, carbonization: adding the mixture obtained in the step S3 into a carbonization furnace, introducing inert gas and carrying out carbonization treatment to obtain a carbonized product;
s5: finishing: and scattering, screening and demagnetizing the carbonized product obtained in the step S4 to obtain the graphite negative electrode material.
2. The method for preparing the negative electrode material of the graphite lithium battery as claimed in claim 1, wherein the binder is any one of asphalt, phenolic resin and epoxy resin.
3. The method for preparing the negative electrode material for the lithium graphite battery as claimed in claim 1, wherein the heat treatment temperature in step S2 is 450-480 ℃ and the heat treatment time is 5-40 h.
4. The method for preparing the negative electrode material of the lithium graphite battery as claimed in claim 1, wherein the weight ratio of the porous spherical graphite to the binder in the step S3 is 1: 0.06-0.25.
5. The method for preparing the negative electrode material for the lithium graphite battery as claimed in claim 1, wherein the stirring time in the step S3 is 60-80 min.
6. The method for preparing the negative electrode material for the lithium graphite battery as claimed in claim 1, wherein the carbonization roasting temperature in step S4 is 900-1200 ℃.
7. The method as claimed in claim 1, wherein the inert gas in step S4 is any one of nitrogen, argon, neon and helium.
8. The method as claimed in claim 1, wherein the oxygen-containing atmosphere in step S2 is composed of a mixed gas containing oxygen.
9. A negative electrode material for a graphite lithium battery, which is characterized by being prepared by the preparation method of the negative electrode material for the graphite lithium battery as claimed in any one of claims 1 to 7.
10. The negative electrode material for a graphite lithium battery as claimed in claim 9, wherein the average particle diameter of the negative electrode material is 15 to 45 μm, and the compacted density is 0.9 to 1.1g/cm3。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115911311A (en) * | 2022-11-16 | 2023-04-04 | 晖阳(贵州)新能源材料有限公司 | Quick-charging graphite composite material for lithium ion battery and preparation method thereof |
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| CN103943860A (en) * | 2014-04-25 | 2014-07-23 | 焦作聚能能源科技有限公司 | Negative pole material for lithium ion power and energy storage battery, as well as preparation method and battery thereof |
| CN104766954A (en) * | 2015-04-24 | 2015-07-08 | 田东 | Method for recycling artificial graphite fine powder as negative pole material |
| CN107069015A (en) * | 2015-05-22 | 2017-08-18 | 许婷 | A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material |
| CN107305949A (en) * | 2016-04-25 | 2017-10-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of porous graphite negative material and preparation method and application |
| CN109950495A (en) * | 2019-03-27 | 2019-06-28 | 溧阳紫宸新材料科技有限公司 | Preparation method, negative electrode material and the lithium ion battery of high magnification graphite cathode material |
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- 2021-04-08 CN CN202110378107.XA patent/CN112952070A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103943860A (en) * | 2014-04-25 | 2014-07-23 | 焦作聚能能源科技有限公司 | Negative pole material for lithium ion power and energy storage battery, as well as preparation method and battery thereof |
| CN104766954A (en) * | 2015-04-24 | 2015-07-08 | 田东 | Method for recycling artificial graphite fine powder as negative pole material |
| CN107069015A (en) * | 2015-05-22 | 2017-08-18 | 许婷 | A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material |
| CN107305949A (en) * | 2016-04-25 | 2017-10-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of porous graphite negative material and preparation method and application |
| CN109950495A (en) * | 2019-03-27 | 2019-06-28 | 溧阳紫宸新材料科技有限公司 | Preparation method, negative electrode material and the lithium ion battery of high magnification graphite cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115911311A (en) * | 2022-11-16 | 2023-04-04 | 晖阳(贵州)新能源材料有限公司 | Quick-charging graphite composite material for lithium ion battery and preparation method thereof |
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