CN111933898A - High-performance graphite negative electrode material for lithium ion battery, and preparation method and application thereof - Google Patents
High-performance graphite negative electrode material for lithium ion battery, and preparation method and application thereof Download PDFInfo
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- CN111933898A CN111933898A CN202010535363.0A CN202010535363A CN111933898A CN 111933898 A CN111933898 A CN 111933898A CN 202010535363 A CN202010535363 A CN 202010535363A CN 111933898 A CN111933898 A CN 111933898A
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/625—Carbon or graphite
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- 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 graphite cathode materials, and particularly relates to a high-performance graphite cathode material for a lithium ion battery, and a preparation method and application thereof. The high-performance graphite cathode material is prepared by crushing graphite powder, mixing the crushed graphite powder with a coating material, and sieving and demagnetizing the mixture after final forming. The preparation method has the advantages of simple and effective preparation process of the graphite cathode material, energy-saving and efficient process operation, good structural stability and isotropy of the coating layer of the prepared graphite cathode material, high lithium ion intercalation and deintercalation efficiency, and prominent rate performance and cycle performance.
Description
Technical Field
The invention belongs to the technical field of graphite cathode materials, and particularly relates to a high-performance graphite cathode material for a lithium ion battery, and a preparation method and application thereof.
Background
The graphite material is the main material of the lithium ion battery cathode at present, and the graphite material is divided into natural graphite and artificial graphite, the latter has relatively high price, and the former is not considered for the time, but the former has the problems of different particle sizes, more surface defects and poor compatibility with electrolyte, if the natural graphite is directly prepared into the lithium ion battery cathode, the capacity is reduced, the cycle life is short, so that a composite graphite material is urgently needed in the market to prepare the lithium ion battery cathode so as to achieve relatively high rate performance and cycle performance.
The Chinese patent with patent publication number CN 110707314A and publication number 2020.01.17 discloses a silicon-carbon composite lithium ion battery cathode material and a preparation method thereof, and the preparation method comprises the following steps: adding micron silicon and a dispersing agent into a solvent, and grinding to obtain nano silicon slurry 1; adding a carbon matrix into the nano silicon slurry 1, and stirring to obtain a mixed slurry 2; wherein the carbon matrix is one or more of flattened artificial graphite, flattened natural graphite and flattened mesocarbon microbeads; and drying the mixed slurry 2, adding the mixed slurry into a fusion machine for fusion, mixing the mixed slurry with a coating agent, granulating, placing the mixture in a protective atmosphere for heat treatment, placing the mixture in the protective atmosphere for high-temperature carbonization, crushing, grading and demagnetizing to obtain the silicon-carbon composite negative electrode material.
However, the lithium ion battery cathode material in the patent of the invention has the problem of poor comprehensive performance.
Disclosure of Invention
The invention aims to provide a high-performance graphite cathode material for a lithium ion battery, and a preparation method and application thereof. The preparation method has the advantages of simple and effective preparation process of the graphite cathode material, energy-saving and efficient process operation, good structural stability and isotropy of the coating layer of the prepared graphite cathode material, high lithium ion intercalation and deintercalation efficiency, and prominent rate performance and cycle performance.
The technical scheme adopted by the invention for solving the problems is as follows: a high-performance graphite cathode material for a lithium ion battery comprises porous graphite powder and a coating layer positioned on the surface of the porous graphite powder, wherein the median particle size of the porous graphite powder is 16-19 mu m, and the compaction density is more than or equal to 1.4g/cm3The first capacity of the graphite cathode material is more than or equal to 353mAh/g, and the first efficiency is more than or equal to 91%.
In the invention, the particle size range of the porous graphite powder is 12-25 μm, the stability of the whole specification is ensured, and the efficiency of the graphite cathode material is more than or equal to 87% after the graphite cathode material is used for 1000 times, which is much higher than that of the prior art, and the advantage of outstanding cycle performance of the graphite cathode material in the invention is reflected.
The further preferred technical scheme is as follows: the porosity of the porous graphite powder is 35-38%, the material of the coating layer comprises petroleum asphalt or coal asphalt, and the thickness of the coating layer is 0.5-1.2 mu m.
In the invention, the coating layer is used for covering various irregular defects on the porous graphite powder so as to further improve the electrochemical performance of the graphite cathode material, such as isotropy, and the characteristic of high porosity of the porous graphite powder is the basis of high capacity and high density of the graphite material.
A preparation method of a high-performance graphite negative electrode material for a lithium ion battery sequentially comprises the following steps:
s1, coarsely crushing the porous graphite powder raw material to obtain qualified porous graphite powder;
s2, mixing the coating raw materials to obtain a coating material;
s3, mixing the porous graphite powder with the coating material to obtain a graphite cathode crude material;
and S4, carrying out screening and demagnetizing operation on the graphite cathode coarse material to obtain the final graphite cathode material.
In step S1 of the present invention, the porous graphite powder is high-quality spherical graphite powder with relatively high compaction density and relatively high porosity, and the coarse crushing operation is performed by using an existing ball mill crusher according to an existing crushing process.
The further preferred technical scheme is as follows: in step S2, the coating layer raw materials include an asphalt base material, a main binder, a binder curing agent, a non-metal oxide filler, a hollow glass microsphere aggregate, a wetting dispersant, and a non-metal coating material.
The further preferred technical scheme is as follows: the asphalt base material is any one of petroleum asphalt or coal asphalt, the main binder is any one or a mixture of phenolic resin, epoxy resin and acrylic resin, the binder curing agent is any one or a mixture of polyisocyanate and phthalic anhydride, the non-metal oxide filler is nano silicon dioxide, the wetting dispersant is isobutylene maleic anhydride copolymer, and the non-metal coating material is nano silicon powder.
In the invention, the asphalt is a main material of the coating layer and is used for forming an amorphous carbon layer to be attached to the surface of the graphite and reducing the active end surface of the graphite material, so that the compatibility of the graphite and an electrolyte is improved, and the main binder and the binder curing agent are used for further enhancing the connection strength of the amorphous carbon layer and graphite powder and avoiding the problem that the amorphous carbon layer is easy to fall off.
In addition, the non-metal oxide filler is used for reinforcing the strength of the coating layer and avoiding the problem of self collapse, the hollow glass microsphere aggregate is used for reinforcing the impact resistance of the coating layer and ensuring the stable and regular appearance of the hollow glass microsphere aggregate during molding, and finally the non-metal coating is uniformly dispersed into the coating layer mainly through high heat resistance and high hardness of the non-metal coating to form a supporting framework.
The further preferred technical scheme is as follows: the coating layer comprises the following raw materials in parts by weight:
45-55 parts of petroleum asphalt,
25-32 parts of epoxy resin,
3-5 parts of phthalic anhydride,
1-2 parts of nano silicon dioxide
1-3 parts of hollow glass microsphere
0.2-0.3 part of isobutylene maleic anhydride copolymer
1-1.5 parts of nano silicon powder.
The further preferred technical scheme is as follows: the isobutylene maleic anhydride copolymer is polycarbonate grafted isobutylene maleic anhydride copolymer, the grafting rate is 1.22-1.35%, the grafting is performed by adopting a molten nitrogen protection method, the melting temperature is 320-440 ℃, the nitrogen introducing time is more than or equal to 15min, and the grafting pressure is 0.5-5.0 bar.
Compared with the common isobutylene maleic anhydride copolymer, the isobutylene maleic anhydride copolymer grafted by the polycarbonate has the advantage of better heat resistance, and the grafting rate can be further improved by a nitrogen protection and high-temperature high-pressure melt grafting mode, wherein the grafting rate of the polycarbonate is 1.22-1.35%, which is far higher than that of polycarbonate in the prior art, which is 0.6-0.8%.
The further preferred technical scheme is as follows: in step S3, the porous graphite powder and the coating material are mixed in a heat treatment reaction kettle, the mixing temperature is 600-920 ℃ and the mixing pressure is 1.2-1.5bar, the mixing time is 5-12h, the heat preservation temperature is 500-800 ℃ and the heat preservation time is 4-6h, and the whole process is mixed under the protection of nitrogen.
The further preferred technical scheme is as follows: in step S4, the sieving and demagnetizing operation is performed by a vibrating screen of 600-800 mesh.
The application of the high-performance graphite negative electrode material for the lithium ion battery is to load the graphite negative electrode material on a negative electrode current collector to prepare the negative electrode of the lithium ion battery.
The high-performance graphite cathode material is prepared by crushing graphite powder, mixing the crushed graphite powder with a coating material, and sieving and demagnetizing the mixture after final forming. The preparation method has the advantages of simple and effective preparation process of the graphite cathode material, energy-saving and efficient process operation, good structural stability and isotropy of the coating layer of the prepared graphite cathode material, high lithium ion intercalation and deintercalation efficiency, and prominent rate performance and cycle performance.
Detailed Description
The following description is only a preferred embodiment of the present invention and is not intended to limit the scope of the present invention.
Example 1
A preparation method of a high-performance graphite negative electrode material for a lithium ion battery sequentially comprises the following steps:
s1, coarsely crushing the porous graphite powder raw material to obtain qualified porous graphite powder;
s2, mixing the coating raw materials to obtain a coating material;
s3, mixing the porous graphite powder with the coating material to obtain a graphite cathode crude material;
and S4, carrying out screening and demagnetizing operation on the graphite cathode coarse material to obtain the final graphite cathode material.
In step S2, the coating layer raw materials include an asphalt base material, a main binder, a binder curing agent, a non-metal oxide filler, a hollow glass microsphere aggregate, a wetting dispersant, and a non-metal coating material.
The asphalt base material is petroleum asphalt, the main binder is epoxy resin, the binder curing agent is phthalic anhydride, the non-metal oxide filler is nano silicon dioxide, the wetting dispersant is polycarbonate grafted isobutylene maleic anhydride copolymer, and the non-metal coating material is nano silicon powder.
The coating layer comprises the following raw materials in parts by weight:
45 portions of petroleum asphalt,
26 parts of epoxy resin,
4 parts of phthalic anhydride,
1 part of nano silicon dioxide
Hollow glass microsphere 2 parts
0.2 part of polycarbonate grafted isobutylene maleic anhydride copolymer
And 1.5 parts of nano silicon powder.
The grafting rate of the polycarbonate grafted isobutylene maleic anhydride copolymer is 1.30%, the copolymer is grafted by adopting a molten nitrogen protection method, the melting temperature is 360 ℃, the nitrogen introduction time is 18min, and the grafting pressure is 1.5 bar.
In step S3, the porous graphite powder and the coating material are mixed in a heat treatment reactor at a mixing temperature of 600 ℃, a mixing pressure of 1.3bar, a mixing time of 6 hours, a heat preservation temperature of 560 ℃, a heat preservation time of 4 hours, and the whole process is mixed under the protection of nitrogen.
In step S4, the sieving is performed by a 600-mesh vibrating screen in the sieving demagnetization operation.
The high-performance graphite cathode material for the lithium ion battery prepared by the method structurally comprises porous graphite powder and a coating layer positioned on the surface of the porous graphite powder, wherein the median particle size of the porous graphite powder is 16 mu m, and the compacted density is 1.5g/cm3The first capacity of the graphite negative electrode material is 365mAh/g, and the first efficiency is 93%.
The porosity of the porous graphite powder is 35%, the material of the coating layer comprises petroleum asphalt or coal asphalt, the thickness of the coating layer is 0.5 mu m, the efficiency after the coating layer is finally used for 1000 times is 88%, and the graphite cathode material has the advantages of large compaction density, large capacity and high efficiency.
The application of the high-performance graphite negative electrode material for the lithium ion battery is to load the graphite negative electrode material on a negative electrode current collector to prepare the negative electrode of the lithium ion battery.
In this embodiment. The graphite negative electrode material is loaded on a negative electrode current collector by the conventional process of the negative electrode of the lithium ion battery, so that the basic use effect of a negative electrode product is realized.
Example 2
A preparation method of a high-performance graphite negative electrode material for a lithium ion battery sequentially comprises the following steps:
s1, coarsely crushing the porous graphite powder raw material to obtain qualified porous graphite powder;
s2, mixing the coating raw materials to obtain a coating material;
s3, mixing the porous graphite powder with the coating material to obtain a graphite cathode crude material;
and S4, carrying out screening and demagnetizing operation on the graphite cathode coarse material to obtain the final graphite cathode material.
In step S2, the coating layer raw materials include an asphalt base material, a main binder, a binder curing agent, a non-metal oxide filler, a hollow glass microsphere aggregate, a wetting dispersant, and a non-metal coating material.
The asphalt base material is coal asphalt, the main binder is phenolic resin, the binder curing agent is polyisocyanate, the non-metal oxide filler is nano silicon dioxide, the wetting dispersant is polycarbonate grafted isobutylene maleic anhydride copolymer, and the non-metal coating material is nano silicon powder.
The coating layer comprises the following raw materials in parts by weight:
49 parts of coal tar pitch,
30 portions of phenolic resin,
5 parts of polyisocyanate,
1 part of nano silicon dioxide
Hollow glass microsphere 2 parts
0.2 part of polycarbonate grafted isobutylene maleic anhydride copolymer
And 1.5 parts of nano silicon powder.
The grafting rate of the polycarbonate grafted isobutylene maleic anhydride copolymer is 1.32%, the copolymer is grafted by adopting a molten nitrogen protection method, the melting temperature is 440 ℃, the nitrogen introduction time is 18min, and the grafting pressure is 2.2 bar.
In step S3, the porous graphite powder and the coating material are mixed in a heat treatment reactor at a mixing temperature of 800 ℃, a mixing pressure of 1.4bar, a mixing time of 12 hours, a heat preservation temperature of 710 ℃, a heat preservation time of 4 hours, and the whole process is mixed under the protection of nitrogen.
In step S4, the sieving is performed by a vibrating screen of 800 mesh in the sieving demagnetization operation.
The high-performance graphite cathode material for the lithium ion battery prepared by the method structurally comprises porous graphite powder and a coating layer positioned on the surface of the porous graphite powder, wherein the median particle size of the porous graphite powder is 17 mu m, and the compacted density is 1.6g/cm3The first capacity of the graphite negative electrode material is 362mAh/g, and the first efficiency is 92%.
The porosity of the porous graphite powder is 35%, the material of the coating layer comprises petroleum asphalt or coal asphalt, the thickness of the coating layer is 0.5 mu m, the efficiency after 1000 times of final use is 89%, and the graphite cathode material has the advantages of large compaction density, large capacity and high efficiency.
The application of the high-performance graphite negative electrode material for the lithium ion battery is to load the graphite negative electrode material on a negative electrode current collector to prepare the negative electrode of the lithium ion battery.
Example 3
A preparation method of a high-performance graphite negative electrode material for a lithium ion battery sequentially comprises the following steps:
s1, coarsely crushing the porous graphite powder raw material to obtain qualified porous graphite powder;
s2, mixing the coating raw materials to obtain a coating material;
s3, mixing the porous graphite powder with the coating material to obtain a graphite cathode crude material;
and S4, carrying out screening and demagnetizing operation on the graphite cathode coarse material to obtain the final graphite cathode material.
In step S2, the coating layer raw materials include an asphalt base material, a main binder, a binder curing agent, a non-metal oxide filler, a hollow glass microsphere aggregate, a wetting dispersant, and a non-metal coating material.
The asphalt base material is coal asphalt, the main binder is acrylic resin, the binder curing agent is polyisocyanate, the non-metal oxide filler is nano silicon dioxide, the wetting dispersant is polycarbonate grafted isobutylene maleic anhydride copolymer, and the non-metal coating material is nano silicon powder.
The coating layer comprises the following raw materials in parts by weight:
52 portions of coal tar pitch,
31 parts of acrylic resin,
3 parts of polyisocyanate,
1 part of nano silicon dioxide
Hollow glass microsphere 3 parts
0.3 part of polycarbonate grafted isobutylene maleic anhydride copolymer
And 1.5 parts of nano silicon powder.
The grafting rate of the polycarbonate grafted isobutylene maleic anhydride copolymer is 1.26%, the copolymer is grafted by adopting a molten nitrogen protection method, the melting temperature is 420 ℃, the nitrogen introduction time is 18min, and the grafting pressure is 3.1 bar.
In step S3, the porous graphite powder and the coating material are mixed in a heat treatment reactor at a mixing temperature of 900 ℃, a mixing pressure of 1.4bar, a mixing time of 11 hours, a heat preservation temperature of 690 ℃, a heat preservation time of 6 hours, and the whole process is mixed under the protection of nitrogen.
In step S4, the sieving is performed by a vibrating screen of 800 mesh in the sieving demagnetization operation.
The high-performance graphite cathode material for the lithium ion battery prepared by the method structurally comprises porous graphite powder and a coating layer positioned on the surface of the porous graphite powder, wherein the median particle size of the porous graphite powder is 18 mu m, and the compacted density is 1.6g/cm3The first capacity of the graphite negative electrode material is 365mAh/g, and the first efficiency is 92%.
The porosity of the porous graphite powder is 35%, the material of the coating layer comprises petroleum asphalt or coal asphalt, the thickness of the coating layer is 0.9 mu m, the efficiency after the coating layer is used for 1000 times is 90%, and the graphite cathode material has the advantages of large compaction density, large capacity and high efficiency.
The application of the high-performance graphite negative electrode material for the lithium ion battery is to load the graphite negative electrode material on a negative electrode current collector to prepare the negative electrode of the lithium ion battery.
In this embodiment. The graphite negative electrode material is loaded on a negative electrode current collector by the conventional process of the negative electrode of the lithium ion battery, so that the basic use effect of a negative electrode product is realized.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various modifications can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. These are non-inventive modifications, which are intended to be protected by patent laws within the scope of the claims appended hereto.
Claims (10)
1. A high-performance graphite negative electrode material for a lithium ion battery is characterized in that: comprises porous graphite powder and a coating layer positioned on the surface of the porous graphite powder, wherein the median particle size of the porous graphite powder is 16-19 mu m, and the compacted density is more than or equal to 1.4g/cm3The first capacity of the graphite cathode material is more than or equal to 353mAh/g, and the first efficiency is more than or equal to 91%.
2. The high-performance graphite anode material for the lithium ion battery according to claim 1, wherein: the porosity of the porous graphite powder is 35-38%, the material of the coating layer comprises petroleum asphalt or coal asphalt, and the thickness of the coating layer is 0.5-1.2 mu m.
3. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery as claimed in claim 1, characterized by sequentially comprising the following steps:
s1, coarsely crushing the porous graphite powder raw material to obtain qualified porous graphite powder;
s2, mixing the coating raw materials to obtain a coating material;
s3, mixing the porous graphite powder with the coating material to obtain a graphite cathode crude material;
and S4, carrying out screening and demagnetizing operation on the graphite cathode coarse material to obtain the final graphite cathode material.
4. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 3, characterized in that: in step S2, the coating layer raw materials include an asphalt base material, a main binder, a binder curing agent, a non-metal oxide filler, a hollow glass microsphere aggregate, a wetting dispersant, and a non-metal coating material.
5. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 4, characterized in that: the asphalt base material is any one of petroleum asphalt or coal asphalt, the main binder is any one or a mixture of phenolic resin, epoxy resin and acrylic resin, the binder curing agent is any one or a mixture of polyisocyanate and phthalic anhydride, the non-metal oxide filler is nano silicon dioxide, the wetting dispersant is isobutylene maleic anhydride copolymer, and the non-metal coating material is nano silicon powder.
6. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 5, wherein the raw material of the coating layer comprises the following components in parts by weight:
45-55 parts of petroleum asphalt,
25-32 parts of epoxy resin,
3-5 parts of phthalic anhydride,
1-2 parts of nano silicon dioxide
1-3 parts of hollow glass microsphere
0.2-0.3 part of isobutylene maleic anhydride copolymer
1-1.5 parts of nano silicon powder.
7. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 5, characterized in that: the isobutylene maleic anhydride copolymer is polycarbonate grafted isobutylene maleic anhydride copolymer, the grafting rate is 1.22-1.35%, the grafting is performed by adopting a molten nitrogen protection method, the melting temperature is 320-440 ℃, the nitrogen introducing time is more than or equal to 15min, and the grafting pressure is 0.5-5.0 bar.
8. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 3, characterized in that: in step S3, the porous graphite powder and the coating material are mixed in a heat treatment reaction kettle, the mixing temperature is 600-920 ℃ and the mixing pressure is 1.2-1.5bar, the mixing time is 5-12h, the heat preservation temperature is 500-800 ℃ and the heat preservation time is 4-6h, and the whole process is mixed under the protection of nitrogen.
9. The preparation method of the high-performance graphite negative electrode material for the lithium ion battery according to claim 3, characterized in that: in step S4, the sieving and demagnetizing operation is performed by a vibrating screen of 600-800 mesh.
10. Use of a high performance graphite anode material according to claim 1 for lithium ion batteries, characterized in that: and loading the graphite negative electrode material on a negative electrode current collector to prepare the negative electrode of the lithium ion battery.
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| CN114976013A (en) * | 2022-06-21 | 2022-08-30 | 惠州锂威新能源科技有限公司 | Preparation method of battery negative electrode material |
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| CN114141993B (en) * | 2021-11-25 | 2024-05-03 | 广东凯金新能源科技股份有限公司 | Processing technology of composite modified graphite negative electrode with good cycle stability |
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| CN114976013B (en) * | 2022-06-21 | 2023-07-04 | 惠州锂威新能源科技有限公司 | Preparation method of battery anode material |
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Denomination of invention: A high-performance graphite negative electrode material for lithium-ion batteries, its preparation method and application Effective date of registration: 20230403 Granted publication date: 20220610 Pledgee: Huzhou bank Limited by Share Ltd. Nan Yuan Branch Pledgor: HUZHOU KAIJIN NEW ENERGY TECHNOLOGY Co.,Ltd. Registration number: Y2023980037333 |