CN111153392A - High-rate lithium ion battery negative electrode material and preparation method thereof - Google Patents
High-rate lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-rate lithium ion battery cathode material and a preparation method thereof, wherein the preparation method of the lithium ion battery cathode material comprises the following steps: s1, uniformly dispersing the carbon nanotubes in a carbon source solution, and performing hydrothermal reaction, washing and drying to obtain a hard carbon precursor material; s2, pyrolyzing the hard carbon precursor material in an inert atmosphere, and then crushing to obtain a hard carbon particle raw material; s3, mixing the hard carbon particle raw material with an asphalt binder, granulating at a medium temperature to obtain secondary particles, then carrying out high-temperature graphitization treatment on the secondary particles to obtain graphitized particles, and then carrying out surface coating modification and carbonization on the graphitized particles by using asphalt. The lithium ion battery cathode material prepared by the invention has the advantages that the structure of the hollow carbon nanotube in the interior can greatly enhance the lithium ion conductivity of the cathode material, improve the defects of low hard carbon capacity and the like, and is beneficial to improving the charge and discharge efficiency and the cycle performance of the graphite cathode.
Description
Technical Field
The invention relates to the technical field of lithium ion battery graphite cathode materials, in particular to a high-rate lithium ion battery cathode material and a preparation method thereof.
Background
The lithium ion battery is widely applied to the field of new energy automobiles, and along with the improvement of requirements of people on high power, high capacity, long cycle, use environment and the like of the lithium ion battery, the improvement of the charge rate, capacity and cycle life of positive and negative materials is taken as a main improvement direction. The negative electrode materials that have been practically used in lithium ion batteries at present are basically carbon materials such as artificial graphite, natural graphite, mesocarbon microbeads, petroleum coke, carbon fibers, pyrolytic resin carbon, and the like. Among them, artificial graphite is widely used in the field of power batteries due to its advantages such as high cycle performance and excellent processability. However, the anisotropic structure of the artificial graphite limits the free diffusion of lithium ions in the graphite structure, so that the exertion of the electrochemical capacity of the graphite negative electrode is limited, and particularly the rate capability of the graphite negative electrode material is influenced.
In order to improve the deficiency of the artificial graphite in charge rate performance, the current mainstream technology improves the conductivity of the surface of the artificial graphite by means of surface coating. Chinese patent CN201510793882.6 discloses a high discharge rate lithium ion battery graphite cathode material and a preparation method thereof, wherein the method is to coat a layer of asphalt on the surface of the graphite cathode material for improving the surface conductivity of artificial graphite and improving the low-temperature performance. However, the method does not solve the problem of poor lithium ion conductivity in the graphite material, and has a limited effect of improving the rate capability.
Compared with the artificial graphite, the hard carbon material has the problems of high cost, low charging rate and the like, has anisotropic structural characteristics, has larger interlayer spacing, can accelerate the diffusion of lithium ions, and has the advantages of better cycle performance and multiplying power, low cost and the like, so that the hard carbon has wide application prospect in the field of lithium ion quick charging.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-rate lithium ion battery cathode material and a preparation method thereof, the obtained lithium ion battery cathode material has the advantages of high rate, high capacity and long cycle life, and the method has simple process and higher practicability.
The invention provides a preparation method of a high-rate lithium ion battery cathode material, which comprises the following steps:
s1, uniformly dispersing the carbon nanotubes in a carbon source solution, and performing hydrothermal reaction, washing and drying to obtain a hard carbon precursor material;
s2, pyrolyzing the hard carbon precursor material in an inert atmosphere, and then crushing to obtain a hard carbon particle raw material;
s3, mixing the hard carbon particle raw material with an asphalt binder, granulating at a medium temperature to obtain secondary particles, then carrying out high-temperature graphitization treatment on the secondary particles to obtain graphitized particles, and then carrying out surface coating modification and carbonization on the graphitized particles by using asphalt to obtain the lithium ion battery negative electrode material.
Preferably, the mass concentration of the carbon source solution is 5-20%.
Preferably, the carbon source is sucrose;
preferably, the mass ratio of the carbon nano tube to the carbon source solution is 1 (10-20).
Preferably, the diameter of the carbon nanotube is 10-60 nm; more preferably, the carbon nanotubes have a diameter of 20 nm.
Preferably, in the step S1, the hydrothermal temperature is 150-; more preferably, the hydrothermal temperature is 180 ℃ and the hydrothermal holding time is 8 h.
Preferably, in the step S2, the pyrolysis temperature is 500-1000 ℃; more preferably, the pyrolysis temperature is 800 ℃.
Preferably, the hard carbon particle raw material has an average particle diameter of 1 to 5 μm.
Preferably, the asphalt binder is coal tar pitch, petroleum pitch, or a mixture thereof.
Preferably, the mass ratio of the asphalt binder to the hard carbon particle raw material is (0.2-0.5): 1.
preferably, in the step S3, the medium-temperature granulation is performed under an inert atmosphere at a temperature of 500-800 ℃.
Preferably, the secondary particles have an average particle diameter of 2.5 to 5 μm.
Preferably, in step S3, the asphalt used for surface coating modification is petroleum asphalt or coal asphalt with a softening temperature point of 80-100 ℃.
Preferably, the mass ratio of the asphalt used for surface coating modification to the graphitized particles is 1: (5-10).
Preferably, in the step S3, the temperature of the high-temperature graphitization treatment is 2800-3200 ℃.
Preferably, in the step S3, the carbonization temperature is 800-.
A high-rate lithium ion battery cathode material is prepared by the preparation method.
According to the invention, carbon tubes/hard carbon cathode materials are formed by carrying out hydrothermal crystallization on carbon sources such as sucrose and the like on carbon nanotubes through pyrolysis, and graphite cathode materials with high multiplying power, high capacity and long cycle life are obtained through high-temperature graphitization. The method has simple process and high practicability.
Drawings
Fig. 1 is a flow chart of the preparation of the high-rate high-capacity negative electrode material of the invention.
Fig. 2 is a rate charging curve diagram of the lithium ion battery of the present invention.
Detailed Description
As shown in fig. 1, fig. 1 is a flow chart of the preparation of the high-rate high-capacity anode material of the invention.
Referring to fig. 1, the invention provides a high-rate lithium ion battery cathode material and a preparation method thereof.
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Uniformly dispersing carbon nanotubes with the diameter of 20nm in a sucrose solution with the mass concentration of 10%, wherein the mass ratio of the carbon nanotubes to the sucrose solution is 1:10, carrying out heat preservation hydrothermal reaction on the obtained slurry solution at 180 ℃ for 8 hours, and washing and drying to obtain a hard carbon precursor material; putting the hard carbon precursor material in inert gas N2Under the protection of (2), the hard carbon particle raw material with the size of 1 mu m is prepared by thermal insulation and pyrolysis for 2h at 800 ℃. Mixing hard carbon granule raw material with powdered petroleum asphaltMixing the binder according to the mass ratio of 1:0.3, mixing for 2h, and then adding inert gas N2Under the protection of (1), heating to 600 ℃ at a constant temperature rate of 5 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing to prepare secondary particles with the average particle size of 2.5 mu m, graphitizing at 2800 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 80 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:5, and carbonizing at 900 ℃ to obtain the lithium ion battery cathode material.
Example 2
Uniformly dispersing carbon nanotubes with the diameter of 10nm in a sucrose solution with the mass concentration of 5%, wherein the mass ratio of the carbon nanotubes to the sucrose solution is 1:15, carrying out heat preservation hydrothermal reaction on the obtained slurry solution at 150 ℃ for 5 hours, washing and drying to obtain a hard carbon precursor material; putting the hard carbon precursor material in inert gas N2Under the protection of (2), the hard carbon particle raw material with the size of 1.5 mu m is prepared by thermal insulation and pyrolysis for 2h at 500 ℃. Mixing the hard carbon particle raw material with a powdered petroleum asphalt binder according to a mass ratio of 1:0.2, mixing for 2 hours, and then adding inert gas N2Under the protection of (1), heating to 600 ℃ at a constant temperature rate of 8 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing, preparing secondary particles with the average particle size of 3 mu m, graphitizing at 3000 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 80 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:8, and carbonizing at 800 ℃ to obtain the lithium ion battery cathode material.
Example 3
Uniformly dispersing carbon nanotubes with the diameter of 30nm in a sucrose solution with the mass concentration of 15%, wherein the mass ratio of the carbon nanotubes to the sucrose solution is 1:20, carrying out heat preservation hydrothermal reaction on the obtained slurry solution at 170 ℃ for 7h, washing and drying to obtain a hard carbon precursor material; putting the hard carbon precursor material in inert gas N2Under the protection of (2), the raw materials are thermally decomposed for 2 hours at 700 ℃ and are crushedThe hard carbon particle raw material with the size of 1.8 mu m is prepared by processing. Mixing the hard carbon particle raw material with a powdered petroleum asphalt binder according to a mass ratio of 1:0.4, mixing for 2 hours, and then adding inert gas N2Under the protection of (1), heating to 500 ℃ at a constant temperature rate of 10 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing to prepare secondary particles with the average particle size of 3.5 microns, graphitizing at 3200 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 90 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:10, and carbonizing at 1000 ℃ to obtain the lithium ion battery cathode material.
Example 4
Uniformly dispersing carbon nanotubes with the diameter of 40nm in a sucrose solution with the mass concentration of 20%, wherein the mass ratio of the carbon nanotubes to the sucrose solution is 1:20, carrying out heat preservation hydrothermal reaction on the obtained slurry solution at 180 ℃ for 9h, washing and drying to obtain a hard carbon precursor material; putting the hard carbon precursor material in inert gas N2Under the protection of (2), the hard carbon particle raw material with the size of 2 mu m is prepared by thermal insulation and pyrolysis for 2h at 900 ℃. Mixing the hard carbon particle raw material with a powdered petroleum asphalt binder according to a mass ratio of 1:0.2, mixing for 2 hours, and then adding inert gas N2Under the protection of (1), heating to 800 ℃ at a constant temperature rate of 15 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing, preparing secondary particles with the average particle size of 4 mu m, graphitizing at 2800 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 100 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:10, and carbonizing at 800 ℃ to obtain the lithium ion battery cathode material.
Example 5
Uniformly dispersing carbon nanotubes with the diameter of 60nm in a 20% sucrose solution, wherein the mass ratio of the carbon nanotubes to the sucrose solution is 1:15, carrying out heat preservation hydrothermal reaction on the obtained slurry solution at 200 ℃ for 10 hours, washing and drying to obtain a hard carbon precursor material; precursor of hard carbonBulk material in inert gas N2Under the protection of (1), the hard carbon particle raw material with the size of 1.7 mu m is prepared by thermal insulation and pyrolysis for 2h at 1000 ℃. Mixing the hard carbon particle raw material with a powdered petroleum asphalt binder according to a mass ratio of 1:0.3, mixing for 2 hours, and then adding inert gas N2Under the protection of (1), heating to 600 ℃ at a constant temperature rate of 20 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing, preparing secondary particles with the average particle size of 5 mu m, graphitizing at 3000 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 100 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:5, and carbonizing at 800 ℃ to obtain the lithium ion battery cathode material.
Comparative example 1
Carrying out heat preservation hydrothermal reaction on 20% of sucrose solution at 200 ℃ for 10h, washing and drying to obtain a hard carbon precursor material; putting the hard carbon precursor material in inert gas N2Under the protection of (1), the hard carbon particle raw material with the size of 1.7 mu m is prepared by thermal insulation and pyrolysis for 2h at 1000 ℃. Mixing the hard carbon particle raw material with a powdered petroleum asphalt binder according to a mass ratio of 1:0.3, mixing for 2 hours, and then adding inert gas N2Under the protection of (1), heating to 600 ℃ at a constant temperature rate of 20 ℃/min, preserving heat for 2h, and then carrying out reaction under the inert gas N2Cooling to room temperature, discharging, crushing, preparing secondary particles with the average particle size of 5 mu m, graphitizing at 3000 ℃ to obtain graphitized particles, coating the surfaces of the graphitized particles with petroleum asphalt with the softening point of 100 ℃, wherein the mass ratio of the petroleum asphalt to the graphitized particles is 1:5, and carbonizing at 800 ℃ to obtain the lithium ion battery cathode material.
Test examples
The lithium ion battery negative electrode materials prepared in examples 1 to 5 and comparative example 1 were processed into batteries for performance testing. And (3) anode material: CMC: SBR: uniformly mixing SP (96.1: 1.3:1.8: 0.8) in an aqueous solution, coating the mixture on a copper foil, drying and rolling to prepare the pole piece. A positive electrode material: PVDF: and uniformly mixing the CNTs (98: 1: 1) in an NMP (N-methyl pyrrolidone) solution, coating the mixture on an aluminum foil, and then drying and rolling the aluminum foil to prepare the pole piece. And assembling the positive and negative pole pieces into an 8Ah soft package battery cell. The electrolyte adopts standard test electrolyte 1molLiPF6+ EC + EMC + DEC, the diaphragm EC is glued with a diaphragm, the 1C-25C multiplying power charging test is adopted, and the charging and discharging voltage range is 2.8-4.2V. The results of the performance tests are shown in Table 1.
Table 1 results of performance testing
As can be seen from table 1, the first efficiency and the discharge capacity of the negative electrode material of the lithium ion battery of comparative example 1 are significantly lower than those of the negative electrode material of the lithium ion battery of the present invention.
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 (10)
1. A preparation method of a high-rate lithium ion battery cathode material is characterized by comprising the following steps:
s1, uniformly dispersing the carbon nanotubes in a carbon source solution, and performing hydrothermal reaction, washing and drying to obtain a hard carbon precursor material;
s2, pyrolyzing the hard carbon precursor material in an inert atmosphere, and then crushing to obtain a hard carbon particle raw material;
s3, mixing the hard carbon particle raw material with an asphalt binder, granulating at a medium temperature to obtain secondary particles, then carrying out high-temperature graphitization treatment on the secondary particles to obtain graphitized particles, and then carrying out surface coating modification and carbonization on the graphitized particles by using asphalt to obtain the lithium ion battery negative electrode material.
2. The preparation method of the high-rate lithium ion battery negative electrode material according to claim 1, wherein the mass concentration of the carbon source solution is 5-20%; preferably, the carbon source is sucrose; preferably, the mass ratio of the carbon nano tube to the carbon source solution is 1 (10-20).
3. The preparation method of the high-rate lithium ion battery negative electrode material according to claim 1 or 2, wherein the diameter of the carbon nanotube is 10-60 nm; preferably, the carbon nanotubes have a diameter of 20 nm.
4. The method for preparing the high-rate lithium ion battery anode material as claimed in any one of claims 1 to 3, wherein in the step S1, the hydrothermal temperature is 150-200 ℃, and the hydrothermal heat preservation time is 5-10 h; preferably, the hydrothermal temperature is 180 ℃ and the hydrothermal heat preservation time is 8 h.
5. The method for preparing the high-rate lithium ion battery anode material as claimed in any one of claims 1 to 4, wherein in the step S2, the pyrolysis temperature is 500-1000 ℃; preferably, the pyrolysis temperature is 800 ℃; preferably, the hard carbon particle raw material has an average particle diameter of 1 to 5 μm.
6. The preparation method of the high-rate lithium ion battery negative electrode material according to any one of claims 1 to 5, wherein the asphalt binder is coal asphalt, petroleum asphalt or a mixture thereof; preferably, the mass ratio of the asphalt binder to the hard carbon particle raw material is (0.2-0.5): 1.
7. the method for preparing the high-rate lithium ion battery anode material as claimed in any one of claims 1 to 6, wherein in the step S3, the medium-temperature granulation is performed under an inert atmosphere at a temperature of 500-800 ℃; preferably, the secondary particles have an average particle diameter of 2.5 to 5 μm.
8. The method for preparing the negative electrode material of the high-rate lithium ion battery according to any one of claims 1 to 7, wherein in the step S3, the asphalt used for surface coating modification is petroleum asphalt or coal asphalt with a softening temperature point of 80-100 ℃; preferably, the mass ratio of the asphalt used for surface coating modification to the graphitized particles is 1: (5-10).
9. The method for preparing the negative electrode material of the high-rate lithium ion battery as claimed in any one of claims 1 to 8, wherein the temperature of the high-temperature graphitization treatment in the step S3 is 2800-3200 ℃; preferably, in the step S3, the carbonization temperature is 800-.
10. A high-rate lithium ion battery negative electrode material, which is characterized by being obtained by the preparation method of any one of claims 1 to 9.
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| CN112713271A (en) * | 2020-12-29 | 2021-04-27 | 上海杉杉科技有限公司 | Modified graphite material, preparation method thereof, lithium ion battery and application |
| CN112713277A (en) * | 2020-12-30 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | Hard carbon material, preparation method and application thereof, and lithium ion battery |
| CN113184828A (en) * | 2021-04-27 | 2021-07-30 | 昆山宝创新能源科技有限公司 | Hard carbon cathode composite material and preparation method and application thereof |
| CN113697804A (en) * | 2021-08-23 | 2021-11-26 | 石家庄尚太科技股份有限公司 | Fast-charging high-first-efficiency hard carbon/artificial graphite negative electrode material and preparation method thereof |
| CN113764645A (en) * | 2021-09-15 | 2021-12-07 | 河北坤天新能源科技有限公司 | Preparation method of hard carbon composite material with three-dimensional structure |
| CN114023958A (en) * | 2021-11-04 | 2022-02-08 | 大连宏光锂业股份有限公司 | Fast-charging graphite negative electrode material based on amorphous carbon coating and preparation method |
| CN114068923A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Modification method of graphite and application of graphite in lithium ion battery |
| CN114497467A (en) * | 2020-10-26 | 2022-05-13 | 湖南中科星城石墨有限公司 | Long-cycle high-rate graphite negative electrode material and preparation method and application thereof |
| CN114899377A (en) * | 2022-05-11 | 2022-08-12 | 广东凯金新能源科技股份有限公司 | Hard carbon negative electrode material coated with carbon nano spherical shell and preparation method thereof |
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| CN114068923A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Modification method of graphite and application of graphite in lithium ion battery |
| CN114497467A (en) * | 2020-10-26 | 2022-05-13 | 湖南中科星城石墨有限公司 | Long-cycle high-rate graphite negative electrode material and preparation method and application thereof |
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| CN112713271B (en) * | 2020-12-29 | 2022-07-05 | 上海杉杉科技有限公司 | Modified graphite material, preparation method thereof, lithium ion battery and application |
| CN112713277A (en) * | 2020-12-30 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | Hard carbon material, preparation method and application thereof, and lithium ion battery |
| CN113184828A (en) * | 2021-04-27 | 2021-07-30 | 昆山宝创新能源科技有限公司 | Hard carbon cathode composite material and preparation method and application thereof |
| CN113697804A (en) * | 2021-08-23 | 2021-11-26 | 石家庄尚太科技股份有限公司 | Fast-charging high-first-efficiency hard carbon/artificial graphite negative electrode material and preparation method thereof |
| CN113764645A (en) * | 2021-09-15 | 2021-12-07 | 河北坤天新能源科技有限公司 | Preparation method of hard carbon composite material with three-dimensional structure |
| CN114023958A (en) * | 2021-11-04 | 2022-02-08 | 大连宏光锂业股份有限公司 | Fast-charging graphite negative electrode material based on amorphous carbon coating and preparation method |
| CN116477598A (en) * | 2022-01-15 | 2023-07-25 | 大连中天新材料科技有限公司 | Hard carbon negative electrode material and preparation method thereof |
| CN114899377A (en) * | 2022-05-11 | 2022-08-12 | 广东凯金新能源科技股份有限公司 | Hard carbon negative electrode material coated with carbon nano spherical shell and preparation method thereof |
| CN114899377B (en) * | 2022-05-11 | 2023-11-24 | 广东凯金新能源科技股份有限公司 | Carbon nano spherical shell coated hard carbon negative electrode material and preparation method thereof |
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