CN115893400B - Preparation method of negative electrode material for long-cycle lithium ion battery - Google Patents
Preparation method of negative electrode material for long-cycle lithium ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method of a negative electrode material for a long-cycle lithium ion battery, which comprises the following steps: firstly, selecting an isotropic coke raw material with an OI value of 1-3, pre-carbonizing for 1-6h at 1000-1200 ℃, heating to 2800 ℃ for graphitizing, crushing, and grading to obtain the particle size distribution (D90-D10)/D50 of less than or equal to 1.2 and the specific surface area of less than or equal to 1.0m 2 And/g, transferring into a plasma generator, and depositing inorganic lithium salt on the surface of the plasma generator. The invention can improve the circulation performance and the power performance.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a preparation method of a negative electrode material for a long-cycle lithium ion battery.
Background
Along with the increase of the cycle times of the lithium ion battery in the energy storage market, the lithium ion battery is required to have the cycle requirements more than or equal to 6000 times, and the cycle capacity loss of the lithium battery mainly comes from three aspects of positive and negative active material loss, active lithium loss and kinetic loss. The long circulation capacity of the material can be improved by the modification methods such as doping and coating of the anode material and the cathode material, and the side reaction in the circulation process can be reduced by adjusting and controlling the components and the structure of the SEI through the optimization of electrolyte, so that the loss of active lithium and the dynamic loss caused by the impedance increase caused by the side reaction are reduced. The lithium ions consumed in the process of cycling the anode material are key factors influencing the battery cycle, such as defects on the surface of the anode material, fine powder, irregular morphology, particle size distribution, lithium ions consumed in the process of expansion and the like, can have an important influence on the cycle of the anode material. Meanwhile, in order to reduce the consumption of lithium ions in the charge and discharge process, enough lithium ions need to be timely supplemented, and the loss of the lithium ions is reduced, so that the service life is prolonged. As disclosed in chinese patent 202011156090.5, a long-cycle high-magnification graphite negative electrode material and a preparation method and application thereof are disclosed, wherein a binder is mainly crushed, mixed with a conductive agent, melted and granulated, crushed, the obtained fusion is mixed with artificial graphite, mechanically fused, carbonized, and an artificial solid electrolyte interface film is deposited on the surface of the carbonized product, so that the long-cycle high-magnification graphite negative electrode material is obtained, and although the cycle and the magnification are improved to some extent, the physical mixing and melting uniformity is poor, the efficiency is low, and the artificial solid electrolyte is nano alumina and cannot provide sufficient lithium ions, the cycle performance is not improved, and meanwhile, the material is not selected from the raw materials and the particle size distribution thereof, so that the expected effect is not achieved.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of a cathode material for a long-cycle lithium ion battery, which can improve cycle performance and power performance.
The invention relates to a preparation method of a negative electrode material for a long-cycle lithium ion battery, which comprises the following steps:
s1: selecting an isotropic coke raw material with an OI value of 1-3, pre-carbonizing for 1-6 hours at 1000-1200 ℃, cooling to room temperature, and crushing to a granularity D50 of less than or equal to 50 mu m to obtain a precursor material A;
s2: the catalyst comprises the following components in percentage by mass: 100, mixing the precursor material A and the catalyst uniformly, heating to 2800 ℃ under inert atmosphere, graphitizing for 24 hours, and then crushing and grading to obtain the particle size distribution (D90-D10)/D50 of less than or equal to 1.2, wherein the specific surface area of less than or equal to 1.0m 2 Graphite precursor material B per gram;
s3: transferring the graphite precursor material B into a plasma generator, vacuumizing at the power of 500-1000W and the vacuum degree of 100-500pa, introducing inorganic lithium salt powder at the flow rate of 50-100L/h, blowing the graphite precursor material B into a suspension state according to the flow rate of 500-1000L/h, mixing for 1-6h, stopping gas mixing, spraying a polymer solution with the concentration of 1-10wt% at the flow rate of 1-10mL/min for 30-200min, transferring into a tube furnace after vacuum drying, carbonizing at the temperature of 900-1200 ℃ for 1-6h under inert gas, naturally cooling to room temperature, and crushing and grading to obtain the product (D90-D10)/D50 is less than or equal to 1.2.
The catalyst in the step S2 is one of ferric chloride, cobalt chloride or nickel chloride.
The polymer solution in the step S3 is one of phenolic resin organic solution, furfural resin organic solution, epoxy resin organic solution or asphalt organic solution; the organic solvent is one of acetone, toluene, xylene, diethyl ether or chloroform.
The inorganic lithium salt powder in the step S3 is one of lithium titanate, lithium hydroxide, lithium carbonate, lithium zirconate, lithium cobaltate or lithium metaaluminate, and the particle size is 0.5-2 mu m.
And in the step S3, the particle size of the graphite precursor material B is 5-10 mu m.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can be adopted as follows: 1) According to the invention, through selecting the isotropic coke (OI value of 1-3), the isotropic coke has the advantages of low expansion, strong structural stability and the like, and meanwhile, the particle size distribution of the material is controlled, namely, the particle size distribution and fine powder of the precursor and the graphite composite material are controlled, the side reaction is reduced, the cycle performance is improved, and the inorganic lithium salt is doped in the material, so that sufficient lithium ions are provided, and the cycle performance is improved. 2) The inorganic lithium salt with smaller particle size and the graphite precursor B with larger particle size are mixed by the plasma generator, and the method has the advantages of uniform mixing, strong physical binding force and the like. 3) The polymer material is sprayed on the outer layer, so that on one hand, the graphite precursor material B and the inorganic lithium salt are fixed, the surface of the graphite precursor material B is carbonized to be coated with amorphous carbon, the specific surface area is reduced, the side reaction is reduced, and the cycle performance and the power performance are improved.
Drawings
Fig. 1 is an SEM image of the graphite composite material prepared in example 1.
Detailed Description
Example 1:
the preparation method of the negative electrode material for the long-cycle lithium ion battery comprises the following steps:
s1: selecting a coal-based petroleum coke raw material with an OI value of 2, pre-carbonizing for 3 hours at 1100 ℃, cooling to room temperature, and crushing to a particle size D50=21 mu m to obtain a precursor material A;
s2: 100g of precursor material A and 1g of ferric chloride catalyst are uniformly mixed, graphitized for 24 hours at the temperature of 2800 ℃ under the inert atmosphere of argon, crushed, and graded to the particle size distribution of (D90-D10)/D50=1.0, and the specific surface area=0.9 m 2 Graphite precursor material B per gram;
s3: transferring 100g of graphite precursor material B into a plasma generator, vacuumizing at the power of 1000W and the vacuum degree of 100pa, introducing 10g of lithium titanate powder with the particle size D50=1mu m (flow rate: 80L/h), simultaneously blowing 100g of graphite precursor material B into a suspension state (flow rate: 800L/h) to be mixed for 3h, stopping gas mixing, spraying 100ml of toluene polymer solution of 5wt% phenolic resin for 60min, vacuum drying at 80 ℃ for 24h, transferring into a tube furnace, carbonizing at the temperature of 1000 ℃ for 3h under argon inert gas, naturally cooling to the room temperature, and crushing and grading to (D90-D10)/D50=1.0.
Example 2:
the preparation method of the negative electrode material for the long-cycle lithium ion battery comprises the following steps:
s1: selecting coal-based asphalt coke raw materials with OI value of 1, pre-carbonizing at 1000 ℃ for 6 hours, cooling to room temperature, and crushing to granularity D50=40 mu m to obtain a precursor material A;
s2: 100g of precursor material A and 0.5g of cobalt chloride catalyst are uniformly mixed, and graphitized for 24 hours at the temperature of 2800 ℃ under the inert atmosphere of argon, and then crushed and graded to the particle size distribution of (D90-D10)/D50=1.2, and the specific surface area=1.0 m 2 Graphite precursor material B per gram;
s3: transferring 100g of graphite precursor material B into a plasma generator, vacuumizing at the power of 500W and the vacuum degree of 500pa, introducing 1g of lithium hydroxide powder with the granularity D50=0.5 mu m (flow rate: 50L/h), simultaneously blowing the graphite precursor material B into a suspension state (flow rate: 500L/h) to mix for 1h, stopping gas mixing, spraying 1% of furfural resin dimethylbenzene polymer solution for 30min, vacuum drying at 80 ℃ for 24h, transferring into a tube furnace, carbonizing at 900 ℃ for 6h under argon inert gas, naturally cooling to room temperature, and crushing and grading to (D90-D10)/D50=1.2.
Example 3:
the preparation method of the negative electrode material for the long-cycle lithium ion battery comprises the following steps:
s1: selecting a coal-based asphalt coke raw material with an OI value of 3, pre-carbonizing for 1h at 1200 ℃, cooling to room temperature, and crushing to a particle size D50=11 mu m to obtain a precursor material A;
s2: 100g of precursor material A and 2g of nickel chloride catalyst are uniformly mixed, and graphitized for 24 hours at the temperature of 2800 ℃ under the inert atmosphere of argon, and then crushed and graded to the particle size distribution of (D90-D10)/D50=0.8, wherein the specific surface area=0.8 m 2 Graphite precursor material B per gram;
s3: transferring 100g of graphite precursor material B into a plasma generator, vacuumizing at the power of 1000W and the vacuum degree of 500pa, introducing 1g of lithium zirconate powder with the granularity D50=0.5 mu m (flow rate: 100L/h), simultaneously blowing 100g of graphite precursor material B into a suspension state (flow rate: 1000L/h) to mix for 6 hours, stopping gas mixing, introducing 10% of epoxy resin to spray polymer solution for 300 minutes, vacuum drying at 80 ℃ for 24 hours, transferring into a tube furnace, carbonizing at the temperature of 1200 ℃ for 1 hour under argon inert gas, naturally cooling to the room temperature, and crushing and grading to (D90-D10)/D50=0.8.
Comparative example:
a preparation method of a graphite composite material comprises the following steps:
s1: selecting a coal-based petroleum coke raw material with an OI value of 2, pre-carbonizing for 3 hours at 1100 ℃, cooling to room temperature, and crushing to a particle size D50=21 mu m to obtain a precursor material A;
s2: graphitizing 100g of precursor material A to 2800 ℃ for 24 hours under an inert argon atmosphere, crushing and grading the precursor material A until the particle size distribution is (D90-D10)/D50=1.5 and the specific surface area=1.4 m 2 Graphite precursor material B per gram;
s3: 100g of graphite precursor material B,10g of lithium titanate powder and 10g of phenolic resin are uniformly mixed, and the mixture is heated to 800 ℃ under the argon atmosphere and carbonized for 3 hours to obtain the graphite composite material.
Test examples
(1) SEM test
SEM test was performed on the graphite composite anode material prepared in example 1, and the results are shown in fig. 1. As can be seen from FIG. 1, the obtained composite material has a granular structure, the grain diameter is between 8 and 15 mu m, and the size distribution is uniform.
(2) Button cell testing
The graphite composite anode materials prepared in examples 1 to 3 and the anode materials of comparative examples were assembled into button cells, respectively, according to the following methods:
adding binder, conductive agent and solvent into the negative electrode material, stirring and mixing uniformly to prepare negative electrode slurry, coating the negative electrode slurry on copper foil, drying, rolling and cutting to prepare the negative electrode plate. The binder is LA132 binder, the conductive agent is SP conductive agent, the solvent is secondary distilled water, and the weight ratio of the anode material, the SP conductive agent, the LA132 binder and the secondary distilled water is 95:1:4:220. The lithium metal sheet is used as a counter electrode, a Polyethylene (PE) film, a polypropylene (PP) film or a polyethylene propylene (PEP) composite film is used as a diaphragm, and LiPF is used 6 /EC+DEC（LiPF 6 The concentration of (2) was 1.3mol/L and the volume ratio of EC and DEC was 1:1) as an electrolyte, and the battery assembly was performed in an argon-filled glove box.
The prepared button cells are respectively arranged on a Wuhan blue electric CT2001A type cell tester, charge and discharge are carried out at a rate of 0.1C, the charge and discharge voltage ranges from 0.005V to 2.0V, and the first discharge capacity and the first discharge efficiency are measured. The rate discharge capacities of 2C and 0.2C were measured, and the rate performance (3C/0.2C) was calculated.
The powder conductivity and the powder OI value of the cathode material are tested according to the national standard GB/T-24533-2019 lithium ion battery graphite cathode material, and the test results are shown in Table 1:
TABLE 1 Properties of the negative electrode materials in examples 1 to 3 and comparative examples
As can be seen from table 1, the discharge capacity of the composite anode materials prepared in examples 1 to 3 is significantly higher than that of the comparative examples; the reason for this is probably because the graphite material increases the conductivity of the material by doping lithium compounds in the material, and decreases the OI value of the powder material, and improves the kinetic properties of the material, thus increasing the specific capacity and first efficiency of the material.
(3) Soft package battery test
Negative electrodes were prepared with the negative electrode materials prepared in examples 1 to 3 and comparative examples, respectively, and were prepared with ternary materials (LiNi 1/3 Co 1/ 3 Mn 1/3 O 2 ) Preparation of positive electrode for positive electrode material with LiPF 6 (the solvent is EC+DEC, the volume ratio is 1:1, the concentration is 1.3 mol/L) is electrolyte, and the cellgard 2400 is a diaphragm to prepare the 2Ah soft package battery.
When the negative electrode is prepared, a binder, a conductive agent and a solvent are added into a negative electrode material, the materials are stirred and mixed uniformly to prepare negative electrode slurry, the negative electrode slurry is coated on a copper foil, and the negative electrode plate is prepared by drying, rolling and cutting. The binder is LA132 binder, the conductive agent is SP conductive agent, the solvent is secondary distilled water, and the weight ratio of the anode material, the SP conductive agent, the LA132 binder and the secondary distilled water is 95:1:4:220.
When the positive electrode is prepared, a binder, a conductive agent and a solvent are added into a positive electrode material, the mixture is stirred and mixed uniformly to prepare positive electrode slurry, the positive electrode slurry is coated on an aluminum foil, the aluminum foil is dried, rolled and cut to prepare a positive electrode plate, the binder is PVDF, the conductive agent is SP, and the solvent is N-methylpyrrolidone. The weight ratio of the positive electrode material, the conductive agent, the binder and the solvent is 93:3:4:140.
1) Rate capability test
The charging and discharging voltage ranges from 2.8V to 4.2V, the testing temperature is 25+/-3.0 ℃, the charging is carried out at 1.0C, 2.0C, 3.0C and 5.0C, the discharging is carried out at 1.0C, the constant current ratio and the temperature of the battery under different charging modes are tested, and the results are shown in Table 2:
table 2 rate performance of examples 1-3 and comparative examples
As can be seen from Table 2, the rate charging performance of the battery pack of the invention is significantly better than that of the comparative example, and the charging time is shorter, which indicates that the composite anode material of the invention has good quick charging performance. The reason may be that the inorganic lithium compound coated on the surface of the material has ion impedance, the low OI value of the powder material of the inorganic lithium compound reduces the impedance, the dynamic performance of the battery is improved, and meanwhile, the active point of the material is improved through gas etching on the surface of the material, the intercalation and deintercalation rate of lithium ions is improved, so that the rate performance is improved.
2) Cycle performance test
The following experiments were performed on the flexible battery fabricated using the anode materials of examples 1 to 3 and comparative example: the capacity retention rate was measured by performing charge and discharge cycles 100 times, 300 times, and 500 times in this order with a charge and discharge rate of 2C/2C and a voltage range of 2.8-4.2V, and the results are shown in Table 3:
table 3 cycle performance of lithium ion batteries of examples 1 to 3 and comparative example
As can be seen from table 3, the cycle performance of the lithium ion battery prepared from the composite anode material prepared by the invention is obviously superior to that of the comparative example in each stage, and the reason is probably that the graphite surface reduces the side reaction and promotes cycle by controlling the particle size distribution and the fine powder, and meanwhile, the material surface coats the inorganic lithium salt on the graphite surface by plasma so as to promote the first efficiency and supplement lithium ions so as to promote the cycle performance.
Although the preferred embodiments of the present invention have been described above with reference to the accompanying drawings, they are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will be apparent to those skilled in the art, and it is intended to cover within the scope of the invention any such modifications, equivalents, and improvements as fall within the spirit and scope of the invention.
Claims (3)
1. The preparation method of the negative electrode material for the long-cycle lithium ion battery comprises the following steps:
s1: selecting an isotropic coke raw material with an OI value of 1-3, pre-carbonizing for 1-6 hours at 1000-1200 ℃, cooling to room temperature, and crushing to a granularity D50 of less than or equal to 50 mu m to obtain a precursor material A;
s2: the catalyst comprises the following components in percentage by mass: 100, mixing the precursor material A and the catalyst uniformly, heating to 2800 ℃ under inert atmosphere, graphitizing for 24 hours, and crushing and grading until the particle size distribution is (D90-D10)/D50 is less than or equal to 1.2, and the specific surface area is less than or equal to 1.0m 2 The graphite precursor material B of/g, wherein the catalyst is one of ferric chloride, cobalt chloride or nickel chloride;
s3: transferring the graphite precursor material B into a plasma generator, vacuumizing at the power of 500-1000W and the vacuum degree of 100-500pa, introducing inorganic lithium salt powder at the flow rate of 50-100L/h, blowing the graphite precursor material B into a suspension state according to the flow rate of 500-1000L/h, mixing for 1-6h, stopping gas mixing, spraying a polymer solution with the concentration of 1-10wt% at the flow rate of 1-10mL/min for 30-200min, transferring into a tube furnace after vacuum drying, carbonizing at the temperature of 900-1200 ℃ for 1-6h under inert gas, naturally cooling to room temperature, and crushing and grading to (D90-D10)/D50 is less than or equal to 1.2, thus obtaining the graphite; wherein the polymer solution is one of phenolic resin organic solution, furfural resin organic solution, epoxy resin organic solution or asphalt organic solution.
2. The method for preparing a negative electrode material for a long-cycle lithium ion battery according to claim 1, wherein: the inorganic lithium salt powder in the step S3 is one of lithium titanate, lithium hydroxide, lithium carbonate, lithium zirconate, lithium cobaltate or lithium metaaluminate, and the particle size is 0.5-2 mu m.
3. The method for preparing a negative electrode material for a long-cycle lithium ion battery according to claim 1, wherein: and in the step S3, the particle size of the graphite precursor material B is 5-10 mu m.
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Effective date of registration: 20230906 Address after: 562499 Xinqiao Industrial Park, Qianxinan High tech Zone, Xinqiao Town, Anlong County, Qianxinan Buyi and Miao Autonomous Prefecture, Guizhou Province Applicant after: Guizhou Huiyang Technology Innovation Research Co.,Ltd. Address before: 562409 group 2, joint venture village, Lutun Town, Yilong new area, Qianxinan Buyei and Miao Autonomous Prefecture, Guizhou Province (next to Yilong Avenue) Applicant before: Huiyang (Guizhou) new energy materials Co.,Ltd. |
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