CN115893400A - Preparation method of negative electrode material for long-cycle lithium ion battery - Google Patents
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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 at 1000-1200 ℃ for 1-6h, heating to 2800 ℃ for graphitization, crushing, and grading until the particle size distribution is (D90-D10)/D50 is less than or equal to 1.2, the specific surface area is less than or equal to 1.0m 2 G, transferAnd (3) putting the mixture into a plasma generator, and depositing inorganic lithium salt on the surface of the mixture to obtain the lithium ion battery. The invention can improve the cycle 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
With the increase of the cycle number requirements of the lithium ion battery in the energy storage market, the lithium ion battery is required to have the cycle requirement of 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 electrode active substance loss, active lithium loss and dynamic loss. The long cycle capacity of the material can be improved by modification methods such as doping and coating of the anode and cathode materials, the components and the structure of the SEI are regulated and controlled by optimizing the electrolyte, the generation of side reactions in the cycle process can be reduced, and further, the loss of active lithium and the kinetic loss caused by the increase of impedance due to the side reactions are reduced. Lithium ions consumed in the cycle process of the negative electrode material are key factors influencing the cycle of the battery, and factors such as defects on the surface of the negative electrode material, fine powder, irregular morphology, particle size distribution, lithium ions consumed in the expansion process and the like can all have important influence on the cycle of the negative electrode material. Meanwhile, in order to reduce the consumption of lithium ions in the charging and discharging processes, enough lithium ions need to be supplemented in time, and the loss of the lithium ions is reduced, so that the service life is prolonged. For example, chinese patent 202011156090.5 discloses a long-circulation high-rate graphite cathode material and a preparation method and application thereof, which mainly comprises the steps of crushing a binder, mixing with a conductive agent, melting, granulating, crushing, mixing the obtained fusion with artificial graphite, mechanically fusing, carbonizing, and depositing an artificial solid electrolyte interface film on the surface of a carbonized product to obtain the long-circulation high-rate graphite cathode material.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of a negative electrode 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 at 1000-1200 ℃ for 1-6h, cooling to room temperature, and crushing to obtain a precursor material A with a particle size D50 of less than or equal to 50 mu m;
s2: according to the mass ratio as a catalyst: precursor material A = (0.5-2): 100, precursor material A and catalyst are mixed evenly, heated to 2800 ℃ under inert atmosphere for graphitization for 24h, crushed and graded until the particle size distribution is (D90-D10)/D50 is less than or equal to 1.2, the specific surface area is less than or equal to 1.0m 2 A graphite precursor material B per gram;
s3: transferring a graphite precursor material B into a plasma generator, vacuumizing under 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 at 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 rate of 1-10mL/min, drying in vacuum, transferring into a tubular furnace, carbonizing at the temperature of 900-1200 ℃ for 1-6h under inert gas, naturally cooling to room temperature, and crushing and grading until (D90-D10)/D50 is less than or equal to 1.2.
And 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 a phenolic resin organic solution, a furfural resin organic solution, an epoxy resin organic solution or an asphalt organic solution; the organic solvent is one of acetone, toluene, xylene, diethyl ether or chloroform.
In the step S3, the inorganic lithium salt powder 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.
The particle size of the graphite precursor material B in the step S3 is 5-10 mu m.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can show that: 1) The method selects the isotropic coke (OI value is 1-3), the isotropic coke has the advantages of low expansion, strong structural stability and the like, 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 advantages of uniform mixing, strong physical binding force and the like are achieved. 3) By spraying the polymer material on the outer layer, on one hand, the graphite precursor material B and the inorganic lithium salt are fixed and carbonized to coat the amorphous carbon on the surface, so that 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:
a preparation method of a negative electrode material for a long-cycle lithium ion battery comprises the following steps:
s1: selecting a coal-series petroleum coke raw material with an OI value of 2, pre-carbonizing for 3h at 1100 ℃, then cooling to room temperature, and crushing to obtain a precursor material A with the particle size D50=21 mu m;
s2: 100g of precursor material A and 1g of ferric chloride catalyst are uniformly mixed, heated to 2800 ℃ under the inert atmosphere of argon, graphitized for 24h, crushed and classified until the particle size distribution is (D90-D10)/D50 =1.0, and the specific surface area =0.9m 2 Per gram of graphite precursor material B;
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 (flow rate: 80L/h) with the particle size of D50=1 mu m, simultaneously blowing 100g of graphite precursor material B to a suspension state (flow rate: 800L/h) for mixing for 3h, stopping gas mixing, spraying 100ml of toluene polymer solution of 5wt% phenolic resin for 60min, transferring into a tube furnace after vacuum drying at 80 ℃ for 24h, carbonizing at 1000 ℃ for 3h under argon inert gas, naturally cooling to room temperature, and crushing and grading to (D90-D10)/D50 =1.0 to obtain the lithium titanate powder.
Example 2:
a preparation method of a negative electrode material for a long-cycle lithium ion battery comprises the following steps:
s1: selecting a coal-series asphalt coke raw material with an OI value =1, pre-carbonizing at 1000 ℃ for 6 hours, cooling to room temperature, and crushing to obtain a precursor material A with a particle size D50=40 mu m;
s2: 100g of precursor material A and 0.5g of cobalt chloride catalyst are uniformly mixed, heated to 2800 ℃ under the inert atmosphere of argon gas for graphitization for 24 hours, and then crushed and classified until the particle size distribution is (D90-D10)/D50 =1.2, and the specific surface area =1.0m 2 A 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 particle size D50=0.5 mu m (flow rate: 50L/h), blowing the graphite precursor material B to a suspension state (flow rate: 500L/h) for mixing for 1h, stopping gas mixing, spraying 1% of furfural resin xylene polymer solution 30min, vacuum-drying at 80 ℃ for 24h, transferring into a tubular 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 to obtain the composite material.
Example 3:
a preparation method of a negative electrode material for a long-cycle lithium ion battery comprises the following steps:
s1: selecting a coal-series asphalt coke raw material with an OI value of 3, pre-carbonizing at 1200 ℃ for 1h, cooling to room temperature, and crushing to obtain a precursor material A with a particle size D50=11 mu m;
s2: uniformly mixing 100g of precursor material A and 2g of nickel chloride catalyst, heating to 2800 ℃ under an argon inert atmosphere for graphitizing for 24h, and then crushing and classifying to obtain particles with the particle size distribution of (D90-D10)/D50 =0.8 and the specific surface area =0.8m 2 Per gram of graphite precursor material B;
s3: transferring 100g of graphite precursor material B into a plasma generator, vacuumizing under the power of 1000W and the vacuum degree of 500pa, introducing 1g of lithium zirconate powder with the particle size 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 6h, stopping gas mixing, introducing 10% of epoxy resin spraying polymer solution to spray for 300min, transferring to a tubular furnace after vacuum drying at 80 ℃ for 24h, carbonizing at 1200 ℃ for 1h under argon inert gas, naturally cooling to room temperature, and crushing and grading to (D90-D10)/D50 =0.8 to obtain the graphite precursor material B.
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 the raw material for 3 hours at the temperature of 1100 ℃, cooling the raw material to room temperature, and crushing the raw material to a particle size D50=21 mu m to obtain a precursor material A;
s2: heating 100g of precursor material A to 2800 ℃ in an argon inert atmosphere, graphitizing for 24h, crushing and grading until the particle size distribution is (D90-D10)/D50 =1.5, and the specific surface area =1.4m 2 Per gram of graphite precursor material B;
s3: and uniformly mixing 100g of graphite precursor material B,10g of lithium titanate powder and 10g of phenolic resin, and heating to 800 ℃ in an argon atmosphere for carbonization for 3h to obtain the graphite composite material.
Test examples
(1) SEM test
The graphite composite negative electrode material prepared in example 1 was subjected to SEM test, and the results are shown in fig. 1. As can be seen from FIG. 1, the obtained composite material has a granular structure, the particle size is between 8 and 15 μm, and the size distribution is uniform.
(2) Button cell test
The graphite composite negative electrode materials prepared in examples 1 to 3 and the negative electrode material of the comparative example were assembled into button cells, respectively, as follows:
adding a binder, a conductive agent and a solvent into the negative electrode material, stirring and mixing uniformly to prepare negative electrode slurry, coating the negative electrode slurry on a copper foil, drying, rolling and cutting to prepare a negative electrode sheet. The binder is a LA132 binder, the conductive agent is an SP conductive agent, the solvent is secondary distilled water, and the weight ratio of the negative electrode material, the SP conductive agent, the LA132 binder and the secondary distilled water is 95. The lithium metal sheet is taken as a counter electrode, a Polyethylene (PE) film, a polypropylene (PP) film or a polyethylene propylene (PEP) composite film is taken as a diaphragm, and LiPF is taken 6 /EC+DEC（LiPF 6 Was 1.3mol/L, the volume ratio of EC and DEC was 1) was 1.
The prepared button cell is respectively arranged on a Wuhan blue electricity CT2001A type cell tester, and is charged and discharged at 0.1C multiplying power, the charging and discharging voltage range is 0.005V to 2.0V, and the first discharge capacity and the first discharge efficiency are measured. The rate discharge capacities of the two materials, 2C and 0.2C, were tested, and the rate performance (3C/0.2C) was calculated.
The powder conductivity and powder OI value of the cathode material are tested according to the national standard GB/T-243357-2019 graphite cathode material of lithium ion batteries, and the test results are shown in Table 1:
TABLE 1 Properties of negative electrode materials in examples 1 to 3 and comparative example
As can be seen from Table 1, the discharge capacities of the composite anode materials prepared in examples 1 to 3 were significantly higher than those of the comparative examples; the reason for this is probably because the graphite material improves the conductivity of the material by doping a lithium compound in the material, and reduces the value of the powder material OI, and improves the dynamic performance of the material, thus improving the specific capacity and the first efficiency of the material.
(3) Pouch cell testing
Cathodes were prepared from the anode materials prepared in examples 1 to 3 and comparative example, respectively, and ternary material (LiNi) 1/3 Co 1/ 3 Mn 1/3 O 2 ) Preparing a positive electrode from a positive electrode material by using LiPF 6 (the solvent is EC + DEC, the volume ratio is 1, and the concentration is 1.3 mol/L) is used as an electrolyte, and celegard2400 is used as a diaphragm to prepare the 2Ah flexible package battery.
When the negative electrode is prepared, the binder, the conductive agent and the solvent are added into the negative electrode material, the negative electrode slurry is prepared by stirring and mixing uniformly, the slurry of the negative electrode slurry is coated on a copper foil, and the negative electrode sheet 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 negative electrode material, the SP conductive agent, the LA132 binder and the secondary distilled water is 95.
When the anode is prepared, adding a binder, a conductive agent and a solvent into an anode material, stirring and mixing uniformly to prepare anode slurry, coating the anode slurry on an aluminum foil, drying, rolling and cutting to prepare an anode sheet, wherein 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.
1) Rate capability test
The charging and discharging voltage range is 2.8-4.2V, the testing temperature is 25 +/-3.0 ℃, the charging is respectively 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 is obviously superior to that of the comparative example, the charging time is short, and the composite negative electrode material has good quick charging performance. The reason may be that the material surface is coated with the inorganic lithium compound with ionic resistivity to reduce the impedance and the low OI value of the powder material thereof to improve the dynamic performance of the battery, and meanwhile, the active points of the material are improved by gas etching on the material surface to improve the insertion and extraction rate of lithium ions, thereby improving the rate performance.
2) Cycle performance test
The following experiment was performed on the pouch batteries manufactured using the negative electrode materials of examples 1 to 3 and comparative example: the capacity retention rate was measured by performing 100, 300, and 500 charge-discharge cycles in sequence at a charge-discharge rate of 2C/2C and a voltage range of 2.8-4.2V, and the results are shown in Table 3:
TABLE 3 cycling Performance of the lithium ion batteries of examples 1-3 and comparative example
It can be seen from table 3 that the cycle performance of the lithium ion battery prepared from the composite negative electrode material prepared by the invention is obviously better than that of the comparative example at each stage, probably because the cycle is improved by controlling the particle size distribution of the graphite surface and controlling fine powder to reduce side reaction of the graphite surface, and the first efficiency is improved and lithium ions are supplemented to improve the cycle performance by coating inorganic lithium salt on the graphite surface through plasma on the material surface.
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 changes may be made by those skilled in the art, and any modifications, equivalents, and improvements made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A preparation method of a negative electrode material for a 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 at 1000-1200 ℃ for 1-6h, cooling to room temperature, and crushing to obtain a precursor material A with a particle size D50 of less than or equal to 50 mu m;
s2: the catalyst comprises the following components in percentage by mass: precursor material A = (0.5-2): 100, precursor material A and catalyst are mixed evenly, heated to 2800 ℃ under inert atmosphere for graphitization for 24h, crushed and graded until the particle size distribution is (D90-D10)/D50 is less than or equal to 1.2, the specific surface area is less than or equal to 1.0m 2 A graphite precursor material B per gram;
s3: transferring a graphite precursor material B into a plasma generator, vacuumizing under 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 at 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 rate of 1-10mL/min, drying in vacuum, transferring into a tubular furnace, carbonizing at the temperature of 900-1200 ℃ for 1-6h under inert gas, naturally cooling to room temperature, and crushing and grading until (D90-D10)/D50 is less than or equal to 1.2.
2. The method of claim 1, wherein: and in the step S2, the catalyst is one of ferric chloride, cobalt chloride or nickel chloride.
3. The method of claim 1 for preparing a negative electrode material for a long-cycle lithium-ion battery, wherein: the polymer solution in the step S3 is one of a phenolic resin organic solution, a furfural resin organic solution, an epoxy resin organic solution or an asphalt organic solution; the organic solvent is one of acetone, toluene, xylene, diethyl ether or chloroform.
4. The method of claim 1, wherein: in the step S3, the inorganic lithium salt powder 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.
5. The method of claim 1, wherein: the particle size of the graphite precursor material B in the step S3 is 5-10 mu m.
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