CN112490399A - Method for pre-lithium of lithium ion battery cathode - Google Patents

Method for pre-lithium of lithium ion battery cathode Download PDF

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CN112490399A
CN112490399A CN202110109821.9A CN202110109821A CN112490399A CN 112490399 A CN112490399 A CN 112490399A CN 202110109821 A CN202110109821 A CN 202110109821A CN 112490399 A CN112490399 A CN 112490399A
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stirring
lithium
speed
suspension
negative electrode
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CN112490399B (en
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刘艳侠
杨幸遇
赵冲冲
高文超
张涛
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Zhengzhou Institute of Emerging Industrial Technology
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    • H—ELECTRICITY
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    • H01M4/02—Electrodes composed of, or comprising, active material
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    • H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
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    • H01—ELECTRIC ELEMENTS
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/00—Electrodes
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    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention provides a method for pre-lithium of a lithium ion battery cathode, which comprises the following steps: (1) adding inert lithium powder into the nonpolar solution at room temperature, and shaking and stirring to form a suspension; (2) stirring the negative active material and the conductive agent at a low speed, and adding a small amount of NMP solvent after uniformly mixing; after stirring uniformly, adding the suspension, and carrying out a low-speed stirring kneading process; (3) adding the conductive suspension into the solution, and stirring at a low speed; adding NMP glue solution of PVDF, and stirring at high speed to prepare negative electrode slurry; (4) coating the negative electrode slurry obtained in the step (3) to prepare an electrode roll; rolling the pole coil; and (4) laminating, welding, packaging, injecting liquid and finally performing chemical composition and volume grading according to the conventional process. According to the invention, the high-efficiency dry mixing process is improved and introduced into the pre-lithium technology, so that the pre-lithiation efficiency and the dispersion uniformity of lithium powder in the electrode slurry can be efficiently improved, a compact SEI film is formed, and the first coulombic efficiency is effectively improved.

Description

Method for pre-lithium of lithium ion battery cathode
Technical Field
The invention relates to the field of lithium batteries, in particular to a method for pre-lithium of a lithium ion battery cathode.
Background
The lithium ion battery adopts an embedded reaction cathode, such as graphite and silicon-based materials, but in the charge and discharge process, especially in the first charge and discharge process, the materials can form an SEI film to consume active lithium ions, and generate large irreversible capacity loss, so that the discharge capacity and energy density of the lithium ion battery can be reduced, and the application of the materials in the high-specific-energy lithium ion battery is restricted.
The negative pole pre-lithium technology provides an effective solution for solving irreversible capacity loss and improving coulombic efficiency and capacity retention rate, and has good application prospect. The application methods which can be searched at present mainly comprise three methods: 1. direct mixing method: adding lithium powder in the anode material homogenizing process. The method is the simplest and direct method, but by the method, a lot of cavities can be left in the pole piece or on the surface of the pole piece by the lithium powder, lithium dendrites can be generated in a thinner area of the pole piece, and safety risk is caused; 2. the spraying method comprises the following steps: the spraying method comprises dry spraying and wet spraying, wherein the dry spraying is to spray inert lithium powder on the surface of the negative pole piece through equipment, and is convenient and direct in practical application operation, but the method has great dust and great potential safety hazard; the lithium powder is dissolved in some organic solvents by wet spraying and is sprayed on the surface of the negative plate, the problem of dust encountered by the dry spraying is effectively solved by the wet spraying, but the lithium powder has low density and is easy to float upwards, the lithium powder is difficult to disperse uniformly when being directly added into the solvents, and the organic solvents are easy to cause certain damage to people and environment after being volatilized; 3. an electrochemical coating method comprises the following steps: and forming a lithium film on the surface of the negative electrode by using methods such as an atomic layer deposition method, a chemical vapor deposition method, a magnetron sputtering method and the like. The lithium supplement amount of the method can be effectively controlled, but additional equipment needs to be purchased, the cost is high, and the method is not beneficial to commercial popularization and application.
Several conventional methods for preparing lithium for the negative electrode have the disadvantages. The direct mixing method has simple process operation, low cost and easy industrialization, but because the lithium powder is light and unstable at normal temperature, the lithium powder is difficult to disperse uniformly in the slurry, the defects of low utilization rate of the lithium powder and low pre-lithium efficiency can be avoided, and dendritic crystals and cavities can be formed on the surface of the pole piece; the spraying method is also difficult to solve the problem of uneven dispersion of the lithium powder, and the effective pre-lithium amount on the surface of the pole piece is not controllable; the electrochemical plating method can control the pre-lithium amount, but needs to introduce expensive equipment, and is not beneficial to commercial promotion.
Disclosure of Invention
The invention provides a method for pre-lithium of a lithium ion battery cathode, which solves the problems of safety risk caused by introduction of metal lithium and uneven dispersion existing in the conventional lithium pre-lithium of the cathode. According to the invention, inert lithium powder is preferably added into a non-polar solvent to prepare stable and uniform lithium powder slurry, a novel pre-lithium technology homogenization process is developed, the inert lithium powder slurry is directly introduced into electrode slurry, and slurry with stable viscosity and solid content and a pole piece with strong binding power and low pole piece impedance are manufactured; and the rolling process is adopted to break the lithium powder coating layer, so that the effective contact of the metal lithium is realized, and the pre-lithiation effect is improved.
The technical scheme for realizing the invention is as follows:
a method for pre-lithium of a lithium ion battery negative electrode comprises the following steps:
(1) adding inert lithium powder into a nonpolar solution at room temperature, and oscillating and stirring to form a stable suspension;
(2) stirring the negative active material and the conductive agent at a low speed, and adding a small amount of NMP solvent after uniformly mixing, so as to wet the slurry after uniformly mixing and be easier to disperse; after uniformly stirring, adding the suspension obtained in the step (1), and carrying out a low-speed stirring kneading process, wherein the step is to uniformly distribute lithium powder in the negative electrode slurry;
(3) adding the conductive suspension into the solution obtained in the step (2), and stirring at a low speed; after the slurry is completely wetted, adding NMP (N-methyl pyrrolidone) glue solution of PVDF (polyvinylidene fluoride) to stir at a high speed, and adjusting the viscosity to prepare cathode slurry capable of being stably coated;
(4) coating by using the negative electrode slurry obtained in the step (3), and controlling the coating temperature and speed to manufacture the pole roll without obvious defects and scratches on the surface; rolling the pole roll, wherein the purpose of the step is to break the inert lithium powder and realize effective contact of the lithium powder and the active material; and (4) laminating, welding, packaging, injecting liquid and finally performing chemical composition and volume grading according to the conventional process.
The particle size of the inert lithium powder in the step (1) is 1 um-100 um, preferably 10 um-30 um; the nonpolar solvent is toluene, hexane, carbon disulfide, carbon tetrachloride or chloroform.
In the step (2), the negative active material is graphite, such as natural graphite, composite graphite and artificial graphite, and silicon-based materials such as one or a mixture of silicon oxide and silicon carbon; the conductive agent is micron or nano-scale powder, and the conductive agent is one or a mixture of a plurality of Super-P, graphene, acetylene black and Ketjen black in any proportion.
In the step (2), the mass ratio of the negative electrode active material to the conductive agent is 95:3, and the ratio of the NMP solvent to the dry powder (the negative electrode active material to the conductive agent) is 1-5%.
In the step (3), the conductive suspension is a suspension of single-walled carbon nanotubes or multi-walled carbon nanotubes, the solid content is 5%, and the solid content of the NMP glue solution of PVDF is 8%.
In the step (3), the rotation speed of the low-speed stirring is 1-50rpm in revolution, and the high-speed stirring is 300-5000rpm in rotation.
The rolling pressure in the step (4) is 0.1-0.5 Mpa.
The dosage of the NMP solvent in the step (2) is 50-100 mL, the rotation speed of the low-speed stirring in the step (3) is revolution 5-15rpm, and the high-speed stirring is rotation 1500-2500 rpm; the rolling pressure in the step (4) is 0.25-0.35 Mpa.
The invention has the beneficial effects that: according to the invention, the high-efficiency dry mixing process is improved and introduced into the pre-lithium technology, so that the high-efficiency coulombic efficiency, the circulating capacity retention rate and the dispersion uniformity of the lithium powder in the electrode slurry can be realized, a compact SEI film is formed, the first coulombic efficiency is effectively improved, meanwhile, the process for introducing the lithium powder into the electrode slurry is simple to operate and low in cost, and the safety risk caused by the contact of the lithium powder and air can be greatly reduced.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 1 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30min, and adding 1% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed 2000rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to obtain negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 2
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30min, and adding 1% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed 2000rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to obtain negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 3
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed 2000rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to obtain negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 4
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 10rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed 2000rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to obtain negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 5
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 10rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the cathode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed 2000rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to obtain negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 6
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a hexane solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a multiwalled carbon nanotube conductive suspension (solid content is 5%) prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at a high speed of 2500rpm for 3h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to prepare negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.25MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(7) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 7
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a toluene solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative electrode active material SiOx/C450 and the conductive agent graphene dry powder at a low speed of 5rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a prepared single-walled carbon nanotube conductive suspension (solid content is 5%) in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at a high speed of 2500rpm for 2.5h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to prepare negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.3MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(8) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Example 8
A novel lithium ion battery negative electrode pre-lithium method comprises the following steps:
(1) adding inert lithium powder with the particle size of 20 mu m into a toluene solution at room temperature, shaking for 1h, and stirring to form a stable suspension;
(2) stirring the negative electrode active material SiOx/C450 and the conductive agent graphene dry powder at a low speed of 5rpm for 30min, and adding 5% of NMP solvent after uniformly mixing, so that the slurry is wetted after uniformly mixing and is easier to disperse;
(3) adding the suspension liquid in the step (1), and stirring at a low speed of 15rpm for 30min to knead, wherein the step is to uniformly distribute the lithium powder in the negative electrode slurry;
(4) adding a prepared single-walled carbon nanotube conductive suspension (solid content is 5%) in advance, and stirring at a low speed of 15rpm for 30 min;
(5) preparing NMP glue solution (the concentration is 8%) of PVDF, stirring at a high speed of 2500rpm for 2.5h, adjusting the viscosity to 5000mPa s after the slurry is completely wetted and making the solid content be 50% to prepare negative electrode slurry capable of being stably coated;
(6) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(7) rolling the pole roll at the rolling pressure of 0.4MPa and the rolling speed of 2m/min to crush the inert lithium powder and realize effective contact between the lithium powder and the active material;
(8) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Comparative example
(1) Firstly, stirring the negative active material SiC 450 and the conductive agent Super-P dry powder at a low speed of 5rpm for 30 min;
(2) adding a multiwalled carbon nanotube conductive suspension prepared in advance, and stirring at a low speed of 15rpm for 30 min;
(3) adding NMP glue solution (the concentration is 8%) of PVDF, stirring at high speed of 2500rpm for 3h, adjusting the viscosity to 5000mPa s, and making into cathode slurry capable of being stably coated, wherein the solid content is 50%;
(4) coating the prepared slurry, and controlling the coating temperature (50-75 ℃) and the coating speed (4 m/min) to manufacture the polar roll without obvious defects and scratches on the surface;
(5) rolling the polar roll at the rolling pressure of 0.3MPa and the rolling speed of 2 m/min;
(6) and (3) laminating, welding, packaging and injecting liquid according to a conventional process, and finally carrying out chemical composition and volume grading and cycle test.
Figure DEST_PATH_IMAGE001
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. A method for pre-lithium of a negative electrode of a lithium ion battery is characterized by comprising the following steps:
(1) adding inert lithium powder into a nonpolar solution at room temperature, and oscillating and stirring to form a stable suspension;
(2) stirring the negative active material and the conductive agent at a low speed, and adding a small amount of NMP solvent after uniformly mixing; after uniformly stirring, adding the suspension obtained in the step (1), and carrying out a low-speed stirring kneading process;
(3) adding the conductive suspension into the solution obtained in the step (2), and stirring at a low speed; adding NMP glue solution of PVDF, stirring at a high speed, and adjusting the viscosity to prepare negative electrode slurry;
(4) coating the negative electrode slurry obtained in the step (3) to prepare an electrode roll; rolling the pole coil; and (4) laminating, welding, packaging, injecting liquid and finally performing chemical composition and volume grading according to the conventional process.
2. The method of claim 1, wherein: in the step (1), the particle size of the inert lithium powder is 1-100 um, and the nonpolar solution is toluene, hexane, carbon disulfide, carbon tetrachloride or chloroform.
3. The method of claim 1, wherein: in the step (2), the negative active material is graphite, the conductive agent is micron-sized or nano-sized powder, and the conductive agent is one or a mixture of more of Super-P, graphene, acetylene black and Ketjen black in any proportion.
4. The method of claim 1, wherein: the mass ratio of the negative electrode active material to the conductive agent in the step (2) is 95: 3.
5. The method of claim 1, wherein: in the step (3), the conductive suspension is a suspension of single-walled carbon nanotubes or multi-walled carbon nanotubes, the solid content is 5%, and the solid content of the NMP glue solution of PVDF is 8%.
6. The method of claim 1, wherein: in the step (3), the rotation speed of the low-speed stirring is 1-50rpm in revolution, and the high-speed stirring is 300-5000rpm in rotation.
7. The method of claim 1, wherein: the rolling pressure in the step (4) is 0.1-0.5 Mpa.
8. The method according to any one of claims 1 to 7, wherein: the dosage of the NMP solvent in the step (2) is 50-100 mL, the rotation speed of the low-speed stirring in the step (3) is revolution 5-15rpm, and the high-speed stirring is rotation 1500-2500 rpm; the rolling pressure in the step (4) is 0.25-0.35 Mpa.
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