CN110492066B - Lithium ion battery negative plate capable of being charged quickly and preparation method thereof - Google Patents

Lithium ion battery negative plate capable of being charged quickly and preparation method thereof Download PDF

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CN110492066B
CN110492066B CN201910708055.0A CN201910708055A CN110492066B CN 110492066 B CN110492066 B CN 110492066B CN 201910708055 A CN201910708055 A CN 201910708055A CN 110492066 B CN110492066 B CN 110492066B
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artificial graphite
negative electrode
stirring
parts
ion battery
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CN110492066A (en
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刘远洲
孙鸿飞
余灵超
潘启明
时洪玲
曹珍
张政
张雪珍
姚琦
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Shenzhen Bak Power Battery Co Ltd
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    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • 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
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a lithium ion battery negative plate capable of being charged quickly and a preparation method thereof, so that a lithium ion battery has the quick charging performance of more than 4C, low temperature rise and excellent cycle performance. The lithium ion battery negative plate comprises a current collector, negative slurry is coated on the current collector, the negative slurry comprises a negative active material, and the negative active material is first artificial graphite and second artificial graphite; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; the mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); the coating surface density of the cathode slurry is 160-170g/m2The compacted density of the negative electrode slurry is 1-2g/cm3。

Description

Lithium ion battery negative plate capable of being charged quickly and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery negative plate capable of being charged quickly and a preparation method thereof.
Background
With the rapid development of portable electronic products and electric automobiles, the market puts higher demands on the rapid charging capability of lithium ion batteries. Currently, commercial lithium ion batteries can only be charged at 0.5C or 0.2C, the charging time is 2 hours or even more than 5 hours, and the charging time is long, so that the use of the lithium ion batteries is limited. With the rapid convergence of people, more and more users expect that the lithium ion battery can be fully charged in a shorter time, and further the cruising anxiety of people is solved from the perspective of rapid charging.
When the existing lithium ion battery is charged for more than 2C, the phenomena of concentration of lithium ions on the surface of a negative electrode, formation of lithium metal, serious electrode polarization, reduction of charging capacity and reduction of cycle life can occur, and meanwhile, the heat production of the battery is increased during large-current charging, the temperature is increased, and the safety problem is caused.
In order to overcome the defect of quick charge of the lithium ion battery, researchers improve the quick charge performance of the lithium ion battery by developing a novel electrolyte, adding an additive and the like. However, the results show that degradation of other properties such as cycle performance and safety performance is inevitably caused in the modification process.
Therefore, how to further shorten the charging time of the lithium ion battery, and simultaneously ensure that the surface temperature of the lithium ion battery rises and falls in the charging process, and the cycle performance of the lithium ion battery is not affected, becomes a problem to be solved urgently.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides the lithium ion battery negative plate capable of being rapidly charged and the preparation method thereof, so that the lithium ion battery has the rapid charging performance of more than 4C, low temperature rise and excellent cycle performance.
The technical problem to be solved by the invention is realized by the following technical scheme:
a lithium ion battery negative plate capable of being rapidly charged comprises a current collector, negative slurry is coated on the current collector and comprises a negative active material, and the negative active material is first artificial graphite and second artificial graphite; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; the mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); the coating surface density of the cathode slurry is 160-170g/m2The compacted density of the negative electrode slurry is 1-2g/cm3。
Further, the particle size D50 of the first artificial graphite was 7 μm, and the particle size D50 of the second artificial graphite was 11 μm; the mass ratio of the first artificial graphite to the second artificial graphite is 71: 23; the coating surface density of the negative electrode slurry is 163g/m2The compacted density of the negative electrode slurry is 1.5g/cm3。
Further, the anode paste further includes a conductive agent, a thickener, and a binder.
Further, the negative electrode slurry comprises the following materials in parts by weight: 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite, 1-2 parts of a conductive agent, 1-2 parts of a thickening agent and 3-4 parts of a binder.
Further, the conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
The invention also provides a preparation method of the lithium ion battery negative plate with the rapid charging function, which comprises the following steps:
s1, adding 70-75 parts of deionized water and 1-2 parts of a thickening agent into a stirrer, stirring until the thickening agent is fully dissolved, and removing bubbles in vacuum to obtain a glue solution for later use;
s2, uniformly stirring 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite and 1-2 parts of conductive agent to obtain powder; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm;
s3, adding 20% of the total mass of the glue solution prepared in the step S1 into the powder, and stirring until the powder is dispersed into particles;
s4, adding 50% of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring until the granular materials are kneaded;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring;
s6, adding deionized water to adjust the viscosity to 2000 plus 4500cp, finally adding 3-4 parts of binder, stirring, removing bubbles in vacuum, and sieving and discharging through a sieve with 200 meshes of 150 plus to obtain cathode slurry;
s7, coating the prepared negative electrode slurry on a current collector, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the cathode slurry is 160-170g/m2(ii) a The compacted density is 1-2g/cm3。
Further, in step S1, stirring with a planetary stirrer, wherein the revolution speed of the stirring is 35rpm, and the stirring time is 150 min; in step S2, the mixture was stirred with a planetary stirrer at a revolution speed of 20rpm, a rotation speed of 200rpm, and a stirring time of 30 min.
Further, in step S3, the revolution speed of stirring is 20rpm, the rotation speed is 500rpm, and the stirring time is 30 min; in step S4, the revolution speed of stirring is 40rpm, the rotation speed is 1500rpm, and the stirring time is 120 min; in step S5, the revolution speed of stirring is 30rpm, the rotation speed is 2000rpm, and the stirring time is 90 min; in step S6, the revolution speed of stirring was 30rpm, the rotation speed was 800rpm, and the stirring time was 30 min.
Further, the current collector is a copper foil with the thickness of 8-12 μm; in step S7, the drying temperature is 60-100 ℃.
Further, the parameters of the vacuum bubble removal are as follows: removing bubbles for 30 minutes under the vacuum degree of less than-0.08 MPa.
The invention has the following beneficial effects:
according to the invention, the negative electrode slurry system, the coating surface density and the compaction density of the negative electrode plate of the lithium ion battery are improved, so that the lithium ion battery using the negative electrode plate has the rapid charging performance of more than 4C, low temperature rise and excellent cycle performance.
According to the invention, the negative active material in the negative slurry adopts two kinds of artificial graphite with different particle sizes, wherein the proportion of the two kinds of artificial graphite is adjusted and mixed, so that the proportion of the small-particle-size artificial graphite is ensured to be large, the proportion of the large-particle-size artificial graphite is small, the artificial graphite with different particle sizes is fully contacted, more small gaps are ensured to exist in the negative plate, and the liquid absorption capacity of the negative plate and the conduction rate of lithium ions are improved. The impedance of the battery is effectively reduced through the synergistic effect of the two kinds of graphite with different particle sizes, so that the battery can be rapidly charged at a temperature of more than 4C, the temperature rise of the battery is controlled, and the cycle life is maintained.
The invention improves the coating surface density and the compaction density which are respectively 160-170g/m2And 1-2g/cm3The thickness and porosity of the negative plate are controlled by controlling the coating surface density and the compaction density, so that the resistance of lithium ions transferred between the positive electrode and the negative electrode in the charge-discharge process is reduced, and the rapid charge is realized.
The invention improves the homogenizing process, which comprises dry mixing, adding glue solution in three steps, adjusting viscosity, sieving, and controlling the stirring time, stirring speed, glue adding proportion and viscosity of the slurry to make the components of the slurry uniformly dispersed and not easy to agglomerate and settle.
Drawings
Fig. 1 is a result of a rate charge performance test of a battery of the present invention comprising the negative electrode sheet of example 1;
fig. 2 is a graph showing the cycle performance test of a battery according to the present invention, which includes the negative electrode sheet of example 1;
fig. 3 shows the charging performance test results of batteries containing different negative electrode sheets.
Detailed Description
In a first aspect, the present invention provides a lithium ion battery negative plate for rapid charging, including a current collector, on which a negative electrode slurry is coated, where the negative electrode slurry includes a negative electrode active material, and the negative electrode active material is first artificial graphite and second artificial graphite.
The particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; more preferably, the particle size D50 of the first artificial graphite is 7 μm, and the particle size D50 of the second artificial graphite is 11 μm.
The mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); more preferably, the mass ratio of the first artificial graphite to the second artificial graphite is 73: 24.
the coating surface density of the cathode slurry is 160-170g/m2More preferably, the coating surface density of the negative electrode slurry is 163g/m2. The inventors found in the research that, if the coating surface density of the negative electrode slurry meets the above specific value range, the obtained lithium ion battery can have both good quick charge performance and good cycle life performance. The coating surface density of the negative electrode slurry is more than 170g/m2The migration path of lithium ions in the charging process of the battery is lengthened, the interface impedance of the battery is increased, the polarization of the battery is increased, and the quick charging is not facilitated; the coating surface density of the negative electrode slurry is less than 160g/m2In time, the capacity of the battery is reduced, and the market competitiveness of the battery is influenced.
The compacted density of the negative electrode slurry is 1-2g/cm3More preferably, the anode slurry has a compacted density of 1.5g/cm3. In the research, the inventor finds that if the compacted density of the negative electrode slurry meets the requirement of the specific value range, the obtained lithium ion battery can have good quick charge performance and good cycle life performance. When the compacted density is less than 1g/cm3The negative plate is stripped and powdered, and the poor electronic conductivity during charging causes lithium precipitation, which affects the quick charging performance of the battery; the compaction density is too high, so that the contact among the components in the cathode slurry is too tight, the electrolyte is difficult to infiltrate, and the charging performance is poor.
In the present invention, the negative electrode slurry further includes a conductive agent, a thickener, and a binder.
Specifically, the negative electrode slurry comprises the following materials in parts by weight: 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite, 1-2 parts of a conductive agent, 1-2 parts of a thickening agent and 3-4 parts of a binder.
And a proper amount of conductive agent is beneficial to the conduction of lithium ions and reduces the resistance of the negative plate. The conductive agent is preferably superconducting carbon black, and the conductive agent of the present invention includes, but is not limited to, the materials listed above, and may be other materials which are not listed in the present invention but are well known to those skilled in the art, and may also be one or more of graphene, conductive graphite, carbon fiber, and carbon nanotube.
The thickener is preferably sodium carboxymethylcellulose, and the thickeners of the present invention include, but are not limited to, the materials listed above, as well as other materials not listed in the present invention but known to those skilled in the art.
The binder can increase the binding power between particles in the negative electrode slurry and the binding power between the negative electrode slurry and the current collector, and keeps good binding property in the volume change process of the charge and discharge negative electrode, thereby avoiding the falling of negative electrode powder, ensuring the structural integrity of the negative electrode plate and being beneficial to improving the cycle life of the battery. In the present invention, the binder is styrene-butadiene rubber emulsion, and the binder of the present invention includes, but is not limited to, the above listed materials, and may be other materials which are not listed in the present invention but are well known to those skilled in the art, for example, acrylic binder.
According to the invention, the negative electrode slurry system, the coating surface density and the compaction density of the negative electrode plate of the lithium ion battery are improved, so that the lithium ion battery using the negative electrode plate has the rapid charging performance of more than 4C, low temperature rise and excellent cycle performance.
In the invention, three parameters of a negative electrode slurry system, coating surface density and compaction density of the lithium ion battery negative electrode plate are correlated and inseparable, the three parameters influence the quick charge and cycle performance of the lithium ion battery together, and the following conditions are met: the negative active materials are first artificial graphite and second artificial graphite; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; the mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); the coating surface density of the cathode slurry is 160-170g/m2The compacted density of the negative electrode slurry is 1-2g/cm3The battery can improve the quick charging capability, and meanwhile, the battery also has good cycle service life; the technical effect is not the simple superposition of the three parameters, which is reflected in that the rapid charging capability and the long cycle life are greatly improved, and 1+1>The technical effect of 3' achieves an unexpected technical effect.
In the prior art, only one kind of artificial graphite is generally used as a negative electrode active material, and the lithium ion battery of the system generally has large resistance, high temperature rise during quick charge and low cycle life. The inventors have found through extensive studies that the use of artificial graphite having different particle diameters as a negative electrode active material has some influence on both the cycle performance and the quick charge capacity of a battery. According to the invention, the negative active material in the negative slurry adopts two kinds of artificial graphite with different particle sizes, and the proportion of the two kinds of artificial graphite is adjusted and mixed to ensure that the proportion of the small-particle-size artificial graphite is large and the proportion of the large-particle-size artificial graphite is small, so that the artificial graphite with different particle sizes is fully contacted, more small gaps are ensured to exist in the negative plate, and the liquid absorption capacity of the negative plate and the conduction rate of lithium ions are improved. The impedance of the battery is effectively reduced through the synergistic effect of the two kinds of graphite with different particle sizes, so that the battery can be rapidly charged at a temperature of more than 4C, the temperature rise of the battery is controlled, and the cycle life is maintained.
The invention improves the coating surface density and the compaction density which are respectively 160-170g/m2And 1.5g/cm3The thickness and porosity of the negative plate are controlled by controlling the coating surface density and the compaction density, so that the impedance of the lithium ion battery is favorably reduced, and the quick charging is favorably realized.
In a second aspect, the present invention further provides a method for preparing the above fast-charging lithium ion battery negative electrode sheet, including the following steps:
s1, adding 70-75 parts of deionized water and 1-2 parts of a thickening agent into a stirrer, stirring until the thickening agent is fully dissolved, and removing bubbles in vacuum to obtain a glue solution for later use;
s2, uniformly stirring 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite and 1-2 parts of conductive agent to obtain powder;
s3, adding 20% of the total mass of the glue solution prepared in the step S1 into the powder, and stirring until the powder is dispersed into particles;
s4, adding 50% of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring until the granular materials are kneaded;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring;
s6, adding deionized water to adjust the viscosity to 2000 plus 4500cp, finally adding 3-4 parts of binder, stirring, removing bubbles in vacuum, and sieving and discharging through a sieve with 200 meshes of 150 plus to obtain cathode slurry;
s7, coating the prepared negative electrode slurry on a current collector, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the cathode slurry is 160-170g/m2(ii) a The compacted density is 1-2g/cm3。
In step S1, a planetary stirrer is used for stirring, the stirring revolution speed is 35rpm, and the stirring time is 150 min; in step S2, a planetary stirrer is used for stirring, the revolution speed of stirring is 20rpm, the rotation speed is 200rpm, and the stirring time is 30 min; in step S3, the revolution speed of stirring is 20rpm, the rotation speed is 500rpm, and the stirring time is 30 min; in step S4, the revolution speed of stirring is 40rpm, the rotation speed is 1500rpm, and the stirring time is 120 min; in step S5, the revolution speed of stirring is 30rpm, the rotation speed is 2000rpm, and the stirring time is 90 min; in step S6, the revolution speed of stirring was 30rpm, the rotation speed was 800rpm, and the stirring time was 30 min.
The deionized water has high purity and less impurities, can ensure that the cathode active material, the binder and the conductive agent dissolved in the deionized water are not easy to generate chemical reaction, and the prepared battery has less side reaction and stable performance.
In the present invention, the current collector is preferably a copper foil, but is not limited thereto, and the current collector of the present invention may be other materials not listed in the present invention but known to those skilled in the art. The thickness of the copper foil is selected by comprehensively considering the factors of the copper foil such as the conductive capability, the heat generation/dissipation capability, the tensile strength, the light weight of the battery and the like, and the thickness of the copper foil is preferably 8-12 μm.
In step S7, the drying temperature is 60-100 deg.C, such as 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C.
The parameters of the vacuum bubble removal are preferably as follows: removing bubbles for 30 minutes under the vacuum degree of less than-0.08 MPa.
The prior art generally comprises dry mixing, one-step or two-step glue adding, viscosity adjusting and sieving, and the slurry prepared by the technology has the defects of uneven dispersion of all components, easy agglomeration and easy sedimentation. The invention improves the homogenizing process, which comprises dry mixing, adding glue solution in three steps, adjusting viscosity, sieving, and controlling the stirring time, stirring speed, glue adding proportion and viscosity of the slurry to make the components of the slurry uniformly dispersed and not easy to agglomerate and settle.
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Example 1
A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 72 parts of deionized water and 1.5 parts of thickening agent into a planetary mixer with the volume of 60L, stirring at the revolution speed of 35rpm for 150 min until the thickening agent is fully dissolved, removing bubbles for 30min under the vacuum degree of less than-0.08 Mpa to prepare glue solution for later use;
s2, adding 71 parts of first artificial graphite, 23 parts of second artificial graphite and 1.6 parts of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle size D50 of the first artificial graphite is 7 μm, and the particle size D50 of the second artificial graphite is 11 μm;
s3, adding 20 percent of the total mass of the glue solution prepared in the step S1 into the powder, and stirring for 30min at a revolution speed of 20rpm and a rotation speed of 500rpm until the powder is dispersed into particles;
s4, adding 50 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring for 120min at a revolution speed of 40rpm and a rotation speed of 1500rpm until the particles are kneaded with each other;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring for 90min at a revolution speed of 30rpm and a rotation speed of 2000rpm until the glue solution is uniformly dispersed;
s6, adding deionized water to adjust the viscosity to 2500cp, finally adding 3.6 parts of a binder, stirring for 30min at a revolution speed of 30rpm and a rotation speed of 800rpm, removing bubbles for 30min under a vacuum degree of less than-0.08 Mpa, and sieving and discharging through a 200-mesh screen to obtain negative electrode slurry;
s7, coating the prepared negative electrode slurry on a copper foil with the thickness of 8 mu m, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the negative electrode slurry is 163g/m2(ii) a The compacted density is 1.5g/cm3(ii) a The drying temperature is 60-100 ℃.
The conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
Example 2
A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 70 parts of deionized water and 1 part of thickening agent into a planetary mixer with the volume of 60L, stirring at the revolution speed of 35rpm for 150 min until the thickening agent is fully dissolved, and removing bubbles for 30min under the vacuum degree of less than-0.08 Mpa to prepare glue solution for later use;
s2, adding 70 parts of first artificial graphite, 21 parts of second artificial graphite and 1 part of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle size D50 of the first artificial graphite is 6 μm, and the particle size D50 of the second artificial graphite is 10 μm;
s3, adding 20 percent of the total mass of the glue solution prepared in the step S1 into the powder, and stirring for 30min at a revolution speed of 20rpm and a rotation speed of 500rpm until the powder is dispersed into particles;
s4, adding 50 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring for 120min at a revolution speed of 40rpm and a rotation speed of 1500rpm until the particles are kneaded with each other;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring for 90min at a revolution speed of 30rpm and a rotation speed of 2000rpm until the glue solution is uniformly dispersed;
s6, adding deionized water to adjust the viscosity to 2000cp, finally adding 3 parts of binder, stirring for 30min at a revolution speed of 30rpm and a rotation speed of 800rpm, removing bubbles for 30min under a vacuum degree of less than-0.08 Mpa, and sieving and discharging through a 150-mesh screen to obtain negative electrode slurry;
s7, coating the prepared negative electrode slurry on a copper foil with the thickness of 12 mu m, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the negative electrode slurry is 160g/m2(ii) a The compacted density is 1g/cm3(ii) a The drying temperature is 60-100 ℃.
The conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
Example 3
A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 75 parts of deionized water and 2 parts of thickening agent into a planetary mixer with the volume of 60L, stirring at the revolution speed of 35rpm for 150 min until the thickening agent is fully dissolved, and removing bubbles for 30min under the vacuum degree of less than-0.08 Mpa to prepare glue solution for later use;
s2, adding 73 parts of first artificial graphite, 25 parts of second artificial graphite and 2 parts of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle size D50 of the first artificial graphite is 8 μm, and the particle size D50 of the second artificial graphite is 12 μm;
s3, adding 20 percent of the total mass of the glue solution prepared in the step S1 into the powder, and stirring for 30min at a revolution speed of 20rpm and a rotation speed of 500rpm until the powder is dispersed into particles;
s4, adding 50 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring for 120min at a revolution speed of 40rpm and a rotation speed of 1500rpm until the particles are kneaded with each other;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring for 90min at a revolution speed of 30rpm and a rotation speed of 2000rpm until the glue solution is uniformly dispersed;
s6, adding deionized water to adjust the viscosity to 4500cp, finally adding 4 parts of binder, stirring for 30min at a revolution speed of 30rpm and a rotation speed of 800rpm, removing bubbles for 30min under a vacuum degree of less than-0.08 Mpa, and sieving and discharging through a 200-mesh screen to obtain negative electrode slurry;
s7, coating the prepared negative electrode slurry on a copper foil with the thickness of 8-12 mu m, drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the negative electrode slurry is 170g/m2(ii) a The compacted density is 2g/cm3(ii) a The drying temperature is 60-100 ℃.
The conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
Example 4
A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 74 parts of deionized water and 1 part of thickening agent into a planetary mixer with the volume of 60L, stirring at the revolution speed of 35rpm for 150 min until the thickening agent is fully dissolved, and removing bubbles for 30min under the vacuum degree of less than-0.08 Mpa to prepare glue solution for later use;
s2, adding 70 parts of first artificial graphite, 25 parts of second artificial graphite and 1 part of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle size D50 of the first artificial graphite is 7 μm, and the particle size D50 of the second artificial graphite is 12 μm;
s3, adding 20 percent of the total mass of the glue solution prepared in the step S1 into the powder, and stirring for 30min at a revolution speed of 20rpm and a rotation speed of 500rpm until the powder is dispersed into particles;
s4, adding 50 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring for 120min at a revolution speed of 40rpm and a rotation speed of 1500rpm until the particles are kneaded with each other;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring for 90min at a revolution speed of 30rpm and a rotation speed of 2000rpm until the glue solution is uniformly dispersed;
s6, adding deionized water to adjust the viscosity to 4500cp of 2000-plus material, finally adding 4 parts of binding agent, stirring for 30min at a revolution speed of 30rpm and a rotation speed of 800rpm, removing bubbles for 30min under a vacuum degree of less than-0.08 Mpa, and sieving and discharging through a sieve with 200 meshes of 150-plus material to obtain cathode slurry;
s7, coating the prepared negative electrode slurry on a copper foil with the thickness of 10 mu m, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the negative electrode slurry is 160g/m2(ii) a The compacted density is 1.5g/cm3(ii) a The drying temperature is 60-100 ℃.
The conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
Comparative example 1
Based on example 1, the difference is only that: step S2 in this comparative example 1 is: adding 94 parts of first artificial graphite and 1.6 parts of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle diameter D50 of the first artificial graphite is 7 μm.
Comparative example 2
Based on example 1, the difference is only that: step S2 in this comparative example 2 is: adding 94 parts of second artificial graphite and 1.6 parts of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle diameter D50 of the second artificial graphite is 11 μm.
Comparative example 3
Based on example 1, the difference is only that: the negative electrode slurry described in comparative example 3 had a coating area density of 200g/m2。
Comparative example 4
Based on example 1, the difference is only that: the coating areal density of the negative electrode slurry described in this comparative example 4 was 150g/m2。
Comparative example 5
Based on example 1, differsThe method is characterized in that: in comparative example 5, the compacted density was 0.8g/cm3。
Comparative example 6
Based on example 1, the difference is only that: in comparative example 6, the compacted density was 3g/cm3。
Comparative example 7
A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 72 parts of deionized water and 1.5 parts of thickening agent into a planetary mixer with the volume of 60L, stirring at the revolution speed of 35rpm for 150 min until the thickening agent is fully dissolved, removing bubbles for 30min under the vacuum degree of less than-0.08 Mpa to prepare glue solution for later use;
s2, adding 71 parts of first artificial graphite, 23 parts of second artificial graphite and 1.6 parts of conductive agent into a planetary mixer with the volume of 60L, and stirring for 30min at the revolution speed of 20rpm and the rotation speed of 200rpm to obtain uniformly mixed powder; wherein the particle size D50 of the first artificial graphite is 7 μm, and the particle size D50 of the second artificial graphite is 11 μm;
s3, adding all the glue solution prepared in the step S1 into the powder, and stirring for 240min at a revolution speed of 30rpm and a rotation speed of 2000rpm until the glue solution is uniformly dispersed;
s4, adding deionized water to adjust the viscosity to 2500cp, finally adding 3.6 parts of a binder, stirring for 30min at a revolution speed of 30rpm and a rotation speed of 800rpm, removing bubbles for 30min under a vacuum degree of less than-0.08 Mpa, and sieving and discharging through a 200-mesh screen to obtain negative electrode slurry;
s7, coating the prepared negative electrode slurry on a copper foil with the thickness of 8 mu m, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the negative electrode slurry is 163g/m2(ii) a The compacted density is 1.5g/cm3(ii) a The drying temperature is 60-100 ℃.
The conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
Test examples
The lithium ion battery negative electrode sheets prepared in the embodiment 1 and the comparative examples 1 to 7 are cut according to the same length and width standard, wound with a conventional positive electrode sheet and a diaphragm to prepare a winding core, assembled into batteries of the same type, injected with the same electrolyte, formed by the same formation process, and subjected to charging performance test and normal temperature cycle test, and the test results are shown in fig. 1 to 3.
In fig. 1, the charging performance test conditions are as follows: detecting the surface temperature of the battery by using a thermistor, standing the battery with the SOC of 30% at 25 ℃ for 10 minutes, discharging the battery to 2.8V at a constant current of 1C for 60 minutes, and charging the battery to a cut-off voltage of 4.2V at a constant current and a constant voltage of 1C when the surface temperature of the battery is recovered to 25 ℃, wherein the cut-off current is 0.05C; after standing for 10 minutes, discharging to 2.8V at a constant current of 1C, standing for 60 minutes, and after the surface temperature of the battery is recovered to 25 ℃, charging to 4.2V at a constant current and a constant voltage of 3C, and stopping the current to 0.05C; after standing for 10 minutes, discharging to 2.8V at a constant current of 1C, standing for 60 minutes, and after the surface temperature of the battery returns to 25 ℃, charging to 4.2V at a constant current and a constant voltage of 5C, and stopping the current at 0.05C; after standing for 10 minutes, discharging to 2.8V at a constant current of 1C, then standing for 60 minutes, and after the temperature of the battery returns to 25 ℃, charging to 4.2V at a constant current and a constant voltage of 8C, and stopping the current at 0.05C; and finishing the multiplying power test, wherein the temperature rise is the difference value between the highest temperature and 25 ℃ in the charging process of each multiplying power.
The charging performance test conditions in fig. 3 are:
5C, 4.2V constant current charge capacity percentage (%): the calculation formula is Cap.CC/Cap.CCCV, wherein the percentage of the capacity charged in the constant current stage to the total capacity in the whole constant current and constant voltage charging stage is shown in the 5C current constant current and constant voltage charging process of the battery;
5C, 4.2V constant-current constant-voltage charging temperature rise (DEG C): the difference value between the highest temperature of the battery and 25 ℃ in the 5C current constant current and constant voltage charging process of the battery is calculated as Tmax-25℃；
Capacity retention (%) after 500 cycles of 4C/-1C, 4.2V/2.8V: the battery is charged to 4.2V and 0.05C at a constant current and a constant voltage of 4C, then discharged to 2.8V at a constant current of 1C, and the ratio of the 500th discharge capacity to the nominal capacity (discharge capacity in the first cycle) is calculated as Cap.discharge (500 th)/Cap.discharge (1st) after 500 charge-discharge cycles.
As can be seen from fig. 1-2, the battery using the negative electrode sheet of example 1 can be rapidly charged at 4C or more while the temperature rise of the battery is controlled and the cycle life is maintained.
As can be seen from fig. 3, in the present invention, three parameters, namely, a negative electrode slurry system, a coating surface density, and a compaction density, of a negative electrode plate of a lithium ion battery are correlated and inseparable, and the three parameters jointly affect the quick charge and cycle performance of the lithium ion battery, and satisfy the following conditions: the negative active materials are first artificial graphite and second artificial graphite; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; the mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); the coating surface density of the cathode slurry is 160-170g/m2The compacted density of the negative electrode slurry is 1-2g/cm3The battery can improve the quick charging capability, and meanwhile, the battery also has good cycle service life; the technical effect is not the simple superposition of the three parameters, which is reflected in that the rapid charging capability and the long cycle life are greatly improved, and 1+1>The technical effect of 3' achieves an unexpected technical effect. Absent any of these three parameters, the battery cannot have good rapid charge capability, good cycling performance, and low temperature rise.
The above-mentioned embodiments only express the embodiments of the present invention, and the description is more specific and detailed, but not understood as the limitation of the patent scope of the present invention, but all the technical solutions obtained by using the equivalent substitution or the equivalent transformation should fall within the protection scope of the present invention.

Claims (8)

1. A lithium ion battery negative plate capable of being rapidly charged comprises a current collector, wherein negative slurry is coated on the current collector and comprises a negative active material; the negative electrode active material is characterized in that the negative electrode active material is first artificial graphite and second artificial graphite; the particle size of the first artificial graphiteD50 is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm; the mass ratio of the first artificial graphite to the second artificial graphite is (70-73): (21-25); the coating surface density of the cathode slurry is 160-170g/m2The compacted density of the negative electrode slurry is 1-2g/cm3；
The negative electrode slurry further comprises a conductive agent, a thickening agent and a binder;
the negative electrode slurry comprises the following materials in parts by weight: 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite, 1-2 parts of a conductive agent, 1-2 parts of a thickening agent and 3-4 parts of a binder.
2. The negative electrode sheet for a rapid-charge lithium ion battery according to claim 1, wherein the particle size D50 of the first artificial graphite is 7 μm, and the particle size D50 of the second artificial graphite is 11 μm; the mass ratio of the first artificial graphite to the second artificial graphite is 71: 23; the coating surface density of the negative electrode slurry is 163g/m2The compacted density of the negative electrode slurry is 1.5g/cm3。
3. The negative electrode sheet for a rapid-charge lithium-ion battery according to claim 1, wherein the conductive agent is superconducting carbon black; the thickening agent is sodium carboxymethyl cellulose; the binder is styrene-butadiene rubber emulsion.
4. A preparation method of a lithium ion battery negative plate capable of being rapidly charged comprises the following steps:
s1, adding 70-75 parts of deionized water and 1-2 parts of a thickening agent into a stirrer, stirring until the thickening agent is fully dissolved, and removing bubbles in vacuum to obtain a glue solution for later use;
s2, uniformly stirring 70-73 parts of first artificial graphite, 21-25 parts of second artificial graphite and 1-2 parts of conductive agent to obtain powder; the particle size D50 of the first artificial graphite is 6-8 μm, and the particle size D50 of the second artificial graphite is 10-12 μm;
s3, adding 20% of the total mass of the glue solution prepared in the step S1 into the powder, and stirring until the powder is dispersed into particles;
s4, adding 50% of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S3, and stirring until the granular materials are kneaded;
s5, adding 30 percent of the total mass of the glue solution prepared in the step S1 into the slurry prepared in the step S4, and stirring;
s6, adding deionized water to adjust the viscosity to 2000 plus 4500cp, finally adding 3-4 parts of binder, stirring, removing bubbles in vacuum, and sieving and discharging through a sieve with 200 meshes of 150 plus to obtain cathode slurry;
s7, coating the prepared negative electrode slurry on a current collector, and drying and rolling to prepare a lithium ion battery negative electrode sheet; wherein the coating surface density of the cathode slurry is 160-170g/m2(ii) a The compacted density is 1-2g/cm3。
5. The method for preparing a negative electrode sheet for a rapid-charging lithium ion battery according to claim 4, wherein in step S1, the negative electrode sheet is stirred by using a planetary stirrer, and the revolution speed of the stirring is 35rpm, and the stirring time is 150 min; in step S2, the mixture was stirred with a planetary stirrer at a revolution speed of 20rpm, a rotation speed of 200rpm, and a stirring time of 30 min.
6. The method for preparing a negative electrode sheet for a rapid-charging lithium ion battery according to claim 4, wherein in step S3, the revolution speed of stirring is 20rpm, the rotation speed is 500rpm, and the stirring time is 30 min; in step S4, the revolution speed of stirring is 40rpm, the rotation speed is 1500rpm, and the stirring time is 120 min; in step S5, the revolution speed of stirring is 30rpm, the rotation speed is 2000rpm, and the stirring time is 90 min; in step S6, the revolution speed of stirring was 30rpm, the rotation speed was 800rpm, and the stirring time was 30 min.
7. The method for preparing a negative electrode sheet for a rapid-charging lithium ion battery according to claim 4, wherein the current collector is a copper foil having a thickness of 8 to 12 μm; in step S7, the drying temperature is 60-100 ℃.
8. The method for preparing a negative electrode sheet of a rapid-charging lithium ion battery according to claim 4, wherein the parameters of the vacuum degassing are as follows: removing bubbles for 30 minutes under the vacuum degree of less than-0.08 MPa.
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