CN114420890A - Lithium supplementing method and application thereof - Google Patents
Lithium supplementing method and application thereof Download PDFInfo
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- CN114420890A CN114420890A CN202210084313.4A CN202210084313A CN114420890A CN 114420890 A CN114420890 A CN 114420890A CN 202210084313 A CN202210084313 A CN 202210084313A CN 114420890 A CN114420890 A CN 114420890A
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- lithium
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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
- 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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
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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
- 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
- H01M4/134—Electrodes based on metals, Si or alloys
Abstract
The invention provides a lithium supplementing method and application thereof, wherein the method comprises the following steps: (1) mixing lithium powder, a binder and a solvent to obtain lithium supplement slurry; (2) point-coating lithium-supplementing slurry on the surface of the negative pole piece to obtain the negative pole piece with point-coated particles; (3) the invention coats a layer of lithium supplement slurry on the surface of the negative pole piece in advance by a point coating method, further coats a layer of solid electrolyte slurry on the lithium supplement slurry layer, and the lithium powder is covered by the coating, thereby ensuring the safety and being applicable to mass production in large scale.
Description
Technical Field
The invention belongs to the technical field of semi-solid batteries, and relates to a lithium supplementing method and application thereof.
Background
The lithium ion battery has the advantages of high energy density, high output voltage, long cycle life, small environmental pollution and the like, and is widely applied to electric automobiles. With the rapid development of electric vehicles, there is an increasing demand for power sources having high energy density. At present, a ternary power battery system usually adopts high-nickel positive electrode matched graphite, and the mass energy density of the ternary power battery system is only close to 290 wh/kg; the negative electrode material of the lithium ion battery is mainly made of graphite, the theoretical specific capacity of the negative electrode material is only 372mAh/g, the graphite negative electrode cannot meet the requirement of an electric vehicle on energy density, and in order to further improve the energy density of the battery, a silicon material gradually becomes the first choice of the negative electrode material of the next generation of lithium ion battery, but the silicon negative electrode material has the defect that the first charge-discharge efficiency is low. In order to improve the first effect, the lithium supplement method is to plate a layer of lithium powder on the surface of the negative electrode by sputtering or spraying, or to supplement lithium on the surface of the negative electrode by using lithium foil.
CN113675363A discloses a method and device for lithium supplement for a pole piece, which comprises rolling two lithium foils by two roller mechanisms, rolling the lithium foils to a predetermined thickness through a first gap between a smooth roller and a concave-convex roller in the roller mechanism and attaching the lithium foils to the two concave-convex rollers, rolling the electrode sheet through a second gap between the two concave-convex rollers for one time, and attaching the lithium foils on the two concave-convex rollers to opposite sides of the electrode sheet during one time of rolling to form a pre-lithium pole piece, thereby completing the lithium supplement operation. However, lithium is supplemented by using lithium foil, the lithium supplementing amount is easy to be excessive, and a metal lithium plating layer can be formed on the surface of a negative electrode due to excessive lithium supplementing, so that the safety of the battery is influenced.
CN113675375A discloses a lithium-supplementing negative plate, a preparation method thereof and a lithium ion battery, wherein the preparation method comprises the following steps: (1) mixing graphite and silicon powder to obtain first negative electrode powder; (2) mixing a conductive agent, lithium powder and the first negative electrode powder obtained in the step (1) to obtain second negative electrode powder; (3) mixing a binder with the second negative electrode powder obtained in the step (2) to obtain third negative electrode powder; (4) rolling the third negative electrode powder obtained in the step (3) to obtain a lithium powder composite membrane; (5) and (4) mutually laminating the lithium powder composite membrane obtained in the step (4) and a negative current collector and rolling together to obtain the lithium-supplement negative plate. In the preparation method, the lithium powder is easy to splash to cause safety risk.
The lithium supplementing methods all have the problem of poor safety performance, so that the development of the lithium supplementing method with good safety performance and good lithium supplementing effect is necessary.
Disclosure of Invention
The invention aims to provide a lithium supplementing method and application thereof, the invention coats a layer of lithium supplementing slurry on the surface of a negative pole piece in advance by a spot coating method, then further coats a layer of solid electrolyte slurry on the lithium supplementing slurry layer, and lithium powder is covered by the coating, thereby ensuring the safety, being applicable to mass production in a large scale, and simultaneously, the solid electrolyte layer can also improve the liquid retention performance of a lithium ion battery, thereby improving the cycle performance of the battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for supplementing lithium, comprising the steps of:
(1) mixing lithium powder, a binder and a solvent to obtain lithium supplement slurry;
(2) point-coating lithium-supplementing slurry on the surface of the negative pole piece to obtain the negative pole piece with point-coated particles;
(3) and coating the solid electrolyte slurry on the surface of the negative pole piece with the spot coating particles, and rolling to obtain the negative pole piece after lithium supplement.
The invention adopts a spot coating method, the spot coating can ensure that the electrolyte layer is fully contacted with the pole piece, the good bonding of the electrolyte layer and the pole piece is ensured, a layer of solid electrolyte layer is coated on the cathode pole piece after the spot coating, and the solid electrolyte powder in the solid electrolyte layer is porous ceramic powder, so that the liquid retention performance of the lithium ion battery can be improved, and the cycle performance of the battery is improved. The lithium supplementing method disclosed by the invention is safe, can improve the lithium supplementing efficiency, can be applied to mass production in a large scale, and can improve the first efficiency of the battery.
Preferably, the particle size of the lithium powder in step (1) is 100-300 nm, for example: 100nm, 150nm, 200nm, 250nm, 300nm, etc.
Preferably, the solvent comprises any one or a combination of at least two of NMP, THF, acetone, DMF, DMAC or ethanol.
Preferably, the binder comprises any one of PVDF, PEO, PS or PMMA, or a combination of at least two of the same.
Preferably, the solid content of the lithium supplementing slurry in the step (1) is 35-85%, for example: 35%, 40%, 50%, 60%, 70%, 85%, etc.
The solid content of the lithium supplementing slurry can influence the lithium supplementing effect, the solid content of the lithium supplementing slurry is controlled to be 35-85%, the lithium supplementing effect is good, if the solid content of the lithium supplementing slurry is too low, uniform slurry cannot be formed well, and if the solid content of the lithium supplementing slurry is too high, the coating thickness is too thick and exceeds the required thickness.
Preferably, the viscosity of the lithium-supplementing slurry is 150 to 2000mPa.s, such as: 150mPa.s, 200mPa.s, 500mPa.s, 1000mPa.s or 2000mPa.s, etc.
Preferably, the dot coating in step (2) comprises blade coating or roll coating.
Preferably, the shape of the spot-coating particles in the step (2) is circular.
Preferably, the spot-coated particles have a diameter of 0.1 to 1mm, for example: 0.1mm, 0.3mm, 0.5mm, 0.8mm, 1mm, or the like.
Preferably, the dot-coated particles have a pitch of 0.5 to 3mm, for example: 0.5mm, 1mm, 2mm, 3mm or more.
Preferably, the thickness of the spot-coating particles is 3 to 10 μm, for example: 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, or 6 μm, etc.
Preferably, the solid electrolyte slurry of step (3) includes a polymer, an electrolyte and a solvent.
Preferably, the polymer comprises PVDF and/or PVDF-HFP.
Preferably, the electrolyte comprises any one of LLZO, LLZTO or LATP or a combination of at least two thereof.
Preferably, the mass fraction of the polymer is 10 to 30% based on 100% by mass of the solids in the solid electrolyte slurry, for example: 10%, 15%, 20%, 25%, 30%, etc.
Preferably, the mass fraction of the electrolyte is 70-90%, such as: 70%, 75%, 80%, 85%, 90%, etc.
Preferably, the solid electrolyte slurry has a solid content of 25 to 40%, for example: 25%, 28%, 30%, 35%, 40%, etc.
Preferably, the viscosity of the solid electrolyte slurry is 300 to 1000mpa.s, for example: 300mPa.s, 500mPa.s, 600mPa.s, 800mPa.s or 1000mPa.s, and the like.
Preferably, the coating thickness of the solid electrolyte slurry is 3-15 μm.
The thickness of the solid electrolyte slurry layer is controlled within the range, so that the lithium powder can be ensured to react in the solid electrolyte slurry layer, no danger is caused, and excessive lithium can not be caused on the surface of the pole piece.
Preferably, the step (3) is performed with a standing treatment in an inert atmosphere before rolling.
Preferably, the standing time is 20-30 h, for example: 20h, 22h, 25h, 28h or 30h and the like.
In a second aspect, the present invention provides a prelithiation negative electrode plate, which is prepared by the lithium supplement method according to the first aspect.
In a third aspect, the present invention provides a semi-solid battery comprising a pre-lithiated negative electrode sheet as described in the second aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) the lithium supplementing method is safe, the lithium powder is covered by the coating, the safety is guaranteed, the lithium supplementing method can be applied to mass production in a large scale, the lithium supplementing slurry is uniformly coated on the surface of the negative electrode, and the consistency of lithium supplementing is guaranteed.
(2) The first effect of the battery prepared by the lithium supplementing method can reach more than 91.37%, the charging DCR can reach less than 2.71m omega, and the 1C/1C cycle can reach more than 825 circles.
Drawings
FIG. 1 is a schematic representation of the dotted particles described in example 1, D being the particle size of the dotted particles and L being the pitch of the dotted particles.
FIG. 2 is a schematic process flow diagram of the lithium replenishment method described in example 1.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a lithium supplementing method, which comprises the following steps:
(1) mixing lithium powder with the particle size of 200nm, PVDF and NMP to obtain lithium supplement slurry, wherein the solid content of the lithium supplement slurry is 50%, and the viscosity of the lithium supplement slurry is 1000 mPa.s;
(2) point-coating lithium-supplementing slurry on the surface of the negative pole piece to obtain the negative pole piece with point-coated particles, wherein the point-coated particles are circular, the diameter D is 0.5mm, the hole pitch L is 2mm, the thickness is 5 mu m, and the schematic diagram of the point-coated particles is shown in figure 1;
(3) mixing LLZO, PVDF and NMP according to the mass ratio of 80:20 to obtain electrolyte slurry with the viscosity of 500mPa.s and the solid content of 30%, coating the solid electrolyte slurry on the surface of the negative pole piece with the spot coating particles, wherein the coating thickness is 8 mu m, standing in argon for 25h, and rolling to obtain the negative pole piece after lithium supplement.
The process flow diagram of the lithium supplementing method is shown in fig. 2.
In an argon protection environment, the lithium supplement coating speed is more than 10m/min, the lithium powder slurry input pipe adjusts the input flow according to the lithium supplement thickness requirement, meanwhile, a scraper or a hob carries out blade coating or roll coating in a point-shaped mesh roller, the lithium powder slurry is coated on a pole piece, then transfer coating or extrusion coating is adopted for coating, finally, the pole piece enters an oven, drying is carried out at the temperature of 40-90 ℃, and the temperature is adjusted according to the actual situation.
Example 2
The embodiment provides a lithium supplementing method, which comprises the following steps:
(1) mixing lithium powder with the particle size of 250nm, PEO and acetone to obtain lithium supplement slurry, wherein the solid content of the lithium supplement slurry is 60%, and the viscosity of the lithium supplement slurry is 1200 mPa.s;
(2) point-coating lithium-supplementing slurry on the surface of the negative pole piece to obtain the negative pole piece with point-coated particles, wherein the point-coated particles are circular, the diameter D is 0.6mm, the hole pitch L is 2.5mm, and the thickness is 6 microns;
(3) mixing LLZTO and PVDF-HFP with acetone according to the mass ratio of 75:25 to obtain electrolyte slurry with the viscosity of 600mPa.s and the solid content of 38%, coating the solid electrolyte slurry on the surface of the negative pole piece with the spot coating particles, wherein the coating thickness is 9 mu m, standing in argon for 25h, and rolling to obtain the negative pole piece after lithium supplement.
Example 3
This example is different from example 1 only in that the thickness of the dot-coated particles in step (2) is 3 μm, and other conditions and parameters are exactly the same as those in example 1.
Example 4
This example is different from example 1 only in that the thickness of the dot-coated particles in step (2) is 8 μm, and other conditions and parameters are exactly the same as those in example 1.
Example 5
This example is different from example 1 only in that the thickness of the electrolyte layer in step (3) is 16 μm, and other conditions and parameters are exactly the same as those in example 1.
Comparative example 1
The comparative example is different from the example 1 only in that the step (2) does not adopt a spot coating method, the lithium supplement slurry is uniformly coated on the surface of the negative pole piece, and other conditions and parameters are completely the same as those of the example 1.
Comparative example 2
This comparative example differs from example 1 only in that no electrolyte layer is applied and the other conditions and parameters are exactly the same as example 1.
And (3) performance testing:
the composition of the positive electrode is as follows: NCM811 SP PVDF 96:2:2, negative electrode composition: graphite: SiOx: conductive agent: adhesive: adhesive: thickener 91.5:3:1.0:2.25: 2.25. And (3) assembling the positive electrode and the negative electrode according to the assembly process of the lithium ion battery by taking the pre-lithiation negative electrode piece obtained in the embodiment 1-5 and the comparative example 1-2, and injecting an electrolyte, wherein the electrolyte comprises the following components: 1mol/L LiPF6/(EC: EMC: DMC 1:1:1), a 10Ah lithium ion battery was prepared.
1. Formation and first effect measurement: charging at 0.05C for 1h, charging at 0.1C for 1h, charging at 0.33C for 4.2V until current is cut off to 0.05C, and discharging at 0.33C for 2.8V
2. Charging DCIR test: 4C charging 10S
3. And (3) circulation: the 1C was charged to 4.2V, the 4.2V was charged to a constant voltage to cut-off current of 0.05C, the 1C was discharged to 2.8V, and the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, in examples 1 to 5, the first effect of the battery prepared by the lithium supplementing method of the present invention can reach 91.37% or more, the charging DCR can reach 2.71 mO or less, and the 1C/1C cycle can reach 825 cycles or more.
Compared with the embodiment 1 and the embodiment 3-4, the thickness of the spot coating particles can influence the lithium supplementing effect, the thickness of the spot coating particles is controlled to be 0.03-3 mm, the lithium supplementing effect is good, if the thickness of the spot coating particles is small, the lithium supplementing effect cannot be achieved, the first effect cannot be fully improved, and if the thickness of the spot coating particles is too large, the excessive lithium supplementing amount causes lithium precipitation and influences the safety of the battery.
Compared with the embodiment 1 and the embodiment 5, the coating thickness of the electrolyte layer can influence the lithium supplementing effect, the coating thickness of the electrolyte layer is controlled to be 3-15 μm, the lithium supplementing effect is good, if the coating thickness of the electrolyte layer is too large, the battery performance is influenced, and if the coating thickness of the electrolyte layer is too small, the lithium powder cannot be effectively covered.
Compared with the comparative example 1, the invention adopts the spot coating process, and the coating is coated after the spot coating, so that the electrolyte layer can be well bonded with the pole piece, and the situation of material falling caused by rolling can not occur.
Compared with the comparative example 2, the invention has the advantages that the electrolyte layer is arranged after spot coating, the liquid retention performance of the lithium ion battery can be improved, the cycle performance of the battery is improved, the lithium powder is covered by the coating, the safety is ensured, and the invention can be applied to mass production in a large scale.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A method of supplementing lithium, the method comprising the steps of:
(1) mixing lithium powder, a binder and a solvent to obtain lithium supplement slurry;
(2) point-coating lithium-supplementing slurry on the surface of the negative pole piece to obtain the negative pole piece with point-coated particles;
(3) and coating the solid electrolyte slurry on the surface of the negative pole piece with the spot coating particles, and rolling to obtain the negative pole piece after lithium supplement.
2. The lithium supplementing method according to claim 1, wherein the particle size of the lithium powder in the step (1) is 100 to 300 nm;
preferably, the solvent comprises any one or a combination of at least two of NMP, THF, acetone, DMF, DMAC, or ethanol;
preferably, the binder comprises any one of PVDF, PEO, PS or PMMA, or a combination of at least two of the same.
3. The lithium replenishing method of claim 1 or 2, wherein the solid content of the lithium replenishing slurry in the step (1) is 35-85%;
preferably, the viscosity of the lithium supplementing slurry is 150-2000 mPa.s.
4. The method according to any one of claims 1 to 3, wherein the dot coating in step (2) comprises blade coating or roll coating.
5. The lithium replenishing method of any one of claims 1 to 4, wherein the dot-coated particles of step (2) are circular in shape;
preferably, the diameter of the dot coating particles is 0.1-1 μm;
preferably, the pitch of the dot coating particles is 50-1000 μm;
preferably, the thickness of the dot coating particles is 1-6 μm.
6. The lithium replenishment method according to any one of claims 1 to 5, wherein the solid electrolyte slurry of step (3) comprises a polymer, an electrolyte and a solvent;
preferably, the polymer comprises PVDF and/or PVDF-HFP;
preferably, the electrolyte comprises any one of LLZO, LLZTO or LATP or a combination of at least two thereof.
7. The method according to claim 6, wherein the mass fraction of the polymer is 10 to 30% based on 100% by mass of the solid in the solid electrolyte slurry;
preferably, the mass fraction of the electrolyte is 70-90%;
preferably, the solid content of the solid electrolyte slurry is 25-40%;
preferably, the viscosity of the solid electrolyte slurry is 300-1000 mPa.s;
preferably, the coating thickness of the solid electrolyte slurry is 3-15 μm.
8. The lithium supplementing method according to any one of claims 1 to 7, wherein the step (3) is performed by a standing treatment in an inert atmosphere before rolling;
preferably, the standing treatment time is 20-30 h.
9. A prelithiation negative electrode tab, characterized in that it is made by a lithium supplementation method according to any one of claims 1 to 8.
10. A semi-solid battery comprising the prelithiated negative electrode tab of claim 9.
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