CN113594419B - Lithium supplementing method for negative electrode and application thereof - Google Patents

Lithium supplementing method for negative electrode and application thereof Download PDF

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CN113594419B
CN113594419B CN202110855682.4A CN202110855682A CN113594419B CN 113594419 B CN113594419 B CN 113594419B CN 202110855682 A CN202110855682 A CN 202110855682A CN 113594419 B CN113594419 B CN 113594419B
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lithium
negative electrode
battery
crystal
supplementing
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CN113594419A (en
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刘良海
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Hunan Lifang New Energy Science and Technology 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
    • 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
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • 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
    • H01M4/38—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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention provides a lithium supplementing method of a negative electrode and application thereof, comprising the following steps of: s1, manufacturing a battery, and charging the battery to ensure that a negative electrode of the battery separates lithium to obtain lithium crystals; s2, stripping the lithium crystal obtained in the step S1; s3, ball-milling the lithium crystal obtained in the step S2, preparing the lithium crystal into a mixed solution, and coating the mixed solution on at least one surface of the negative electrode to be supplemented with lithium; and completing lithium supplement of the negative electrode. Compared with the conventional lithium powder for lithium supplement, the lithium supplement method adopts the compact granular lithium crystal for lithium supplement, the specific surface area is far smaller than that of the lithium powder, and the granules are not easy to agglomerate, so that the problem of easy agglomeration of the lithium powder in the early mixing process is solved.

Description

Lithium supplementing method for negative electrode and application thereof
Technical Field
The invention relates to the field of lithium batteries, in particular to a lithium supplementing method for a negative electrode and application thereof.
Background
Lithium ion batteries are widely used by people because of their characteristics of high operating voltage, large specific energy, long cycle life, no memory effect, etc. At present, lithium ion batteries are generally applied to the fields of 3C digital consumer electronics, power batteries and the like. However, with the popularization of lithium ion batteries, the performance requirements of consumers on lithium ion batteries are continuously improved, the graphite negative electrode cannot meet the requirements of consumers due to the limitation of the energy of the graphite negative electrode, and is concerned more and more due to the higher energy density of silicon, the silicon negative electrode is also expected to be a negative electrode material for effectively improving the energy density of the lithium ion batteries, but the first cycle efficiency of silicon is low, and the performance of the silicon negative electrode is improved by a common lithium supplement technology at present. The commonly used lithium supplementing method is carried out by means of lithium powder, lithium tapes or lithium slurry, wherein the lithium powder and lithium slurry method still has the problems that the slurry is difficult to disperse and the lithium powder is safe to use.
In view of the above, it is necessary to provide a technical solution to the above problems.
Disclosure of Invention
One of the objects of the present invention is: the invention provides a lithium supplementing method for a negative electrode, which solves the problem that slurry is difficult to disperse in the conventional lithium supplementing technology for the negative electrode, and effectively solves the problem that the slurry is easy to agglomerate in the mixing process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lithium supplementing method for a negative electrode comprises the following steps:
s1, manufacturing a battery, and charging the battery to ensure that lithium is separated from a negative electrode of the battery to obtain lithium crystals;
s2, stripping the lithium crystal obtained in the step S1;
s3, ball-milling the lithium crystal obtained in the step S2, preparing the lithium crystal into a mixed solution, and coating the mixed solution on at least one surface of the negative electrode to be supplemented with lithium; and completing lithium supplement of the negative electrode.
Preferably, in step S1, the particle size of the obtained lithium crystal is 1 μm to 1cm.
Preferably, in step S1, the negative electrode of the battery includes a negative electrode current collector and a conductive carbon layer coated on at least one surface of the negative electrode current collector, and the lithium crystals are precipitated on the surface of the conductive carbon layer.
Preferably, in step S2, the exfoliated lithium crystals are doped with a carbon source.
Preferably, in step S3, an electrolyte solvent is mixed with the lithium crystal to prepare a mixed solution, and the mixed solution is diluted and coated on at least one surface of the negative electrode to be supplemented with lithium.
Preferably, in step S3, the coating method is spray coating or gravure printing.
Preferably, in step S3, the electrolyte solvent includes at least one of ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl methyl carbonate, ethyl propionate, propyl propionate, ethyl acetate, ethyl n-butyrate, and γ -butyrolactone.
Preferably, in step S3, after the coating is completed, the temperature is decreased, so that the electrolyte solvent is cooled to be solid.
Another object of the present invention is to provide a method for manufacturing a battery, including the method for supplementing lithium to the negative electrode described above.
It is a further object of the present invention to provide a lithium ion battery manufactured by the above-described method for manufacturing a battery, wherein the negative electrode active material of the lithium ion battery is a graphite material or a silicon-based material.
Compared with the prior art, the invention has the beneficial effects that:
1) The lithium supplement method provided by the invention takes the fact that lithium returns from the battery as a guide idea, obtains a lithium supplement source from the battery, breaks through a conventional lithium supplement design idea, and takes a lithium crystal which is forbidden by the battery originally as the lithium supplement source.
2) In addition, the lithium supplementing method provided by the invention also adopts the mixing of the electrolyte solvent and the lithium crystal, and the electrolyte solvent can form a certain protection effect on the lithium crystal after being cooled and solidified, so that the lithium crystal is prevented from being oxidized or reacting with water, and the use safety performance of the battery is improved.
Drawings
FIG. 1 is a flow chart of a lithium supplementing method according to the present invention.
FIG. 2 is an SEM image of a lithium crystal obtained by the present invention.
Fig. 3 is a graph of capacity retention rates of example 1 of the present invention and comparative example 1.
Fig. 4 is a graph showing discharge curves of example 1 of the present invention and comparative example 1.
Detailed Description
The first aspect of the present invention provides a method for supplementing lithium to a negative electrode, as shown in fig. 1, including the following steps:
s1, manufacturing a battery, and charging the battery to ensure that lithium is separated from a negative electrode of the battery to obtain lithium crystals;
s2, stripping the lithium crystal obtained in the step S1;
s3, ball-milling the lithium crystal obtained in the step S2, preparing the lithium crystal into a mixed solution, and coating the mixed solution on at least one surface of the negative electrode to be supplemented with lithium; and completing lithium supplement of the negative electrode.
Further, in step S1, the particle size of the obtained lithium crystal is 1 μm to 1cm. The particle size of the lithium crystal can be adjusted by a lithium separation method, the charging current of the lithium separation can be 0.01-3C, the voltage can be 2-5V according to different voltages of the anode and cathode active materials, and the charging time can be 1 min-12 h. The amount of lithium supplement can be determined according to the need. The particle size of the obtained lithium crystal is not limited too much, and when the particle size is too large, the lithium crystal is milled to be small in the subsequent ball milling process.
Further, in step S1, the negative electrode of the battery includes a negative electrode current collector and a conductive carbon layer coated on at least one surface of the negative electrode current collector, and the lithium crystals are precipitated on the surface of the conductive carbon layer. The negative current collector may be a copper foil, and the conductive carbon layer may be a conductive layer of conductive carbon or graphite. The carbon-containing conducting layer on the surface of the negative electrode has the advantages that the conducting layer can conduct electricity and further enables lithium crystals to be separated out, the separated lithium crystals can be attached to the surface of carbon, and when the lithium crystals are subsequently separated, the carbon and the lithium crystals are separated together, so that the separation is more convenient, and the industrial production and application are more facilitated.
Further, in step S2, the exfoliated lithium crystals are doped with a carbon source. The carbon source is the carbon on the conductive carbon layer. The active material layer coated on the battery negative plate is one or more of graphite, soft carbon, hard carbon, carbon fiber, mesocarbon microbeads, silicon-based materials and the like. Wherein, the graphite can be selected from one or more of artificial graphite, natural graphite and modified graphite; silicon-based materials are also typically doped with carbon source materials such as graphite. Even if the stripped lithium crystal is doped with a carbon source, the lithium supplementing effect cannot be influenced, the carbon source also belongs to a common active material of the negative electrode, and the doped carbon source is also beneficial to protecting the active lithium crystal and improving the safety performance of the battery.
Further, in step S3, an electrolyte solvent is mixed with the lithium crystal to prepare a mixed solution, and the mixed solution is diluted and then coated on at least one surface of the negative electrode to be supplemented with lithium. The electrolyte solvent is adopted as a solvent to mix and dilute the lithium crystal to prepare a mixed solution, the electrolyte solvent and the lithium crystal are mixed together to play a role in protecting the lithium crystal, and the electrolyte solvent can be rapidly cooled to become a solid and is frozen to cover the surface of the lithium crystal or is mixed with the lithium crystal to be frozen together so as to play a role in protecting the lithium crystal, avoid the contact of the lithium crystal with air and improve the safety performance of a lithium supplementing environment and a battery. The diluted concentration can be adjusted according to the content of the lithium supplement, and is not limited too much here.
Further, in step S3, the coating method is spray coating or gravure printing. The specific method can be referred to the existing lithium supplement coating process of the negative electrode, and redundant description is omitted here.
Further, in step S3, the electrolyte solvent includes at least one of Ethylene Carbonate (EC), propylene Carbonate (PC), diethyl carbonate (DEC), ethyl Methyl Carbonate (EMC), ethyl Propionate (EP), propyl Propionate (PP), ethyl Acetate (EA), ethyl n-butyrate (EB), and γ -butyrolactone (GBL). Further preferably, the electrolyte solvent is Ethylene Carbonate (EC) or Propylene Carbonate (PC). Still more preferably, the electrolyte solvent is Ethylene Carbonate (EC).
Further, in step S3, after the coating is completed, the temperature is decreased, so that the electrolyte solvent is cooled to be solid. The Ethylene Carbonate (EC) is an organic solvent with excellent performance, can dissolve various polymers, is used as a lithium crystal mixing and diluting solvent, can be cooled after coating, and is cooled into a solid to be coated on the surface of the lithium crystal or mixed with the lithium crystal, so that the lithium crystal is protected to a certain extent, and the lithium crystal is prevented from being oxidized or reacted with water to reduce the lithium supplementing effect.
A second aspect of the present invention provides a method for manufacturing a battery, including the method for supplementing lithium to the negative electrode described in any one of the above.
In a third aspect of the present invention, there is provided a lithium ion battery manufactured by the above-described method for manufacturing a battery, wherein a negative electrode active material of the lithium ion battery is a graphite material or a silicon-based material. Particularly for silicon-based materials, the problem of low first cycle efficiency exists, and after lithium is supplemented by the lithium supplementing method, lithium ions can supplement lithium ions consumed by an SEI (solid electrolyte interface) film formed by a negative electrode in time, so that the first cycle efficiency of the silicon-based negative electrode is effectively improved, and more possibilities are provided for application of the silicon-based negative electrode.
Wherein, the positive active material of the lithium ion battery can be a compound including but not limited to a chemical formula such as Li a Ni x Co y M z O 2-b N b (wherein 0.95. Ltoreq. A. Ltoreq.1.2. X>0,y ≧ 0, z ≧ 0, and x + y + z =1,0 ≦ b ≦ 1, M is selected from one or more of Mn, al in combination, N is selected from one or more of F, P, S in combination), the positive electrode active material may also be a combination including but not limited to LiCoO 2 、LiNiO 2 、LiVO 2 、LiCrO 2 、LiMn 2 O 4 、LiCoMnO 4 、Li 2 NiMn 3 O 8 、LiNi 0.5 Mn 1.5 O 4 、LiCoPO 4 、LiMnPO 4 、LiFePO 4 、LiNiPO 4 、LiCoFSO 4 、CuS 2 、FeS 2 、MoS 2 、NiS、TiS 2 And the like. The positive electrode active material may be further modified, and the method of modifying the positive electrode active material is known to those skilled in the art, for example, the positive electrode active material may be modified by coating, doping, and the like, and the material used in the modification may be one or a combination of more of Al, B, P, zr, si, ti, ge, sn, mg, ce, W, and the like.
The separator used in the lithium ion battery may be any material suitable for a lithium ion battery separator in the art, and for example, may be one or a combination of more of polyethylene, polypropylene, polyvinylidene fluoride, aramid, polyethylene terephthalate, polytetrafluoroethylene, polyacrylonitrile, polyimide, polyamide, polyester, natural fiber, and the like.
In order to make the technical solutions and advantages of the present invention clearer, the present invention and its advantages will be described in further detail below with reference to specific embodiments and drawings of the specification, but the embodiments of the present invention are not limited thereto.
Example 1
A lithium supplementing method for a negative electrode comprises the following steps:
s1, coating a layer of conductive carbon or a conductive layer mixed with graphite on a copper foil to prepare a negative plate, coating a positive active substance on at least one surface of a positive current collector to prepare a conventional positive plate, sequentially placing the positive plate, a diaphragm and the negative plate to be wound or laminated to prepare a battery, and charging the battery to ensure that the negative electrode of the battery separates lithium to obtain a lithium crystal; wherein, the charging current can be 0.01-3C, the voltage can be 2-5V, and the charging time can be 1 min-12 h;
s2, stripping the obtained lithium crystal from the copper foil, and stripping the conductive carbon layer on the copper foil together;
s3, ball-milling the lithium crystal and carbon obtained in the step S2 to obtain a mixture of lithium crystal particles and carbon with a certain particle size, wherein EC is used as a solvent for mixing to prepare a mixed solution containing lithium crystal, carbon and EC, diluting, and coating the mixed solution on at least one surface of copper foil of the negative electrode to be compensated with lithium by adopting a spraying or gravure printing mode;
and S4, after coating is finished, cooling to enable the electrolyte solvent to be cooled into a solid, and finishing lithium supplement of the negative electrode.
The lithium supplementing method is applied to a battery manufacturing method to obtain the lithium ion battery.
Comparative example 1
A method for manufacturing a battery, which is a conventional battery manufacturing method and to which lithium is not added to the negative electrode.
The performance test was performed on the lithium ion batteries obtained in example 1 and comparative example 1, and the test results are shown in fig. 2 to 4.
As can be seen from FIG. 2, the crystal structure of the lithium source lithium prepared by the invention is compact strip-shaped particles, the particles are not easy to agglomerate, the particles are easy to disperse when the particles are dispersed to prepare a mixed solution, and the difficulty of lithium supplement is greatly reduced.
As can be seen from the test results of FIG. 3 and FIG. 4, the capacity retention rate of the battery is higher and the number of cycles is more after the lithium is supplemented by the lithium supplementing method of the present invention. Therefore, if the lithium supplementing method is applied to the silicon-based negative electrode lithium ion battery, the first cycle efficiency of silicon can be effectively improved, and more possibilities are provided for the application of the silicon-based negative electrode battery.
In conclusion, the lithium supplementing method provided by the invention takes the fact that lithium comes back from the battery as a guiding idea, and takes the lithium crystal particles generated in the battery as a lithium supplementing source to supplement lithium, so that the traditional lithium supplementing method of lithium powder, a lithium belt and a lithium sheet is replaced, the problem that lithium powder slurry is difficult to disperse is solved, the problem of safe use of lithium is effectively solved, and the lithium supplementing method is simpler.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious modifications, substitutions or alterations based on the present invention will fall within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (7)

1. A lithium supplementing method for a negative electrode is characterized by comprising the following steps:
s1, manufacturing a battery, charging the battery, and separating lithium from a negative electrode of the battery to obtain lithium crystals, wherein the negative electrode of the battery comprises a negative electrode current collector and a conductive carbon layer coated on at least one surface of the negative electrode current collector, and the lithium crystals are separated out of the surface of the conductive carbon layer;
s2, stripping the lithium crystal obtained in the step S1, wherein the stripped lithium crystal is doped with a carbon source;
s3, ball-milling the lithium crystal obtained in the step S2, mixing an electrolyte solvent with the lithium crystal to prepare a mixed solution, and coating the mixed solution on at least one surface of the negative electrode to be supplemented with lithium after dilution; and completing lithium supplement of the negative electrode.
2. The method for supplementing lithium to the negative electrode according to claim 1, wherein the lithium crystal obtained in step S1 has a particle size of 1 μm to 1cm.
3. The method for supplementing lithium to the negative electrode according to claim 1, wherein the coating method in step S3 is spray coating or gravure printing.
4. The method for supplementing lithium to the negative electrode according to claim 1, wherein in step S3, the electrolyte solvent comprises at least one of ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl methyl carbonate, ethyl propionate, propyl propionate, ethyl acetate, ethyl n-butyrate, and γ -butyrolactone.
5. The method for supplementing lithium to the negative electrode according to claim 3 or 4, wherein in step S3, after the coating is completed, the temperature is reduced so that the electrolyte solvent is cooled to be solid.
6. A method for producing a battery, comprising the method for supplementing lithium to the negative electrode according to any one of claims 1 to 5.
7. A lithium ion battery manufactured by the method for manufacturing a battery according to claim 6, wherein a negative electrode active material of the lithium ion battery is a graphite material or a silicon-based material.
CN202110855682.4A 2021-07-28 2021-07-28 Lithium supplementing method for negative electrode and application thereof Active CN113594419B (en)

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