CN114023945A - Lithium ion battery cathode lithium supplementing method and application thereof - Google Patents
Lithium ion battery cathode lithium supplementing method and application thereof Download PDFInfo
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- CN114023945A CN114023945A CN202111324554.3A CN202111324554A CN114023945A CN 114023945 A CN114023945 A CN 114023945A CN 202111324554 A CN202111324554 A CN 202111324554A CN 114023945 A CN114023945 A CN 114023945A
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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
- H01M10/42—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
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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
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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
- H01M4/36—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
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/669—Steels
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- 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
Abstract
The invention provides a lithium ion battery cathode lithium supplementing method and application thereof. The lithium ion battery cathode lithium supplement method comprises the following steps: s1: dissolving a lithium-containing reducing agent in an organic solvent to prepare a lithium supplementing solution; s2: processing the negative pole piece by adopting a lithium supplementing solution; wherein, the lithium-containing reducing agent is selected from at least one of lithium naphthalene, lithium aluminum hydride and lithium borohydride. The lithium supplementing method can enable the negative pole piece to be embedded with a certain amount of lithium before the lithium ion battery is manufactured so as to make up the irreversible capacity loss caused by the SEI (solid electrolyte interphase) film formed by the negative pole in the first cycle of the lithium ion battery, and the negative pole material after lithium supplementation is beneficial to improving the first coulombic efficiency of the lithium ion battery and improving the cycle stability of the lithium ion battery in the process of embedding and extracting lithium ions; in addition, the lithium supplementing process can reduce the probability of reaction between a lithium source and water, improve the safety and stability of the lithium supplementing process and improve the energy of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery cathode lithium supplementing method and application thereof.
Background
The lithium ion battery is a secondary battery which mainly depends on lithium ions moving between a positive electrode and a negative electrode to work, and has the advantages of high energy density, high safety, long cycle life, environmental friendliness and the like, so the lithium ion battery is widely applied to the fields of portable electronic products, large-scale energy storage, electric automobiles and the like. At present, lithium ions of a positive electrode material are inserted into a negative electrode to form an SEI film during first charging, and the lithium ions cannot be reversibly extracted, so that the lithium ion battery has the problems of low first coulombic efficiency, poor cycle stability and the like.
Aiming at the problem of irreversible capacity caused by the SEI film formed by the first charge and discharge, the lithium supplement method is usually adopted at present, wherein the lithium supplement method for the negative electrode comprises the steps of spraying or coating passivated lithium powder on the surface of a negative electrode plate, rolling a pure lithium foil and the negative electrode plate together, forming a primary battery by using the negative electrode plate wetted by the lithium foil and the electrolyte, forming the primary battery by using the negative electrode plate wetted by the positive electrode plate and the electrolyte, and the like. However, the first coulombic efficiency and the cycle stability of the lithium ion battery prepared by the existing lithium supplement method still need to be further improved.
Because the specific surface area of the lithium powder is large, the lithium powder is easy to spray and is unsafe because of the risk of being inhaled by a human body; the lithium belt can not be pressed to be thin, so that excessive lithium supplement can be caused, and potential safety hazards exist after long-term use; the lithium is supplemented electrochemically, and the efficiency is too low. By liquid-solid phase lithium supplement, a uniform lithium-containing compound interface is generated on a solid-liquid interface, so that the side reaction of the negative pole piece in the electrolyte of the battery can be effectively improved, a certain lithium source is provided to make up the first irreversible lithium, and the safety problem in the lithium supplement process is solved.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a lithium ion battery cathode lithium supplementing method and application thereof. The lithium supplementing process is easier to control the safety problem, the probability of the reaction of a lithium source and water can be reduced, the safety and stability of the lithium supplementing process are improved, the requirement on the processing environment is reduced, the obtained lithium supplementing negative plate is applied to the lithium ion battery, the energy of the lithium ion battery can be improved, the first coulomb efficiency of the lithium ion battery is improved, and the cycling stability of the lithium ion battery is improved.
The invention provides a lithium ion battery cathode lithium supplementing method, which comprises the following steps:
s1: dissolving a lithium-containing reducing agent in an organic solvent to prepare a lithium supplementing solution;
s2: and (4) processing the negative pole piece by adopting a lithium supplementing solution.
The lithium supplementing method adopts the lithium supplementing solution containing the lithium-containing reducing agent to supplement lithium for the negative pole piece, and compared with other inorganic lithium salts (such as lithium bicarbonate, lithium nitride and the like) and organic lithium salts (such as n-butyl lithium, phenyl lithium and the like), the lithium-containing reducing agent with strong reducibility can enable a certain amount of lithium to be embedded into the negative pole piece formed by lithium supplementation, so that irreversible capacity loss caused by an SEI (solid electrolyte interphase) film formed by the negative pole in the first cycle of the lithium ion battery is well compensated. Experiments prove that: the lithium-containing reducing agent is adopted for lithium supplement, so that the first coulomb efficiency of lithium ion can be obviously improved, and the cycle stability of the battery can be improved.
The lithium-containing reducing agent used in the present invention should have strong reducing property, and is not strictly limited, and may be, for example, at least one selected from lithium naphthalene, lithium aluminum hydride, and lithium borohydride. Further, the organic solvent in which the lithium-containing reducing agent is dissolved is also not particularly limited, and may be selected from at least one of tetrahydrofuran, ethanol, and diethyl ether, for example, and tetrahydrofuran is preferable.
In the present invention, the concentration of the lithium-containing reducing agent in the lithium replenishing solution may be controlled to 0.01 to 0.2mol/L, preferably 0.01 to 0.05mol/L, and more preferably 0.01 to 0.15 mol/L. In the preparation of the lithium-supplementing solution, the preparation can be carried out in a specific environment such as a glove box with water content less than 1ppm and oxygen content less than 1 ppm. The lithium supplement is to make up irreversible lithium in the first cycle, the effect of lithium supplement can be controlled by adjusting the concentration of the lithium-containing reducing agent, and better first coulombic efficiency can be obtained by supplementing a specific amount of lithium.
The method for processing the negative pole piece by the lithium supplement solution is not strictly limited, and a conventional lithium supplement method in the field can be adopted; specifically, step S2 of the present invention may include: placing the negative pole piece in a lithium supplement solution for soaking for 1-2 hours, and then carrying out DMC leaching and drying; the drying conditions are not particularly restricted, and the drying temperature may be, for example, 60 to 100 ℃ and the drying time may be 1 to 4 hours.
In the invention, the amount of lithium supplement to the negative pole piece can be accurately controlled according to the concentration of the lithium-containing reducing agent in the lithium supplement solution and the soaking time of the negative pole piece in the lithium supplement solution; lithium is supplemented in a manner of soaking the negative pole piece in the lithium supplementing solution, so that uniform lithium supplementation of the negative pole piece is facilitated. The DMC leaching is mainly used for removing the residual lithium supplement solution on the negative pole piece, and the leaching can be carried out in a conventional mode; further, the drying conditions are not strictly limited, and the drying conditions conventional in the art may be employed.
In the invention, the cathode pole piece can be prepared by adopting a conventional method in the field; specifically, the preparation method of the negative electrode plate may include: coating a negative active material on a current collector to prepare a negative pole piece; wherein, the negative active material can be selected from at least one of metallic lithium and alloy materials thereof, hard carbon, soft carbon, natural graphite, artificial graphite, Si, SiO, SiC, silicon-carbon composite material and lithium silicide composite material; the current collector may be selected from at least one of copper foil, carbon-coated copper foil, stainless steel mesh, and nickel foil.
The invention also provides a lithium-supplement negative pole piece which is prepared by the lithium-supplement method for the negative pole of the lithium ion battery; preferably, the lithium supplementing amount of the lithium supplementing negative pole piece is 3-6%. The lithium supplement amount is beneficial to improving the energy of the lithium ion battery, improving the first coulombic efficiency of the lithium ion battery and improving the cycle stability of the lithium ion battery.
The invention also provides a lithium ion battery, which comprises the lithium-supplementing negative pole piece; preferably, the first coulombic efficiency of the lithium ion battery is 90-94%; the retention rate of the 500-week circulation capacity is 88-96%.
The implementation of the invention has at least the following advantages:
1. the lithium ion battery negative pole lithium supplementing method can enable the negative pole piece to be embedded with a certain amount of lithium before the lithium ion battery is manufactured so as to make up the irreversible capacity loss caused by the SEI (solid electrolyte interphase) film formed by the negative pole in the first cycle of the lithium ion battery, and the negative pole material after lithium supplementation is beneficial to improving the first coulombic efficiency of the lithium ion battery and improving the cycle stability of the lithium ion battery in the process of embedding and extracting lithium ions;
2. the lithium supplement amount of the lithium supplement negative pole piece is 3-6%, and the first coulombic efficiency of the lithium ion battery containing the lithium supplement negative pole piece is 90-94%; the 500-week circulation capacity retention rate is 88-96%, and the comprehensive performance is excellent;
3. the lithium supplementing process is easier to control the safety problem, the probability of the reaction of a lithium source and water can be reduced, the safety and stability of the lithium supplementing process are improved, the requirement on the processing environment is reduced, the obtained lithium supplementing negative plate is applied to the lithium ion battery, the energy of the lithium ion battery can be improved, the first coulomb efficiency of the lithium ion battery is improved, and the cycling stability of the lithium ion battery is improved.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms also include the plural forms unless the context clearly dictates otherwise, and further, it is understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The lithium supplementing method of the embodiment comprises the following steps:
a) preparation of negative electrode plate
According to a conventional mode, preparing the silicon oxide/graphite negative pole piece by sizing, coating, baking, rolling and slitting SiO, graphite, CMC, acrylate and SBR.
b) Preparation of lithium-supplementing solution
And adding naphthalene lithium into a tetrahydrofuran solvent in a glove box with the water content of less than 1ppm and the oxygen content of less than 1ppm to prepare a lithium supplement solution, wherein the concentration of the naphthalene lithium is 0.10 mol/L.
c) Prelithiation
And b), putting the silicon oxide/graphite negative pole piece prepared in the step a) into the lithium supplement solution prepared in the step b) for soaking for 2 hours.
d) Cleaning of
Leaching the pre-lithiated silicon oxide/graphite negative pole piece obtained in the step c) by using a DMC solvent, and then drying to obtain a lithium-supplement negative pole piece; through detection, the lithium supplement amount of the lithium supplement negative pole piece is 3%.
Example 2
The lithium supplementing method of the embodiment comprises the following steps:
a) preparation of negative electrode plate
According to a conventional mode, the graphite negative pole piece is prepared by sizing, coating, baking, rolling and slitting the artificial graphite, the CMC and the SBR.
b) Preparation of lithium-supplementing solution
And adding naphthalene lithium into a tetrahydrofuran solvent in a glove box with the water content of less than 1ppm and the oxygen content of less than 1ppm to prepare a lithium supplement solution, wherein the concentration of the naphthalene lithium is 0.14 mol/L.
c) Prelithiation
And b), putting the graphite negative pole piece prepared in the step a) into the lithium supplement solution prepared in the step b) for soaking for 2 hours.
d) Cleaning of
Leaching the graphite negative pole piece pre-lithiated in the step c) by using a DMC solvent, and then drying to prepare a lithium supplement negative pole piece; through detection, the lithium supplement amount of the lithium supplement negative pole piece is 5%.
Example 3
The lithium supplementing method of the embodiment comprises the following steps:
a) preparation of negative electrode plate
According to a conventional mode, the graphite negative pole piece is prepared by sizing, coating, baking, rolling and slitting the artificial graphite, the CMC and the SBR.
b) Preparation of lithium-supplementing solution
Lithium aluminum hydride is added into tetrahydrofuran solvent in a glove box with water content less than 1ppm and oxygen content less than 1ppm to prepare lithium supplementing solution, wherein the concentration of the lithium aluminum hydride is 0.12 mol/L.
c) Prelithiation
And b), putting the graphite negative pole piece prepared in the step a) into the lithium supplement solution prepared in the step b) for soaking for 2 hours.
d) Cleaning of
Leaching the graphite negative pole piece pre-lithiated in the step c) by using a DMC solvent, and then drying to prepare a lithium supplement negative pole piece; through detection, the lithium supplement amount of the lithium supplement negative pole piece is 4%.
Comparative example 1
The negative electrode piece of silica/graphite prepared in step a) of example 1 was used as a control.
Comparative example 2
The graphite negative electrode piece prepared in step a) of example 2 was used as a control.
Test example 1
The negative electrode pieces prepared in examples 1 to 3 and comparative examples 1 to 2 were mixed with 1mol/L LiPF6The three-component mixed solvent is prepared according to the following formula of EC: DMC, EMC 1: 1: 1 (volume ratio) of the mixed solution is used as electrolyte, and a metal lithium sheet is used as a counter electrode to prepare LIR2430 in a glove box filled with argon gas for capacity test and cycle performance test.
The capacity test and the cycle performance test of each lithium ion battery are carried out according to the following methods:
the charge and discharge voltage range is 0.005-2V, the charge and discharge rate is 0.1C to test the capacity, and the charge and discharge rate is 1C to test the cycle performance.
The results are shown in Table 1.
Table 1 performance test results of each lithium ion battery
From the data in table 1 above, it can be seen that:
1. compared with each comparative example, the first discharge capacity, the first coulombic efficiency and the 500-week circulation capacity retention rate in the examples 1 to 3 are obviously improved;
2. from the results of examples 1-3, it can be seen that the concentration of the lithium replenishing solution has a certain influence on lithium replenishment, and the lithium replenishing effect is reduced after the concentration is increased to a certain degree, which indicates that the concentration of the lithium replenishing solution has a better effect only when being controlled within a proper range;
3. compared with the comparative examples 1-2, the first coulombic efficiency of the examples 1-2 is obviously improved, and the lithium supplement provides part of lithium to increase the reversible capacity.
In summary, the lithium ion battery negative electrode lithium supplementing method of the present invention can enable a certain amount of lithium to be inserted into the negative electrode plate before the lithium ion battery is manufactured so as to compensate for the irreversible capacity loss caused by the SEI film formed on the negative electrode in the first cycle of the lithium ion battery, and the negative electrode material after lithium supplementation is beneficial to improving the first coulombic efficiency of the lithium ion battery and improving the cycle stability of the lithium ion battery in the process of lithium ion insertion and extraction.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A lithium ion battery cathode lithium supplement method is characterized by comprising the following steps:
s1: dissolving a lithium-containing reducing agent in an organic solvent to prepare a lithium supplementing solution;
s2: processing the negative pole piece by adopting a lithium supplementing solution;
preferably, the lithium-containing reducing agent is selected from at least one of lithium naphthalene, lithium aluminum hydride, and lithium borohydride.
2. The lithium ion battery negative electrode lithium supplementing method according to claim 1, wherein the organic solvent is at least one selected from tetrahydrofuran, ethanol and diethyl ether, and is preferably tetrahydrofuran.
3. The lithium ion battery negative electrode lithium supplementing method according to claim 1, wherein the concentration of the lithium-containing reducing agent in the lithium supplementing solution is 0.01-0.2mol/L, preferably 0.01-0.15 mol/L.
4. The lithium ion battery negative electrode lithium supplementing method according to claim 1, wherein step S1 is performed in an environment with a water content of <1ppm and an oxygen content of <1 ppm.
5. The lithium ion battery negative electrode lithium supplementing method according to claim 1, wherein step S2 includes: and (3) placing the negative pole piece in a lithium supplement solution for soaking for 1-2 hours, and then carrying out DMC leaching and drying.
6. The lithium ion battery negative electrode lithium supplementing method according to claim 1, wherein the preparation method of the negative electrode sheet comprises the following steps: and coating the negative active material on a current collector to prepare a negative pole piece.
7. The lithium ion battery negative electrode lithium supplementing method according to claim 6, wherein the negative electrode active material is at least one selected from metallic lithium and alloy materials thereof, hard carbon, soft carbon, natural graphite, artificial graphite, Si, SiO, SiC, silicon carbon composite material, and lithium silicide composite material.
8. The lithium ion battery negative electrode lithium supplementing method according to claim 6, wherein the current collector is selected from at least one of copper foil, carbon-coated copper foil, stainless steel mesh and nickel foil.
9. A lithium-supplement negative electrode piece is characterized by being prepared by the lithium-supplement method for the negative electrode of the lithium ion battery according to any one of claims 1 to 8.
10. A lithium ion battery comprising the lithium-supplemented negative electrode tab of claim 9.
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