CN111261836A - Method for pre-lithiating negative electrode of lithium ion battery and preparation method of pre-lithiated lithium ion battery - Google Patents
Method for pre-lithiating negative electrode of lithium ion battery and preparation method of pre-lithiated lithium ion battery Download PDFInfo
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- CN111261836A CN111261836A CN201911338394.0A CN201911338394A CN111261836A CN 111261836 A CN111261836 A CN 111261836A CN 201911338394 A CN201911338394 A CN 201911338394A CN 111261836 A CN111261836 A CN 111261836A
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for pre-lithiation of a negative electrode of a lithium ion battery, which comprises the following steps of: A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state; B) and B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment. The application also provides a preparation method of the lithium ion battery subjected to pre-lithiation. According to the lithium ion battery, the negative plate is pre-lithiated, the SEI film can be generated, lithium removed from the positive electrode in the formation process can not be consumed for forming the SEI film, active lithium consumed by reaction with electrolyte and lithium consumed by other irreversible side reactions can be reduced, irreversible capacity is reduced, and the first efficiency and capacity of the lithium ion battery are improved.
Description
Technical Field
The invention relates to the technical field of manufacturing of high-energy-density lithium ion batteries, in particular to a method for pre-lithiating a negative electrode of a lithium ion battery and a method for preparing the pre-lithiated lithium ion battery.
Background
Lithium ion batteries have the advantages of high energy density, good cycle performance, and the like, and thus have received much attention. With the popularization of mobile internet devices, the popularization of electric automobiles and other electric vehicles, and the development of aerospace technologies such as unmanned aerial vehicles and space detectors, the performance of lithium ion batteries faces higher development requirements, and how to improve the volume energy density and the mass energy density of lithium batteries becomes a key breakthrough direction of high-performance lithium ion batteries.
Most researchers have used silicon-based anode materials with high gram-capacity for the anode. However, the silicon-based negative electrode material with high gram capacity has low first efficiency, and the energy density of 400Wh/kg is difficult to reach under the design condition of a limit process, so that the method for solving the problem only carries out pre-lithiation on the negative electrode material or the battery cell, and improves the first efficiency. Meanwhile, the control of water content in the manufacturing process of the battery cell is also particularly important, and the current pole piece is time-consuming, labor-consuming and high in cost when dried. The moisture content also has a large impact on the overall performance of the battery. However, some of the existing prelithiation technologies either cannot be prepared in large quantities or are time-consuming, which is not favorable for improving the production efficiency of the cell and saving the cost.
Disclosure of Invention
The invention aims to provide a method for pre-lithiating a lithium ion battery cathode, which can solve the problem of low initial efficiency of a lithium ion battery and can improve the preparation efficiency of a pre-lithiated battery cell.
In view of the above, the present application provides a method for prelithiation of a negative electrode of a lithium ion battery, comprising the steps of:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) and B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment.
Preferably, the water content of the negative electrode sheet is 300ppm to 2000 ppm.
Preferably, the water content of the negative electrode plate is 1000ppm to 1600 ppm.
Preferably, the thickness of the lithium foil is 2-10 μm.
Preferably, standing is further included after the vacuum pumping treatment, and the standing time is 5-72 hours.
Preferably, the standing time is 10-24 h.
The application also provides a preparation method of the lithium ion battery subjected to pre-lithiation, which comprises the following steps:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment;
C) and D) assembling the negative plate and the positive plate obtained in the step B), injecting electrolyte, standing, and then forming into a component and a capacity to obtain the lithium ion battery.
Preferably, the standing temperature is 20-75 ℃.
Preferably, the standing temperature is 25-45 ℃.
Preferably, the formation and capacity grading process specifically comprises the following steps:
standing the lithium ion battery after standing for t1, then charging to U1 with a current constant current of 0.02C, then discharging to U2 with a current constant current of 0.1C, then charging to a current of 0.02C with a voltage constant voltage of U2, standing for t2, discharging to U3 with a voltage constant current of 0.1C, decompressing, exhausting, sealing, and finishing formation;
t1 is 12-24 h, U1 is 3.5-4.3V, U2 is 4.6V, U3 is 2-2.5V, and t2 is 1-5 min.
The application provides a method for pre-lithiation of a lithium ion battery cathode, which comprises the steps of firstly pressing a lithium foil on a cathode plate, wherein the cathode plate is in a semi-dry state, and then placing the cathode plate in a closed bag for vacuumizing treatment; according to the method, the negative plate is subjected to pre-lithiation by the steps, residual trace moisture in the negative plate is used for reacting with the ultrathin metal lithium foil, the products are lithium carbonate, lithium silicate, lithium fluoride and residual active metal lithium, and the components are just main components of SEI (solid electrolyte interphase), so that lithium separated from the positive electrode in the formation process cannot be consumed to form an SEI (solid electrolyte interphase) film, the irreversible capacity is reduced, and the primary efficiency and capacity of the battery are improved.
Drawings
FIG. 1 is a schematic flow chart of the lithium ion battery preparation according to the present invention;
FIG. 2 is a photograph of the negative electrode sheet before and after pre-lithiation in example 1 of the present invention;
FIG. 3 is a graph comparing the first efficiency and capacity of a lithium ion battery prepared in example 1 of the present invention;
FIG. 4 is a graph comparing the cycling curves of a lithium ion battery prepared in example 1 of the present invention and a lithium ion battery prepared in a comparative example;
fig. 5 is a graph comparing the primary efficiency and capacity of the lithium ion battery prepared in example 5 of the present invention and the lithium ion battery prepared in the comparative example.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the problems of prelithiation in the prior art, the application provides a method for prelithiation of a negative electrode of a lithium ion battery, which forms an SEI film by introducing a lithium foil and controlling the water content of a negative electrode plate, thereby avoiding the problem that the first efficiency and the first capacity are influenced by the extraction of positive electrode lithium. Specifically, the method for pre-lithiating the negative electrode of the lithium ion battery comprises the following steps:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) and B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment.
In the process of pre-lithiation of the negative electrode of the lithium ion battery, firstly, a lithium foil is pressed on a negative electrode sheet, and the negative electrode sheet is in a semi-dry state; in the process, the lithium foil is mainly used as a lithium source for forming an SEI film, and the thickness of the lithium foil is 2-10 mu m. The negative plate is in a semi-dry state, specifically, the water content of the negative plate is 300ppm to 2000ppm, and in a specific embodiment, the water content of the negative plate is 1000ppm to 1600 ppm. The micro moisture on the surface of the negative plate reacts with the ultrathin lithium metal foil, and the product is the main component of the SEI film, so that the consumption of positive lithium for SEI formation and some other side reactions are avoided. In the process, the moisture content of the negative plate is strictly controlled, the moisture content in the lithium ion battery is not random, if the moisture content is too much, water and electrolyte can generate side reaction, the gas generation seriously influences the capacity exertion of the battery, and the cost of the pre-lithiation is increased. The water content of the negative plate realizes the pre-lithiation process on one hand, and obviously improves the flatulence in the formation component capacity and the later cycle process on the other hand; therefore, the water content of the negative plate is strictly controlled in the pre-lithiation process. For the ultrathin lithium foil, active lithium still remains because the lithium foil does not completely react with water in the negative plate in the pre-lithiation process, a part of the lithium foil forms an SEI film, and the remaining active lithium can also be embedded into the negative electrode to realize further lithium supplement by utilizing the action of potential difference of the electrolyte after the SEI film is formed. The application of the ultrathin lithium foil can remove trace moisture in the lithium ion battery, and the effect of subsequent moisture on electrolyte is guaranteed. The above-mentioned pressing process, which is well known to those skilled in the art, may be performed on one side of the negative electrode sheet, or may be performed on both sides of the negative electrode sheet, and the present application is not particularly limited thereto.
The application then places the negative plate in a sealed bag for vacuuming to avoid oxidation of the negative plate. In the practical application process, the negative plate is preferably arranged in an aluminum plastic film packaging bag and vacuumized on an automatic sealing machine for later direct use in the assembly of the lithium ion battery. The vacuum-pumping treatment is followed by still standing treatment, wherein the still standing time is 5-72 hours, and more specifically, the still standing time is 10-24 hours. The standing time is a pre-lithiation process of the lithium ion battery, and is a process of generating an SEI film by moisture in the negative plate and the lithium foil.
After the negative electrode of the lithium ion battery is pre-lithiated, the present application performs the preparation of the lithium ion battery, specifically as shown in fig. 1, and the present application also provides a preparation method of the lithium ion battery subjected to the pre-lithiation, which includes the following steps:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment;
C) and D) assembling the negative plate and the positive plate obtained in the step B), injecting electrolyte, standing, and then forming into a component and a capacity to obtain the lithium ion battery.
In the present application, after the lithium ion battery is pre-lithiated, conventional preparation is performed, and the step a) and the step B) are described in detail above, and are not described herein again.
According to the invention, after the negative plate is pre-lithiated, the negative plate and the positive plate are assembled and then injected with electrolyte, and the mixture is stood and then formed into a partial volume, thus obtaining the lithium ion battery. The positive electrode sheet is well known to those skilled in the art, and specific materials thereof are not particularly limited in this application. The assembly and the electrolyte injection process are conventional technical means for those skilled in the art, and the present application is not particularly limited thereto. The standing temperature is 20-75 ℃, and more specifically, the standing temperature is 25-45 ℃. And standing and then forming into a component and a volume to obtain the lithium ion battery. The formation component capacity is a conventional method for the formation component capacity of a lithium ion battery in the prior art, for example, the lithium ion battery after standing is stood for t1, then is charged to U1 by a current constant current of 0.02C, then is discharged to U2 by a current constant current of 0.1C, then is charged to a current of 0.02C by a voltage constant voltage of U2, is stood for t2, and is discharged to U3 by a current constant current of 0.1C, and is subjected to pressure reduction, air suction and sealing, and formation is finished; the t1 is 12-24 h, U1 is 3.5-4.3V, U2 is 4.6V, U3 is 2-2.5V, and t2 is 1-5 min.
The application provides a method for pre-lithiating a negative electrode of a lithium ion battery and a preparation method of the lithium ion battery subjected to pre-lithiation; the method for pre-lithiating the lithium ion battery negative electrode material can solve the problem of low first efficiency of a high-energy density lithium ion battery, and can improve the preparation efficiency of a pre-lithiated battery cell.
In order to further understand the present invention, the method for prelithiating the negative electrode of the lithium ion battery and the method for preparing the lithium ion battery provided by the present invention are described in detail below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
Lithium-rich manganese is used as a positive electrode material, and silicon carbon is used as a negative electrode material;
coating the positive electrode and the negative electrode on a current collector; tabletting and cutting to obtain a negative plate (with the water content of 600-1000 ppm) and a positive plate; pressing an ultrathin lithium foil (3-7 microns) on the cut negative plate by a rolling method, vacuumizing, standing for 12 hours, and assembling the battery with the cut lithium-rich positive plate; and then injecting electrolyte, standing for 12-24 hours at 20-45 ℃, and then carrying out formation and grading to obtain the lithium ion battery.
Fig. 2 is photographs of the negative electrode sheet of this example before and after pre-lithiation, and it can be seen from fig. 2 that the lithium foil on the surface of the negative electrode sheet is used up after pre-lithiation.
Example 2
The same preparation method as in example 1 is adopted, except that: the negative electrode material is hard carbon; the water content of the negative plate is 1000 ppm-1500 ppm; the thickness of the lithium foil is 5 to 10 μm.
Example 3
The same preparation method as in example 1 is adopted, except that: the negative electrode material is graphite; the water content of the negative plate is 1200ppm to 1600 ppm; the thickness of the lithium foil is 4 to 11 μm.
Example 4
The same preparation method as in example 1 is adopted, except that: the cathode material is a tin base; the water content of the negative plate is 1350ppm to 1600 ppm; the thickness of the lithium foil is 2-8 μm.
Example 5
The same preparation method as in example 1 is adopted, except that: the positive electrode material was ternary NCM 811S 85E. The test result shows that the reversible capacity of the lithium ion battery prepared by the embodiment is 1150 mAh/g.
The above-described positive electrode material may be any conventional positive electrode material such as ternary materials (NCM111, NCM532, NCM622, NCM811, and NCA), lithium iron phosphate, and lithium cobaltate.
Comparative example
Taking a lithium-rich manganese anode material and silicon carbon as a cathode material;
coating the positive electrode and the negative electrode on a current collector, taking silicon carbon as a negative electrode material, then assembling into a soft package battery, and carrying out formation and grading operation to record the first efficiency.
Lithium-rich manganese is used as a positive electrode material, and silicon carbon is used as a negative electrode material; coating the positive electrode and the negative electrode on a current collector, and pressing, cutting, laminating and packaging to obtain the battery. And carrying out chemical composition and grading treatment on the battery.
The slurry viscosity was 4500 and the solid content was 63% for the positive electrode (LRM: SP: KS-6: PVDF: 96%: 0.8%: 1.2%: 2%); the negative electrode was found to have an N/P ratio of 1.08 (SIO: SP: SWCNT: PAA: 94%: 1.04%: 0.06%: 4.9%).
As shown in fig. 3, fig. 3 is a graph comparing the first efficiency and capacity of the lithium ion battery prepared in example 1 and the lithium ion battery prepared in the comparative example; FIG. 4 is a graph comparing the cycling curves of a lithium ion battery prepared in example 1 of the present invention and a lithium ion battery prepared in a comparative example; fig. 5 is a comparison graph of the first efficiency and the capacity of the lithium ion battery prepared in example 5 of the present invention and the lithium ion battery prepared in the comparative example, and it can be seen from fig. 3 to 5 that the first efficiency is improved by 8 to 15%, the capacity is improved by 12 to 20%, the energy is improved by 12 to 20%, the highest energy density can reach 400Wh/kg, and the energy density in the lithium ion battery published at present is the highest.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method of prelithiation of a lithium ion battery negative electrode, comprising the steps of:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) and B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment.
2. The method according to claim 1, wherein the water content of the negative electrode sheet is 300ppm to 2000 ppm.
3. The method according to claim 1 or 2, wherein the water content of the negative electrode sheet is 1000ppm to 1600 ppm.
4. The method of claim 1, wherein the lithium foil has a thickness of 2 to 10 μm.
5. The method according to claim 1, wherein the vacuuming treatment is followed by standing for 5-72 hours.
6. The method according to claim 5, wherein the standing time is 10-24 h.
7. A method of preparing a prelithiated lithium ion battery comprising the steps of:
A) pressing lithium foil on the negative plate; the negative plate is in a semi-dry state;
B) placing the negative plate obtained in the step A) in a closed bag for vacuumizing treatment;
C) and D) assembling the negative plate and the positive plate obtained in the step B), injecting electrolyte, standing, and then forming into a component and a capacity to obtain the lithium ion battery.
8. The method according to claim 7, wherein the temperature of the standing is 20 to 75 ℃.
9. The method according to claim 7 or 8, wherein the temperature of the standing is 25 to 45 ℃.
10. The preparation method according to claim 7, wherein the process of component capacity is specifically as follows:
standing the lithium ion battery after standing for t1, then charging to U1 with a current constant current of 0.02C, then discharging to U2 with a current constant current of 0.1C, then charging to a current of 0.02C with a voltage constant voltage of U2, standing for t2, discharging to U3 with a voltage constant current of 0.1C, decompressing, exhausting, sealing, and finishing formation;
t1 is 12-24 h, U1 is 3.5-4.3V, U2 is 4.6V, U3 is 2-2.5V, and t2 is 1-5 min.
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| CN111912736A (en) * | 2020-07-23 | 2020-11-10 | 蜂巢能源科技有限公司 | Method for testing negative electrode degassing capacity of lithium ion battery |
| CN111969179A (en) * | 2020-07-31 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Pre-lithiation method, high-energy-density lithium ion battery and preparation method of high-energy-density lithium ion battery |
| CN112701253A (en) * | 2020-12-29 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Pre-lithiation composite negative plate and preparation method and application thereof |
| CN112786971A (en) * | 2021-02-04 | 2021-05-11 | 湖南立方新能源科技有限责任公司 | Preparation method of negative electrode pre-lithiation lithium ion battery and negative electrode pre-lithiation lithium ion battery |
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| CN112786971A (en) * | 2021-02-04 | 2021-05-11 | 湖南立方新能源科技有限责任公司 | Preparation method of negative electrode pre-lithiation lithium ion battery and negative electrode pre-lithiation lithium ion battery |
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