CN112038579A - Metal lithium composite electrode, preparation method thereof and electrochemical energy storage device - Google Patents
Metal lithium composite electrode, preparation method thereof and electrochemical energy storage device Download PDFInfo
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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
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 discloses a metal lithium composite electrode, a preparation method thereof and an electrochemical energy storage device, wherein the metal lithium composite electrode comprises a negative current collector and an active material layer at least loaded on one side of the negative current collector; the active material layer comprises the following substances in percentage by mass: 0.5-20% of metal lithium, 60-95% of negative electrode material, 1-10% of binder and 1-10% of conductive agent; the invention also discloses an electrochemical energy storage device containing the metal lithium composite electrode. The metal lithium composite electrode prepared by the method does not contain any solvent component, so that the side reaction of the lithium ion battery caused by solvent residue in the charging and discharging processes is avoided, and the potential safety hazard is eliminated; according to the invention, metal lithium is introduced into the negative active material through a dry process, and the lithium can be used as a lithium source except for the positive electrode in the first charging process to compensate the irreversible capacity loss caused by the first charging and discharging, so that the capacity of the lithium ion battery is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a metal lithium composite electrode, a preparation method thereof and an electrochemical energy storage device.
Background
Lithium ion batteries are widely applied to electric vehicles at present, and higher requirements are also put forward on the energy density and the safety performance of the lithium ion batteries. If the energy density of the battery is further improved, an active material with higher specific capacity needs to be adopted, and for a negative active material, silicon and oxide thereof are more feasible to be adopted as the negative active material.
However, in the case of a negative electrode material using silicon and its oxide as an active material, a significant portion of lithium inserted into the negative electrode from the positive electrode participates in an irreversible reaction during the first charge, resulting in a low ratio of reversible capacity to charge capacity, which limits its application. It is necessary to compensate for lithium consumed by the anode reaction by additionally supplementing lithium element.
The current popular strategy is to adopt metal lithium powder on the surface of the negative electrode material (CN1889288A, CN 103022413). Are typically placed on a surface in two ways: 1. the lithium powder needs to be dissolved in a solvent to prepare a slurry, and then the slurry is coated on the surface of the negative electrode material layer, but the contained solvent cannot be completely volatilized, and part of the solvent is remained in an electrode, so that the influence on the battery is realized. 2. The lithium powder is directly sprayed on the surface of the negative electrode material layer, and because the lithium powder is light, the lithium powder is difficult to be completely attached to the surface, and a small part of the lithium powder can permeate the air, so that the lithium battery has great potential safety hazard. Meanwhile, lithium on the surface of the negative electrode material can only be in full contact with the outermost layer of the negative electrode material, so that the problem that the lithium cannot be completely reacted exists, and redundant residual lithium powder which cannot be reacted can form lithium dendrites on the surface, so that the safety performance is influenced.
Disclosure of Invention
In view of the defects of the prior art, the present invention aims to provide a lithium metal composite electrode, which can significantly improve the capacity of a lithium ion battery and avoid the problems in the background art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a lithium metal composite electrode comprises a negative electrode current collector and an active material layer loaded on at least one side of the negative electrode current collector; the active material layer comprises the following substances in percentage by mass: 0.5-20% of metal lithium, 60-95% of negative electrode material, 1-10% of binder and 1-10% of conductive agent; the adhesive comprises a main adhesive and an auxiliary adhesive, wherein the main adhesive accounts for 40-80% of the total mass of the adhesive.
According to a preferable technical scheme, the negative current collector is one of an electrolytic copper foil, a rolled copper foil, a copper-nickel alloy foil, a copper surface nickel-plated foil and a copper foil with holes.
Preferably, the thickness of the negative current collector is 4-12 μm. The thickness range can meet certain processing performance, and meanwhile, the proportion of the whole current collector in the metal lithium composite electrode plate is not high, and the energy density of the metal lithium composite electrode plate is not influenced.
Preferably, the thickness of the active material layer is 50 to 500 μm.
Preferably, the lithium metal is at least one of lithium powder, a lithium metal tape, a lithium metal rod, lithium metal particles and a lithium metal foil, the surface of which is coated with a lithium carbonate layer.
Preferably, the negative electrode material is at least one of graphite, soft carbon, hard carbon, tin oxide, silicon and silicon oxide. The content of lithium metal varies depending on the loss of irreversible capacity caused by the first charge and discharge of each negative electrode material. According to the theoretical discharge capacity of the metallic lithium 3860mAh/g, the content of the metallic lithium to be added can be calculated. If the irreversible capacity lost by the initial charge and discharge is 608mAh/g for a silica negative electrode, 100g of silica and 60800mAh for the irreversible capacity lost by the charge and discharge are required, and the amount of lithium metal required is about 15.7 g.
Preferably, the primary binder is polytetrafluoroethylene, and the secondary binder is one of polyvinylidene fluoride, hexafluoropropylene and polyethylene oxide. The secondary binder is firstly mixed with the metal lithium, the negative electrode material and the conductive agent to form the bonding between material particles and particles, then the primary binder is added for continuous mixing, and fibrillation is carried out through high-speed shearing force to form a bonding network similar to a spider web, so that all materials of the electrode active layer are bonded with one another to form a high-viscosity mixture similar to a dough, and the mixture can be directly pressed on a current collector without any solvent. In this process, the mixture needs to be heated to a temperature, typically 180 ℃ to 230 ℃, at which the lithium metal becomes very soft (close to liquid) and can be uniformly dispersed in the mixture.
As a preferable technical solution, the conductive agent is at least one of conductive carbon black, conductive acetylene black, graphene, and carbon nanotubes.
The invention also aims to provide a preparation method of the metal lithium composite electrode, which belongs to a dry process, namely, the preparation method does not involve a solvent, and comprises the following steps: primarily mixing the lithium metal, the negative electrode material, the secondary binder and the conductive agent, adding the main binder, and continuously mixing to obtain a mixed material; extruding and stirring the mixed materials by using a double-screw extruder, shearing at a high speed, simultaneously increasing the temperature to 180-230 ℃, and cooling to ensure that high-viscosity mixed slurry is formed; and pressing the mixed slurry on one side or two sides of the negative current collector to obtain the metal lithium composite electrode.
The invention also provides an electrochemical energy storage device which is a lithium ion battery and comprises a positive plate, a negative plate, a diaphragm, electrolyte and a shell, wherein the negative plate is the metal lithium composite electrode.
The negative electrode current collector such as electrolytic copper foil or rolled copper foil, the lithium metal such as lithium powder, lithium metal ribbon or lithium metal rod coated with a lithium carbonate layer, the negative electrode material such as graphite, soft carbon, hard carbon, tin oxide, silicon oxide or silicon oxide, and various binders listed above are commercially available.
Compared with the prior art, the invention has the following beneficial effects:
the metal lithium composite electrode prepared by the method does not contain any solvent component, so that the side reaction of the lithium ion battery caused by solvent residue in the charging and discharging processes is avoided, and the potential safety hazard is eliminated; in the preparation process, metal lithium is introduced into the negative active material through a dry process, and the lithium can be used as a lithium source except for the positive electrode in the first charging process to compensate the irreversible capacity loss caused by the first charging and discharging of the negative electrode, so that the capacity of the lithium ion battery is improved. In addition, the preparation process of the metal lithium composite electrode is simple, the input cost is low, and industrial production can be realized.
Drawings
Fig. 1 is a charge and discharge curve of a lithium ion battery made of the metallic lithium composite electrode prepared in example 1 and a general lithium ion battery.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. 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. The material proportions in the following examples are in percent by mass unless otherwise specified.
Example 1
Mixing a silicon oxide/graphite negative electrode material (a mixture of silicon oxide and graphite negative electrode powder in a weight ratio of 2: 8), metal lithium powder with a lithium carbonate layer coated on the surface, polyethylene oxide and conductive agent superconducting carbon black in a ratio of 92%, 2% and 1%, uniformly stirring, adding 3% of polytetrafluoroethylene, extruding and stirring by adopting a double screw, carrying out high-speed shearing at a stirring speed of 3000rpm/min, increasing the temperature to 180 ℃ at the same time, continuing for 90 minutes, and cooling to room temperature to form high-viscosity mixed slurry. And pressing the slurry on two sides of a copper foil with the thickness of 150 mu m to prepare the lithium metal composite negative electrode. Then assembled with a conventional NCM positive electrode, PE separator, and a conventional commercial electrolyte was added. And (5) preparing the lithium ion battery.
Example 2
Mixing a silicon oxide/graphite negative electrode material (a mixture of silicon oxide and graphite negative electrode powder in a weight ratio of 2: 8), cubic metal lithium particles with the side length of 2cm, polyethylene oxide and a conductive agent superconducting carbon black in a ratio of 92%, 2% and 1%. After the mixture is uniformly stirred, 3 percent of polytetrafluoroethylene is added, and extrusion stirring and high-speed shearing are carried out by adopting a double screw, wherein the stirring speed is 3000rpm/min, at the moment, a strong shearing force exists, the temperature is increased to 230 ℃, and after 70 minutes, the mixture is cooled to the room temperature, so as to form the high-viscosity mixed slurry. And pressing the slurry on two sides of a copper foil with the thickness of 150 mu m to prepare the lithium metal composite negative electrode. And then assembling the lithium ion battery with a conventional NCM positive electrode and a PE diaphragm, and adding a conventional commercial electrolyte to prepare the lithium ion battery.
Comparative example 1
Mixing a silicon oxide/graphite negative electrode material (a mixture of silicon oxide and graphite negative electrode powder in a weight ratio of 2: 8), polyethylene oxide and a conductive agent in a proportion of 94%, 2% and 1%, uniformly stirring, adding 3% of polytetrafluoroethylene, extruding and stirring by adopting a double screw, and shearing at a high speed, wherein the stirring speed is 3000rpm/min, a strong shearing force exists, the temperature is increased to 180 ℃, the stirring is continued for 90 minutes, and then, the mixture is cooled to room temperature to form high-viscosity mixed slurry. And pressing the slurry on a copper foil with the thickness of 150 mu m to obtain the conventional negative pole piece. And then assembling the lithium ion battery with a conventional NCM positive electrode and a PE diaphragm, and adding a conventional commercial electrolyte to prepare the lithium ion battery.
And (3) charge and discharge test:
the battery was charged to 4.2V at a current of 0.1C and then charged at a constant voltage until the current reached 0.05C. After a subsequent 30min hold, discharge to 2.5V at a current of 0.1C. And obtaining the charging capacity and the discharging capacity, wherein the ratio of the discharging capacity divided by the charging capacity is the first coulombic efficiency.
The lithium ion batteries in the comparative example 1 and the comparative example 1 are subjected to charge and discharge performance tests, and the results are shown in fig. 1, and it can be seen from fig. 1 that the capacity of the lithium ion battery made of the metal lithium composite electrode prepared in the example 1 is obviously improved. It can be seen that the lithium metal introduced into the negative active material of the present invention can be used as a lithium source to supplement lithium consumption caused by the first charge-discharge process, the discharge capacity of the lithium ion battery prepared in example 1 is increased from 13.2Ah to 17.4Ah, and the first coulombic efficiency is increased from 66% to 88%. The batteries of example 1 and comparative example 1 were disassembled at full charge and found to have almost the same negative sheet state, indicating that the negative sheet made by the method of the present invention performed well without the fine traces of lithium powder as occurs when metallic lithium powder was supported on the surface of the active material layer.
Appropriate changes and modifications to the embodiments described above will become apparent to those skilled in the art from the disclosure and teachings of the foregoing description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims 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 (10)
1. A lithium metal composite electrode, characterized by: the negative electrode comprises a negative electrode current collector and an active material layer loaded on at least one side of the negative electrode current collector; the active material layer comprises the following substances in percentage by mass: 0.5-20% of metal lithium, 60-95% of negative electrode material, 1-10% of binder and 1-10% of conductive agent; the adhesive comprises a main adhesive and an auxiliary adhesive, wherein the main adhesive accounts for 40-80% of the total mass of the adhesive.
2. The lithium metal composite electrode according to claim 1, wherein: the negative current collector is one of electrolytic copper foil, rolled copper foil, copper-nickel alloy foil, copper surface nickel-plated foil and copper foil with holes.
3. The lithium metal composite electrode according to claim 1, wherein: the thickness of the negative current collector is 4-12 mu m.
4. The lithium metal composite electrode according to claim 1, wherein: the thickness of the active material layer is 50-500 μm.
5. The lithium metal composite electrode according to claim 1, wherein: the metal lithium is at least one of lithium powder, a metal lithium tape, a metal lithium rod, metal lithium particles and metal lithium foil of which the surface is coated with a lithium carbonate layer.
6. The lithium metal composite electrode according to claim 1, wherein: the negative electrode material is at least one of graphite, soft carbon, hard carbon, tin oxide, silicon and silicon oxide.
7. The lithium metal composite electrode according to claim 1, wherein: the main binder is polytetrafluoroethylene, and the auxiliary binder is one of polyvinylidene fluoride, hexafluoropropylene and polyethylene oxide.
8. The lithium metal composite electrode according to claim 1, wherein: the conductive agent is at least one of conductive carbon black, conductive acetylene black, graphene and carbon nano tubes.
9. The method of making a lithium metal composite electrode of any of claims 1 to 8, wherein: the method comprises the following steps: preliminarily mixing the lithium metal, the negative electrode material, the secondary binder and the conductive agent, adding the main binder, and continuously mixing to obtain a mixed material; extruding, stirring and shearing the mixed materials at a high speed by adopting a double-screw extruder to form high-viscosity mixed slurry; and pressing the mixed slurry on one side or two sides of the negative current collector to obtain the metal lithium composite electrode.
10. An electrochemical energy storage device, characterized by: the lithium metal composite electrode comprises a positive plate, a negative plate, a diaphragm, electrolyte and a shell, wherein the negative plate is the lithium metal composite electrode as claimed in any one of claims 1 to 8.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113258038A (en) * | 2021-06-16 | 2021-08-13 | 上海瑞浦青创新能源有限公司 | Method for preparing lithium-supplementing negative plate of lithium battery by dry method |
CN113675375A (en) * | 2021-08-12 | 2021-11-19 | 湖北亿纬动力有限公司 | Lithium-supplement negative plate, preparation method thereof and lithium ion battery |
CN113948674A (en) * | 2021-10-28 | 2022-01-18 | 郑州中科新兴产业技术研究院 | Safe lithium supplement negative plate, preparation method and lithium battery |
WO2023170108A1 (en) * | 2022-03-10 | 2023-09-14 | Volkswagen Ag | Method for the continuous production of a battery electrode |
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