CN110993947A - Modified anode material and lithium ion battery - Google Patents
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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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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- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M2004/028—Positive 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the field of lithium ion batteries, in particular to a modified anode material and a lithium ion battery. The modified cathode material of the invention comprises: a granular positive electrode material and a self-healing solid electrolyte layer covering the positive electrode material. The modified positive electrode material can self-repair cracks appearing in the circulation process, slow down the impedance rising rate of the battery, improve the capacity retention rate of the battery and improve the first coulomb efficiency of the battery.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a modified anode material and a lithium ion battery.
Background
A lithium ion battery is a type of secondary battery that mainly operates by movement of lithium ions between a positive electrode and a negative electrode. During charging and discharging, Li+Intercalation and deintercalation to and from two electrodes: upon charging, Li+The lithium ion battery is extracted from the positive electrode and is inserted into the negative electrode through the electrolyte, and the negative electrode is in a lithium-rich state; the opposite is true during discharge. Lithium ion batteries have the outstanding advantages of high energy density, long cycle life, no pollution and the like, and have become the mainstream of the battery market.
Energy density is a major concern of lithium ion batteries as one of the most obvious advantages, and since the commercialization of lithium ion batteries in the nineties of the twentieth century, the energy density of lithium ion batteries is almost improved by increasing the content of active materials and reducing the content of inactive materials in slurry, but in recent years, the bottleneck period is reached in the direction, and the content ratio of active materials is difficult to increase.
Therefore, people aim at improving the first coulombic efficiency and the cycle capacity retention rate of the battery, wherein the first coulombic efficiency of the battery refers to that a layer of solid electrolyte membrane is formed on the surface of an electrode material in the first charging and discharging process of the battery, and a considerable part of lithium ions are lost in the process of forming the solid electrolyte membrane, so that the capacity of the lithium battery is reduced, and the energy density of the battery is further reduced. At present, two methods for improving the first coulombic efficiency of lithium batteries mainly comprise negative electrode lithium supplement and electrode material pre-coated solid electrolyte membrane layers, the negative electrode lithium supplement process and operation are complex, at present, commercialization is not realized very much, and the material pre-coated method is a conventional material modification method and is easy to realize. The surface of the electrode material is coated with a layer of solid electrolyte membrane in advance, so that the reaction of electrolyte during the first charge and discharge can be prevented, the first coulombic efficiency of the battery is greatly improved, the structure can be optimized by utilizing the strong controllability of the artificial solid electrolyte membrane, the method is a method for improving the first effect of the battery and is an important direction for modifying the electrode material in the future. The capacity retention rate of the battery in the circulation process is a necessary way for realizing high energy density, and the material can continuously expand and contract in the circulation process to cause cracks, so that the electrolyte penetrates through the artificial solid electrolyte membrane to further react, and the electrochemical properties of the battery such as impedance, capacity retention rate and the like are further influenced.
At present, researchers mainly coat the negative electrode with a solid electrolyte membrane, neglecting a large amount of side reactions of the positive electrode material, the impedance increase mainly comes from the positive electrode in the battery cycle process, and the side reactions of the positive electrode material have a non-negligible effect on the overall impedance increase of the battery.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the modified positive electrode material can self-repair cracks appearing in the circulation process, slow down the impedance rising rate of the battery, improve the capacity retention rate of the battery and improve the first coulombic efficiency of the battery.
The invention provides a modified cathode material, which comprises: a granular positive electrode material and a self-healing solid electrolyte layer covering the positive electrode material.
Preferably, the material of the self-healing solid electrolyte layer is a material which is designed based on reversible chemical bonds or an irreversible system of micro/nano containers and can pass lithium ions and can not pass electrons.
Preferably, the material of the self-healing solid electrolyte layer is a self-healing ceramic or a polymer having self-healing properties.
Preferably, the self-healing solid electrolyte layer has a thickness of 0.001 to 5 μm.
Preferably, the mass of the self-healing solid electrolyte layer accounts for 0.001-10% of the total mass of the modified cathode material.
Preferably, the positive electrode material includes LiNixCoyMzO2Lithium iron phosphate and vanadium phosphateOne or more of lithium; wherein M is manganese or aluminum, x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 0 and less than or equal to 1.
The invention provides a preparation method of a modified anode material, which comprises the following steps:
dissolving the self-healing solid electrolyte material in a solvent, mixing with a granular positive electrode material, and drying to obtain a modified positive electrode material; or
And synthesizing the self-healing solid electrolyte material on the granular positive electrode material in situ to obtain the modified positive electrode material.
Preferably, when the self-healing solid electrolyte material is dissolved in the solvent, the mass percentage of the self-healing solid electrolyte material in the solvent is 0.1% to 80%.
The invention also provides a lithium ion battery which comprises the anode made of the modified anode material.
Compared with the prior art, the modified cathode material comprises the following components: a granular positive electrode material and a self-healing solid electrolyte layer covering the positive electrode material. The positive electrode material is wrapped by the solid electrolyte layer with the self-healing property, so that cracks caused by the separation and the embedding of lithium ions can be continuously repaired in the battery circulation process, the capacity loss generated by the further reaction of electrolyte is further organized, and the capacity retention rate of the battery in the circulation process is improved. In addition, compared with the solid electrolyte membrane which continuously grows in the circulation, the self-healing solid electrolyte layer can weaken the impedance increase caused by the growth of the solid electrolyte membrane, further reduce the self-discharge, polarization and the like of the battery, and achieve the purpose of improving the electrochemical performance of the battery.
Drawings
Fig. 1 is a schematic cross-sectional view of a modified cathode material according to an embodiment of the invention;
legends note:
1 is a positive electrode material, and 2 is a self-healing solid electrolyte layer.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention in conjunction with the following examples, but it will be understood that the description is intended to illustrate the features and advantages of the invention further, and not to limit the invention.
The embodiment of the invention discloses a modified anode material, which comprises the following components: a granular positive electrode material and a self-healing solid electrolyte layer covering the positive electrode material.
In the invention, the solid electrolyte layer has self-healing property, and can automatically repair cracks in the process of lithium ion intercalation-deintercalation or when cracks are generated by other stress, so that the electrolyte is prevented from further reaction to cause impedance rise and capacity consumption, and the aim of improving the electrochemical performance of the anode material is fulfilled.
In the present invention, the material of the self-healing solid electrolyte layer may be a material designed based on reversible chemical bonds or an irreversible system of micro/nano containers, which can pass lithium ions, which cannot pass electrons. Preferably, a self-healing ceramic or a polymer having self-healing properties may be selected.
The polymer with self-healing and property is a single, cross-linked, copolymerized, grafted, blocked or polymer adopting two or more of the above functions prepared by utilizing hydrogen bonds, ionic bonds, pi-pi interactions, van der waals forces, electrostatic interactions, charge transfer interactions.
Optionally, the polymer with self-healing properties is a polyamide polymer, an epoxy resin, or an acrylate polymer.
Preferably, the self-healing solid electrolyte layer has a thickness of 0.001 to 5 μm. Too low a thickness of the self-healing solid electrolyte does not allow complete coating, and too high a thickness reduces the energy density of the material. The self-healing electrolyte layer is therefore selected to have a thickness of 0.001 to 5 μm.
Preferably, the mass of the self-healing solid electrolyte layer accounts for 0.001-10% of the total mass of the modified cathode material. The quality of the self-healing solid electrolyte layer should not be too low or too high, too low to completely coat, and too high to reduce the energy density of the material.
In the present invention, the positive electrode material may be LiNixCoyMzO2One or more of lithium iron phosphate and lithium vanadium phosphate; wherein M is manganese or aluminum, x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 0 and less than or equal to 1.
The particle shape of the positive electrode material is not particularly limited in the present invention, and may be spherical, ellipsoidal, or irregular.
The embodiment of the invention discloses a preparation method of a modified anode material, which comprises the following steps:
dissolving the self-healing solid electrolyte material in a solvent, mixing with a granular positive electrode material, and drying to obtain a modified positive electrode material; or
And synthesizing the self-healing solid electrolyte material on the granular positive electrode material in situ to obtain the modified positive electrode material.
In the first preparation method, when the self-healing solid electrolyte material is dissolved in a solvent, the mass percentage of the self-healing solid electrolyte material in the solvent is 0.1% to 80%.
The solvent is selected according to the kind of the self-healing solid electrolyte material, and specifically comprises two or more of hydrocarbons, halogenated alkanes, ethers, aldehydes, ketones, esters, amides, amines, alcohols, phenols, sulfonic acids, carboxylic acids, furan, and sulfones. The solvent is selected from the above classes, and is a liquid compound at room temperature.
The second preparation method may be in-situ growth or in-situ polymerization, but is not limited to the two in-situ synthesis methods, depending on the self-healing solid electrolyte material to be synthesized.
The embodiment of the invention also discloses a lithium ion battery which comprises the anode made of the modified anode material.
According to the invention, the modified positive electrode material, the binder, the conductive agent and the graphite are dissolved in the solvent to prepare slurry, and then the slurry is coated on the current collector to prepare the positive electrode.
In order to further understand the present invention, the modified cathode material, the preparation method thereof and 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
The polyamide-based polymer having self-healing properties is dissolved in phenol to form a solution. The mass fraction of the polyamide-based polymer having the self-healing property was 0.5%. And uniformly stirring and mixing with prepared lithium cobaltate, wherein the mass ratio of the polyamide polymer to the lithium cobaltate is 1:60, and drying the material after uniform stirring to obtain the required electrode material with the self-healing polyamide polymer solid electrolyte layer. The thickness of the self-healing polyamide-based polymer solid electrolyte layer was 1 μm.
Comparative example 1
Lithium cobaltate is directly used as a positive electrode material.
Example 2
Dissolving the epoxy resin with the self-healing performance in ethyl acetate to prepare a solution, wherein the mass fraction of the epoxy resin with the self-healing performance in the solution is 3%. And adding the solution into lithium iron phosphate after uniformly stirring, wherein the mass ratio of the epoxy resin to the lithium iron phosphate is 1: and 60, uniformly mixing, drying, and evaporating the ethyl acetate solvent to obtain the required lithium iron phosphate cathode material with the self-healing epoxy resin artificial solid electrolyte layer. The thickness of the self-healing epoxy artificial solid electrolyte layer was 2.5 μm.
Comparative example 2
Lithium iron phosphate is used as a positive electrode material.
Example 3
Dispersing acrylate monomer in butanone, and mixing the solution with prepared LiNi0.6Co0.21Mn0.2O2Electrode material was mixed homogeneously, acrylic monomer mass and LiNi0.8Co0.1Mn0.1O2The mass ratio of the electrode material is 1:40, then initiator dibenzoyl peroxide is added to initiate the copolymerization of acrylic monomer to form acrylic copolymer with self-healing performance, and the mixture is stirred all the time in the reaction processThe step can lead the monomer to be evenly polymerized in situ on LiNi0.8Co0.1Mn0.1O2On the electrode material, LiNi with a self-healing polyacrylic polymer solid electrolyte layer can be successfully prepared0.8Co0.1Mn0.1O2An electrode material. The thickness of the self-healing polyacrylic polymer solid electrolyte layer was 5 μm.
Comparative example 3
With LiNi0.8Co0.1Mn0.1O2As a positive electrode material.
Example 4
Dispersing amide monomer in N, N-dimethylformamide, wherein the mass fraction of the amide monomer is 10%, and adding the solution into pre-mixed lithium cobaltate and LiNi0.6Co0.21Mn0.2O2And (3) adding an initiator azobisisobutyronitrile into the mixed electrode material after uniformly stirring to initiate polymerization reaction, thereby preparing the modified anode material of the polyamide solid electrolyte layer (the thickness is 15nm) with self-healing property. The mass of the polyamide solid electrolyte layer with the self-healing property accounts for 5% of the total mass of the modified cathode material.
Comparative example 4
With lithium cobaltate and LiNi0.6Co0.21Mn0.2O2The mixed material is used as a positive electrode material.
The positive electrode materials in all the above examples and comparative examples were mixed with a binder, a conductive agent and graphite, and made into a positive electrode, and carbon was used as a negative electrode to form a lithium ion battery. And the lithium ion battery is tested for the first coulombic efficiency, the cycle capacity retention rate (1000 times) and the impedance increase rate after the cycle (1000 times), and the specific results are shown in table 1.
TABLE 1
| First coulombic efficiency | Retention rate of circulating capacity | Rate of increase of impedance | |
| Example 1 | 95.9％ | 85.4％ | 12.5％ |
| Comparative example 1 | 93.4％ | 80.7％ | 22.4％ |
| Example 2 | 93.2％ | 90.3％ | 9.5％ |
| Comparative example 2 | 92.8％ | 85.4％ | 15.6％ |
| Example 3 | 94.5％ | 83.3％ | 14.8％ |
| Comparative example 3 | 90.7％ | 76.8％ | 25.7％ |
| Example 4 | 93.7％ | 83.9％ | 10.3％ |
| Comparative example 4 | 91.2％ | 78.1％ | 18.5％ |
As can be seen from the experimental results in table 1, the modified cathode material formed by coating the solid electrolyte layer with the self-healing performance on the surface of the cathode material can effectively improve the first coulomb efficiency, the retention rate of the cyclic capacity and the impedance increase rate of the lithium ion battery, and has a positive effect on the electrochemical performance of the lithium ion battery.
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 (9)
1. A modified positive electrode material, comprising: a granular positive electrode material and a self-healing solid electrolyte layer covering the positive electrode material.
2. The modified cathode material according to claim 1, wherein the self-healing solid electrolyte layer is made of a material that is designed based on a reversible chemical bond or an irreversible system of micro/nano-containers and that can pass lithium ions and not pass electrons.
3. The modified positive electrode material according to claim 1, wherein the material of the self-healing solid electrolyte layer is a self-healing ceramic or a polymer having a self-healing property.
4. The modified positive electrode material according to claim 1, wherein the self-healing solid electrolyte layer has a thickness of 0.001 to 5 μm.
5. The modified positive electrode material according to claim 1, wherein the self-healing solid electrolyte layer accounts for 0.001 to 10% by mass of the total mass of the modified positive electrode material.
6. The modified cathode material according to claim 1, wherein the cathode material comprises LiNixCoyMzO2One or more of lithium iron phosphate and lithium vanadium phosphate; wherein M is manganese or aluminum, x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 0 and less than or equal to 1.
7. The preparation method of the modified cathode material is characterized by comprising the following steps:
dissolving the self-healing solid electrolyte material in a solvent, mixing with a granular positive electrode material, and drying to obtain a modified positive electrode material; or
And synthesizing the self-healing solid electrolyte material on the granular positive electrode material in situ to obtain the modified positive electrode material.
8. The production method according to claim 7, wherein when the self-healing solid electrolyte material is dissolved in the solvent, the self-healing solid electrolyte material is present in the solvent in an amount of 0.1 to 80% by mass.
9. A lithium ion battery comprising a positive electrode made of the modified positive electrode material according to any one of claims 1 to 6.
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| CN112201791A (en) * | 2020-10-23 | 2021-01-08 | 江苏大学 | Method for improving ternary cathode material of lithium ion battery by oxygen-absorbing self-healing film |
| CN114573053A (en) * | 2022-05-05 | 2022-06-03 | 南通金通储能动力新材料有限公司 | Dynamic repairing method for spherical cracking high-nickel ternary precursor |
| CN115714200A (en) * | 2022-11-10 | 2023-02-24 | 哈尔滨工业大学 | Method for preparing solid-state battery through selective curing |
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Address after: 519180 No. 209 Pearl Peak Avenue, Jingan Town, Doumen District, Zhuhai City, Guangdong Province Applicant after: Zhuhai Guanyu Battery Co., Ltd Address before: 519180 No. 209 Pearl Peak Avenue, Jingan Town, Doumen District, Zhuhai City, Guangdong Province Applicant before: ZHUHAI COSLIGHT BATTERY Co.,Ltd. |
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Application publication date: 20200410 |