CN111697223A - Surface modified lithium ion battery anode material and preparation method thereof - Google Patents
Surface modified lithium ion battery anode material and preparation method thereof Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- 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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The surface-modified lithium ion battery anode material consists of a base material and a surface coating material coated on the surface of the base material. The surface coating material is a hydrophobic organic silicon material. The hydrophobic organosilicon material is one or a mixture of more than two of multi-component copolymerized high molecular silane, siloxane, a silane coupling agent and a siloxane coupling agent. The mass ratio of the surface coating material to the base material is 0.000001-0.05: 1, the thickness of the surface coating layer is nano-scale, and the nano-scale surface coating material can prevent the anode material from absorbing water and carbon dioxide, so that the processing performance of the anode material is improved, and the pH value of the anode material and the carbonate and hydroxyl content (or residual lithium content) on the surface of the anode material are reduced. The invention also provides a preparation method of the surface modified lithium ion battery anode material.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a surface-modified lithium ion battery positive electrode material and a preparation method thereof.
Background
The lithium ion battery is used as a new generation of green and environment-friendly power supply, has the advantages of high energy density, high voltage, small self-discharge, no memory effect and the like, and is widely applied to products such as mobile phones, cameras, notebook computers, electric tools, electric bicycles, electric automobiles and the like. With the rapid development of electronic products, the requirements on the energy and power of the lithium ion battery are higher and higher, and the anode material of the lithium ion battery is an important component of the lithium ion battery and is one of the main influencing factors of the performance of the lithium ion battery.
At present, the most applied lithium ion battery positive electrode materials mainly comprise ternary materials of lithium cobaltate, lithium nickelate, lithium manganate and lithium nickel cobalt manganese. Lithium cobaltate is the earliest industrialized and commercialized material, and has the advantages of stable electrochemical performance, good conductivity, high voltage platform, good cycle performance and compacted density of 4.0g/cm3However, the specific capacity of lithium cobaltate is relatively low, only 140mAh/g, the cobalt toxicity is high, cobalt resources are scarce, the price is high, and the overcharge safety performance is poor. Lithium nickelate is difficult to synthesize, the reproducibility of the material is poor, the layered lithium manganate has high specific capacity but poor structural stability, and the spinel lithium manganate has low specific capacity and is unstable in structure at high temperature and needs to be reinforced. The lithium nickel cobalt manganese oxide ternary material integrates the performance performances of lithium cobaltate, lithium nickelate and lithium manganate, has good thermal stability and high specific capacity (the higher the nickel content is), but the high-alkalinity high-nickel material is easy to absorb water and carbon dioxide from the surrounding air. After water and carbon dioxide are absorbed, on one hand, the processing performance problems of jelly and the like easily occur in slurry mixing coating during the manufacturing of the lithium ion battery, and on the other hand, the technical parameters of safety, circulation and the like of the high-nickel battery cell are further deteriorated.
At present, the main stream in the industry is to reduce the surface alkali residue and the PH value of the high nickel material by adopting a water washing and twice burning method, however, the result of this is that the production cost is significantly increased, and other properties of the battery cell, such as cycle and even safety, are also sacrificed. Therefore, the application and popularization of the current high nickel material in the market are not expected.
Disclosure of Invention
In view of the above, there is a need to provide a lithium ion battery cathode material and a preparation method thereof, which can overcome the above mentioned unfavorable surface modification, so as to overcome the deficiencies of the prior art, and the material with good hydrophobic property is adopted to coat and modify an active substance to improve the tolerance of the material to the environmental humidity, thereby improving the processing performance of the material slurry coating, and further improving the high temperature storage performance and the safety performance of the material.
The surface modified lithium ion battery anode material consists of a base material and a surface coating material coated on the surface of the base material. The matrix material is one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel cobalt oxide or lithium nickel manganese oxide. The surface coating material is a hydrophobic organic silicon material. The hydrophobic organosilicon material is one or a mixture of more than two of multi-component copolymerized macromolecular silane, siloxane, a silane coupling agent and a siloxane coupling agent. The mass ratio of the surface coating material to the base material is 0.000001-0.05: 1, the thickness of the surface coating layer is nano-scale, and the nano-scale surface coating material is coated on the outer surface of the granular base material.
Further, the surface coating material is one or a mixture of more than two of silane, siloxane, a silane coupling agent and a siloxane coupling agent with the molecular weight of less than 1 million.
Further, when the surface coating material is a silane and/or siloxane coupling agent mixture, the material coated on the surface of the base material is organic silane.
Further, the molecular formula of the organo-silane is
Further, the molecular formula of the organo-silane is
Further, the hydrophobic organosilicon material is in a liquid state or a solid state.
A preparation method of a surface modified lithium ion battery anode material comprises the following steps:
s1: providing a base material, wherein the base material is one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium manganese iron phosphate, lithium nickel cobalt oxide or lithium nickel manganese oxide;
s2, providing a surface coating material, wherein the surface coating material is one or a mixture of more than two of multi-copolymerization macromolecular silane, siloxane, a silane coupling agent and a siloxane coupling agent;
s3, heating the surface coating material at 100-400 ℃;
s4, providing a reaction pot, mixing the surface coating material and the substrate material in the reaction pot and reacting to coat, wherein the coating time is less than 10 minutes to coat the surface coating material on the surface of the substrate material to form the surface modified lithium ion battery anode material.
Further, the reaction vessels are filled with air or oxygen.
Further, the surface coating material is heated to be gasified, the gasified surface coating material is introduced from the bottom or the side part of the reaction vessel, and the substrate material is sprayed from the top of the reaction vessel for coating.
Furthermore, the surface coating material and the substrate material are directly and uniformly mixed and reacted in the reaction vessel at a certain temperature to generate a coating layer.
Compared with the prior art, the surface-modified lithium ion battery anode material provided by the invention has the advantages that the surface coating material is coated on the surface of the base material, and the surface coating material is a hydrophobic nano material, so that the coating layer can isolate external water from the anode material and simultaneously can enable lithium ions to freely pass through, and further the anode material can be prevented from absorbing water and carbon dioxide while charging and discharging are completed, so that the processing performance of the anode material is improved, and the pH value of the anode material and the carbonate and hydroxyl contents (or residual lithium contents) on the surface of the anode material are reduced. In addition, the synthesis process can be completed only by uniformly mixing and heating in one reaction tank, so that the method is simple and easy to implement, has low equipment requirement, sufficient and cheap raw material resources and no pollution, and has good industrial application prospect.
Detailed Description
Specific examples of the present invention will be described in further detail below. It should be understood that the description herein of embodiments of the invention is not intended to limit the scope of the invention.
The surface modified lithium ion battery anode material provided by the invention consists of a base material and a surface coating material. The matrix material can be one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel cobalt oxide or lithium nickel manganese oxide. The nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel cobalt oxide or lithium nickel manganese oxide is used as an active substance of the lithium ion battery positive electrode material, which is the prior art, and the characteristics and the forming process thereof are not described herein again. In manufacturing, the matrix material should first be crushed to particles of a suitable size. The material degree of the base material is 0.1-30 microns. The surface coating material can be a hydrophobic organic silicon material, and can be in a liquid state or a solid state. The hydrophobic organosilicon material can be one or a mixture of more than two of multi-component copolymerized macromolecular silane, siloxane, a silane coupling agent and a siloxane coupling agent. The mass ratio of the surface coating material to the base material is 0.000001-0.05: 1.
The surface coating material is coated on the outer surface of the granular base material so as to form the surface modified lithium ion battery anode material. The surface coating material is coated on the surface of the base material, and the surface coating material is a hydrophobic nano material, so that the coating layer can enable lithium ions to freely pass through while isolating external water and the anode material, and further can prevent the anode material from absorbing water and carbon dioxide while finishing charging and discharging, thereby not only improving the processing performance of the anode material, but also reducing the pH value of the anode material and the contents of carbonate and hydroxyl (or residual lithium) on the surface of the anode material.
The invention also provides a preparation method of the surface modified lithium ion battery anode material, which comprises the following steps:
s1: providing a base material, wherein the base material is one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium manganese iron phosphate, lithium nickel cobalt oxide or lithium nickel manganese oxide;
s2, providing the surface coating material, wherein the surface coating material is one or a mixture of more than two of multi-copolymerization macromolecular silane, siloxane, a silane coupling agent and a siloxane coupling agent;
s3, heating the surface coating material at 100-400 ℃;
s4, providing a reaction pot, mixing the surface coating material and the substrate material in the reaction pot for reaction to carry out coating, wherein the coating time is less than 10 minutes to coat the surface coating material on the surface of the substrate material to form the surface modified lithium ion battery anode material.
In step S4, the reactor is filled with air or oxygen. In addition, when the surface coating material is heated to be gasified, the gasified surface coating material can be introduced from the bottom or the side of the reaction vessel, and the substrate material is sprayed from the top of the reaction vessel for coating.
In specific implementation, the method may be implemented in any one of the following embodiments.
The first embodiment is as follows:
silane coupling agent with molecular weight of 5 ten thousand is preheated to 250 deg.c, and the material is decomposed slowly into gas state. Introducing dry air to continuously bring the gaseous silane coupling agent into the closed chamber filled with the base material. The silane coupling agent is fed in from the bottom, while the base material is sprinkled in from the top, thereby forming a closed ring. In the process of introducing, a coating layer of a nano layer is gradually and uniformly formed on the surface of the matrix material, the coating time is 1 minute, and the matrix material in the closed cavity is converted into the anode material of the surface nano-coating hydrophobic material.
The pH value and the surface residual lithium content of the material before and after coating are respectively tested by a pH meter and a titration method. The pH value after coating is reduced by 0.4 compared with the pH value before coating; the content of residual lithium on the surface of the material is reduced by 0.05 percent before coating compared with that after coating. The electrochemical performance of the material is tested by adopting a blue battery testing system at 25 ℃, and the testing voltage range is 3-4.3V; multiplying power performance test conditions: charging and discharging once at 0.2C, and discharging once at 0.2C and 1C; the specific discharge capacity of the material under the multiplying power of 0.2C is 200mAh/g, and the specific discharge capacity under the multiplying power of 1C is 190 mAh/g.
Example 2:
a mixture of silane and siloxane coupling agent having a molecular weight of 10 ten thousand was preheated to 300 ℃ and the mixture was slowly decomposed into a gaseous state. Dry oxygen is introduced to continuously bring the gaseous mixture into the closed chamber containing the substrate material. The silane and siloxane coupling agent mixture is passed in from the side, while the matrix material is sprayed in from the top, forming a closed ring. And (3) gradually and uniformly forming an organic silicon alkane coating of a nano layer on the surface of the substrate material, wherein the coating time is 10 minutes, and the substrate material in the closed cavity is converted into a cathode material of which the surface is coated with a nano hydrophobic material.
The molecular formula of the organic silane is
Example 3:
uniformly mixing siloxane with the molecular weight of 1000 and a matrix material in advance, heating to 200 ℃, preserving heat for 30 seconds, cooling, and generating the cathode material with the surface nano-coated hydrophobic material after cooling. In this embodiment, the surface coating material and the substrate material are directly and uniformly mixed and reacted in the reaction vessel at a certain temperature to form a coating layer.
Example 4:
a mixture of siloxane and silane coupling agent having a molecular weight of 30 ten thousand was previously heated to 350 degrees, and the mixture was slowly decomposed into a gaseous state. Dry oxygen is introduced to continuously bring the gaseous mixture into the closed chamber containing the substrate material. The silane and siloxane coupling agent mixture is passed in from the side, while the matrix material is sprayed in from the top, forming a closed ring. And (3) gradually and uniformly forming an organic silicon alkane coating of a nano layer on the surface of the matrix material, wherein the coating time is 5 minutes, and the matrix material in the closed cavity is converted into the cathode material of which the surface is coated with the nano hydrophobic material.
The molecular formula of the organic silane is
Compared with the prior art, the surface-modified lithium ion battery anode material provided by the invention has the advantages that the surface coating material is coated on the surface of the base material, and the surface coating material is a hydrophobic nano material, so that the coating layer can isolate external water from the anode material and simultaneously can enable lithium ions to freely pass through, and further the anode material can be prevented from absorbing water and carbon dioxide while charging and discharging are completed, so that the processing performance of the anode material is improved, and the pH value of the anode material and the carbonate and hydroxyl contents (or residual lithium contents) on the surface of the anode material are reduced. In addition, the synthesis process can be completed only by uniformly mixing and heating in one reaction tank, so that the method is simple and easy to implement, has low equipment requirement, sufficient and cheap raw material resources and no pollution, and has good industrial application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications, equivalents or improvements that are within the spirit of the present invention are intended to be covered by the following claims.
Claims (10)
1. A surface modified lithium ion battery anode material is characterized in that: the surface-modified lithium ion battery positive electrode material is composed of a base material and a surface coating material coated on the surface of the base material, wherein the base material is one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel cobalt lithium or lithium nickel manganese, the surface coating material is a hydrophobic organic silicon material, the hydrophobic organic silicon material is one or a mixture of more than two of multi-copolymerization high polymer silane, siloxane, a silane coupling agent and a siloxane coupling agent, the mass ratio of the surface coating material to the base material is 0.000001-0.05: 1, the thickness of the surface coating layer is nano-scale, and the nano-scale surface coating material is coated on the outer surface of the granular base material.
2. The surface-modified lithium ion battery positive electrode material of claim 1, wherein: the surface coating material is one or a mixture of more than two of silane, siloxane, a silane coupling agent and a siloxane coupling agent with the molecular weight less than 1 million.
3. The surface-modified lithium ion battery positive electrode material of claim 2, wherein: when the surface coating material is a silane and/or siloxane coupling agent mixture, the material coated on the surface of the base material is organic silicon alkane.
4. The surface-modified lithium ion battery positive electrode material of claim 3, wherein: the molecular formula of the organic silane is
5. The surface-modified lithium of claim 3The positive electrode material of the ion battery is characterized in that: the molecular formula of the organic silane is
6. The surface-modified lithium ion battery positive electrode material of claim 1, wherein: the hydrophobic organosilicon material is in a liquid state or a solid state.
7. A preparation method of a surface modified lithium ion battery anode material comprises the following steps:
s1: providing a base material, wherein the base material is one or a mixture of more than two of nickel cobalt manganese aluminum acid lithium, nickel cobalt lithium manganate, nickel cobalt aluminum acid lithium, lithium manganate, lithium cobaltate, lithium iron phosphate, lithium manganese iron phosphate, lithium nickel cobalt oxide and lithium nickel manganese oxide;
s2, providing a surface coating material, wherein the surface coating material is one or a mixture of more than two of multi-copolymerization macromolecular silane, siloxane, a silane coupling agent and a siloxane coupling agent;
s3, heating the surface coating material at 100-400 ℃;
s4, providing a reaction pot, mixing the surface coating material and the substrate material in the reaction pot and reacting to coat, wherein the coating time is less than 10 minutes to coat the surface coating material on the surface of the substrate material to form the surface modified lithium ion battery anode material.
8. The method of preparing the surface-modified lithium ion battery positive electrode material of claim 7, wherein: the reaction vessel is filled with air or oxygen.
9. The method of preparing the surface-modified lithium ion battery positive electrode material of claim 7, wherein: the surface coating material is heated to be gasified, the gasified surface coating material is introduced from the bottom or the side part of the reaction vessel, and the substrate material is sprinkled from the top of the reaction vessel for coating.
10. The method of preparing the surface-modified lithium ion battery positive electrode material of claim 7, wherein: the surface coating material and the substrate material are directly and uniformly mixed and reacted in the reaction vessel at a certain temperature to generate a coating layer.
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Cited By (6)
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| CN113889618A (en) * | 2021-09-30 | 2022-01-04 | 中国电子科技集团公司第十八研究所 | Hydrophobic anode material modified by organic silicide and preparation method thereof |
| CN114824268A (en) * | 2022-03-29 | 2022-07-29 | 中国科学院上海硅酸盐研究所 | Hydrophobic protective layer on surface of negative electrode of metal-air battery and preparation method and application thereof |
| CN116154169A (en) * | 2023-01-13 | 2023-05-23 | 江苏正力新能电池技术有限公司 | MXene coated positive electrode material, preparation method thereof, positive electrode plate and lithium ion battery |
| WO2023184355A1 (en) * | 2022-03-31 | 2023-10-05 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, preparation method therefor, and positive electrode plate, secondary battery, and electric device comprising same |
| CN117117160A (en) * | 2023-10-24 | 2023-11-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, preparation method thereof, positive electrode plate, battery and electricity utilization device |
| WO2024087872A1 (en) * | 2022-10-24 | 2024-05-02 | 天津巴莫科技有限责任公司 | Ternary positive electrode material, and preparation method therefor and use thereof |
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Application publication date: 20200922 |