CN109728278B - Positive active material, preparation method thereof and lithium ion battery - Google Patents
Positive active material, preparation method thereof and lithium ion battery Download PDFInfo
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Abstract
The invention provides a positive active material, a preparation method thereof and a lithium ion battery, wherein the positive active material comprises the following components: a positive electrode active material substrate; and a coating layer that completely covers an outer surface of the positive electrode active material substrate, the coating layer being formed of at least a metal oxide. The surface of the positive active material is formed with the continuously coated metal oxide, thereby avoiding the side reaction of the core and the electrolyte, reducing the initial irreversible capacity, improving the cycle performance and improving the performance of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a positive active material, a preparation method thereof and a lithium ion battery.
Background
The lithium ion battery has the advantages of high specific energy, long service life, safety, environmental protection and the like, and is widely applied to the fields of notebook computers, mobile phones, digital cameras, electric automobiles, energy storage and the like. With the continuous development of the demands of computers, mobile phones, electric vehicles and the like, batteries are required to have higher performance.
Currently, as a positive electrode active material for a lithium secondary battery, a lithium composite metal compound is widely used, and lithium impurities inevitably exist on the surface thereof. The lithium impurities remaining on the surface cause a negative reaction with the electrolyte solution, change the surface structure of the lithium composite metal compound, eventually form an initial irreversible capacity, and hinder the movement of lithium ions on the surface, which is a factor of generating gas.
In order to solve this problem, studies have been made on surface treatment of the positive electrode active material with a metal, a metal oxide, a metal phosphate, a metal fluoride, a carbon compound, or the like. In this connection, surface treatment methods are known: the material to be surface treated is dissolved in the solution directly, and then mixed with the positive active material directly, and the mixture is dried and coated on the surface of the positive active material.
However, if the positive electrode active material is coated by the above method, island-shaped coating layers are easily formed on a part of the surface of the positive electrode active material, and lithium impurities remain on the uncoated part, which cannot fundamentally solve the problem of side reactions with the electrolyte solution.
Therefore, currently, the positive active material of the lithium ion battery is still under study.
Disclosure of Invention
In view of the above, the present invention is directed to a positive electrode active material to solve the island-shaped coating (partial coating) problem.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the positive active material according to an embodiment of the present invention includes: a positive electrode active material substrate; and a coating layer that completely covers an outer surface of the positive electrode active material substrate, the coating layer being formed of at least a metal oxide.
According to some embodiments of the invention, the positive active material matrix is a nickel-cobalt-manganese ternary material.
According to some embodiments of the present invention, the particle size of the positive electrode active material matrix is 3 to 20 μm.
According to some embodiments of the invention, the metal oxide is selected from metal-formed oxides of at least one of: li, Al, Zr, Ni, Mn, Co, Ca, Ti, Cr, Fe, Zn, Y, Ba, La, Ce, Sm, Gd, Yb, Mg, Sr and Cu.
According to some preferred embodiments of the invention, the metal oxide is selected from oxides formed of Al.
According to some embodiments of the invention, the raw material for forming the metal oxide comprises: a metal salt, which is a salt formed by the metal; and alcohol compounds.
According to some embodiments of the invention, the alcohol compound is selected from at least one of the following: methanol, ethanol, ethylene glycol, glycerol, benzyl alcohol, isoamyl alcohol and isopropanol.
According to some preferred embodiments of the invention, the alcohol compound is selected from ethylene glycol.
Compared with the prior art, the positive active material has the following advantages:
the surface of the positive active material matrix is completely coated with the metal oxide, so that the side reaction of the core and the electrolyte is avoided, the initial irreversible capacity is reduced, the cycle performance is improved, and the performance of the lithium ion battery is integrally improved.
Another object of the present invention is to provide a method for preparing the positive electrode active material as described above.
The method for preparing the aforementioned positive active material according to an embodiment of the present invention includes: mixing the metal salt and the alcohol compound to obtain a first mixture; polymerizing the first mixture to obtain a polymer; coating the polymer and the positive active material matrix to obtain a second mixture; and carrying out heat treatment on the second mixed material so as to form a coating layer on the outer surface of the positive active material matrix, thereby obtaining the battery positive active material.
According to some embodiments of the invention, the concentration of the metal salt in the first mixture is 0.05-2 mol/L.
According to some embodiments of the invention, the polymerization is carried out at 60 to 120 ℃ for 10 minutes to 10 hours.
According to some embodiments of the invention, the coating treatment time is 1 minute to 2 hours.
According to some embodiments of the invention, the heat treatment is performed at 400 to 700 ℃ for 10 minutes to 20 hours.
According to some embodiments of the invention, the method further comprises: diluting the polymer by using an organic solvent, and coating the obtained diluent and the positive active material matrix; and before the heat treatment, drying the second mixture.
According to some embodiments of the invention, the concentration of the polymer in the diluent is 0.001 to 0.1 mol/L.
According to some embodiments of the invention, the mass ratio of the diluent to the positive electrode active material matrix is (0.1-10): 1.
According to some embodiments of the invention, the temperature of the drying treatment is 60 to 180 ℃ and the time is 1 to 48 hours.
Compared with the prior art, the method for preparing the positive active material has the following advantages:
the preparation method of the invention is not to directly coat the metal oxide on the surface of the matrix of the positive active material, but combines the coating of the high molecular polymer and the heat treatment, so as to form the continuous coated metal oxide on the surface of the matrix of the positive active material. Moreover, the method is simple, convenient and quick to operate, low in cost and suitable for large-scale production.
The invention further aims to provide a lithium ion battery.
The lithium ion battery according to an embodiment of the present invention contains the aforementioned positive electrode active material.
Compared with the prior art, the lithium ion battery has the following advantages:
the surface of the positive active material in the lithium ion battery is continuously coated with the metal oxide, so that the initial irreversible capacity can be reduced, the cycle performance is improved, and the performance of the lithium ion battery is integrally improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural view of a positive electrode active material according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a method of preparing a positive electrode active material according to an embodiment of the present invention;
FIG. 3 is a schematic view of cycle retention analysis according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of first charge-discharge specific capacity analysis according to an embodiment of the present invention.
Description of reference numerals:
a positive electrode active material substrate 100, and a coating layer 200.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention provides a positive active material, a method for preparing the same, and a lithium ion battery, which will be described in detail below.
Positive electrode active material
In one aspect of the present invention, a positive active material is provided. According to an embodiment of the present invention, referring to fig. 1, the positive active material includes: a positive electrode active material substrate 100; and a coating layer 200, the coating layer 200 completely coating the outer surface of the positive electrode active material substrate 100, the coating layer 200 being formed of at least a metal oxide. By continuously coating the metal oxide on the surface of the matrix of the positive active material, the side reaction of the core and the electrolyte is avoided, the initial irreversible capacity is reduced, the cycle performance is improved, and the performance of the lithium ion battery is integrally improved.
According to some embodiments of the invention, the metal oxide is a metal oxideAn oxide of a metal selected from at least one of: li, Al, Zr, Ni, Mn, Co, Ca, Ti, Cr, Fe, Zn, Y, Ba, La, Ce, Sm, Gd, Yb, Mg, Sr and Cu. Preferably, the metal oxide is selected from Al2O3. Therefore, the raw materials are cheap and easy to obtain, the source is wide, the operation is simple, and the coating is stable.
According to some embodiments of the invention, the raw material for forming the metal oxide comprises: a metal salt, which is a salt formed by the metal; and alcohol compounds. The metal salt can be combined with a part of alcohol compounds to form a monomer, and the monomer is polymerized with the rest of alcohol compounds to form a high molecular polymer.
According to some embodiments of the invention, the alcohol compound is selected from at least one of the following: methanol, ethanol, ethylene glycol, glycerol, benzyl alcohol, isoamyl alcohol and isopropanol. Preferably, the alcohol compound is selected from ethylene glycol. Therefore, the raw materials are easy to obtain, the operation is simple, and the polymerization reaction is easy to occur.
According to some embodiments of the invention, the positive active material matrix is a nickel-cobalt-manganese ternary material. Specifically, the particle size of the positive electrode active material matrix is 3-20 μm. Thereby, excellent performance is imparted to the battery containing the positive electrode active material.
Method for preparing positive electrode active material
In still another aspect of the present invention, the present invention provides a method for preparing the positive electrode active material described above. According to an embodiment of the invention, referring to fig. 2, the method comprises:
s100 hybrid processing
In this step, a metal salt and an alcohol compound are mixed to obtain a first mixed material.
According to some embodiments of the invention, the concentration of the metal salt in the first mixture is 0.05-2 mol/L. Thereby, the polymerization reaction with the alcohol compound can be sufficiently performed.
S200 polymerization
In this step, the first compounded material is subjected to a polymerization reaction to obtain a polymer. The metal salt can be combined with a part of alcohol compounds to form a monomer, and the monomer is polymerized with the rest of alcohol compounds to form a high molecular polymer.
According to some embodiments of the invention, the polymerization is carried out at 60 to 120 ℃ for 10 minutes to 10 hours. Thus, the metal salt can be sufficiently polymerized with the alcohol compound to form a high molecular weight polymer.
S300 coating treatment
In this step, the polymer and the positive electrode active material matrix are subjected to a coating treatment to obtain a second mixture material. Thus, a loose, irregular, and intermittent coating layer is formed on the surface of the positive electrode active material substrate.
According to some embodiments of the invention, the coating treatment time is 1 minute to 2 hours. The materials are continuously stirred in the coating treatment process, so that an intermittent and unstable coating layer is formed on the surface of the positive active material matrix.
According to some embodiments of the present invention, the polymer is subjected to a dilution treatment using an organic solvent, and the resulting dilution and the positive electrode active material matrix are subjected to the coating treatment. The polymer is diluted so as to be coated on the surface of the matrix of the positive active material more uniformly.
Specifically, the concentration of the polymer in the diluent is 0.001-0.1 mol/L, and the mass ratio of the diluent to the positive electrode active material matrix is (0.1-10): 1. Thereby, the surface of the positive electrode active material substrate is coated more uniformly.
According to some embodiments of the invention, the second mix is subjected to a drying process prior to the heat treatment. Specifically, the drying treatment temperature is 60-180 ℃, and the drying treatment time is 1-48 hours. Thereby, the solvent is completely volatilized.
S400 Heat treatment
In this step, the second mixed material is subjected to heat treatment to form a coating layer on the outer surface of the positive active material matrix, resulting in a battery positive active material. Thereby, the polymer is oxidized to an oxide by the heat treatment, and a coating layer is formed to be continuously and stably bonded to the positive electrode active material substrate.
According to some embodiments of the present invention, the heat treatment is performed at 400 to 700 ℃ for 10 minutes to 20 hours. Thereby, a coating layer is formed to be continuously and stably closely combined with the positive electrode active material substrate.
It will be understood by those skilled in the art that the features and advantages described above with respect to the positive electrode active material are equally applicable to the method of preparing the positive electrode active material and will not be described in detail herein.
Lithium ion battery
In yet another aspect of the present invention, a lithium ion battery is presented. According to an embodiment of the present invention, the lithium ion battery contains the positive electrode active material described above. According to the lithium ion battery provided by the embodiment of the invention, the surface of the positive electrode active material is continuously coated with the metal oxide, so that the initial irreversible capacity can be reduced, the cycle performance is improved, and the performance of the lithium ion battery is integrally improved.
It will be appreciated by those skilled in the art that the features and advantages described above for the positive active material are equally applicable to the lithium ion battery and will not be described in detail here.
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
In this example, a lithium ion battery was prepared as follows:
1. aluminum nitrate was mixed with ethylene glycol, wherein the molar concentration of aluminum nitrate was 0.5M.
2. The mixture obtained above was reacted at 100 ℃ for 10 hours to obtain a high molecular polymer.
3. The high molecular polymer was added to ethanol and diluted to a concentration of 0.01M.
4. And mixing the diluent obtained in the previous step with a nickel-cobalt-manganese ternary material, wherein the mass ratio of the diluent to the ternary material is 3:1, and drying at 100 ℃ for 8 hours.
5. And (3) carrying out heat treatment on the dried substance obtained in the previous step at 550 ℃ for 400 minutes to obtain the positive electrode active material.
6. The lithium ion battery is prepared by taking a positive active material, a negative electrode and a diaphragm as a gluing diaphragm based on a PE base film.
Example 2
The lithium ion battery obtained in example 1 was subjected to a performance test.
1. The test is carried out by adopting a blue battery test system at the temperature of 25 ℃, the test voltage range is 3V-4.3V, the charge and discharge are carried out for 2 times at 0.1C, then the charge is carried out at 0.5C, and the discharge is carried out for 50 times at 1C. The capacity retention rate after 50 cycles is more than 94%, and the cycle performance is better (figure 3).
2. The test is carried out by adopting a blue battery test system at 25 ℃, the test voltage range is 3V-4.3V, the charge and discharge are carried out for 2 times at 0.1C, the first charge specific capacity is about 230mAh/g, the first discharge specific capacity is about 208mAh/g, the first efficiency is more than 90 percent, and the first discharge specific capacity and the first efficiency are both higher (figure 4).
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (16)
1. A positive electrode active material, comprising:
a positive electrode active material substrate; and
a coating layer completely coating the outer surface of the positive active material substrate,
the coating layer is at least formed by metal oxide;
the metal oxide is selected from oxides formed from at least one of the following metals:
li, Al, Zr, Ni, Mn, Co, Ca, Ti, Cr, Fe, Zn, Y, Ba, La, Ce, Sm, Gd, Yb, Mg, Sr and Cu;
the raw materials for forming the metal oxide include:
a metal salt, which is a salt formed by the metal; and
an alcohol compound;
the method of preparing the positive active material includes:
mixing the metal salt and the alcohol compound to obtain a first mixture;
polymerizing the first mixture to obtain a polymer;
coating the polymer and the positive active material matrix to obtain a second mixture; and
and carrying out heat treatment on the second mixed material so as to form a coating layer on the outer surface of the positive active material matrix, thereby obtaining the positive active material.
2. The positive electrode active material according to claim 1, wherein the positive electrode active material matrix is a nickel-cobalt-manganese ternary material.
3. The positive electrode active material according to claim 1, wherein the particle diameter of the positive electrode active material matrix is 3 to 20 μm.
4. The positive electrode active material according to claim 1, wherein the metal oxide is selected from oxides formed of Al.
5. The positive electrode active material according to claim 1, wherein the alcohol compound is selected from at least one of: ethylene glycol and glycerol.
6. The positive electrode active material according to claim 1, wherein the alcohol compound is selected from ethylene glycol.
7. A method for producing the positive electrode active material according to any one of claims 1 to 6, comprising:
mixing the metal salt and the alcohol compound to obtain a first mixture;
polymerizing the first mixture to obtain a polymer;
coating the polymer and the positive active material matrix to obtain a second mixture; and
and carrying out heat treatment on the second mixed material so as to form a coating layer on the outer surface of the positive active material matrix, thereby obtaining the positive active material.
8. The method according to claim 7, wherein the concentration of the metal salt in the first mixture is 0.05-2 mol/L.
9. The method according to claim 7, wherein the polymerization is carried out at 60 to 120 ℃ for 10 minutes to 10 hours.
10. The method of claim 7, wherein the coating treatment time is 1 minute to 2 hours.
11. The method according to claim 7, wherein the heat treatment is performed at 400 to 700 ℃ for 10 minutes to 20 hours.
12. The method of claim 7, further comprising:
diluting the polymer by using an organic solvent, and coating the obtained diluent and the positive active material matrix;
and before the heat treatment, drying the second mixture.
13. The method according to claim 12, wherein the concentration of the polymer in the diluent is 0.001 to 0.1 mol/L.
14. The method according to claim 12, wherein the mass ratio of the diluent to the positive electrode active material matrix is (0.1-10): 1.
15. The method according to claim 12, wherein the drying treatment is carried out at a temperature of 60 to 180 ℃ for 1 to 48 hours.
16. A lithium ion battery comprising the positive electrode active material according to any one of claims 1 to 6.
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| CN110165166B (en) * | 2019-05-13 | 2021-03-16 | 北京石油化工学院 | Method for in-situ coating of lithium ion battery anode material assisted by microemulsion |
| CN111048773B (en) * | 2019-12-19 | 2021-06-15 | 中冶瑞木新能源科技有限公司 | Core-double-shell structure composite nickel-cobalt-manganese ternary positive electrode material, lithium battery and vehicle |
| CN111536767B (en) * | 2020-05-08 | 2021-06-04 | 潍坊学院 | Integrative device of drying cooling of preparation cladding type nickel cobalt lithium manganate cathode material |
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