CN112164774A - Composite high-nickel ternary cathode material and preparation method thereof - Google Patents
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Abstract
The invention discloses a composite high-nickel ternary cathode material and a preparation method thereof. The invention effectively solves the problem of poor cycle stability of the high-nickel ternary material, and the coating treatment process is relatively simple and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of lithium battery anode materials, in particular to a composite high-nickel ternary anode material and a preparation method thereof.
Background
High nickel ternary positive electrode materials are commonly referred to as NixCoyMn1-x-y(OH)2(x is more than or equal to 0.8) and mainly contains three elements of Ni, Mn and Co, wherein the Ni element containsThe higher the amount, the higher the capacity of the material, but the poorer the stability of the corresponding material, and in particular the stability of the material/electrolyte interface is also reduced accordingly, resulting in the occurrence of side reactions, which affect the cycling stability of the material. This is also a significant reason why high nickel ternary materials, especially NMC811 materials, have not become popular. Surface coating is a common method for improving the interface stability of materials, and common coating materials comprise MgO and Al2O3、TiO2、SiO2、ZnO、SnO2、ZrO2The main action principle of surface coating is to prevent the material surface from directly contacting with electrolyte, reduce the occurrence of side reaction, inhibit the phase change of the material, and improve the structural stability of the material, thereby improving the circulation stability of the material. However, the cycle stability of the high nickel ternary cathode material cannot be significantly improved by a single metal oxide coating.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a composite high-nickel ternary cathode material and a preparation method thereof.
The invention provides a composite high-nickel ternary cathode material which is composed of a high-nickel ternary cathode material, a metal oxide layer coated on the surface of the high-nickel ternary cathode material and a sulfonate layer coated on the surface of the metal oxide layer.
Preferably, the mass ratio of the metal oxide layer to the high-nickel ternary cathode material is (0.1-5): 1000, and the mass ratio of the sulfonate layer to the high-nickel ternary cathode material is (1-5): 1000.
preferably, the high-nickel ternary cathode material is LiNixCoyMn1-x-yO2Wherein x is more than or equal to 0.8 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.2.
Preferably, the metal oxide is Al2O3、TiO2、SiO2、ZnO、SnO2And ZrO.
Preferably, the sulfonate is at least one of alpha-olefin sulfonate, N-dimethyl pyrrolidine methyl sulfonate and fatty acid methyl ester sulfonate; the mass ratio of the sulfonate to the primary calcined product is (1-5): 1000.
the invention also provides a preparation method of the composite high-nickel ternary cathode material, which comprises the following steps:
s1, uniformly mixing the high-nickel ternary precursor, a lithium source and a metal oxide to obtain a precursor mixture;
s2, carrying out primary calcination on the precursor mixture to obtain a primary calcined product;
s3, mixing the primary calcined product with sulfonate and a solvent to coat the sulfonate on the surface of the primary calcined product to obtain mixed slurry;
and S4, filtering the mixed slurry, drying a filter cake, and then carrying out secondary calcination to obtain the composite high-nickel ternary cathode material.
Preferably, the high-nickel ternary precursor is NixCoyMn1-x-y(OH)2、NixCoyMn1-x-yCO3Or a combination thereof, wherein x is more than or equal to 0.8 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.2.
Preferably, the lithium source is Li2CO3LiOH, or a combination thereof; the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in the lithium source is 1 (1.01-1.07).
Preferably, the solvent is N-methylpyrrolidone.
Preferably, the solid content of the mixed slurry is 40-55%.
Preferably, in the step S2, the temperature of the primary calcination is 750 to 850 ℃, and the time is 10 to 12 hours; in the step S4, the temperature of the secondary calcination is 450-600 ℃, and the time is 6-8 h.
Preferably, in the steps S2 and S4, the atmosphere of the primary calcination and the secondary calcination is a high-purity oxygen atmosphere, and the oxygen concentration is greater than or equal to 96%.
Preferably, in the step S3, after the primary calcined product is mixed with sulfonate and a solvent, the mixture is stirred at a high speed in vacuum for 2 to 3 hours, so that the sulfonate is coated on the surface of the primary calcined product, thereby obtaining a mixed slurry.
The invention has the following beneficial effects:
the preparation method comprises the steps of uniformly mixing a high-nickel ternary precursor, a lithium source and a metal oxide to obtain a precursor mixture, then carrying out primary calcination, forming a high-nickel ternary positive electrode material coated with a metal oxide layer in the primary calcination process, namely a primary calcination product, mixing the primary calcination product with sulfonate and a solvent, carrying out vacuum high-speed stirring to enable the sulfonate to be coated on the surface of the primary calcination product to obtain mixed slurry, filtering the mixed slurry, drying a filter cake, and carrying out secondary calcination.
According to the invention, the high-nickel ternary material is coated by the metal oxide and the sulfonate, on one hand, the coating of the metal oxide can obviously reduce the surface residual alkali content of the lithium ion battery, reduce the surface pH value of the material and improve the processing performance of the material, so that the safety of the whole battery system is improved, on the other hand, the sulfonate-based surface coating layer can well inhibit the decomposition of electrolyte in the circulation process and improve the circulation performance of the high-nickel ternary material, and the coating layer can also promote Li+The purpose of improving the rate capability of the material is achieved by diffusion; in conclusion, the method effectively solves the problem of poor circulation stability of the high-nickel ternary material by utilizing the synergistic effect of co-coating of the metal oxide and the sulfonate, and is relatively simple in coating treatment process and suitable for large-scale industrial production.
Drawings
Fig. 1 is a cycle curve obtained by assembling the materials obtained in example 1, comparative example 1 and comparative example 2 as positive electrode active materials into a battery and performing a cycle test.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A composite high-Ni ternary positive electrode material is prepared from LiNi0.8Co0.1Mn0.1O2MaterialCoated with LiNi0.8Co0.1Mn0.1O2Al of material surface2O3And coating with Al2O3Alpha-olefin sulfonate of the surface, wherein Al2O3And LiNi0.8Co0.1Mn0.1O2The mass ratio of the material is 1:1000, and the alpha-olefin sulfonate and the LiNi are0.8Co0.1Mn0.1O2The mass ratio of the materials is 1: 1000.
the preparation method of the composite high-nickel ternary cathode material comprises the following steps:
s1, chemical formula is Ni0.8Co0.1Mn0.1(OH)2High nickel ternary precursor, LiOH and Al2O3Mixing for 20min under the condition of 500r/min to obtain a precursor mixture, wherein the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in LiOH is 1: 1.01;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 750 ℃ and the primary calcination time is 10 hours;
s3, crushing the primary calcined product, mixing the crushed primary calcined product with alpha-alkenyl sulfonate and N-methyl pyrrolidone, and stirring the mixture for 2 hours at a high speed in vacuum to obtain mixed slurry with the solid content of 40%;
s4, filtering the mixed slurry, drying a filter cake, performing secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, and then crushing and demagnetizing to obtain the composite high-nickel ternary cathode material, wherein the secondary calcination temperature is 450 ℃ and the time is 6 hours.
Example 2
A composite high-Ni ternary positive electrode material is prepared from LiNi0.85Co0.1Mn0.05O2Material coated with LiNi0.85Co0.1Mn0.05O2ZrO of material surface2And cladding at ZrO2Surface of N, N-dimethylpyrrolidine methanesulfonate, wherein ZrO2And LiNi0.85Co0.1Mn0.05O2The mass ratio of the material is 3:1000, and the N, N-dimethyl pyrrolidine methyl sulfonate and LiNi are0.85Co0.1Mn0.05O2The mass ratio of the materials is 3: 1000.
the preparation method of the composite high-nickel ternary cathode material comprises the following steps:
s1, chemical formula is Ni0.85Co0.1Mn0.05(OH)2High nickel ternary precursor, Li0H and ZrO2Mixing for 20min at 500r/min to obtain a precursor mixture, wherein the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in the lithium source is 1: 1.03;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 800 ℃ and the primary calcination time is 12 hours;
s3, crushing the primary calcined product, mixing the crushed primary calcined product with N, N-dimethyl pyrrolidine methyl sulfonate and N-methyl pyrrolidone, and stirring the mixture for 2.5 hours at a high speed in vacuum to obtain mixed slurry with the solid content of 42%;
s4, filtering the mixed slurry, drying a filter cake, performing secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, and then crushing and demagnetizing to obtain the composite high-nickel ternary cathode material, wherein the secondary calcination temperature is 500 ℃ and the time is 6.5 hours.
Example 3
A composite high-Ni ternary positive electrode material is prepared from LiNi0.9Co0.05Mn0.05O2Material coated with LiNi0.9Co0.05Mn0.05O2TiO on the surface of the material2And coating on TiO2Fatty acid methyl ester sulfonate of the surface, wherein TiO2And LiNi0.9Co0.05Mn0.05O2The mass ratio of the material is 5:1000, and the mass ratio of the fatty acid methyl ester sulfonate to the LiNi is0.9Co0.05Mn0.05O2The mass ratio of the materials is 5: 1000.
the preparation method of the composite high-nickel ternary cathode material comprises the following steps:
s1, chemical formula is Ni0.9Co0.05Mn0.05(OH)2High nickel ternary precursor, Li0H and TiO2Mixing for 20min at 500r/min to obtain a precursor mixture;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 850 ℃, the primary calcination time is 10.5h, and the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in the lithium source is 1: 1.07;
s3, crushing the primary calcined product, mixing the crushed primary calcined product with fatty acid methyl ester sulfonate and N-methyl pyrrolidone, and stirring the mixture for 3 hours at a high speed in vacuum to obtain mixed slurry with the solid content of 45%;
s4, filtering the mixed slurry, drying a filter cake, performing secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, crushing, and demagnetizing to obtain the composite high-nickel ternary cathode material, wherein the secondary calcination temperature is 550 ℃ and the time is 8 hours.
Example 4
A composite high-Ni ternary positive electrode material is prepared from LiNi0.8Co0.1Mn0.1O2Material coated with LiNi0.8Co0.1Mn0.1O2Al of material surface2O3And coating with Al2O3Alpha-olefin sulfonate of the surface, wherein Al2O3And LiNi0.8Co0.1Mn0.1O2The mass ratio of the material is 0.1:1000, and the alpha-olefin sulfonate and the LiNi are0.8Co0.1Mn0.1O2The mass ratio of the materials is 1: 1000.
the preparation method of the composite high-nickel ternary cathode material comprises the following steps:
s1, chemical formula is Ni0.8Co0.1Mn0.1(OH)2High nickel ternary precursor, Li2CO3And Al2O3Mixing at 500r/min for 20min to obtain precursor mixtureTotal amount of metal ions in medium-high nickel ternary precursor and Li2CO3The mass ratio of the lithium ion in the lithium ion battery is 1: 1.01;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 750 ℃ and the primary calcination time is 10 hours;
s3, crushing the primary calcined product, mixing the crushed primary calcined product with alpha-alkenyl sulfonate and N-methyl pyrrolidone, and stirring the mixture for 2 hours at a high speed in vacuum to obtain mixed slurry with the solid content of 55%;
s4, filtering the mixed slurry, drying a filter cake, performing secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, and then crushing and demagnetizing to obtain the composite high-nickel ternary cathode material, wherein the secondary calcination temperature is 600 ℃ and the time is 7 hours.
Comparative example 1
LiNi0.8Co0.1Mn0.1O2The preparation method of the material comprises the following steps:
s1, chemical formula is Ni0.8Co0.1Mn0.1(OH)2The high nickel ternary precursor and LiOH are mixed for 20min under the condition of 500r/min to obtain a precursor mixture, wherein the ratio of the total amount of metal ions in the high nickel ternary precursor to the amount of lithium ions in the LiOH is 1: 1.01;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 750 ℃ and the primary calcination time is 10 hours;
s3, crushing the primary calcined product, then carrying out secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, and then crushing and demagnetizing to obtain LiNi0.8Co0.1Mn0.1O2The material, wherein the temperature of the secondary calcination is 450 ℃, and the time is 6 h.
Comparative example 2
A composite high-Ni ternary positive electrode material is prepared from LiNi0.8Co0.1Mn0.1O2Material coated with LiNi0.8Co0.1Mn0.1O2Al of material surface2O3Is composed of Al2O3And LiNi0.8Co0.1Mn0.1O2The mass ratio of the materials is 1: 1000.
The preparation method of the composite high-nickel ternary cathode material comprises the following steps:
s1, chemical formula is Ni0.8Co0.1Mn0.1(OH)2High nickel ternary precursor, LiOH and Al2O3Mixing for 20min under the condition of 500r/min to obtain a precursor mixture, wherein the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in LiOH is 1: 1.01;
s2, carrying out primary calcination on the precursor mixture in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96% to obtain a primary calcined product, wherein the primary calcination temperature is 750 ℃ and the primary calcination time is 10 hours;
and S3, crushing the primary calcined product, then carrying out secondary calcination in a high-purity oxygen atmosphere with the oxygen concentration of more than or equal to 96%, and then crushing and demagnetizing to obtain the composite high-nickel ternary cathode material, wherein the temperature of the secondary calcination is 450 ℃ and the time is 6 hours.
The materials prepared in example 1, comparative example 1 and comparative example 2 were used as positive electrode active materials, assembled into batteries, and subjected to cycle test at 25 ℃ under 0.5C/1C and 2.8-4.2V, and the test results are shown in FIG. 1. As can be seen from fig. 1, the cycle performance of the metal oxide-sulfonate co-coated high nickel ternary cathode material in example 1 of the present invention is significantly higher than that of the uncoated high nickel ternary cathode material in comparative example 1, and that of the high nickel ternary cathode material coated with only the metal oxide in comparative example 2.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The composite high-nickel ternary cathode material is characterized by comprising a high-nickel ternary cathode material, a metal oxide coated on the surface of the high-nickel ternary cathode material and a sulfonate layer coated on the surface of the metal oxide.
2. The composite high-nickel ternary cathode material according to claim 1, wherein the mass ratio of the metal oxide to the high-nickel ternary cathode material is (0.1-5): 1000, and the mass ratio of the sulfonate to the high-nickel ternary cathode material is (1-5): 1000.
3. the composite high-nickel ternary positive electrode material according to claim 1 or 2, wherein the high-nickel ternary positive electrode material is LiNixCoyMn1-x-yO2Wherein x is more than or equal to 0.8 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.2.
4. The composite high-nickel ternary positive electrode material according to any one of claims 1 to 3, wherein the metal oxide is Al2O3、TiO2、SiO2、ZnO、SnO2At least one of ZrO; the sulfonate is at least one of alpha-olefin sulfonate, N-dimethyl pyrrolidine methyl sulfonate and fatty acid methyl ester sulfonate.
5. A method for preparing the composite high-nickel ternary positive electrode material according to any one of claims 1 to 4, comprising the following steps:
s1, uniformly mixing the high-nickel ternary precursor, a lithium source and a metal oxide to obtain a precursor mixture;
s2, carrying out primary calcination on the precursor mixture to obtain a primary calcined product;
s3, mixing the primary calcined product with sulfonate and a solvent to coat the sulfonate on the surface of the primary calcined product to obtain mixed slurry;
and S4, filtering the mixed slurry, drying a filter cake, and then carrying out secondary calcination to obtain the composite high-nickel ternary cathode material.
6. The method for preparing the composite high-nickel ternary cathode material according to claim 5, wherein the high-nickel ternary precursor is NixCoyMn1-x-y(OH)2、NixCoyMn1-x-yCO3Or a combination thereof, wherein x is more than or equal to 0.8 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 0.2.
7. The method of claim 5 or 6, wherein the lithium source is Li2CO3LiOH, or a combination thereof; the ratio of the total amount of metal ions in the high-nickel ternary precursor to the amount of lithium ions in the lithium source is 1 (1.01-1.07).
8. The preparation method of the composite high-nickel ternary cathode material as claimed in any one of claims 5 to 7, wherein the solid content of the mixed slurry is 40-55%.
9. The preparation method of the composite high-nickel ternary cathode material according to any one of claims 5 to 8, wherein in the step S2, the temperature of primary calcination is 750 to 850 ℃, and the time is 10 to 12 hours; in the step S4, the temperature of the secondary calcination is 450-600 ℃, and the time is 6-8 h.
10. The method for preparing the composite high-nickel ternary cathode material according to any one of claims 5 to 9, wherein in the steps S2 and S4, the atmosphere of primary calcination and secondary calcination is a high-purity oxygen atmosphere, and the oxygen concentration is not less than 96%.
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| WO2024090148A1 (en) * | 2022-10-24 | 2024-05-02 | パナソニックＩｐマネジメント株式会社 | Non-aqueous electrolyte secondary battery |
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