CN115140784A - Lithium-rich ternary cathode material and preparation method and application thereof - Google Patents
Lithium-rich ternary cathode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a lithium-rich ternary cathode material and a preparation method and application thereof, belonging to the field of inorganic materials. According to the invention, a lithium source, a nickel source, a cobalt source and a manganese source are mixed and then are subjected to dry grinding to obtain mixed powder with uniformly mixed components and smaller particle size, the mixed powder is subjected to wet grinding after being mixed with water to further promote the mixing uniformity and the particle size uniformity of the components so as to improve the electrical property of the subsequently prepared lithium-rich ternary positive electrode material, a mixed slurry is obtained, and then the lithium-rich ternary positive electrode material with a layered crystal structure is obtained through calcination. The method provided by the invention combines dry grinding, wet grinding and calcining, belongs to a semi-solid phase method, does not generate waste liquid, is green and environment-friendly, has high production efficiency and simple process, and is suitable for large-scale production. The specific capacity of the prepared lithium-rich ternary cathode material is more than 200 mAh/g.
Description
Technical Field
The invention relates to the field of electrode materials, in particular to a lithium-rich ternary cathode material and a preparation method and application thereof.
Background
The ternary material has a wide application prospect in the field of new energy automobiles, and compared with lithium cobaltate and lithium iron phosphate anode materials, the ternary anode material has obvious advantages in the aspect of energy density. The lithium content of the lithium-rich ternary cathode material is increased compared with that of a common ternary material, so that the energy density of the lithium-rich ternary cathode material is obviously improved compared with that of the conventional ternary cathode material. However, lithium-rich ternary cathode materials have not yet been implemented for large-scale commercial applications, and are mainly found in literature reports.
The preparation method of the lithium-rich ternary cathode material reported in the literature at present is mainly a liquid phase mixing method, namely, a lithium compound, a nickel compound, a cobalt compound and a manganese compound are mixed in organic liquid or aqueous solution, and then the mixed solution is dried. Therefore, how to prepare the lithium-rich ternary cathode material with high specific capacity in a simple process, high efficiency, environmental protection and no pollution mode is a problem which needs to be solved in the prior art.
Disclosure of Invention
The preparation method of the lithium-rich ternary cathode material belongs to a semi-solid phase method, is simple in process, high in production efficiency, free of waste liquid treatment problem, green and environment-friendly, and has high specific capacity.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a lithium-rich ternary cathode material, which comprises the following steps:
(1) Mixing a lithium source, a nickel source, a cobalt source and a manganese source, and then carrying out dry grinding to obtain mixed powder;
(2) Mixing the mixed powder obtained in the step (1) with water, and then carrying out wet milling to obtain mixed slurry;
(3) And (3) calcining the mixed slurry obtained in the step (2) to obtain the lithium-rich ternary cathode material.
Preferably, the ratio of the amounts of the lithium source, the nickel source, the cobalt source and the manganese source in the step (1) is (200-300): (25-40): (90-130).
Preferably, the average particle size of the mixed powder in the step (1) is 200 μm or less.
Preferably, the wet milling time in the step (2) is 10 to 130min.
Preferably, the mixed slurry in the step (2) is a viscous paste which is mixed uniformly.
Preferably, the mass fraction of water in the mixed slurry in the step (2) is 15-70%.
Preferably, before the calcining in the step (3), the method further comprises the step of preheating the mixed slurry.
Preferably, the calcination in the step (3) is carried out in an air atmosphere, the calcination temperature is 800-1000 ℃, and the calcination time is 10-14 h.
The invention also provides the lithium-rich ternary cathode material prepared by the preparation method in the technical scheme. In the invention, the lithium-rich ternary cathode material is Li with a layered crystal structure 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
The invention also provides the application of the lithium-rich ternary cathode material in the technical scheme in a lithium ion battery.
The invention has the beneficial effects that:
the invention provides a preparation method of a lithium-rich ternary cathode material, which comprises the steps of mixing a lithium source, a nickel source, a cobalt source and a manganese source, then carrying out dry grinding to obtain mixed powder with uniformly mixed components and smaller particle size, mixing the mixed powder with water, then carrying out wet grinding to further promote the mixing uniformity and the particle size uniformity of the components so as to improve the electrical property of the subsequently prepared lithium-rich ternary cathode material to obtain mixed slurry, then carrying out calcination, and decomposing and compounding the lithium source, the nickel source, the cobalt source and the manganese source to finally obtain the lithium-rich ternary cathode material with a layered crystal structure, namely the Li ternary cathode material 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 . The method provided by the invention combines dry grinding, wet grinding and calcining, belongs to a semi-solid phase method, does not generate waste liquid, is green and environment-friendly, has high production efficiency and simple process, and is suitable for large-scale production. The results of the embodiment show that the method provided by the invention has the advantages of high production efficiency, no waste liquid, environmental protection, and excellent electrical properties, and the prepared lithium-rich ternary cathode material has the specific capacity of more than 200 mAh/g.
Drawings
FIG. 1 is an X-ray diffraction spectrum of a lithium-rich ternary cathode material prepared in example 1 of the present invention;
FIG. 2 is a graph comparing the charge and discharge performance of the lithium-rich ternary cathode materials prepared in examples 1-4 of the present invention and the ternary cathode material prepared in comparative example 2;
FIG. 3 is a graph of rate performance of a lithium-rich ternary cathode material prepared in example 1 of the present invention;
fig. 4 is an SEM image of the lithium-rich ternary cathode material prepared in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of a lithium-rich ternary cathode material, which comprises the following steps:
(1) Mixing a lithium source, a nickel source, a cobalt source and a manganese source, and then carrying out dry grinding to obtain mixed powder;
(2) Mixing the mixed powder obtained in the step (1) with water, and then carrying out wet milling to obtain mixed slurry;
(3) And (3) calcining the mixed slurry obtained in the step (2) to obtain the lithium-rich ternary cathode material.
In the present invention, the raw materials used are all commercial products which are conventional in the art, unless otherwise specified.
The method mixes the lithium source, the nickel source, the cobalt source and the manganese source and then carries out dry grinding to obtain mixed powder.
In the present invention, the lithium source is preferably one or more of lithium nitrate, lithium carbonate, lithium acetate and lithium sulfate. In the present invention, the nickel source is preferably one or more of nickel nitrate, nickel carbonate, nickel acetate, and nickel sulfate. In the present invention, the cobalt source is preferably one or more of cobalt nitrate, cobalt carbonate, cobalt acetate, and cobalt sulfate. In the present invention, the manganese source is preferably one or more of manganese nitrate, manganese carbonate, manganese acetate and manganese sulfate.
In the present invention, the ratio of the amounts of the lithium source, the nickel source, the cobalt source and the manganese source is (200-300): (25-40): (90-130), more preferably (230-280): (28-38): (95-125), still more preferably (240-260): (30-35): 95-120). According to the invention, the ratio of the quantities of the lithium source, the nickel source, the cobalt source and the manganese source is controlled within the range, so that the specific capacity performance of the subsequently prepared lithium-rich ternary cathode material is improved, and the lithium-rich ternary cathode material with excellent electrical properties is obtained.
The invention has no special limit on the mixing mode of the lithium source, the nickel source, the cobalt source and the manganese source, and can realize the uniform mixing of all the components.
In the present invention, the dry milling is preferably ball milling. The dry-milling time is not particularly limited, and the purpose of obtaining a mixed powder having a uniform particle size and an average particle size of 200 μm or less can be achieved.
In the present invention, the average particle diameter of the mixed powder is preferably 200 μm or less, and more preferably 180 μm or less. The invention controls the average grain diameter of the mixed powder within the upper range, which is beneficial to ensuring the uniformity of the dry-milled product.
After the mixed powder is obtained, the mixed powder and water are mixed and then wet-milled to obtain mixed slurry.
In the present invention, the water is preferably deionized water. In the present invention, the mass fraction of water in the mixed slurry is preferably 15 to 70%, more preferably 18 to 68%. The invention controls the mass fraction of water in the mixed slurry within the range, thereby being beneficial to ensuring the uniformity of mixed materials and reducing wastes.
The invention has no characteristic limit on the mixing mode of the mixed powder and water, and the components are uniformly mixed.
In the present invention, the wet milling is preferably performed by ball milling. In the present invention, the time for the wet milling is preferably 10 to 130min, more preferably 20 to 120min. According to the invention, the wet milling time is controlled within the range, so that the mixing uniformity and the particle size uniformity of each component are further promoted, and the electrical property of the lithium-rich ternary cathode material prepared subsequently is improved.
In the present invention, the mixed slurry is preferably in the form of a viscous paste which is uniformly mixed.
After the mixed slurry is obtained, the mixed slurry is preferably calcined to obtain the lithium-rich ternary cathode material.
In the invention, the pre-heating treatment of the mixed slurry is further carried out before the calcination, so as to obtain the pre-heated mixed slurry.
In the present invention, the preheating treatment is preferably performed in an air atmosphere. In the present invention, the temperature of the preheating treatment is preferably 300 to 500 ℃, more preferably 350 to 450 ℃. In the present invention, the time of the preheating treatment is preferably 4 to 7 hours, and more preferably 4.5 to 6 hours. According to the invention, the temperature and time of the preheating treatment are controlled within the above ranges, so that the full decomposition of each component in the mixed slurry and the occurrence of a composite reaction are facilitated, and the lithium-rich ternary cathode material with high specific capacity, a layered structure and high crystallinity is obtained.
In the present invention, the calcination is preferably carried out in an air atmosphere. In the present invention, the temperature of the calcination is preferably 800 to 1000 ℃, more preferably 850 to 950 ℃. In the present invention, the time for the calcination is preferably 10 to 14 hours, and more preferably 11 to 13 hours. According to the invention, the calcining temperature and time are controlled within the above ranges, so that the material can be kept in high uniformity and crystallinity, and the lithium-rich ternary cathode material with excellent electrical properties can be obtained.
The invention also provides the lithium-rich ternary cathode material prepared by the preparation method in the technical scheme. In the invention, the lithium-rich ternary cathode material is Li with a layered crystal structure 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
The invention also provides the application of the lithium-rich ternary cathode material in the technical scheme in a lithium ion battery.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Preparation method of lithium-rich ternary cathode material
(1) Mixing 1.72g of lithium nitrate, 0.62g of nickel nitrate, 0.59g of cobalt nitrate and 1.88g of manganese acetate, and then carrying out ball milling to obtain mixed powder with the average particle size of below 200 mu m;
the mass ratio of the lithium nitrate to the nickel nitrate to the cobalt nitrate to the manganese acetate is 249: 34: 32: 109;
(2) Mixing the mixed powder obtained in the step (1) with 1.15g of deionized water, and then carrying out ball milling for 120min to obtain pink mixed slurry which is uniformly mixed and is in a thick paste shape; the mass fraction of the deionized water in the mixed slurry is 19%;
(3) And (3) in an air atmosphere, carrying out preheating treatment on the mixed slurry obtained in the step (2) at 450 ℃ for 5h, and then calcining at 900 ℃ for 12h to obtain the lithium-rich ternary cathode material.
FIG. 1 is an X-ray diffraction spectrum of the lithium-rich ternary cathode material prepared in example 1, and it can be seen from FIG. 1 that the lithium-rich ternary cathode material prepared in example 1 has a peak (003) at 18 degrees, a peak (101) at 37 degrees, a peak (104) at 45 degrees and Li prepared by a liquid phase mixing method reported in the literature 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 The diffraction peaks are consistent, which shows that the Li-rich ternary cathode material successfully prepared in example 1 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
Fig. 3 is a rate performance graph of the lithium-rich ternary cathode material prepared in example 1, and it can be seen from fig. 3 that the specific capacity of the lithium-rich ternary cathode material prepared in example 1 can reach more than 200mAh/g at a current density of 15mA/g, and is about 150mAh/g at a current density of 150 mA/g.
Fig. 4 is an SEM image of the lithium-rich ternary cathode material prepared in example 1, and it can be seen from fig. 4 that the lithium-rich ternary cathode material prepared in example 1 has a layered crystal structure and a size of 100 to 500nm.
Example 2
Preparing a lithium-rich ternary cathode material according to the method of example 1;
unlike example 1, the deionized water in step (2) was 2.3g, and the mass fraction of the deionized water in the mixed slurry was 32%.
Example 3
Preparing a lithium-rich ternary cathode material according to the method of example 1;
unlike example 1, the deionized water in step (2) was 4.6g, and the mass fraction of the deionized water in the mixed slurry was 49%.
Example 4
Preparing a lithium-rich ternary cathode material according to the method of example 1;
unlike example 1, the deionized water in step (2) was 9.2g, and the mass fraction of the deionized water in the mixed slurry was 66%.
Comparative example 1
Preparing a ternary cathode material;
(1) Mixing 1.72g of lithium nitrate, 0.62g of nickel nitrate, 0.59g of cobalt nitrate, 1.88g of manganese acetate and 1.15g of deionized water, and then carrying out ball milling for 120min to obtain pink and uniformly mixed thick pasty mixed slurry; the mass ratio of the lithium nitrate to the nickel nitrate to the cobalt nitrate to the manganese acetate is 249: 34: 32: 109; the mass fraction of the deionized water in the mixed slurry is 21%;
(2) And (3) in an air atmosphere, carrying out preheating treatment on the mixed slurry obtained in the step (2) at 450 ℃ for 5h, and then calcining at 900 ℃ for 12h to obtain the ternary cathode material.
Comparative example 2
(1) Mixing 1.72g of lithium nitrate, 0.62g of nickel nitrate, 0.59g of cobalt nitrate and 1.88g of manganese acetate, and then carrying out ball milling for 120min to obtain mixed powder with the average particle size of below 200 mu m; the mass ratio of the lithium nitrate, the nickel nitrate, the cobalt nitrate and the manganese acetate is 249: 34: 32: 109;
(2) And (2) in an air atmosphere, carrying out preheating treatment on the mixed powder obtained in the step (1) at 450 ℃ for 5h, and then calcining at 900 ℃ for 12h to obtain the ternary cathode material.
Fig. 2 is a comparison graph of charge and discharge performances of the lithium-rich ternary cathode materials prepared in examples 1 to 4 and the ternary cathode material prepared in comparative example 2, and it can be seen from fig. 2 that the capacity performance of the electrode is improved with the increase of the mass fraction of deionized water in the mixed slurry within a certain range, and the specific capacity of the lithium-rich ternary cathode materials prepared in examples 1 to 4 is more than 200 mAh/g.
The embodiment shows that the method provided by the invention has the advantages of high production efficiency, no waste liquid, environmental protection, and excellent electrical property, and the specific capacity of the prepared lithium-rich ternary cathode material is more than 200 mAh/g. The preparation method of the lithium-rich ternary cathode material provided by the invention combines dry grinding, wet grinding and calcining, belongs to a semi-solid phase method, does not generate waste liquid, is green and environment-friendly, has high production efficiency and simple process, and is suitable for large-scale production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the lithium-rich ternary cathode material is characterized by comprising the following steps of:
(1) Mixing a lithium source, a nickel source, a cobalt source and a manganese source, and then carrying out dry grinding to obtain mixed powder;
the mass ratio of the lithium source to the nickel source to the cobalt source to the manganese source is (200-300) to (25-40) to (90-130);
(2) Mixing the mixed powder obtained in the step (1) with water, and then carrying out wet milling to obtain mixed slurry;
(3) And (3) calcining the mixed slurry obtained in the step (2) to obtain the lithium-rich ternary cathode material.
2. The method according to claim 1, wherein the ratio of the amounts of the lithium source, the nickel source, the cobalt source and the manganese source in step (1) is (230-280) to (28-38) to (95-125).
3. The production method according to claim 1, wherein the average particle diameter of the mixed powder in the step (1) is 200 μm or less.
4. The method according to claim 1, wherein the time for wet milling in the step (2) is 10 to 130min.
5. The method according to claim 1, wherein the mixed slurry in the step (2) is in a viscous paste shape which is uniformly mixed.
6. The method according to claim 1 or 5, wherein the mass fraction of water in the mixed slurry in the step (2) is 15 to 70%.
7. The method according to claim 1, wherein the step (3) of pre-heating the mixed slurry before calcining.
8. The preparation method according to claim 1, wherein the calcination in the step (3) is carried out in an air atmosphere, the calcination temperature is 800-1000 ℃, and the calcination time is 10-14 h.
9. The lithium-rich ternary cathode material prepared by the preparation method of any one of claims 1 to 8, wherein the lithium-rich ternary cathode material is Li with a layered crystal structure 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
10. Use of the lithium-rich ternary cathode material of claim 9 in a lithium ion battery.
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