CN115140784B - Lithium-rich ternary positive electrode material and preparation method and application thereof - Google Patents
Lithium-rich ternary positive electrode material and preparation method and application thereof Download PDFInfo
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- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- 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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- H01M4/525—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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- H01M4/02—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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Abstract
The invention provides a lithium-rich ternary positive electrode material, and a preparation method and application thereof, and belongs 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 subjected to dry grinding to obtain mixed powder with uniform and smaller particle size, the mixed powder is mixed with water and then subjected to wet grinding, so that the mixing uniformity of the components and the uniformity of the particle size are further promoted, the electrical property of the lithium-rich ternary positive electrode material prepared subsequently is improved, mixed slurry is obtained, and 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 calcination, belongs to a semi-solid phase method, has no waste liquid, is 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 positive electrode 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 anode material, and a preparation method and application thereof.
Background
The ternary material has wide application prospect in the field of new energy automobiles, and compared with the lithium cobaltate and lithium iron phosphate positive electrode materials, the ternary positive electrode material has obvious advantages in the aspect of energy density. The lithium content of the lithium-rich ternary positive electrode material is increased compared with that of the common ternary material, so that the energy density of the lithium-rich ternary positive electrode material is obviously improved compared with that of the conventional ternary positive electrode material. However, lithium-rich ternary cathode materials have not achieved large-scale commercial application, and are mainly reported in literature.
The preparation method of the lithium-rich ternary cathode material reported in the current literature mainly comprises a liquid phase mixing method, namely mixing a lithium compound, a nickel compound, a cobalt compound and a manganese compound in an organic liquid or an aqueous solution, and drying the mixed solution. Therefore, how to realize simple process, high efficiency, environmental protection and no pollution to prepare the lithium-rich ternary positive electrode material with high specific capacity is a problem to be solved in the prior art.
Disclosure of Invention
The invention aims to provide a lithium-rich ternary positive electrode material, a preparation method and application thereof, and the preparation method of the lithium-rich ternary positive electrode material provided by the invention 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 higher 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 positive electrode 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 performing wet grinding to obtain mixed slurry;
(3) And (3) calcining the mixed slurry obtained in the step (2) to obtain the lithium-rich ternary anode material.
Preferably, the ratio of the amounts of the substances of the lithium source, the nickel source, the cobalt source and the manganese source in the step (1) is (200-300) to (25-40) to (90-130).
Preferably, the average particle diameter of the mixed powder in the step (1) is 200 μm or less.
Preferably, the wet milling time in the step (2) is 10-130 min.
Preferably, in the step (2), the mixed slurry is in a pasty state.
Preferably, the mass fraction of water in the mixed slurry in the step (2) is 15-70%.
Preferably, the step (3) further comprises preheating the slurry mixture before calcination.
Preferably, the calcination in the step (3) is performed 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 anode material prepared by the preparation method. In the invention, the lithium-rich ternary positive electrode material is Li with layered crystal structure 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
The invention also provides application of the lithium-rich ternary anode material in a lithium ion battery.
The beneficial effects of the invention are as follows:
the invention provides a preparation method of a lithium-rich ternary positive electrode material, which comprises the steps of firstly mixing a lithium source, a nickel source, a cobalt source and a manganese source, carrying out dry grinding to obtain mixed powder with uniform and smaller particle size of each component, mixing the mixed powder with water, carrying out wet grinding to further promote the mixing uniformity and the particle size uniformity of each component so as to improve the electrical property of the lithium-rich ternary positive electrode material prepared later, obtain mixed slurry, and then calcining, wherein the lithium source, the nickel source, the cobalt source and the manganese source are decomposed and compounded to finally obtain the lithium-rich ternary positive electrode material with a layered crystal structure, namely Li 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 calcination, belongs to a semi-solid phase method, has no waste liquid, is 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 high production efficiency, no waste liquid generation, green and environment-friendly performance, and the prepared lithium-rich ternary positive electrode material has specific capacity of more than 200mAh/g and excellent electrical performance.
Drawings
FIG. 1 is an X-ray diffraction spectrum of a lithium-rich ternary cathode material prepared in example 1 of the invention;
FIG. 2 is a graph showing the charge and discharge performance of the lithium-rich ternary cathode materials prepared in examples 1 to 4 according to the present invention and the ternary cathode material prepared in comparative example 2;
FIG. 3 is a graph showing the rate performance of the 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 positive electrode 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 performing wet grinding to obtain mixed slurry;
(3) And (3) calcining the mixed slurry obtained in the step (2) to obtain the lithium-rich ternary anode material.
In the present invention, the raw materials used are all conventional commercial products in the art unless otherwise specified.
According to the invention, a lithium source, a nickel source, a cobalt source and a manganese source are mixed and then subjected to dry grinding, so that mixed powder is obtained.
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, nickel source, cobalt source and 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). The invention controls the mass ratio of the lithium source, the nickel source, the cobalt source and the manganese source in the range, which is beneficial to improving the specific capacity performance of the lithium-rich ternary positive electrode material prepared subsequently so as to obtain the lithium-rich ternary positive electrode material with excellent electrical performance.
The invention has no special limitation on the mixing mode of the lithium source, the nickel source, the cobalt source and the manganese source, and can realize uniform mixing of all the components.
In the present invention, the dry milling is preferably performed by ball milling. The time of the dry milling is not particularly limited, and the purpose of obtaining a mixed powder having a uniform particle diameter and an average particle diameter 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, 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-grinding 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 slurry mixture 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, which is beneficial to reducing waste while guaranteeing the uniformity of mixing.
The invention has no characteristic limitation on the mixing mode of the mixed powder and water, and can realize uniform mixing of all the components.
In the present invention, the wet milling is preferably performed by ball milling. In the present invention, the time of the wet milling is preferably 10 to 130 minutes, more preferably 20 to 120 minutes. The invention controls the wet milling time within the range, which is beneficial to further promoting the mixing uniformity of each component and the uniformity of particle size, so as to improve the electrical property of the lithium-rich ternary positive electrode material prepared subsequently.
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 anode material.
In the invention, the method further comprises the step of carrying out preheating treatment on the mixed pulp before calcination to obtain preheated mixed pulp.
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, more preferably 4.5 to 6 hours. The invention controls the temperature and time of the preheating treatment in the above range, which is beneficial to promoting the full decomposition of each component in the mixed slurry and the occurrence of the composite reaction, thereby obtaining the lithium-rich ternary positive electrode material with high specific capacity, layered structure and high crystallinity.
In the present invention, the calcination is preferably performed 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 calcination time is preferably 10 to 14 hours, more preferably 11 to 13 hours. The invention controls the calcination temperature and time within the above range, which is beneficial to keeping the material with higher uniformity and crystallinity, and the lithium-rich ternary positive electrode material with excellent electrical property is obtained.
The invention also provides the lithium-rich ternary anode material prepared by the preparation method. In the invention, the lithium-rich ternary positive electrode material is Li with layered crystal structure 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
The invention also provides application of the lithium-rich ternary anode material in a lithium ion battery.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation method of lithium-rich ternary positive electrode 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 performing ball milling to obtain mixed powder with the average particle size 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) Mixing the mixed powder obtained in the step (1) with 1.15g of deionized water, and performing ball milling for 120min to obtain pink mixed slurry which is uniformly mixed and is in a thick paste shape; the mass fraction of deionized water in the mixed slurry is 19%;
(3) And (3) in an air atmosphere, preheating the mixed slurry obtained in the step (2) for 5 hours at 450 ℃, and calcining for 12 hours at 900 ℃ to obtain the lithium-rich ternary anode material.
FIG. 1 is an X-ray diffraction spectrum of the lithium-rich ternary cathode material prepared in example 1. As can be seen from FIG. 1, the lithium-rich ternary cathode material prepared in example 1 was prepared by a liquid phase mixing method of 18 DEG (003) peak, 37 DEG (101) peak, 45 DEG (104) peak and literature 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 Diffraction peaks are consistent, which shows that example 1 successfully prepares the lithium-rich ternary positive electrode material Li 1.2 Ni 0.13 Co 0.13 Mn 0.54 O 2 。
Fig. 3 is a graph of the rate performance of the lithium-rich ternary cathode material prepared in example 1, and as can be seen from fig. 3, 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 the specific capacity 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 as can be seen from fig. 4, the lithium-rich ternary cathode material prepared in example 1 has a layered crystal structure and a size of 100-500 nm.
Example 2
A lithium-rich ternary cathode material was prepared as in example 1;
unlike example 1, the deionized water in step (2) was 2.3g, and the mass fraction of deionized water in the slurry mixture was 32%.
Example 3
A lithium-rich ternary cathode material was prepared as in example 1;
unlike example 1, the deionized water in step (2) was 4.6g, and the mass fraction of deionized water in the slurry mixture was 49%.
Example 4
A lithium-rich ternary cathode material was prepared as in example 1;
unlike example 1, the deionized water in step (2) was 9.2g, and the mass fraction of deionized water in the slurry mixture was 66%.
Comparative example 1
Preparing a ternary positive electrode 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 performing ball milling for 120min to obtain pink mixed slurry which is a thick paste with uniform mixing; the mass ratio of the lithium nitrate, the nickel nitrate, the cobalt nitrate and the manganese acetate is 249:34:32:109; the mass fraction of deionized water in the mixed slurry is 21%;
(2) And (3) in an air atmosphere, preheating the mixed slurry obtained in the step (2) for 5 hours at 450 ℃, and then calcining for 12 hours at 900 ℃ to obtain the ternary positive electrode 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 performing ball milling for 120min to obtain mixed powder with the average particle size 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 (3) in an air atmosphere, preheating the mixed powder obtained in the step (1) for 5 hours at 450 ℃, and then calcining for 12 hours at 900 ℃ to obtain the ternary positive electrode material.
Fig. 2 is a graph comparing charge and discharge performance of the lithium-rich ternary cathode materials prepared in examples 1 to 4 and that of the ternary cathode material prepared in comparative example 2, and it can be seen from fig. 2 that the electrode capacity performance is improved along 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 generation, environment friendliness, and excellent electrical property, and the specific capacity of the prepared lithium-rich ternary positive electrode material is more than 200 mAh/g. The preparation method of the lithium-rich ternary cathode material combines dry grinding, wet grinding and calcination, belongs to a semi-solid phase method, generates no waste liquid, is environment-friendly, has high production efficiency and simple process, and is suitable for large-scale production.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The preparation method of the lithium-rich ternary positive electrode 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 average particle diameter of the mixed powder is below 200 mu m;
the mass ratio of the lithium source, the nickel source, the cobalt source and 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 performing wet grinding to obtain mixed slurry; the mass fraction of water in the mixed slurry is 49-70%;
(3) Calcining the mixed slurry obtained in the step (2) to obtain a lithium-rich ternary anode material; the mixed slurry is subjected to preheating treatment before calcination; the temperature of the preheating treatment is 300-500 ℃.
2. The method according to claim 1, wherein the amount of the lithium source, nickel source, cobalt source and manganese source in the step (1) is (230-280): (28-38): (95-125).
3. The method according to claim 1, wherein the wet milling in the step (2) is performed for 10 to 130 minutes.
4. The method according to claim 1, wherein the mixed slurry in the step (2) is a viscous paste which is uniformly mixed.
5. The method according to claim 1, wherein the calcination in the step (3) is performed in an air atmosphere at 800 to 1000 ℃ for 10 to 14 hours.
6. The lithium-rich ternary cathode material prepared by the preparation method according to any one of claims 1 to 5, 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 。
7. The use of the lithium-rich ternary cathode material of claim 6 in a lithium ion battery.
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