CN112768683A - Polyanion-doped manganese-rich ternary cathode material and preparation method thereof - Google Patents
Polyanion-doped manganese-rich ternary cathode material and preparation method thereof Download PDFInfo
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- H01M4/52—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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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a polyanion-doped manganese-rich ternary cathode material and a preparation method thereof. The chemical formula of the polyanion-doped manganese-rich ternary material is as follows: (LiNi)2Co2Mn5)1‑bMgbO2‑x(BO3) x; wherein b and x are mole fractions, b is more than or equal to 0 and less than or equal to 0.01, and x is more than or equal to 0.1 and less than or equal to 0.2. The preparation method comprises the following steps: (1): mixing carbonates of Mn, Ni and Co with the molar ratio of 5:3:2 with NaOH solution with equal concentration for precipitation reaction; (2): adding Mg sulfate in proportion and mixing with NaOH solution with equal concentration to obtain precipitate, and cleaning for later use; (3): adding Li to the product obtained in (2)3BO3Dissolving the solution and deionized water, reacting, and drying; (4): adding Li to the product obtained in (3)2CO3Mixing and reacting the mixture in the absolute ethyl alcohol solution, and drying the mixture; (5): sintering under oxygen atmosphere. The polyanion-doped manganese-rich ternary cathode material has good dispersibility, uniform granularity, stable electrical property and high energy density; the preparation method is simple and easy to operate, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a polyanion-doped manganese-rich ternary cathode material and a preparation method thereof.
Background
Lithium ion batteries have gained wide attention as new energy sources and have developed very rapidly in recent years. According to the action mechanism, the positive electrode material determines the overall performance of the lithium battery, so that the development of a new high-performance positive electrode material is a key for further promoting the development of the lithium ion battery. At present, commercial cathode materials such as lithium manganate have good safety performance, but have low energy density, and can be irreversibly converted to a spinel structure in the battery charging and discharging process, so that the cycle performance of the battery is seriously influenced. Lithium cobaltate has higher performance, but the development of lithium cobaltate is influenced due to poor safety performance of lithium cobaltate. The defects of the positive electrode material only containing single elements of Mn, Ni and Co are gradually exposed in the use process, and the requirements of people on the performance of the lithium battery can not be met. With ternary material LiNi1-x-yCoxMnyO2The defect of the single-element anode material is overcome, and the lithium battery anode material becomes a main force of the lithium battery anode material.
The traditional NCM ternary materials, including 523, 622, 811 and the like have certain advantages in energy density and comprehensive electrical property, particularly 811, and the gram capacity of the traditional NCM ternary materials can reach 195 mAh/g. However, the thermal stability of the high-nickel ternary material is poor, and the product with high requirements on the safety performance of the battery cannot meet the safety requirements of the battery. In addition, the Ni content is too high, so that part of Ni can occupy the 3a position of Li, and the phenomenon of ion mixing and discharging is caused, thereby leading to Li in the charging and discharging process+Cannot be re-embedded, resulting in severe capacity fading. However, the three metal elements of Ni, Co and Mn have synergistic effect, and can exert the advantages of the three metal oxides to the maximum extent. Therefore, it is difficult and important to adjust the ratio of the three metal materials to achieve the best safety performance and energy density.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a polyanion-doped manganese-rich ternary cathode material which has stable electrical property, higher energy density and outstanding safety performance. The invention also aims to provide a preparation method of the polyanion-doped manganese-rich ternary cathode material, which is simple and easy to operate, can provide a stable crystal structure material and obtain the modified manganese-rich ternary cathode material doped with a metal ion phase and a polyanion surface gradient.
The purpose of the invention is realized by the following technical scheme: a polyanion-doped manganese-rich ternary cathode material is characterized in that the chemical formula of the polyanion-doped manganese-rich ternary cathode material is as follows: (LiNi)2Co2Mn5)1-bMgbO2-x(BO3) x; wherein b and x are mole fractions, b is more than or equal to 0 and less than or equal to 0.01, and x is more than or equal to 0.1 and less than or equal to 0.2.
The polyanion-doped manganese-rich ternary cathode material provided by the invention has the advantages of good dispersibility, uniform granularity, stable electrical property, high energy density and outstanding safety performance.
Preferably, 0. ltoreq. b.ltoreq.0.005, 0.1. ltoreq. x.ltoreq.0.2.
A preparation method of a polyanion-doped manganese-rich ternary cathode material comprises the following steps:
(1): mixing carbonates of Mn, Ni and Co with the molar ratio of 5:3:2 with NaOH solution with equal concentration, adjusting the pH to 10-12, standing for 2-4h, performing suction filtration to obtain a precipitate, and cleaning for later use;
(2): adding Mg sulfate in proportion, mixing with NaOH solution with equal concentration, adjusting pH to 10-12, standing for 2-4h, suction filtering to obtain precipitate, and cleaning for use;
(3): adding Li to the product obtained in the step (2)3BO3Dissolving the solution and deionized water, reacting, and drying;
(4): adding Li to the product obtained in the step (3)2CO3Mixing and reacting the mixture in the absolute ethyl alcohol solution, and drying the mixture;
(5): sintering in an oxygen atmosphere to obtain (LiNi)2Co2Mn5)1-bMgbO2-x(BO3)x， 0≤b≤0.005，0.1≤x≤0.2。
The invention firstly prepares the manganese-rich ternary material by a coprecipitation method, and then dopes Mg into a precursor2+And BO3 3-. First, Mg2+The doping of the ternary material has a certain stabilizing effect on the structure of the ternary material, reduces the side reaction of the ternary material and the organic electrolyte, reduces the impedance of the battery in the charging and discharging processes, and ensures that the battery has more stable cycle performance; second, BO3 3-The material belongs to polyanion, has larger gaps for other metal ions to occupy, has crystal structure stability, adopts a doping mode to replace partial oxygen atoms in the ternary material, and can inhibit oxygen precipitation of the material in the first charging process and improve the first charge-discharge efficiency of the material due to the stronger covalent bond structure; meanwhile, the structure of the ternary material is also stabilized by the higher bond energy of the ternary material.
Further, BO is contained in the mixed solution obtained in the step (3)3 3-The concentration is 0.1-0.2 mol/L.
Inventive regulating BO3 3-The concentration is 0.1-0.2mol/L, so that the finally obtained manganese-rich ternary material has stable electrical property, higher energy density and outstanding safety performance.
Further, in the step (4), the obtained product is reacted with Li2CO3Mixing according to a molar ratio of 1: 1.05.
The invention adjusts the obtained substance in the step (4) and Li2CO3The molar ratio is 1:1.05, so that the phenomenon that Li + cannot be re-embedded in the charging and discharging process due to the phenomenon of ion mixing and discharging after part of Ni occupies the position 3a of Li is effectively avoided, and the capacity attenuation condition is effectively avoided.
Further, in the step (5), the mixture is sintered for 5-8h at the temperature of 400-500 ℃ and then heated to the temperature of 800-1000 ℃ for 16-20 h.
According to the invention, through two-step sintering, the internal structure of the material is changed stably, and the crystal phase structure is more stable.
Further, the temperature rising rate of the step (5) from room temperature to 400-500 ℃ is 2-5 ℃/min.
Further, the temperature rise rate of 400-500 ℃ to 800-1000 ℃ in the step (5) is 2-5 ℃/min.
Further, the cleaning process in the step (1) and the step (2) is to clean 1 to 3 times by using deionized water and clean 1 to 3 times by using absolute ethyl alcohol.
Further, the drying process in the step (3) and the step (4) is natural airing at room temperature or baking at 40-50 ℃ for 1-5 h.
Compared with the prior art, the invention has the advantages that: the polyanion-doped manganese-rich ternary cathode material provided by the invention has the advantages of good dispersibility, uniform granularity, stable electrical property, high energy density and outstanding safety performance;
the preparation method obtains the modified manganese-rich ternary material with stable electrical property, higher energy density and outstanding safety performance in a polyanion gradient doping mode, and is simple and easy to operate and suitable for large-scale production.
Drawings
FIG. 1 is a SEM photograph of the material obtained in example 1;
FIG. 2 photograph of HAADF-STEM of the material obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of a polyanion-doped manganese-rich ternary cathode material comprises the following steps. (1) preparing carbonate of Mn, Ni and Co (5: 3: 2) into a mixed solution with the total concentration of 2.5mol/L according to the stoichiometric ratio, mixing the mixed solution with an NaOH solution with equal concentration, keeping the pH of the mixed solution at 11, standing for 4h, carrying out precipitation reaction, carrying out suction filtration after standing to obtain a precipitate, washing with deionized water for 3 times, and washing with absolute ethyl alcohol for 2 times for later use.
(2) Adding sulfate doped with Mg into the precursor obtained in the step (1), wherein the molar ratio of the added Mg to (Ni + Mn + Co) in the precursor obtained in the step (1) is 0.0015:0.9985, adding NaOH solution with the concentration of 2.5mol/L, mixing, keeping the pH of the mixed solution at 11, standing for 4 hours, carrying out precipitation reaction, carrying out suction filtration after standing to obtain a precipitate, washing with deionized water for 3 times, and washing with absolute ethyl alcohol for 2 times to obtain the Mg-doped precursor.
(3) Mixing the precursor obtained in the step (2) with 0.13mol of Li3BO3Separately dissolved and mixed in deionized water, and then dried.
(4) Drying the product obtained in the step (3) and Li2CO3Uniformly mixing the components in the molar ratio of 1:1.05 in absolute ethyl alcohol and drying.
(5) Placing the mixture obtained in the step (4) in a muffle furnace, sintering in an oxygen atmosphere, raising the temperature to 400 ℃ at a heating rate of 2 ℃/min, preserving the heat for 8 hours, raising the temperature to 800 ℃ at the same heating rate, preserving the heat for 20 hours, and finally obtaining (LiNi)2Co2Mn5)0.9985Mg0.0015O1.87(BO3)0.13。
Example 2
A preparation method of a polyanion-doped manganese-rich ternary cathode material comprises the following steps.
(1) Preparing carbonate of Mn, Ni and Co (5: 3: 2) into mixed solution with the total concentration of 2.5mol/L according to the stoichiometric ratio, mixing the mixed solution with NaOH solution with equal concentration, keeping the mixed solution at the pH value of 11, standing for 4 hours, and carrying out precipitation reaction. Standing, performing suction filtration to obtain precipitate, washing with deionized water for 3 times, and washing with anhydrous ethanol for 2 times. It should be noted that the solvent of the solution mentioned in the present invention is deionized water without specific description.
(2) Adding sulfate doped with Mg into the precursor obtained in the step (1), wherein the molar ratio of the added Mg to (Ni + Mn + Co) in the precursor obtained in the step (1) is 0.0023:0.9977, adding NaOH solution with the concentration of 2.5mol/L, mixing, keeping the pH value of the mixed solution at 11, standing for 4h, and carrying out precipitation reaction. Standing, performing suction filtration to obtain a precipitate, washing with deionized water for 3 times, and then washing with absolute ethanol for 2 times to obtain a Mg-doped precursor.
(3) And (3) mixing the precursor obtained in the step (2) with 0.16mol of Li3BO3Separately dissolved and mixed in deionized water, and then dried.
(4) Drying the product obtained in the step (3) and Li2CO3Uniformly mixing the components in the molar ratio of 1:1.05 in absolute ethyl alcohol and drying.
(5) And (3) placing the mixture obtained in the step (4) in a muffle furnace, sintering in an oxygen atmosphere, raising the temperature to 400 ℃ at a heating rate of 2 ℃/min, preserving the heat for 8 hours, raising the temperature to 800 ℃ at the same heating rate, preserving the heat for 20 hours, and finally obtaining (LiNi)2Co2Mn5)0.9977Mg0.0023O1.84(BO3)0.16。
Example 3
A preparation method of a polyanion-doped manganese-rich ternary cathode material comprises the following steps.
(1) Preparing carbonate of Mn, Ni and Co (5: 3: 2) into mixed solution with the total concentration of 2.5mol/L according to the stoichiometric ratio, mixing the mixed solution with NaOH solution with equal concentration, keeping the mixed solution at the pH value of 11, standing for 4 hours, and carrying out precipitation reaction. Standing, performing suction filtration to obtain precipitate, washing with deionized water for 3 times, and washing with anhydrous ethanol for 2 times. It should be noted that the solvent of the solution mentioned in the present invention is deionized water without specific description.
(2) Adding sulfate doped with Mg into the precursor obtained in the step (1), wherein the molar ratio of the added Mg to (Ni + Mn + Co) in the precursor obtained in the step (1) is 0.0017:0.9985, adding NaOH solution with the concentration of 2.5mol/L, mixing, keeping the pH of the mixed solution at 11, standing for 4 hours, and carrying out precipitation reaction. Standing, performing suction filtration to obtain a precipitate, washing with deionized water for 3 times, and then washing with absolute ethanol for 2 times to obtain a Mg-doped precursor.
(3) And (3) mixing the precursor obtained in the step (2) with 0.15mol of Li3BO3Separately dissolved and mixed in deionized water, and then dried.
(4) Drying the product obtained in the step (3) and Li2CO3Uniformly mixing the components in the molar ratio of 1:1.05 in absolute ethyl alcohol and drying.
(5) And (3) placing the mixture obtained in the step (4) in a muffle furnace, sintering in an oxygen atmosphere, raising the temperature to 500 ℃ at a heating rate of 3 ℃/min, preserving the heat for 5 hours, raising the temperature to 1000 ℃ at the same heating rate, preserving the heat for 16 hours, and finally obtaining (LiNi)2Co2Mn5)0.9983Mg0.0017O1.85(BO3)0.15。
The polyanion-doped manganese-rich ternary cathode material prepared in the above example was subjected to performance testing, and the test results are shown in fig. a, which is an SEM photograph of the material obtained in example 1, fig. b, which is an HAADF-STEM photograph of the material obtained in example 1, and table 1, which is an index of performance of the material obtained in example 1.
TABLE 1
The test data shows that the polyanion-doped manganese-rich ternary cathode material prepared by the invention has the advantages of good dispersibility, uniform granularity, high capacity density, high electrical property, temperature and strong reliability. The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A polyanion-doped manganese-rich ternary cathode material is characterized in that the chemical formula of the polyanion-doped manganese-rich ternary cathode material is as follows: (LiNi)2Co2Mn5)1-bMgbO2-x(BO3) x; wherein b and x are mole fractions, b is more than or equal to 0 and less than or equal to 0.01, and x is more than or equal to 0.1 and less than or equal to 0.2.
2. The polyanion-doped manganese-rich ternary positive electrode material of claim 1, wherein b is 0. ltoreq. b.ltoreq.0.005, and x is 0.1. ltoreq. x.ltoreq.0.2.
3. The preparation method of the polyanion-doped manganese-rich ternary cathode material according to any one of claims 1 to 2, comprising the following steps:
(1): mixing carbonates of Mn, Ni and Co with the molar ratio of 5:3:2 with NaOH solution with equal concentration, adjusting the pH to 10-12, standing for 2-4h, performing suction filtration to obtain a precipitate, and cleaning for later use;
(2): adding Mg sulfate in proportion, mixing with NaOH solution with equal concentration, adjusting pH to 10-12, standing for 2-4h, suction filtering to obtain precipitate, and cleaning for use;
(3): adding Li to the product obtained in the step (2)3BO3And deionized water, and drying after dissolution reaction;
(4): adding Li to the product obtained in the step (3)2CO3Mixing and reacting the mixture in the absolute ethyl alcohol solution, and drying the mixture;
(5): sintering in an oxygen atmosphere to obtain (LiNi)2Co2Mn5)1-bMgbO2-x(BO3)x，0≤b≤0.01，0.1≤x≤0.2。
4. The method for preparing the polyanion-doped manganese-rich ternary cathode material according to claim 3, wherein BO is contained in the mixed solution obtained in the step (3)3 3-The concentration is 0.1-0.2 mol/L.
5. The method for preparing the polyanion-doped manganese-rich ternary cathode material according to claim 4, wherein in the step (4), the obtained product is mixed with Li2CO3Mixing according to a molar ratio of 1: 1.05.
6. The method as claimed in claim 5, wherein the step (5) comprises sintering at 400-500 ℃ for 5-8h, and then heating to 800-1000 ℃ for 16-20 h.
7. The method as claimed in claim 6, wherein the temperature increase rate of the step (5) from room temperature to 400-500 ℃ is 2-5 ℃/min.
8. The method as claimed in claim 7, wherein the temperature increase rate of the temperature increase from 400-500 ℃ to 800-1000 ℃ in the step (5) is 2-5 ℃/min.
9. The method for preparing the polyanion-doped manganese-rich ternary cathode material according to claim 8, wherein the washing process in the step (1) and the step (2) is washing with deionized water for 1-3 times, and then washing with absolute ethyl alcohol for 1-3 times.
10. The method for preparing the polyanion-doped manganese-rich ternary cathode material according to claim 9, wherein the drying process in the step (3) and the step (4) is natural airing at room temperature or baking at 40-50 ℃ for 1-5 h.
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