CN114394631A - Preparation method of ternary cathode material precursor - Google Patents
Preparation method of ternary cathode material precursor Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a preparation method of a ternary anode material precursor, which comprises the following steps of preparing a raw material metal salt solution, an alkali liquor and a complexing agent solution, adding the raw material metal salt solution, the alkali liquor and the complexing agent into a reaction kettle for coprecipitation reaction, and adjusting the pH value in the reaction process, wherein the preparation method comprises the following steps: the pH value is 11.9-12.5 until the nucleation is finished; after the nucleation is finished, reducing the pH value to 11.2-11.7, and suspending feeding until the average particle size of the particles grows to the target particle size; and (3) after the pH value is adjusted to 11.9-12.5, continuing feeding, re-nucleating for 5-18 h, then reducing the pH value to 11.2-11.7, continuing reacting until the average particle size of the particles grows to the target particle size, and stopping feeding to obtain the solution containing the precursor material. According to the invention, only the pH value is adjusted in the coprecipitation reaction process, other reaction conditions are not changed, and the tap density of the prepared precursor of the positive electrode material is more than 2.10g/cm3While the specific surface area is more than 18.5m2The shape is controllable, the particle size distribution is uniform, and the capacity and the charge-discharge performance of the lithium ion battery are greatly improved.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a preparation method of a precursor of a ternary anode material.
Background
The demand of lithium ion batteries in electric automobiles, electric bicycles and mobile phone batteries is increasing day by day, and lithium battery products are developing continuously towards the directions of high specific capacity, high energy density, high capacity retention rate and better safety performance. The performance of the positive electrode material in the lithium battery is a decisive factor of the battery performance, and the energy density, the cycle performance and the safety of the battery are closely related to the performance of the positive electrode material. The specific discharge capacity, the working platform voltage, the filling property of the powder material and the like are several key factors influencing the energy density. By increasing the density of the positive electrode material, the volumetric energy density of the lithium battery can be increased. The ternary cathode material has low cost, high capacity and environmental friendliness, and has a very wide market in the field of power batteries.
In the preparation process of the anode material, the preparation process of the precursor accounts for 60%, and the quality of the precursor directly influences the performance of the anode material. The common positive electrode material is prepared by mixing and calcining secondary spherical particles formed by agglomeration of fine grains of nickel-cobalt-manganese hydroxide and lithium hydroxide. At present, the production of precursor mainly adopts coprecipitation method, i.e. nickel salt, cobalt salt, manganese salt or aluminium salt is prepared into salt solution according to a certain proportion, nickel hydroxide cobalt manganese \ aluminium precipitate is formed under the condition of alkali liquor and complexing agent, and then the qualified product is obtained through the steps of centrifugal washing, slurrying, drying and the like. The tap density, size, morphology, particle size, impurity content and the like of the precursor of the anode material have direct influence on the technical index of the ternary battery material, and the quality and the physical and chemical properties of the precursor of the anode material determine the performance of the battery material to a great extent. Wherein, coprecipitation is a key stage for controlling the morphological structure and tap density of the precursor.
The anode material is required to have uniform particle size, high tap density, large specific surface area and stable structure, so that the power battery has high requirements on long endurance, high cycle characteristic, high safety, short charging time and the like. The higher the tap density is, the higher the capacity is, and the stronger the cruising ability is; the larger the specific surface area, the larger the charge-discharge time magnification, and the shorter the charge time. The specific surface area and tap density of the ternary cathode material precursor product are in a negative correlation relationship on theoretical properties. The specific surface area of the product is reduced in the case of preparing the high tap density ternary cathode material precursor, and the tap density of the product is reduced in the case of preparing the high specific surface area. The battery performance cannot simultaneously meet the requirements of high compaction density and high rate discharge performance. The specific surface area of the traditional high specific surface area product is 20-30m2The tap density is 1.3-1.7g/cm3The traditional high tap density product has tap density of 1.8-2.4g/cm3The specific surface area is 5-13m2(ii) in terms of/g. For example, the Chinese patent application with the publication number of CN107640792A discloses a high-density small-particle-size nickel-cobalt-manganese hydroxide and a preparation method thereof, the particle size of the obtained precursor particle d10 is more than or equal to 2 microns (mum), and d50 is 2.5-4Micron (mum), d90 is less than or equal to 6 microns (mum), and tap density is more than or equal to 1.4g/cm3The specific surface area is 5-20m2And/g, the shape is spherical or spheroidal. It is prepared through raising reaction temperature, pH value and stirring speed in the nucleation stage, controlling the stirring speed in the growth process,The reaction temperature, pH and flow rate enable the small crystal nuclei to grow slowly, so that the high-compactness small-particle-size nickel-cobalt-manganese hydroxide is obtained, but the specific surface area and the tap density are still small, particularly the tap density is only 1.4g/cm3Therefore, how to increase the specific surface area while ensuring that the tap density of the ternary cathode material precursor is increased, thereby ensuring the endurance time of the lithium ion battery and shortening the charging time is a technical problem to be solved at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a ternary cathode material precursor, wherein the ternary cathode material precursor prepared by the method has high tap density and large specific surface area.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a ternary cathode material precursor comprises the steps of preparing a raw material metal salt solution, an alkali liquor and a complexing agent solution, adding the raw material metal salt solution, the alkali liquor and the complexing agent into a reaction kettle, and introducing inert shielding gas for coprecipitation reaction, wherein in the coprecipitation reaction process, the feeding flow of the metal salt solution is controlled to be 200-800L/h, the stirring speed is 600-1100 r/min, the temperature of the reaction kettle is 40-70 ℃, the ammonia concentration is 2-5 g/L, and the pH value in the coprecipitation reaction process is adjusted by the following steps:
s1: the pH value is 11.9-12.5 until the nucleation is finished; the secondary particles of the product in the electron microscope picture are in a sphere-like shape, and then nucleation is completed;
s2: after the nucleation is finished, reducing the pH value to 11.2-11.7, and suspending feeding until the average particle size of the particles grows to the target particle size;
s3: and (3) after the pH value is adjusted to 11.9-12.5, continuing feeding, re-nucleating for 5-18 h, then reducing the pH value to 11.2-11.7, continuing reacting until the average particle size of the particles grows to a target particle size, stopping feeding to obtain a solution containing a precursor material, and then aging, washing, drying, screening and deironing to obtain the precursor of the anode material.
Since the pH is first increased to re-nucleate at S3, the particle size is reduced, the pH is again decreased, and the reaction is continued until the average particle size of the particles grows to the target particle size.
Further, the step S3 may be repeated until the tap density meets the design requirement.
Further, the total concentration of metal ions in the metal salt solution is 1-3 mol/L, and the metal salt solution is an aqueous solution containing nickel salt, cobalt salt or nickel salt, cobalt salt and manganese salt.
Further, the nickel salt, the cobalt salt and the manganese salt are at least one of sulfate, nitrate and halogen salt.
Further, the raw material also comprises an aluminum salt solution.
Further, the alkali liquor is a mixed solution of one or more of potassium hydroxide, lithium hydroxide and sodium hydroxide, and the concentration of the alkali liquor is 3-12 mol/L; the complexing agent solution is ammonia water, and the concentration of the complexing agent solution is 10-30%.
Furthermore, the average particle size of the particles is a particle size distribution D50 value, and the target particle size is 3-15 μm.
Further, the inert protective gas is nitrogen, helium or argon.
Further, the nucleation reaction time of the step S1 is 0-10 h.
The invention has the beneficial effects that: according to the invention, only the pH value is adjusted in the coprecipitation reaction process, other reaction conditions are not changed, and the tap density of the prepared precursor of the positive electrode material is more than 2.10g/cm3While the specific surface area is more than 18.6m2The shape is controllable, the particle size distribution is uniform, and the capacity and the charge-discharge performance of the lithium ion battery are greatly improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH of the base solution to 11.90, then adding an ammonia water solution to adjust the ammonia value of the base solution to 3g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel, cobalt and manganese is 1: 1) at the flow rate of 300L/h, introducing 32% of liquid caustic soda solution and 16% of ammonia water solution, continuously introducing nitrogen into a reaction container, keeping the pH value of the reaction kettle at 11.90 and 3g/L of ammonia value 3 hours before reaction, and reducing the pH value of the reaction kettle to 11.40 after 3 hours until the granularity D50 of a product reaches 4 mu m; then keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the pH value of the reaction kettle to 11.90, then restarting the feeding and nucleating for 10 hours, and then reducing the pH value to 11.40 without changing other parameters to continue the reaction until the product granularity D50 reaches 4 mu m. The product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
Example 2:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH of the base solution to 12.05, then adding an ammonia water solution to prepare the base solution to be 3g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. And simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel to cobalt to manganese is 57: 13: 20), 32% of liquid caustic soda solution and 16% of ammonia water solution at the flow rate of 300L/h, keeping the pH value of the reaction kettle at 12.05 and the ammonia value at 3.5g/L within 1.5 hours before reaction, and reducing the pH value of the reaction kettle to 11.60 after 3 hours until the particle size D50 of the product reaches 4 mu m. Then keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the pH value of the reaction kettle to 12.05, then restarting the feeding and nucleating for 10 hours, and reducing the pH value to 11.60 without changing other parameters to continue the reaction until the product granularity D50 reaches 4 mu m. And repeating the third step, keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of the mixed salt, the ammonia and the alkali, restarting the feeding and the nucleation for 10 hours after the pH value of the reaction kettle is increased to 12.05, and continuously reacting until the particle size D50 of the product reaches 4um after the pH value of other parameters is unchanged and is reduced to 11.60. The product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
Example 3:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH of the base solution to 12.3, then adding an ammonia water solution to adjust the ammonia value of the base solution to 5g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1100r/min to prepare the base solution for the coprecipitation reaction. Simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel, cobalt and manganese is 84: 11: 5) at the flow rate of 300L/h, introducing 32% of liquid caustic soda solution and 16% of ammonia water solution, continuously introducing nitrogen into a reaction container, keeping the pH value of the reaction kettle at 12.3 and 4.5g/L in 1 hour before the reaction, and reducing the pH value of the reaction kettle to 11.20 after 3 hours until the granularity D50 of the product reaches 4 mu m; then keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the pH value of the reaction kettle to 12.2, then restarting the feeding and nucleating for 10 hours, and then reducing the pH value to 11.20 without changing other parameters to continue the reaction until the product granularity D50 reaches 4 mu m. The product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
Comparative example 1:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH of the base solution to 11.90, then adding an ammonia water solution to adjust the ammonia value of the base solution to 3g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel, cobalt and manganese is 1: 1) at the flow rate of 300L/h, introducing 32% of liquid caustic soda solution and 16% of ammonia water solution, continuously introducing nitrogen into a reaction container, keeping the pH value of the reaction kettle at 11.90 and 3g/L of ammonia value 3 hours before reaction, and reducing the pH value of the reaction kettle to 11.60 after 3 hours until the granularity D50 of a product reaches 4 mu m; the product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
Comparative example 2:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH value of the base solution to 12.7, then adding an ammonia water solution to adjust the ammonia value of the base solution to 3g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel, cobalt and manganese is 1: 1) at the flow rate of 300L/h, introducing 32% of liquid caustic soda solution and 16% of ammonia water solution, continuously introducing nitrogen into a reaction container, keeping the pH value of the reaction kettle at 12.7 and the ammonia value at 3 g/L3 hours before the reaction, and reducing the pH value of the reaction kettle to 11.9 after 3 hours until the granularity D50 of the product reaches 4 mu m; then keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the pH value of the reaction kettle to 12.7, then restarting the feeding and nucleating for 10 hours, and then continuously reacting until the particle size D50 of the product reaches 4 mu m after the pH value of other parameters is unchanged and is reduced to 11.9. The product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
Comparative example 3:
adding deionized water into a reaction kettle, heating to 60 ℃, then adding the prepared liquid alkali solution to adjust the pH of the base solution to 11.80, then adding an ammonia water solution to adjust the ammonia value of the base solution to 3g/L, and uniformly mixing stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Simultaneously adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel, cobalt and manganese is 1: 1) at the flow rate of 300L/h, introducing 32% of liquid caustic soda solution and 16% of ammonia water solution, continuously introducing nitrogen into a reaction container, keeping the pH value of the reaction kettle at 11.80 and 3g/L of ammonia value 3 hours before reaction, and reducing the pH value of the reaction kettle to 11.60 after 3 hours until the granularity D50 of a product reaches 4 mu m; then keeping the temperature, the ammonia value and the rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the pH value of the reaction kettle to 11.80, then restarting the feeding and nucleating for 10 hours, and then reducing the pH value to 11.60 without changing other parameters to continue the reaction until the product granularity D50 reaches 4 mu m. The product is subjected to centrifugation, drying, material mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of opening the kettle by using the clear mother liquor discharged by the thickener in the previous round of reaction.
The precursor products obtained in the examples and comparative examples were tested for D50, tap density, and specific surface area, and the results are shown in table 1.
TABLE 1
| D50/μm | Tap density g/cm3 | Specific surface area m2/g | Morphology of | |
| Example 1 | 4 | 2.23 | 20.15 | Spherical shape |
| Example 2 | 4 | 2.37 | 18.6 | Spherical shape |
| Example 3 | 4 | 2.1 | 22.0 | Spherical shape |
| Comparative example 1 | 4 | 1.65 | 15.6 | Spherical shape |
| Comparative example 2 | 4 | 1.41 | 19.4 | Spherical shape |
| Comparative example 3 | 4 | 1.62 | 14.9 | Spherical shape |
Claims (9)
1. A preparation method of a ternary anode material precursor comprises the steps of preparing a raw material metal salt solution, an alkali liquor and a complexing agent solution, adding the raw material metal salt solution, the alkali liquor and the complexing agent into a reaction kettle, and introducing inert shielding gas for coprecipitation reaction, wherein in the coprecipitation reaction process, the feeding flow of the metal salt solution is controlled to be 200-800L/h, the stirring speed is 600-1100 r/min, the temperature of the reaction kettle is 40-70 ℃, and the ammonia concentration is 2-5 g/L, and the preparation method is characterized in that the pH value in the coprecipitation reaction process comprises the following steps:
s1: the pH value is 11.9-12.5 until the nucleation is finished;
s2: after the nucleation is finished, reducing the pH value to 11.2-11.7, and suspending feeding until the average particle size of the particles grows to the target particle size;
s3: and (3) after the pH value is adjusted to 11.9-12.5, continuing feeding, re-nucleating for 5-18 h, then reducing the pH value to 11.2-11.7, continuing reacting until the average particle size of the particles grows to a target particle size, stopping feeding to obtain a solution containing a precursor material, and then aging, washing, drying, screening and deironing to obtain the precursor of the anode material.
2. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the step S3 may be repeated until the tap density meets the design requirement.
3. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the total concentration of metal ions in the metal salt solution is 1-3 mol/L, and the metal salt solution is an aqueous solution containing nickel salt, cobalt salt or nickel salt, cobalt salt and manganese salt.
4. The method for preparing a precursor of a ternary positive electrode material according to claim 3, wherein: the nickel salt, the cobalt salt and the manganese salt are at least one of sulfate, nitrate and halogen salt.
5. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the raw material also comprises an aluminum salt solution.
6. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the alkali liquor is a mixed solution of one or more of potassium hydroxide, lithium hydroxide and sodium hydroxide, and the concentration of the alkali liquor is 3-12 mol/L; the complexing agent solution is ammonia water, and the concentration of the complexing agent solution is 10-30%.
7. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the average particle size of the particles is a particle size distribution D50 value, and the target particle size is 3-15 mu m.
8. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the inert protective gas is nitrogen, helium or argon.
9. The method for preparing a precursor of a ternary positive electrode material according to claim 1, wherein: the nucleation reaction time of the step S1 is 0-10 h.
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| CN115092974A (en) * | 2022-06-20 | 2022-09-23 | 天津巴莫科技有限责任公司 | Doped ternary precursor and preparation method thereof, ternary cathode material and lithium ion battery |
| CN115490273A (en) * | 2022-08-17 | 2022-12-20 | 四川顺应动力电池材料有限公司 | Method for continuously preparing large-ratio table ternary precursor and precursor prepared by method |
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| CN115092974A (en) * | 2022-06-20 | 2022-09-23 | 天津巴莫科技有限责任公司 | Doped ternary precursor and preparation method thereof, ternary cathode material and lithium ion battery |
| CN115092974B (en) * | 2022-06-20 | 2024-03-19 | 天津巴莫科技有限责任公司 | Doped ternary precursor, preparation method thereof, ternary positive electrode material and lithium ion battery |
| CN115092976A (en) * | 2022-07-08 | 2022-09-23 | 金驰能源材料有限公司 | Preparation method of precursor with high specific surface area and high tap density |
| CN115092976B (en) * | 2022-07-08 | 2023-10-24 | 金驰能源材料有限公司 | Preparation method of precursor with high specific surface area and high tap density |
| CN115490273A (en) * | 2022-08-17 | 2022-12-20 | 四川顺应动力电池材料有限公司 | Method for continuously preparing large-ratio table ternary precursor and precursor prepared by method |
| CN115490273B (en) * | 2022-08-17 | 2023-09-22 | 四川顺应动力电池材料有限公司 | Method for continuously preparing ternary precursor with large specific surface and prepared precursor |
| WO2024040908A1 (en) * | 2022-08-25 | 2024-02-29 | 广东邦普循环科技有限公司 | Porous spherical ternary precursor and preparation method therefor, ternary positive electrode material, positive electrode plate and battery |
| WO2024055513A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Positive electrode material precursor, positive electrode material, method for preparing same, and use thereof |
| CN115893515A (en) * | 2022-10-14 | 2023-04-04 | 宜宾光原锂电材料有限公司 | Novel positive electrode material precursor and preparation method thereof |
| CN115893515B (en) * | 2022-10-14 | 2024-03-26 | 宜宾光原锂电材料有限公司 | Preparation method of nickel-cobalt-containing hydroxide positive electrode material precursor |
| CN116462243A (en) * | 2023-06-19 | 2023-07-21 | 宜宾光原锂电材料有限公司 | Battery, ternary positive electrode material thereof, precursor thereof and preparation method |
| CN116462243B (en) * | 2023-06-19 | 2023-09-26 | 宜宾光原锂电材料有限公司 | Battery, ternary positive electrode material thereof, precursor thereof and preparation method |
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