CN114394631B - Preparation method of ternary positive electrode material precursor - Google Patents
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Abstract
The invention discloses a preparation method of ternary positive electrode material precursors, which comprises the steps of preparing a raw material metal salt solution, an alkali solution and a complexing agent solution, adding the raw material metal salt solution, the alkali solution 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 completed; after nucleation is completed, the pH value is reduced to 11.2-11.7, and feeding is stopped after the average particle size of the particles grows to the target particle size; and (3) continuously feeding after the pH value is adjusted to 11.9-12.5, re-nucleating for 5-18 h, then reducing the pH value to 11.2-11.7, continuously 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. The pH value is only regulated in the coprecipitation reaction process, other reaction conditions are not changed, and the tap density of the prepared positive electrode material precursor is more than 2.10g/cm 3 At the same time the specific surface area is more than 18.5m 2 And/g, the morphology is controllable, the granularity distribution is uniform, and the capacity and the charge and 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 ternary anode material precursor.
Background
The demand of lithium ion batteries in electric automobiles, electric bicycles and mobile phone batteries is increasing, and lithium battery products are also developing towards high specific capacity, high energy density, high capacity retention rate and better safety performance. The performance of the positive electrode material in a lithium battery is a decisive factor for the performance of the battery, and the energy density, cycle performance and safety of the battery are relevant. Wherein specific discharge capacity, working platform voltage, filling property of powder material and the like are several key factors influencing energy density. By increasing the density of the positive electrode material, the volumetric energy density of the lithium battery can be increased. The ternary positive electrode 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 positive electrode material, the preparation process of the precursor accounts for 60 percent, and the advantages and disadvantages of the precursor directly influence the performance of the positive electrode material. The common positive electrode material is formed by mixing secondary spherical particles formed by agglomeration of fine crystal grains of nickel cobalt manganese hydroxide with lithium hydroxide and calcining. At present, a coprecipitation method is mainly adopted for producing a precursor, namely nickel salt, cobalt salt, manganese salt or aluminum salt is prepared into a salt solution according to a certain proportion, cobalt nickel manganese/aluminum hydroxide precipitate is formed under the existence of alkali liquor and complexing agent, and qualified products are obtained through the steps of centrifugal washing, slurrying, drying and the like. The tap density, the size, the morphology, the particle size, the impurity content and the like of the precursor of the positive electrode material directly influence the technical indexes of the ternary battery material, and the quality and the physical and chemical properties of the precursor of the positive electrode material determine the performance of the battery material to a great extent. Wherein, coprecipitation is a key stage for controlling the morphology structure and tap density of the precursor.
The positive electrode material requires uniform particle size, high tap density, large specific surface area and stable structure, and can ensure the powerThe battery has high requirements for long endurance, high cycle characteristics, high safety, short charging time, and the like. Because the higher the tap density, the higher the capacity, the stronger the cruising ability; the larger the specific surface area is, the larger the charge-discharge time multiplying power is, and the shorter the charge time is. The specific surface area and tap density of the ternary positive electrode material precursor product show negative correlation in theoretical properties. The specific surface area of the product is reduced when the high-tap ternary cathode material precursor is prepared, and the tap density of the product is reduced when the high-specific surface area is prepared. The battery performance cannot meet the requirements of high compacted density and high-rate discharge performance at the same time. The specific surface area of the traditional high specific surface area product is 20-30m 2 Per gram, tap density of 1.3-1.7g/cm 3 The vibration density of the traditional high tap density product is 1.8-2.4g/cm 3 Specific surface area of 5-13m 2 And/g. The Chinese patent application with publication No. CN107640792A discloses a high-density nickel-cobalt-manganese hydroxide with small particle size and a preparation method thereof, and the particle size d10 of the obtained precursor particles is more than or equal to 2 micrometers (mu m), d50=2.5 -4 Micrometer (mum), d90 is less than or equal to 6 micrometers (mum), and tap density is more than or equal to 1.4g/cm 3 Specific surface area of 5-20m 2 And/g, the shape is spherical or spheroid. The method is characterized in that the reaction temperature, the pH value and the stirring rate are increased in the nucleation stage, and the stirring rotation speed, the reaction temperature, the pH value and the flow rate are controlled in the growth process, so that small crystal nuclei slowly grow, and the high-compactness small-particle-size nickel cobalt manganese hydroxide is obtained, but the specific surface area and the tap density are still small, and especially the tap density is only 1.4g/cm 3 Therefore, how to ensure the improvement of the tap density of the ternary cathode material precursor and the improvement of the specific surface area, thereby ensuring the endurance time of the lithium ion battery and shortening the charging time is a technical problem to be solved urgently at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a ternary positive electrode material precursor, and the ternary positive electrode material precursor prepared by the method has high tap density and large specific surface area.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of ternary positive electrode material precursor comprises the steps of preparing a raw material metal salt solution, an alkali solution and a complexing agent solution, adding the raw material metal salt solution, the alkali solution and the complexing agent into a reaction kettle, and introducing inert protective gas to perform 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 rotating 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 completed; the secondary particles of the product in the electron microscope picture are in a sphere-like shape, namely, the nucleation is completed;
s2: after nucleation is completed, the pH value is reduced to 11.2-11.7, and feeding is stopped after the average particle size of the particles grows to the target particle size;
s3: and (3) continuously feeding after the pH value is adjusted to 11.9-12.5, re-nucleating for 5-18 hours, then reducing the pH value to 11.2-11.7, continuously reacting until the average particle size of the particles grows to the target particle size, stopping feeding to obtain a solution containing a precursor material, and then aging, washing, drying, screening and removing iron to obtain a precursor of the positive electrode material.
Since the pH is first raised to re-nucleation at S3, the particle size is reduced, the pH is lowered again, 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 a water solution containing nickel salt, cobalt salt or nickel salt, cobalt salt and manganese salt.
Further, the nickel salt, cobalt salt and manganese salt are at least one of sulfate, nitrate and halogen salt.
Further, the raw materials also comprise aluminum salt solution.
Further, the alkali liquor is one or a mixed solution of more than one 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%.
Further, the average particle diameter of the particles is a D50 value of particle size distribution, and the target particle diameter is 3-15 mu m.
Further, the inert shielding gas is nitrogen, helium or argon.
Furthermore, the nucleation reaction time in the step S1 is 0-10 h.
The beneficial effects of the invention are as follows: the pH value is only regulated in the coprecipitation reaction process, other reaction conditions are not changed, and the tap density of the prepared positive electrode material precursor is more than 2.10g/cm 3 At the same time the specific surface area is more than 18.6m 2 And/g, the morphology is controllable, the granularity distribution is uniform, and the capacity and the charge and discharge performance of the lithium ion battery are greatly improved.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared liquid-alkali solution to adjust the pH of the base solution to 11.90, adding ammonia water solution to adjust the liquid ammonia value of the base solution to 3g/L, and uniformly mixing the stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Meanwhile, adding 120g/L of nickel-cobalt-manganese mixed salt solution (molar ratio of nickel to cobalt to manganese is 1:1) at a flow rate of 300L/h, introducing 32% of aqueous alkali solution and 16% of ammonia solution, continuously introducing nitrogen into a reaction container, keeping the ph value of the reaction container at 11.90 and the ammonia value of 3g/L for 3 hours before the reaction, and reducing the ph value of the reaction container to 11.40 until the granularity D50 of the product reaches 4 mu m after 3 hours; then maintaining the temperature, ammonia value and rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the temperature ph of the reaction kettle to 11.90, restarting feeding and nucleating for 10 hours, and continuously reacting until the granularity D50 of the product reaches 4 mu m. And the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
Example 2:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared aqueous alkali to adjust the pH of the base solution to 12.05, adding the aqueous ammonia solution to prepare the base solution to 3g/L, and uniformly mixing the base solution with stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Meanwhile, 120g/L of nickel-cobalt-manganese mixed salt solution (molar ratio of nickel to cobalt to manganese is 57:13:20), 32% aqueous alkali solution and 16% aqueous ammonia solution are added at a flow rate of 300L/h, the ph value of a reaction kettle is kept at 12.05 and the ammonia value is 3.5g/L for 1.5 hours before the reaction, and the ph value of the reaction kettle is reduced to 11.60 after 3 hours until the granularity D50 of the product reaches 4 mu m. Then maintaining the temperature, ammonia value and rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the temperature ph of the reaction kettle to 12.05, restarting feeding and nucleating for 10 hours, and continuously reacting until the granularity D50 of the product reaches 4 mu m without changing other parameters to reduce the ph to 11.60. And step three, 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 temperature ph of the reaction kettle to 12.05, restarting feeding and nucleating for 10 hours, and keeping the other parameters unchanged, reducing the ph to 11.60, and continuing the reaction until the granularity D50 of the product reaches 4um. And the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
Example 3:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared liquid-alkali solution to adjust the pH of the base solution to 12.3, adding ammonia water solution to adjust the liquid ammonia value of the base solution to 5g/L, and uniformly mixing the stirring blades in the reaction kettle at the rotating speed of 1100r/min to prepare the base solution for the coprecipitation reaction. Meanwhile, adding 120g/L of nickel-cobalt-manganese mixed salt solution (the molar ratio of nickel to cobalt to manganese is 84:11:5) at the flow rate of 300L/h, introducing 32% of aqueous alkali solution and 16% of ammonia solution, continuously introducing nitrogen into a reaction container, keeping the ph value of the reaction kettle at 12.3 and the ammonia value at 4.5g/L for 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 maintaining the temperature, ammonia value and rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the temperature ph of the reaction kettle to 12.2, restarting feeding and nucleating for 10 hours, and continuously reacting until the granularity D50 of the product reaches 4 mu m without changing other parameters to reduce the ph to 11.20. And the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
Comparative example 1:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared liquid-alkali solution to adjust the pH of the base solution to 11.90, adding ammonia water solution to adjust the liquid ammonia value of the base solution to 3g/L, and uniformly mixing the stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Meanwhile, adding 120g/L of nickel-cobalt-manganese mixed salt solution (molar ratio of nickel to cobalt to manganese is 1:1) at a flow rate of 300L/h, introducing 32% of aqueous alkali solution and 16% of ammonia solution, continuously introducing nitrogen into a reaction container, keeping the ph value of the reaction container at 11.90 and the ammonia value of 3g/L for 3 hours before the reaction, and reducing the ph value of the reaction container to 11.60 until the granularity D50 of the product reaches 4 mu m after 3 hours; and the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
Comparative example 2:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared liquid-alkali solution to adjust the pH value of the base solution to 12.7, adding ammonia water solution to adjust the pH 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. Meanwhile, adding 120g/L of nickel-cobalt-manganese mixed salt solution (molar ratio of nickel to cobalt to manganese is 1:1) at a flow rate of 300L/h, introducing 32% of aqueous alkali solution and 16% of ammonia solution, continuously introducing nitrogen into a reaction container, keeping the ph value of the reaction container at 12.7 and the ammonia value of 3g/L for 3 hours before the reaction, and reducing the ph value of the reaction container to 11.9 until the granularity D50 of the product reaches 4 mu m; then maintaining the temperature, ammonia value and rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the temperature ph of the reaction kettle to 12.7, restarting feeding and nucleating for 10 hours, and continuously reacting until the granularity D50 of the product reaches 4 mu m without changing other parameters to reduce the ph to 11.9. And the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
Comparative example 3:
adding deionized water into a reaction kettle, heating to 60 ℃, adding the prepared liquid-alkali solution to adjust the pH of the base solution to 11.80, adding ammonia water solution to adjust the liquid ammonia value of the base solution to 3g/L, and uniformly mixing the stirring blades in the reaction kettle at the rotating speed of 1000r/min to prepare the base solution for the coprecipitation reaction. Meanwhile, adding 120g/L of nickel-cobalt-manganese mixed salt solution (molar ratio of nickel to cobalt to manganese is 1:1) at a flow rate of 300L/h, introducing 32% of aqueous alkali solution and 16% of ammonia solution, continuously introducing nitrogen into a reaction container, keeping the ph value of the reaction container at 11.80 and the ammonia value at 3g/L for 3 hours before the reaction, and reducing the ph value of the reaction container to 11.60 until the granularity D50 of the product reaches 4 mu m after 3 hours; then maintaining the temperature, ammonia value and rotating speed of the reaction kettle unchanged, suspending the introduction of mixed salt, ammonia and alkali, raising the temperature ph of the reaction kettle to 11.80, restarting feeding and nucleating for 10 hours, and continuously reacting until the granularity D50 of the product reaches 4 mu m. And the product is subjected to centrifugation, drying, mixing, screening, iron removal and packaging to obtain the ternary material precursor product. And opening the kettle along the next round of kettle opening, and discharging clear mother liquor by a thickener in the previous round of reaction process.
The precursor products obtained in examples and comparative examples were examined for D50, tap density and specific surface area, and the results are shown in table 1.
TABLE 1
| D50/μm | Tap density g/cm 3 | Specific surface area m 2 /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 (8)
1. The preparation method of ternary positive electrode material precursor comprises the steps of preparing a raw material metal salt solution, an alkali solution and a complexing agent solution, adding the raw material metal salt solution, the alkali solution and the complexing agent into a reaction kettle, and introducing inert protective gas to perform 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 rotating 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 preparation method is characterized in that the pH value adjustment in the coprecipitation reaction process comprises the following steps:
s1: the pH value is 11.9-12.5 until the nucleation is completed;
s2: after nucleation is completed, the pH value is reduced to 11.2-11.7, and feeding is stopped after the average particle size of the particles grows to the target particle size;
s3: and (3) continuously feeding after the pH value is adjusted to 11.9-12.5, re-nucleating for 5-18 hours, then reducing the pH value to 11.2-11.7, continuously reacting until the average particle size of the particles grows to the target particle size, stopping feeding to obtain a solution containing a precursor material, and then aging, washing, drying, screening and removing iron to obtain a precursor of the positive electrode material.
2. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: and step S3 is repeatedly performed until the tap density meets the design requirement.
3. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: the total concentration of metal ions in the metal salt solution is 1-3 mol/L, and the metal salt solution is nickel salt, cobalt salt or aqueous solution containing nickel salt, cobalt salt and manganese salt.
4. A method for preparing a ternary positive electrode material precursor according to claim 3, wherein: the nickel salt, cobalt salt and manganese salt are at least one of sulfate, nitrate and halogen salt.
5. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: the raw materials also comprise aluminum salt solution.
6. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: the alkali liquor is one or a mixed solution of more than one 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 ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: the average particle size of the particles is the D50 value of the particle size distribution, and the target particle size is 3-15 mu m.
8. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the method comprises the following steps: the inert shielding gas is nitrogen, helium or argon.
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| 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 |
| 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 |
| 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 |
| CN115403076A (en) * | 2022-08-25 | 2022-11-29 | 广东邦普循环科技有限公司 | Porous spherical ternary precursor and preparation method thereof, ternary positive electrode material, positive electrode plate and battery |
| CN115504518A (en) * | 2022-09-15 | 2022-12-23 | 广东邦普循环科技有限公司 | Positive electrode material precursor, positive electrode material, and preparation method and application of positive electrode material |
| 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 |
| 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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