CN114655998A - Preparation method of high-nickel ternary positive electrode precursor - Google Patents
Preparation method of high-nickel ternary positive electrode precursor Download PDFInfo
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- CN114655998A CN114655998A CN202210200777.7A CN202210200777A CN114655998A CN 114655998 A CN114655998 A CN 114655998A CN 202210200777 A CN202210200777 A CN 202210200777A CN 114655998 A CN114655998 A CN 114655998A
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- C—CHEMISTRY; METALLURGY
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- C01G53/00—Compounds of nickel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a preparation method of a high-nickel ternary cathode precursor, which comprises the following steps of: weighing Ni salt, metal A salt and metal B salt in a molar ratio of x, y and z in sequence, wherein x is more than or equal to 0.5 and less than or equal to 0.98, and x + y + z is 1 to prepare a transition metal salt solution; adding the base solution into a reaction kettle, sealing the reaction kettle, introducing inert gas, heating, raising the temperature, adding a precipitator, a complexing agent and the obtained transition metal salt solution into the reaction kettle for reaction, and then stirring at constant temperature; taking out the obtained product, cleaning until the supernatant is neutral, filtering, and drying the filter cake to obtain the final product. According to the preparation method of the high-nickel ternary cathode precursor, provided by the invention, the precursor particles with regular appearance, compact particles and concentrated particle size distribution can be prepared by adopting a single-kettle preparation mode and controlling the pH value, the ammonia concentration, the reaction time and the dropping speed of the raw materials in the reaction process.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to a preparation method of a high-nickel ternary positive electrode precursor.
Background
With the improvement of the requirement on the driving mileage of the electric automobile, it is very important to develop a battery material with high energy density, wherein the ternary cathode material has received wide attention due to its high energy density and low cost. At present, the mainstream preparation method of the ternary cathode material is a coprecipitation method and a high-temperature solid phase method, a ternary cathode precursor is prepared by the coprecipitation method, and then a lithium source is added to synthesize the ternary cathode material by the high-temperature solid phase method, wherein the quality of the precursor has the greatest influence on the performance of the ternary cathode material, so that the preparation of the qualified precursor is the premise of producing the high-performance ternary cathode material. The existing ternary precursor preparation generally adopts multi-kettle preparation, and has long production cycle, wide product particle size distribution and irregular appearance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-nickel ternary cathode precursor, which solves the problems of long production cycle, wide product particle size distribution and irregular appearance caused by the existing preparation method.
The technical scheme adopted by the invention is as follows: the preparation method of the high-nickel ternary positive electrode precursor comprises the following steps:
step 2, adding the base solution into the reaction kettle, sealing the reaction kettle, introducing inert gas, heating, raising the temperature, adding the precipitator, the complexing agent and the transition metal salt solution obtained in the step 1 into the reaction kettle for reaction, and then stirring at constant temperature;
and 3, taking out the product obtained in the step 2, cleaning until the supernatant is neutral, performing suction filtration, and drying the filter cake to obtain the filter cake.
The present invention is also characterized in that,
in the metal A salt and the metal B salt in the step 1, the metal A and the metal B are selected from any two of Co, Mn, Zn, Al, Mg and Fe; the salt forming type of the Ni salt, the metal A salt and the metal B salt is one of sulfate, chloride or nitrate.
In the step 1, deionized water is added to prepare a transition metal salt solution with the concentration of 1-3 mol/L.
And 2, adding the base solution in the step (2) by volume accounting for 20-80% of the volume of the reaction kettle.
The inert gas in the step 2 is N2Introduction of N2And completely discharging the air in the reaction kettle.
Heating to 45-60 ℃ in the step 2, and stirring at constant temperature for 2-50 h.
The base solution in the step 2 is ammonia water with the concentration of 0.1-0.7mol/L, the precipitator is NaOH solution with the concentration of 2-8mol/L, and the complexing agent is ammonia water with the concentration of 1-7 mol/L.
And 2, adding the precipitator, the complexing agent and the transition metal salt solution obtained in the step 1 into a reaction kettle in a parallel flow manner through a peristaltic pump, controlling the dropping speed between V ml/min and the volume V L of the reaction kettle to be 0.5-2V/V, controlling the pH to be 10-12 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.1-0.7mol/L, and stirring at the speed of 400-1200 r/min.
And 3, washing the product by deionized water until the pH of the supernatant is neutral, detecting the conductivity of the supernatant, and performing suction filtration after no impurity metal ions exist.
And 3, drying the obtained filter cake in a drying box for 8-24h at the temperature of 60-150 ℃.
The invention has the beneficial effects that: according to the preparation method of the high-nickel ternary cathode precursor, provided by the invention, the precursor particles with regular appearance, compact particles and concentrated particle size distribution can be prepared by adopting a single-kettle preparation mode and controlling the pH value, the ammonia concentration, the reaction time and the dropping speed of the raw materials in the reaction process.
Drawings
FIG. 1 is a 5000 × SEM image of a ternary positive electrode precursor prepared according to the present invention;
fig. 2 is a 20000 × SEM image of the ternary positive electrode precursor prepared by the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a high-nickel ternary positive electrode precursor, which comprises the steps of weighing Ni salt, Co salt and Mn salt according to a molar ratio of x: y: z (x is more than or equal to 0.5 and less than or equal to 0.98, and x + y + z is 1), adding deionized water, and preparing 1-3mol/L transition metal salt solution, wherein the latter two metal salts can be replaced by other transition metal salt solutions, such as Zn, Al, Mg, Fe salt and the like, and the metal salt types comprise sulfate, chloride and nitrate. Preparing 2-8mol/L NaOH solution as precipitant, preparing 1-7mol/L ammonia water as complexing agent, using 0.1-0.7mol/L ammonia water as base solution, adding a certain volume of base solution into a reaction kettle, wherein the base solution amount is 20-80% of the volume of the reaction kettle, introducing N into the reaction kettle2The air in the reaction kettle is discharged, a heating switch is turned on, the temperature in the kettle is controlled to be 45-60 ℃, and the transition metal salt solution, the precipitator and the complexing agent are added into the reaction kettle in a parallel flow mode through a peristaltic pump. Controlling the pH value to be between 10 and 12 in the reaction process, controlling the total ammonia concentration in the reaction kettle to be between 0.1 and 0.7mol/L, controlling the rotating speed of a stirring paddle in the kettle to be 400-1200r/min, controlling the V/V between the dropping speed V ml/min of raw materials and the volume V L of the reaction kettle to be between 0.5 and 2, controlling the dropping time of the reaction to be between 8 and 50 hours, stopping feeding after dropping, keeping the preset temperature of between 45 and 60 ℃ and continuing stirring for 2 to 50 hours, taking out a product after the reaction is finished, washing the precipitation product by deionized water until the pH value of a supernatant is neutral, detecting the conductivity of the supernatant, determining that no other impurity metal ions exist in the supernatant, carrying out suction filtration on the washed precipitation product, placing the obtained filter cake in a drying box to be dried for 8 to 24 hours at the temperature of between 60 and 150 ℃, and then passing the dried product through a screen, and packaging the sieved product.
By adopting the mode, the preparation method of the high-nickel ternary cathode precursor disclosed by the invention overcomes the problems of long production period, wide product particle size distribution, irregular and non-uniform appearance caused by multi-kettle preparation by adopting a single kettle preparation mode; in addition, the pH value, the ammonia concentration, the reaction time and the raw material dripping speed are controlled in the reaction process, precursor particles with regular appearance, compact particles and concentrated particle size distribution can be prepared, and parameters such as the raw material adding amount, the dripping speed and the like are directly related to the volume of the reaction kettle, so that the method is suitable for reaction kettles with different volumes.
As shown in fig. 1 and 2, the product is a spheroidal or spherical particle with D50 ranging from 3 to 20 microns, conventionally referred to as a spherical particle as a secondary particle, on which spindle-shaped (or described as stripe, plate, needle-shaped) primary particles are distributed, the whole secondary particle being composed of the primary particles. The primary particles are tightly packed, the tap density is high, and the characteristic can be inherited to a positive electrode material prepared subsequently, so that the energy density of the battery can be improved.
Example 1
Mixing NiSO4·6H2O、FeSO4·7H2O、MnSO4·H2Weighing O at a molar ratio of 8:1:1, adding deionized water to prepare a transition metal salt solution of 2mol/L, weighing NaOH to prepare a solution of 4mol/L as a precipitator, preparing ammonia water of 2.5mol/L as a complexing agent, preparing a base solution with the volume of 50% of the reaction kettle by using the ammonia water, adding the base solution into the reaction kettle, sealing the reaction kettle, introducing nitrogen to open a heating switch, heating to 55 ℃ after air in the kettle is completely discharged, adding the transition metal salt solution, the precipitating agent and the complexing agent into the reaction kettle in a concurrent flow manner through a peristaltic pump, controlling the pH to be 11.2 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.5mol/L, stirring at a feeding speed of 800r/min, keeping the reaction temperature at 55 ℃ for 20 hours, closing the peristaltic pump after feeding is finished, and continuously stirring at 55 ℃ for 12 hours. And after the reaction is finished, taking out the product, washing the product by using deionized water until the supernatant is neutral, carrying out suction filtration on the cleaned product, and drying the filter cake in a drying oven at 100 ℃ for 12h to obtain the ternary cathode precursor with the molar ratio of Ni to Fe to Mn of 8:1: 1.
Example 2
Mixing NiSO4·6H2O、CoSO4·7H2O、MnSO4·H2Weighing O at a molar ratio of 98:1:1, adding deionized water to prepare a 2mol/L transition metal salt solution, weighing NaOH to prepare a 6mol/L solution as a precipitator, preparing 2mol/L ammonia water as a complexing agent, preparing a 30% base solution by using the ammonia water, adding the base solution into a reaction kettle, sealing the reaction kettle, introducing nitrogen gasAnd opening a heating switch, after the air in the kettle is completely discharged and the temperature is raised to 55 ℃, adding the transition metal salt solution, the precipitator and the complexing agent into the reaction kettle in a parallel flow manner through a peristaltic pump, controlling the pH to be 11.4 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.55mol/L, stirring at the speed of 800r/min, keeping the reaction temperature at 55 ℃, feeding for 24 hours, closing the peristaltic pump after the feeding is finished, and continuously stirring at 55 ℃ for 12 hours. And after the reaction is finished, taking out the product, washing the product by using deionized water until the supernatant is neutral, carrying out suction filtration on the washed product, and drying the filter cake in a drying oven at 100 ℃ for 12 hours to obtain the ternary anode precursor with the molar ratio of Ni to Co to Mn being 98:1: 1.
Example 3
Mixing NiSO4·6H2O、FeSO4·7H2O、MnSO4·H2Weighing O at a molar ratio of 6:2:2, adding deionized water to prepare 1mol/L transition metal salt solution, weighing NaOH to prepare 2mol/L solution serving as a precipitator, preparing 1mol/L ammonia water serving as a complexing agent, preparing 20% base solution of the volume of a reaction kettle by using the ammonia water, adding the base solution into the reaction kettle, sealing the reaction kettle, introducing nitrogen to open a heating switch, heating to 45 ℃ after air in the kettle is completely discharged, adding the transition metal salt solution, the precipitating agent and the complexing agent into the reaction kettle in a parallel flow manner through a peristaltic pump, controlling the pH to be 10 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.1mol/L, stirring at a speed of 400r/min, keeping the reaction temperature at 45 ℃, feeding time to be 8h, closing the peristaltic pump after feeding is finished, and continuing stirring at 45 ℃ for 2 h. And after the reaction is finished, taking out the product, washing the product by using deionized water until the supernatant is neutral, carrying out suction filtration on the cleaned product, and drying the filter cake in a drying oven at 60 ℃ for 24h to obtain the ternary cathode precursor with the molar ratio of Ni to Fe to Mn of 6:2: 2.
Example 4
Mixing NiSO4·6H2O、CoSO4·7H2O、MnSO4·H2Weighing O according to the molar ratio of 5:2:3, adding deionized water to prepare a transition metal salt solution of 3mol/L, weighing NaOH to prepare a solution of 8mol/L as a precipitator, preparing ammonia water of 7mol/L as a complexing agent, and preparing a base solution with 80% of the volume of the reaction kettle by using the ammonia waterAdding the base solution into a reaction kettle, sealing the reaction kettle, introducing nitrogen to open a heating switch, after the air in the kettle is completely discharged and the temperature is raised to 60 ℃, adding a transition metal salt solution, a precipitator and a complexing agent into the reaction kettle in a parallel flow manner through a peristaltic pump, controlling the pH to be 12 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.7mol/L, stirring at the speed of 1200r/min, keeping the reaction temperature at 60 ℃, feeding for 50h, closing the peristaltic pump after the feeding is finished, and continuing to stir at 60 ℃ for 50 h. And after the reaction is finished, taking out the product, washing the product by using deionized water until the supernatant is neutral, carrying out suction filtration on the cleaned product, and drying the filter cake in a drying oven at 150 ℃ for 8h to obtain the ternary cathode precursor with the molar ratio of Ni to Co to Mn of 5:2: 3.
Example 5
Mixing Ni (NO)3)2·6H2O、Co(NO3)2·6H2O、Mg(NO3)2·H2Weighing O according to a molar ratio of 85:10:5, adding deionized water to prepare a 2.5mol/L transition metal salt solution, weighing NaOH to prepare a 6mol/L solution as a precipitator, preparing 5mol/L ammonia water as a complexing agent, preparing a 20% base solution by using the ammonia water, adding the base solution into a reaction kettle, sealing the reaction kettle, introducing nitrogen to open a heating switch, heating to 50 ℃ after air in the kettle is completely discharged, adding the transition metal salt solution, the precipitating agent and the complexing agent into the reaction kettle in a concurrent flow manner through a peristaltic pump, controlling the pH value to be 10.8 in the reaction process, controlling the ammonia concentration in the reaction kettle to be 0.2mol/L, stirring at a stirring speed of 700r/min, keeping the reaction temperature at 50 ℃, keeping the feeding time for 30 hours, closing the peristaltic pump after the feeding is finished, and continuing to stir at 50 ℃ for 40 hours. And after the reaction is finished, taking out the product, washing the product by using deionized water until the supernatant is neutral, carrying out suction filtration on the washed product, and drying the filter cake in a drying oven at 120 ℃ for 20h to obtain the ternary cathode precursor with the molar ratio of Ni, Co and Mg of 85:10: 5.
Claims (10)
1. The preparation method of the high-nickel ternary cathode precursor is characterized by comprising the following steps of:
step 1, weighing Ni salt, metal A salt and metal B salt in a molar ratio of x: y: z in sequence, wherein x is more than or equal to 0.5 and less than or equal to 0.98, and x + y + z is 1 to prepare a transition metal salt solution;
step 2, adding the base solution into the reaction kettle, sealing the reaction kettle, introducing inert gas, heating, raising the temperature, adding the precipitator, the complexing agent and the transition metal salt solution obtained in the step 1 into the reaction kettle for reaction, and then stirring at constant temperature;
and 3, taking out the product obtained in the step 2, cleaning until the supernatant is neutral, performing suction filtration, and drying the filter cake to obtain the filter cake.
2. The method for preparing the high-nickel ternary cathode precursor according to claim 1, wherein the metal a and the metal B in the metal a salt and the metal B salt of step 1 are selected from any two of Co, Mn, Zn, Al, Mg and Fe; the salt forming type of the Ni salt, the metal A salt and the metal B salt is one of sulfate, chloride or nitrate.
3. The method for preparing the high-nickel ternary positive electrode precursor according to claim 1, wherein a transition metal salt solution with a concentration of 1-3mol/L is prepared in the step 1 by adding deionized water.
4. The method for preparing a high-nickel ternary positive electrode precursor according to claim 1, wherein the addition volume of the electrolyte in the step 2 is 20-80% of the volume of the reaction kettle.
5. The method for preparing the high-nickel ternary positive electrode precursor according to claim 1, wherein the inert gas in the step 2 is N2Introduction of N2And completely discharging the air in the reaction kettle.
6. The preparation method of the high-nickel ternary positive electrode precursor according to claim 1, wherein the heating in the step 2 is carried out to 45-60 ℃, and the stirring time at constant temperature is 2-50 h.
7. The method for preparing the high-nickel ternary positive electrode precursor according to claim 1, wherein the base solution in the step 2 is ammonia water with a concentration of 0.1-0.7mol/L, the precipitant is NaOH solution with a concentration of 2-8mol/L, and the complexing agent is ammonia water with a concentration of 1-7 mol/L.
8. The method for preparing the high-nickel ternary positive electrode precursor as claimed in claim 7, wherein the precipitant, the complexing agent and the transition metal salt solution obtained in step 1 are co-flowed into the reaction kettle through a peristaltic pump in step 2, the dropping speed V ml/min and the volume V L of the reaction kettle are controlled between 0.5-2V/V, the pH is controlled to be 10-12 during the reaction, the ammonia concentration in the reaction kettle is 0.1-0.7mol/L, and the stirring speed is 400-1200 r/min.
9. The method for preparing the high-nickel ternary positive electrode precursor according to claim 1, wherein in the step 3, the product is washed by deionized water until the pH of the supernatant is neutral, the conductivity of the supernatant is detected, and the supernatant is filtered after no impurity metal ions exist.
10. The method for preparing the high-nickel ternary positive electrode precursor according to claim 1, wherein the filter cake obtained in the step 3 is dried in a drying oven at 60-150 ℃ for 8-24 h.
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