CN111463425A - Ternary positive electrode material precursor and preparation method thereof - Google Patents
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The application discloses a preparation method of a ternary cathode material precursor, which comprises the following steps: 1) preparing a mixed solution of metal salt; 2) preparing an alkali metal hydroxide solution and an ammonia solution; 3) adding a foaming agent or a defoaming agent into the metal salt mixed solution, the alkali metal oxide solution or the ammonia solution, and uniformly stirring; 4) mixing the solutions prepared in the steps 1) to 3), stirring and reacting to generate slurry containing a precursor of the ternary cathode material; 5) and carrying out post-treatment on the slurry to obtain a ternary cathode material precursor. The application also discloses a ternary cathode material prepared by using the method.
Description
Technical Field
The application relates to the field of battery materials, in particular to a ternary cathode material precursor and a preparation method thereof.
Background
In recent years, lithium ion batteries have been widely used in electronic digital products such as mobile phones and tablet computers, and gradually become the preferred power source in the fields of energy storage devices, electric vehicles, and the like due to their advantages of high specific energy, high output voltage, high-current charging and discharging, no memory effect, long cycle life, low self-discharge rate, environmental protection, and the like.
In 2018, the yield of the ternary cathode material is 14.12 ten thousand tons, and compared with the increase of 33% in the same ratio in 2017, the ternary precursor is a necessary product for synthesizing the ternary battery cathode material, the performance of the battery material is directly influenced, the battery cycle performance of the current high-nickel product (the nickel content is greater than 80%) is gradually deteriorated along with the increase of the nickel content, and the compressive strength of the high-nickel cathode material is also deteriorated.
The production of the ternary cathode material precursor adopts cobalt sulfate crystals, nickel sulfate crystals and the like as main raw materials, and the problems of poor battery cycle performance and low compressive strength of the high-nickel ternary cathode material at present are that the service life of the battery is shortened.
Patent application publication No. CN 109485104 a discloses a method for reducing the crystallinity of a ternary material precursor by increasing the specific surface area (BET) of the ternary precursor through a micro bubble device, which physically purges an oxidizing gas to the liquid phase portion of a reaction solution, oxidizes cobalt elements and additive elements, increases the specific surface area (BET) of the precursor, and simultaneously reduces the crystallinity. However, this method requires the addition of special equipment for increasing the oxidizing gas, and only the porosity can be increased directionally, which cannot be reduced, and the blowing of air by physical means cannot ensure the uniform distribution of gas inside the solution.
Disclosure of Invention
The application mainly aims to provide a ternary cathode material precursor and a preparation method thereof, and aims to solve the problems that the internal porosity of the precursor is difficult to directly regulate and control, and a sample sintered from a cathode has low compressive strength in the related technology.
In order to achieve the above object, according to a first aspect of the present application, there is provided a method for preparing a ternary positive electrode material precursor, characterized by comprising the steps of:
1) preparing a mixed solution of metal salt;
2) preparing an alkali metal hydroxide solution and an ammonia solution;
3) adding a foaming agent or a defoaming agent into the metal salt mixed solution, the alkali metal oxide solution or the ammonia solution, and uniformly stirring;
4) mixing the solutions prepared in the steps 1) to 3), stirring and reacting to generate slurry containing a precursor of the ternary cathode material;
5) and carrying out post-treatment on the slurry to obtain a ternary cathode material precursor.
Preferably, the foaming agent or defoamer is added in an amount such that, upon mixing in step 4), the concentration of the foaming agent or defoamer is from 0.01 g/L to 10 g/L.
Preferably, the foaming agent is selected from at least one of sodium dodecyl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate, amino acid and derivatives thereof, and the defoaming agent is selected from at least one of trialkyl melamine, cyanuric chloride melamine, copolymer of ethylene oxide and propylene oxide, and polydimethylsiloxane.
Preferably, the total concentration of metal ions in the metal salt mixed solution is 1-3 mol/L, and the metal salt is preferably a salt of three metals of nickel, cobalt and manganese.
Preferably, the concentration of the alkali metal hydroxide solution is 1 to 15 mol/L, and the concentration of the ammonia solution is 5 to 10 mol/L.
Preferably, the reaction in the step 4) is carried out at 40-80 ℃, the reaction time is 15-26h, and the pH value of the reaction system is controlled at 10-12.
The reaction time is the volume of all solutions entering the reaction kettle in the actual use volume of the reaction kettle per unit time, and the volume of all solutions entering the reaction kettle in unit time is the volume of the transition metal salt solution entering the reaction kettle in unit time + the volume of the alkali metal solution entering the reaction kettle in unit time + the volume of the ammonia solution entering the reaction kettle in unit time.
Preferably, the reaction of step 4) is carried out in the absence of oxygen, and preferably, an inert gas is introduced into the reactor to remove oxygen before mixing the solutions.
Preferably, the post-treatment in the step 5) comprises the steps of carrying out solid-liquid separation on the slurry, and then washing and drying to obtain the product.
According to another aspect of the application, the ternary cathode material precursor prepared by the preparation method of the ternary cathode material precursor is characterized in that the general formula of the ternary cathode material precursor is NixCoyMz(OH)2+aWherein x + y + z is 1, x is more than or equal to 0.5 and less than or equal to 0.95, y is more than or equal to 0 and less than or equal to 0.3, z is more than or equal to 0 and less than or equal to 0.5, a is more than or equal to 0 and less than or equal to 0.5, and M is a metal element and is selected from at least one of Mg, Ca, Al, Ti, Mn, Zr and Zn.
Preferably, the precursor of the ternary cathode material is a sphere formed by aggregation of fibrous primary crystal grains, the diameter of the primary crystal grains is 0.1-1 μm, the average particle diameter of the precursor of the ternary cathode material is 5 μm-20 μm, and the tap density of the precursor of the ternary cathode material is 1-3g/cm3。
The precursor of the ternary cathode material and the preparation method thereof have the following advantages:
1. the gas content in the reaction solution is increased by adding a physical foaming agent or a chemical foaming agent, and finally, the porosity in the precursor is increased, so that the sintered cathode material has good pressure resistance, the cycle performance of the battery is improved, and for the precursor material without pores, the gas in the reaction solution can be removed by using a defoaming agent.
2. The preparation method is convenient to popularize in chemical production, and is more convenient and direct for changing the characteristics of the product.
3. The preparation method is a method capable of directionally changing the porosity of the ternary material precursor, so that fine pores can be uniformly distributed in the prepared precursor, the battery cycle performance of the ternary anode material sintered at the later stage is obviously improved, and the compressive strength of the anode material is also improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, serve to provide a further understanding of the application and to enable other features, objects, and advantages of the application to be more apparent. The drawings and their description illustrate the embodiments of the invention and do not limit it. In the drawings:
FIG. 1 is a particle section electron microscope image of a ternary cathode material precursor;
FIG. 2 is a sectional electron microscope image of particles of a precursor of a ternary cathode material provided according to an embodiment of the present application;
FIG. 3 is a sectional electron microscope image of particles of a precursor of a ternary cathode material provided according to an embodiment of the present application;
fig. 4 is a sectional electron microscope image of particles of a precursor of a ternary cathode material provided in an embodiment of the present application.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example 1
Preparing a solution 200L with a nickel-cobalt-manganese molar ratio of 8:1:1 and a total nickel-cobalt-manganese molar concentration of 1.5 mol/L by using nickel sulfate, cobalt sulfate and manganese sulfate, preparing a solution 5.0 mol/L sodium hydroxide solution 200 liters by using sodium hydroxide, adding the prepared nickel sulfate, cobalt sulfate, manganese sulfate aqueous solution, sodium hydroxide solution and a complexing agent ammonia water (10 mol/L) into a reaction kettle in parallel through a metering pump, controlling the reaction temperature in the reaction kettle to be 60 +/-5 ℃, controlling the ammonia water concentration to be 10 +/-2 g/L and the reaction pH value to be 11.0 +/-0.5, reacting for 50 hours, filtering the precipitate, washing the precipitate with pure hot water at 60 ℃, drying the precipitate in a drying box at 110 ℃ for 10 hours, drying the precipitate, and screening the precipitate with 200 meshes to obtain the nickel-cobalt-manganese composite hydroxide.
The physicochemical data are as follows:
| test index | Ni(mol％) | Co(mol％) | Mn(mol％) | D50(μm) | BET(m2/g) |
| Value of | 80.2 | 9.9 | 9.9 | 10.3 | 9.5 |
As shown in FIG. 1, when no chemical foaming agent or defoaming agent is added, the inside of the film is slightly porous and the distribution of the film is not uniform.
Example 2
Preparing a solution 200L with a nickel-cobalt-manganese molar ratio of 8:1:1 and a total nickel-cobalt-manganese molar concentration of 1.5 mol/L by using nickel sulfate, cobalt sulfate and manganese sulfate, preparing a solution 5.0 mol/L sodium hydroxide solution 200 liters by using sodium hydroxide, adding trialkyl trise into the prepared nickel-cobalt-manganese sulfate solution to obtain cyanamide with a concentration of 2 g/L, adding the prepared nickel-cobalt-manganese sulfate solution, sodium hydroxide solution and complexing agent ammonia water (10 mol/L) into a reaction kettle in a cocurrent flow manner through a metering pump, controlling the reaction temperature in the reaction kettle to be 60 +/-5 ℃, controlling the ammonia water concentration to be 10 +/-2 g/L and the reaction pH value to be 11.0 +/-0.5, filtering the precipitate after reacting for 50 hours, washing the precipitate with pure hot water at 60 ℃, drying the precipitate in a drying oven at 110 ℃ for 10 hours, and screening the precipitate with 200 meshes to obtain the manganese-cobalt-manganese composite hydroxide.
The physicochemical data are as follows:
| test index | Ni(mol％) | Co(mol％) | Mn(mol％) | D50(μm) | BET(m2/g) |
| Value of | 80.2 | 9.9 | 9.9 | 10.2 | 4.3 |
After addition of the antifoam, it can be seen from the particle section electron micrograph that the internal pores are substantially eliminated, as shown in FIG. 2.
Example 3
Preparing a solution 200L with a nickel-cobalt-manganese molar ratio of 8:1:1 and a total nickel-cobalt-manganese molar concentration of 1.5 mol/L from nickel sulfate, cobalt sulfate and manganese sulfate, preparing a sodium hydroxide solution 5.0 mol/L with sodium hydroxide for 200 liters, adding sodium dodecyl sulfate with a concentration of 2 g/L into the prepared nickel-cobalt-manganese sulfate solution, adding the prepared nickel-cobalt-manganese sulfate solution, the sodium hydroxide solution and a complexing agent ammonia water (10 mol/L) into a reaction kettle in a parallel flow manner through a metering pump, controlling the reaction temperature in the reaction kettle to be 60 +/-5 ℃, the ammonia water concentration to be 10 +/-2 g/L and the reaction pH value to be 11.0 +/-0.5, filtering the precipitate after reacting for 50 hours, washing the precipitate with pure hot water at 60 ℃, drying the precipitate in a drying oven at 110 ℃ for 10 hours, and screening the dried precipitate with 200 meshes to obtain the nickel-cobalt-manganese composite hydroxide.
The physicochemical data are as follows:
| test index | Ni(mol％) | Co(mol％) | Mn(mol％) | D50(μm) | BET(m2/g) |
| Value of | 80.2 | 9.9 | 9.9 | 10.3 | 15.9 |
After the foaming agent is added, the pores are present in a large area and are uniformly distributed as seen in a section electron microscope image of the particles, as shown in FIG. 3.
Example 4
Preparing a solution 200L with a nickel-cobalt-manganese molar ratio of 8:1:1 and a total nickel-cobalt-manganese molar concentration of 1.5 mol/L from nickel sulfate, cobalt sulfate and manganese sulfate, preparing a 5.0 mol/L sodium hydroxide solution 200 liters from sodium hydroxide, adding sodium dodecyl sulfate with a concentration of 5 g/L into the prepared nickel-cobalt-manganese sulfate solution, adding the prepared nickel-cobalt-manganese sulfate solution, sodium hydroxide solution and complexing agent ammonia water (10 mol/L) into a reaction kettle in a parallel flow manner through a metering pump, controlling the reaction temperature in the reaction kettle to be 60 +/-5 ℃, the ammonia water concentration to be 10 +/-2 g/L and the reaction pH value to be 11.0 +/-0.5, filtering the precipitate after reacting for 50 hours, washing the precipitate with pure hot water at 60 ℃, drying the precipitate in a drying oven at 110 ℃ for 10 hours, and screening the dried precipitate with 200 meshes to obtain the nickel-cobalt-manganese composite hydroxide.
The physicochemical data are as follows:
| test index | Ni(mol％) | Co(mol％) | Mn(mol％) | D50(μm) | BET(m2/g) |
| Value of | 80.2 | 9.9 | 9.9 | 10.2 | 25.3 |
The porosity can be increased by increasing the concentration of the blowing agent sodium lauryl sulfate, and the same conclusion can be drawn from the corresponding BET variation, from which it can be seen from the particle profile electron micrograph that the pores are present in large areas and are uniformly distributed, as shown in fig. 4.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a ternary cathode material precursor is characterized by comprising the following steps:
1) preparing a mixed solution of metal salt;
2) preparing an alkali metal hydroxide solution and an ammonia solution;
3) adding a foaming agent or a defoaming agent into the metal salt mixed solution, the alkali metal hydroxide solution or the ammonia solution, and uniformly stirring;
4) mixing the solutions prepared in the steps 1) to 3), stirring and reacting to generate slurry containing a precursor of the ternary cathode material;
5) and carrying out post-treatment on the slurry to obtain a ternary cathode material precursor.
2. The method for preparing a ternary positive electrode material precursor according to claim 1, wherein the foaming agent or defoaming agent is added in an amount such that the concentration of the foaming agent or defoaming agent is 0.01 g/L to 10 g/L when mixing in step 4).
3. The method for preparing the ternary cathode material precursor according to claim 1, wherein the foaming agent is at least one selected from sodium dodecyl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate, amino acid and derivatives thereof, and the antifoaming agent is at least one selected from trialkyl melamine, cyanuric chloride melamine, copolymer of ethylene oxide and propylene oxide, and polydimethylsiloxane.
4. The method for preparing the precursor of the ternary cathode material according to claim 1, wherein the total concentration of metal ions in the metal salt mixed solution is 1-3 mol/L, and/or the metal salt is a salt of three metals of nickel, cobalt and manganese.
5. The method for producing a ternary positive electrode material precursor according to claim 1, wherein the concentration of the alkali metal hydroxide solution is 1 to 15 mol/L and/or the concentration of the ammonia solution is 5 to 10 mol/L.
6. The method for preparing the ternary cathode material precursor of claim 1, wherein the reaction in the step 4) is carried out at 40-80 ℃, the reaction time is 15-26h, and the pH value of the reaction system is controlled to be 10-12.
7. The method for preparing a ternary cathode material precursor according to claim 1, wherein the reaction of step 4) is performed under oxygen-free conditions, and preferably, an inert gas is introduced into the reactor to remove oxygen before mixing the solutions.
8. The method for preparing the ternary cathode material precursor of claim 1, wherein the post-treatment in the step 5) comprises performing solid-liquid separation on the slurry, and then washing and drying to obtain the product.
9. The precursor of the ternary cathode material prepared by the method for preparing the precursor of the ternary cathode material according to any one of claims 1 to 8, wherein the general formula of the precursor of the ternary cathode material is NixCoyMz(OH)2+aWherein x + y + z is 1, x is more than or equal to 0.5 and less than or equal to 0.95, y is more than or equal to 0 and less than or equal to 0.3, z is more than or equal to 0 and less than or equal to 0.5, a is more than or equal to 0 and less than or equal to 0.5, and M is a metal element and is selected from at least one of Mg, Ca, Al, Ti, Mn, Zr and Zn.
10. The precursor of the ternary positive electrode material according to claim 9, wherein the precursor of the ternary positive electrode material is a sphere formed by aggregation of fibrous primary crystal grains, the diameter of the primary crystal grains is 0.1 to 1 μm, the average particle diameter of the precursor of the ternary positive electrode material is 5 μm to 20 μm, and the tap density of the precursor of the ternary positive electrode material is 1 to 3g/cm3。
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| CN114084917A (en) * | 2022-01-24 | 2022-02-25 | 金驰能源材料有限公司 | Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof |
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| CN112542328A (en) * | 2020-12-02 | 2021-03-23 | 浙江大学 | Ternary layered metal hydroxide @ polyaniline composite electrode material and preparation method and application thereof |
| CN112542328B (en) * | 2020-12-02 | 2022-07-05 | 浙江大学 | Ternary layered metal hydroxide @ polyaniline composite electrode material and preparation method and application thereof |
| CN113896255A (en) * | 2021-09-30 | 2022-01-07 | 宁波容百新能源科技股份有限公司 | Annular-pore ternary positive electrode precursor and preparation method thereof |
| CN113896255B (en) * | 2021-09-30 | 2023-10-13 | 宁波容百新能源科技股份有限公司 | Annular pore ternary positive electrode precursor and preparation method thereof |
| CN114084917A (en) * | 2022-01-24 | 2022-02-25 | 金驰能源材料有限公司 | Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof |
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