CN114349069B - High-nickel ternary positive electrode material precursor and preparation method thereof - Google Patents
High-nickel ternary positive electrode material precursor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-nickel ternary positive electrode material precursor which is of a concentric sphere structure formed by mutually combining concentric spheres, wherein the interval between layers of the concentric sphere structure is 0.01-1 mu m, and the thickness of each layer of concentric sphere is 1-5 mu m. The precursor of the high-nickel ternary cathode material is prepared under the condition of not changing the rotating speed, the ammonia value and the pH value of the reaction, and the lithium ion battery prepared from the precursor of the concentric sphere structure improves the rate capability while ensuring the battery capacity and the cycle retention rate.
Description
Technical Field
The invention relates to a ternary positive electrode material precursor, in particular to a high-nickel ternary positive electrode material precursor.
Background
The lithium ion battery is widely applied due to the advantages of good circulation performance, high capacity, low price, convenient use, safety, environmental protection and the like. Today, with the increasing demand of high-performance batteries, such as high energy density, in the market and the increasing popularity of electric vehicles, the market demand of battery cathode materials has presented a rapidly growing situation. The ternary positive electrode material is a material with the highest potential and the most development prospect in the current positive electrode materials in mass production due to the characteristics of high energy density, relatively low cost, excellent cycle performance and the like, so that the performance of the ternary precursor is improved. In order to better exert the excellent performance of the ternary cathode material, the quality of the precursor is important to the production of the ternary cathode material, because the quality (morphology, particle size distribution, specific surface area, impurity content, tap density and the like) of the precursor directly determines the physicochemical index of the final sintered product. The production of ternary positive electrode material precursor mainly adopts hydroxide coprecipitation process, and is characterized by that after the raw material is dissolved in deionized water, and proportioned according to a certain mole ratio, naOH is used as precipitant, ammonia water is used as complexing agent so as to produce high-density spherical hydroxide precursor.
In the aspect of ternary precursor performance, the higher the nickel content in the material, the higher the energy density of the battery, the service time of the battery after single charging can be greatly improved, the endurance mileage of the vehicle-mounted power battery and the like, the high-nickel power battery solves the problem of light weight of the battery, the space saving capability is far better than that of a common ternary battery, and meanwhile, the use of cobalt is reduced due to the improvement of the nickel proportion, so that the production cost is reduced to a certain extent. The high-nickel ternary positive electrode material has high energy density and becomes an industry development hot spot, in order to improve the energy density of the high-nickel ternary positive electrode material, the adopted atmosphere and parameters can ensure that the precursor particles have continuous and compact internal structure during growth, the precursor of the high-nickel positive electrode material has higher dispersing requirement, and the compactness of the product particles is further enhanced by adopting high-rotating speed for production. Although the method improves the tap density of the precursor, the more compact the inside of the precursor, the lithium ions are difficult to migrate in the material after the prepared lithium ion battery, so that the performance of the high-nickel ternary positive electrode material can not be completely released, the battery has low charge and discharge capability and poor multiplying power performance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the high-nickel ternary positive electrode material precursor which can ensure the energy density of the lithium ion battery and improve the multiplying power performance of the lithium ion battery.
The technical scheme adopted for solving the technical problems is as follows: the ternary positive electrode material precursor is a concentric sphere structure formed by mutually combining concentric spheres, the interval between layers of the concentric sphere structure is 0.01-1 mu m, and the thickness of each layer of concentric sphere is 1-5 mu m.
The preparation method of the high-nickel ternary positive electrode material precursor comprises the following steps of:
(1) Preparing a metal salt solution, a precipitator solution, a complexing agent solution and a hydrogen peroxide solution, wherein the metal salt solution is an aqueous solution containing nickel salt, cobalt salt, manganese salt or aluminum salt;
(2) Adding a metal salt solution, a precipitator solution and a complexing agent solution into a reaction kettle for coprecipitation reaction, continuously introducing inert protective gas into the reaction kettle in the reaction process, starting to introduce hydrogen peroxide solution when the particle size of particles in the reaction kettle grows to 1-5 mu m, then continuously carrying out the reaction to prepare an interlayer structure of 0.01-1 mu m, then stopping introducing the hydrogen peroxide solution, continuously carrying out the reaction to prepare concentric spheres with the thickness of 1-5 mu m, repeating the preparation of the interlayer structure and the concentric spheres until the particle size D50 of the particles grows to the target particle size diameter, and stopping feeding to obtain a solution containing a precursor material;
(3) And (3) aging, washing, drying, screening and deironing the solution containing the precursor material to obtain the high-nickel ternary positive electrode material precursor with the concentric sphere structure.
Further, in the step (2), the pH value of the reaction system is controlled to be 10.0-12.5, the ammonia value is controlled to be 2-20 g/L, the temperature is controlled to be 40-80 ℃, and the rotating speed is controlled to be 100-1000 rpm.
Further, the total concentration of metal ions in the metal salt solution is 1-2.5 mol/L, the metal salt solution is an aqueous solution containing nickel salt, cobalt salt and manganese salt, and the introducing rate of the metal salt solution is 2-10L/h.
Further, the metal salt solution comprises a nickel-cobalt salt solution and an aluminum salt solution, wherein the total concentration of metal ions in the nickel-cobalt salt solution is 1-2.5 mol/L, the concentration of aluminum in the aluminum salt solution is 0.05-0.3 mol/L, the introducing rate of the nickel-cobalt salt solution is 2-10L/h, and the introducing rate of the aluminum salt solution is 0.5-4L/h.
Further, the inert shielding gas is nitrogen.
Further, the precipitant solution is a sodium hydroxide solution with the mass concentration of 28-34%, and the complexing agent solution is an ammonia water solution with the mass concentration of 16-25%.
Further, the concentration of the hydrogen peroxide solution is 3-15%, and the flow rate of the hydrogen peroxide solution is 0.2-2L/h.
The beneficial effects of the invention are as follows: the precursor of the high-nickel ternary cathode material is prepared under the condition of not changing the rotating speed, ammonia value and pH of the reaction, and the lithium ion battery prepared from the precursor of the concentric sphere structure improves the rate capability while ensuring the battery capacity and the cycle retention rate.
Drawings
FIG. 1 is a schematic cross-sectional structure of a ternary positive electrode material precursor obtained by the invention;
fig. 2 is a schematic cross-sectional structure of a ternary cathode material precursor obtained in example 1 of the present invention.
Detailed Description
The invention will be further described with reference to the drawings and examples.
Example 1:
and simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring speed is 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 90:5:5, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 5 μm, the designed concentric circles were 2 μm/layer, the interlayer spacing was 0.02 μm, and the D50 growth rate per hour was 0.12 μm/h. And continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 2 mu m, continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 4 mu m, keeping parameters such as pH, ammonia value, reaction temperature, rotating speed and the like unchanged in the process, and ending the reaction when the granularity D50 grows to 5 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, and then mixing and sintering the precursor material with lithium salt to form a positive electrode material, wherein the buckling electricity measurement discharge capacity is 0.1C:215.4mAh/g;0.2C:211.7mAh/g;0.5C:204.4mAh/g; the cycle retention at 1C was 94.4% at 50 weeks at 1C of 200.5 mAh/g.
Example 2:
and simultaneously introducing nickel cobalt sulfate solution, sodium metaaluminate solution, ammonia water and sodium hydroxide solution into a reaction kettle, introducing nitrogen for protection, setting the pH of a reaction system to be 12.2, setting the ammonia value to be 15g/L, and setting the reaction temperature to be 50 ℃ and the rotating speed to be 850rpm, wherein the concentration of the nickel cobalt sulfate is 1.6mol/L, the concentration of the sodium metaaluminate solution is 0.3mol/L, introducing two metal solutions into the reaction kettle according to a certain flow, wherein the mass percentage concentration of the sodium hydroxide solution is 32%, the mass percentage concentration of the ammonia water is 21%, and the mole ratio of each ion of nickel cobalt sulfate and aluminum salt solution after mixing is 94:3:3.
The product target D50 was 6 μm, the designed concentric circles were 2.5 μm/layer, the interlayer spacing was 0.02 μm, and the D50 growth rate per hour was 0.2 μm/h. And continuously introducing hydrogen peroxide for 6min when the granularity D50 grows to 2.5 mu m, continuously introducing hydrogen peroxide for 6min when the granularity D50 grows to 5 mu m, keeping parameters such as pH, ammonia value, reaction temperature, rotating speed and the like unchanged in the process, and ending the reaction when the granularity D50 grows to 6 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, mixing and sintering with lithium salt to form a positive electrode material, and carrying out buckling measurement on the positive electrode material to obtain a discharge capacity of 0.1C:224.7mAh/g;0.2C:220.8mAh/g;0.5C:214.8mAh/g; the cycle retention rate at 1C was 93.9% at 1C of 208.1mAh/g for 50 weeks.
Example 3:
and simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring rotation speed to be 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 95:3:2, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 15 μm, the designed concentric circles were 5 μm/layer, the interlayer spacing was 0.02 μm, and the D50 growth rate per hour was 0.12 μm/h. And continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 5 mu m, continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 10 mu m, keeping parameters such as pH, ammonia value, reaction temperature, rotating speed and the like unchanged in the process, and ending the reaction when the granularity D50 grows to 15 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, mixing and sintering with lithium salt to form a positive electrode material, and measuring the discharge capacity of 0.1C:223.4mAh/g;0.2C:220.5mAh/g;0.5C:214.8mAh/g; the cycle retention rate at 1C was 92.9% at 1C of 208.1mAh/g for 50 weeks.
Comparative example 1: (without interlayer Structure)
And simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring speed is 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 90:5:5, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 5 μm and the D50 growth rate per hour was 0.12 μm/h. The parameters such as pH, ammonia value, reaction temperature, rotating speed and the like are kept unchanged in the process, and the reaction is ended when the D50 grows to 5 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, mixing and sintering with lithium salt to form a positive electrode material, and carrying out buckling measurement on the positive electrode material to obtain a discharge capacity of 0.1C:214.7mAh/g;0.2C:206.5mAh/g;0.5C:196.14mAh/g; the 1C rate was 186.3mAh/g, and the 50-week cycle retention rate at 1C was 93.5%.
Comparative example 2: (Concentric circle thickness is less than 1 μm)
And simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring speed is 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 90:5:5, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 5 μm, the designed concentric circles were 0.5 μm/layer, the interlayer spacing was 0.02 μm, and the D50 growth rate per hour was 0.12 μm/h. Continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 2 mu m, continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 2.5 mu m, keeping parameters such as pH, ammonia value, reaction temperature, rotating speed and the like unchanged in the process, repeatedly preparing concentric circles and interlayers, and ending the reaction when the granularity D50 grows to 5 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, and then mixing and sintering the precursor material with lithium salt to form a positive electrode material, wherein the discharge capacity of the buckling test is 0.1C:215.8mAh/g;0.2C:212.7mAh/g;0.5C:206.9mAh/g;1C 199.4mAh/g, and a 50-week cycle retention of 86.7% at 1C.
Comparative example 3: (Concentric circle thickness is greater than 5 μm)
And simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring rotation speed to be 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 95:3:2, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 15 μm, the designed concentric circles were 6 μm/layer, the interlayer spacing was 0.02 μm, and the D50 growth rate per hour was 0.12 μm/h. Continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 6 mu m, continuously introducing hydrogen peroxide for 10min when the granularity D50 grows to 12 mu m, keeping parameters such as pH, ammonia value, reaction temperature, rotating speed and the like unchanged in the process, preparing particles with concentric sphere structures by repeating the operation of introducing hydrogen peroxide solution, and ending the reaction when the granularity D50 grows to 15 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, mixing and sintering with lithium salt to form a positive electrode material, and carrying out buckling measurement on the positive electrode material to obtain a discharge capacity of 0.1C:221.9mAh/g;0.2C:215.4mAh/g;0.5C:208.5mAh/g;1C 200.2mAh/g, 50 week cycle retention at 1C 94.8%.
Comparative example 4: (interlayer structure is larger than 1 μm)
And simultaneously introducing the nickel-cobalt-manganese salt mixed solution, ammonia water and sodium hydroxide into a reaction kettle, introducing nitrogen for protection, setting the pH value of the reaction system to be 12.0, setting the ammonia value to be 10g/L, and setting the reaction temperature to be 55 ℃, wherein the stirring rotation speed to be 800rpm, the concentration of the metal salt solution is 2.1mol/L, the molar ratio of nickel-cobalt-manganese ions in the metal salt solution is 95:3:2, the mass percentage concentration of the sodium hydroxide solution is 32%, and the mass percentage concentration of the ammonia water is 21%.
The product target D50 was 15 μm, the designed concentric circles were 5 μm/layer, the interlayer spacing was 1.5 μm, and the D50 growth rate per hour was 0.12 μm/h. Hydrogen peroxide is continuously fed for 12.5 hours when the granularity D50 grows to 5 mu m, hydrogen peroxide is continuously fed for 12.5 hours when the granularity D50 grows to 11.5 mu m, parameters such as pH, ammonia value, reaction temperature, rotating speed and the like are kept unchanged in the process, and the reaction is ended when the granularity D50 grows to 15 mu m.
Placing the kettle material in an aging kettle for aging, filtering, adding alkali liquor with a certain concentration into a filter cake for pulping, filtering and washing until the pH value of the filtrate is less than 9, drying, screening and demagnetizing to obtain a precursor material with a concentric sphere structure, and then mixing and sintering the precursor material with lithium salt to form a positive electrode material, wherein the discharge capacity of the buckling test is 0.1C:224.1mAh/g;0.2C:221.7mAh/g;0.5C:215.6mAh/g; the 1C 206.8mAh/g, 50 week cycle retention at 1C was 84.1%.
The electrochemical performance detection method comprises the following steps:
1. the five precursors prepared in examples 1 to 3 and comparative examples 1 to 4 and lithium hydroxide are uniformly mixed according to the molar ratio of M (Ni+Co+Mn): M (Li) =1:1.03, presintered for 4 hours at 450 ℃, taken out and ground, calcined for 20 hours at 750 ℃, taken out and ground to finally obtain five positive electrode materials, which are respectively marked as A1, A2, A3, D1, D2, D3 and D4;
2. six positive electrode materials A1, A2, A3, D1, D2, D3 and D4 are prepared according to the following positive electrode materials: conductive carbon: polyvinylidene fluoride (PVDF) =90: 5:5 preparing into slurry to prepare a positive pole piece (the compacted density of the pole piece is 3.3 g/cm) 2 ) Selecting a metal lithium sheet as a negative electrode material, and assembling the metal lithium sheet into a 2025 button cell;
3. the electrochemical performance test of the battery is carried out in a blue-ray test system, and the charge and discharge tests of 0.1C, 0.2C, 0.5C and 1C are respectively carried out in the voltage range of 3.0-4.3V;
4. at 1m LiPF6 EC: DEC: dmc=1: 1:1 (V%) is an electrolyte, and after three cycles of activation at a 1C magnification, the electrolyte was cycled 50 times at a 1C magnification, and the discharge capacity at the 1 st cycle and the discharge capacity at the 50 th cycle were measured, respectively, to calculate the capacity retention rate at 50 cycles.
5. The calculation formula is as follows: the specific capacity and cycle retention of the materials obtained by cycling 50 times the capacity retention (%) =discharge capacity at 50 th cycle/discharge capacity at 1 st cycle ×100% are shown in table 1, and the electrochemical performance measurement results of the five positive electrode materials are shown in table 1.
Table 1 electrochemical properties of the positive electrode materials obtained in examples and comparative examples
As can be seen from table 1, the lithium ion batteries prepared from the precursor of concentric sphere structure prepared in examples 1-3 have improved rate capability while ensuring battery capacity and cycle retention. As in example 1, the capacity was 215.4mAh/g, the percentage of discharge capacity of 0.1C/0.2C was 98.3% and the cycle retention rate at 50 weeks was 94.4%, and the comparative example had a good capacity and cycle retention rate but poor rate performance and the comparative example had a good rate performance but low cycle retention rate.
Claims (5)
1. The preparation method of the high-nickel ternary positive electrode material precursor is characterized in that the ternary positive electrode material precursor is of a concentric sphere structure formed by mutually combining concentric spheres, the interval between layers of the concentric sphere structure layer and the layer is 0.01-1 mu m, and the thickness of each layer of concentric sphere is 1-5 mu m, and the preparation method is characterized by comprising the following steps:
(1) Preparing a metal salt solution, a precipitator solution, a complexing agent solution and a hydrogen peroxide solution, wherein the metal salt solution is an aqueous solution containing nickel salt, cobalt salt, manganese salt or aluminum salt;
(2) Adding a metal salt solution, a precipitator solution and a complexing agent solution into a reaction kettle for coprecipitation reaction, continuously introducing inert protective gas into the reaction kettle in the reaction process, starting introducing hydrogen peroxide solution when the particle size of particles in the reaction kettle grows to 1-5 mu m, then continuously carrying out the reaction to prepare an interlayer structure of 0.01-1 mu m, stopping introducing the hydrogen peroxide solution, continuously carrying out the reaction to prepare concentric spheres with the thickness of 1-5 mu m, repeating the preparation of the interlayer structure and the concentric spheres until the particle size D50 of the particles grows to the target particle size, and stopping feeding to obtain a solution containing a precursor material; controlling the pH value of the reaction system to be 10.0-12.5, the ammonia value to be 2-20 g/L, the temperature to be 40-80 ℃ and the rotating speed to be 100-1000 rpm; the concentration of the hydrogen peroxide solution is 3-15%, and the flow rate of the hydrogen peroxide solution is 0.2-2L/h;
(3) And (3) aging, washing, drying, screening and deironing the solution containing the precursor material to obtain the high-nickel ternary positive electrode material precursor with the concentric sphere structure.
2. The method for preparing the high-nickel ternary cathode material precursor according to claim 1, wherein the method comprises the following steps: the total concentration of metal ions of the metal salt solution is 1-2.5 mol/L, the metal salt solution is an aqueous solution containing nickel salt, cobalt salt and manganese salt, and the introducing rate of the metal salt solution is 2-10L/h.
3. The method for preparing the high-nickel ternary cathode material precursor according to claim 1, wherein the method comprises the following steps: the metal salt solution comprises a nickel-cobalt salt solution and an aluminum salt solution, wherein the total concentration of metal ions in the nickel-cobalt salt solution is 1-2.5 mol/L, the concentration of aluminum in the aluminum salt solution is 0.05-0.3 mol/L, the introducing rate of the nickel-cobalt salt solution is 2-10L/h, and the introducing rate of the aluminum salt solution is 0.5-4L/h.
4. The method for preparing the high-nickel ternary cathode material precursor according to claim 1, wherein the method comprises the following steps: the inert shielding gas is nitrogen.
5. The method for preparing the high-nickel ternary cathode material precursor according to claim 1, wherein the method comprises the following steps: the precipitant solution is a sodium hydroxide solution with the mass concentration of 28-34%, and the complexing agent solution is an ammonia water solution with the mass concentration of 16-25%.
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