CN114583141A - Precursor material with three-layer structure, preparation method thereof and anode material - Google Patents
Precursor material with three-layer structure, preparation method thereof and anode material Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion battery materials, and discloses a precursor material with a three-layer structure and a preparation method thereof. The preparation method of the precursor is simple and easy to control, equipment and a field are not increased, and the cycle performance of the battery containing the anode material is greatly improved after the obtained precursor material is baked into the anode material.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a precursor material and a preparation method thereof.
Background
Among the advanced cathode materials, nickel-rich layered transition metal oxide has been one of the best choices for cathode materials for electric vehicles due to its superior energy density and green and pollution-free characteristics. However, the practical capacity of many commercial nickel-rich anodes is still limited to 200 mAhg-1In order to overcome the limitation, increasing the content of Ni in the material is a good way to improve the capacity of the material; meanwhile, Co plays an important role in the ternary material, so that the material is ensured to have a longer cycle life, but the price of Co is always high, and the production cost of the ternary material is increased.
To address these issues, increasing the Ni content in the material while reducing the use of Co is a common strategy. While materials with higher Ni content exhibit faster chemical-mechanical degradation during charge and discharge cycles, such as microcracking of secondary particles, resulting in poor battery cycling stability. Therefore, it remains a challenge to prepare high nickel anodes with good cycling stability.
Disclosure of Invention
In view of the problems in the prior art, it is an object of the present invention to provide a precursor material with a three-layer structure, in which the primary particles of the precursor have a sheet-like structure and the secondary particles have a complete round shape.
The second purpose of the invention is to provide a preparation method of the precursor material with a three-layer structure.
The invention also aims to provide a positive electrode material.
In order to achieve the above object, the present invention provides the following technical solutions.
The precursor material comprises an inner core, an intermediate layer and a shell, wherein the inner core and the intermediate layer are both cobalt-doped nickel hydroxide, the shell is nickel-cobalt-manganese hydroxide, the content of nickel in the inner core, the intermediate layer and the shell is consistent, the content of cobalt in the inner core, the intermediate layer and the shell is inconsistent, and the cobalt content in the intermediate layer is higher than that of the inner core.
Preferably, the particle size of the inner core of the precursor material is 1/4-1/3 of the particle size of the precursor material; the size of particles formed by the inner core and the middle layer of the precursor material is 1/2-2/3 of the size of the particles of the precursor material.
Preferably, the molar percentage of nickel in the precursor material is not less than 60%, the molar percentage of cobalt is not more than 10%, and the molar percentage of manganese is not more than 30%.
A preparation method of a precursor material with a three-layer structure comprises the following steps:
step S1, preparing a nickel salt solution, a manganese salt solution and a cobalt salt solution; preparing a precipitator solution and a complexing agent solution;
step S2, preparing a reaction kettle bottom solution;
step S3, adding a nickel salt solution, a cobalt salt solution, a precipitator solution and a complexing agent solution into the bottom liquid of the reaction kettle in a parallel flow manner to perform a one-stage coprecipitation reaction until the particle size D50 of the reaction slurry is 1/4-1/3 of the target particle size D50 value of the precursor material;
step S4, after the first-stage coprecipitation reaction is finished, adding a nickel salt solution, a cobalt salt solution, a precipitator solution and a complexing agent solution in a parallel flow manner to perform a second-stage coprecipitation reaction until the particle size D50 of the reaction slurry is 1/2-2/3 of the target particle size D50 value of the precursor material;
step S5, after the two-stage coprecipitation reaction is finished, adding a nickel salt solution, a cobalt salt solution, a manganese salt solution, a precipitator solution and a complexing agent solution in a parallel flow manner to carry out the three-stage coprecipitation reaction until the granularity D50 of the reaction slurry reaches the target granularity D50 value of the precursor material, and stopping the reaction;
step S6, carrying out solid-liquid separation on the reaction slurry to obtain a solid phase, washing and drying the solid phase to obtain a precursor material with a three-layer structure;
wherein, the total molar weight of the nickel element added into the reaction kettle in the steps S3, S4 and S5 is kept consistent, and the total molar weight of the cobalt element added into the reaction kettle is different; the total molar amount of the cobalt element added in the step S4 is greater than the total molar amount of the cobalt element added in the step S3; and controlling the pH value of a reaction system in the coprecipitation reaction process of the steps S3, S4 and S5 to be 10-12.5 and the ammonia concentration to be 6-10 g/L.
Preferably, the concentration of nickel in the nickel salt solution is 4-8 mol/L; the manganese concentration of the manganese salt solution is 3-6 mol/L; the concentration of cobalt in the cobalt salt solution is 1-5 mol/L.
Preferably, the coprecipitation reactions of the steps S3, S4 and S5 are performed for the same time, the flow rates of the nickel salt solutions are kept consistent, and the flow rates of the cobalt salt solutions are different; the flow rate of the cobalt salt solution in step S4 is greater than the flow rate of the cobalt salt solution in step S3.
Preferably, the precipitator is NaOH, and the concentration of the precipitator solution is 4-8 mol/L; the complexing agent solution is an ammonia water solution, and the concentration of the complexing agent solution is 3-6 mol/L.
Preferably, the pH value of the reaction kettle bottom liquid is 10-12.5, and the ammonia concentration is 6-10 g/L.
In the process of coprecipitation reaction, the flow rate of the raw material salt can be designed according to the total content of each element in the designed precursor material, the molar concentration of the raw material salt and the time of coprecipitation reaction needed by obtaining the precursor material with the target particle size according to experience.
Preferably, the target particle size D50 value of the precursor material is 3-7 μm.
The anode material is prepared by mixing and sintering the precursor material with the three-layer structure or the precursor material with the three-layer structure prepared by the preparation method.
Compared with the prior art, the invention has the most important beneficial effects that:
the primary particles of the precursor are of a sheet structure, and the secondary particles are complete and round; the use of Co is well controlled, and the theoretical capacity is high; the preparation method of the precursor provided by the invention is simple and easy to operate and control, equipment and field are not increased, and the cycle performance of the battery containing the anode material is greatly improved after the obtained precursor material is baked into the anode material.
Drawings
FIG. 1 is an SEM image of a positive electrode precursor obtained in example 1 of the present invention;
FIG. 2 is an SEM image of a positive electrode precursor obtained in comparative example 1 of the present invention;
FIG. 3 is an SEM image of a positive electrode precursor obtained in comparative example 2 of the present invention;
FIG. 4 is an SEM image of a positive electrode precursor obtained in comparative example 3 of the present invention;
FIG. 5 is a graph showing cycle performance of the batteries obtained in example 1 and comparative examples 1 to 4.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific embodiments, wherein only some, but not all embodiments of the invention are described, and the embodiments should not be construed as limiting the scope of the claims of the present application. All other changes and modifications which can be made by one skilled in the art based on the embodiments of the present invention without inventive faculty are within the scope of the claims of the present application.
Example 1
The chemical general formula of the precursor material is designed to be Ni0.99Co0.01(OH)2@Ni0.98Co0.02(OH)2@Ni0.8Co0.05Mn0.15(OH)2The precursor material comprises an inner core, an intermediate layer and a shell, wherein the inner core and the intermediate layer are both cobalt-doped nickel hydroxide, the shell is nickel-cobalt-manganese hydroxide, the content of nickel in the inner core, the intermediate layer and the shell is consistent, and the cobalt content in the intermediate layer is higher than that of the inner core.
The preparation of the precursor designed above is realized by the following steps:
preparing a nickel sulfate solution with the nickel concentration of 5mol/L, a manganese sulfate solution with the manganese concentration of 5mol/L and a cobalt sulfate solution with the cobalt concentration of 5 mol/L; preparing 4mol/L NaOH solution; preparing 4mol/L ammonia water solution.
Regulating and controlling the pH value of the bottom liquid of the reaction kettle to be 11.5 and the ammonia concentration to be 9 g/L.
Controlling the pH value of a reaction system to be 11.5 and the ammonia concentration to be 9g/L in the coprecipitation reaction process, and specifically:
adding a nickel sulfate solution, a cobalt sulfate solution, a precipitator solution and a complexing agent solution into the bottom liquid of the reaction kettle in a parallel flow manner to perform a one-stage coprecipitation reaction for 4 hours until the granularity D50 of the reaction slurry reaches 1-2 mu m, wherein the flow rate of the nickel sulfate solution is fixed to be 300L/h, and the flow rate of the cobalt sulfate solution is 3.03L/h;
after the first-stage coprecipitation reaction is finished, adding a nickel sulfate solution, a cobalt salt solution, a precipitator solution and a complexing agent solution in parallel for carrying out second-stage coprecipitation reaction for 4 hours until the granularity D50 of the reaction slurry reaches 2-3 mu m, wherein the flow rate of the nickel sulfate solution is fixed to be 300L/h, and the flow rate of the cobalt sulfate solution is adjusted to be 6.12L/h;
after the two-stage coprecipitation reaction is finished, adding a nickel salt solution, a cobalt salt solution, a manganese salt solution, a precipitator solution and a complexing agent solution in a parallel flow manner to perform three-stage coprecipitation reaction for 4 hours, wherein the flow rate of a nickel sulfate solution is fixed to be 300L/h, the flow rate of a cobalt sulfate solution is adjusted to be 18.75L/h, and the flow rate of a manganese sulfate solution is 56.18L/h;
after the reaction is carried out for 12 hours, the granularity D50 of the reaction slurry reaches 3-7 mu m, and the reaction is stopped.
And filtering the reaction slurry, washing the solid phase, and drying the solid phase to obtain the precursor material.
An SEM image of the precursor material prepared in the embodiment is shown in FIG. 1, the particle surface has no cracks, and the particle size is 3-7 μm.
Precursor material and LiOH in a ratio of 1: 1.05, and sintering at 830 ℃ for 10 hours to obtain the cathode material.
Comparative example 1
Comparative example 1 differs from example 1 only in that: in the first stage of coprecipitation reaction, a cobalt sulfate solution is not required to be added; finally obtaining ternary positive electrode precursor Ni (OH)2@Ni0.98Co0.02(OH)2@Ni0.8Co0.05Mn0.15(OH)2。
An SEM image of the precursor obtained in the comparative example is shown in FIG. 2, the particle surface has no cracks, the particle size is 3-7 μm, and the appearance of the primary particles is different from that of the precursor obtained in example 1.
Mixing a precursor material with LiOH in a ratio of 1: 1.05, and sintering at 830 ℃ for 10 hours to obtain the cathode material.
Comparative example 2
Comparative example 2 differs from example 1 only in that: in the two-stage coprecipitation reaction, a cobalt sulfate solution is not added; finally obtaining ternary positive precursor Ni0.99Co0.01(OH)2@Ni(OH)2@Ni0.8Co0.05Mn0.15(OH)2。
An SEM image of the precursor obtained in the comparative example is shown in FIG. 3, the particle surface has no cracks, the particle size is 3-7 μm, and the appearance of the primary particles is different from that of the precursor obtained in example 1.
Mixing a precursor material with LiOH in a ratio of 1: 1.05, and sintering at 830 ℃ for 10 hours to obtain the cathode material.
Comparative example 3
Comparative example 3 differs from example 1 only in that: cobalt sulfate solution is not added in the first-stage coprecipitation reaction and the second-stage coprecipitation reaction; finally obtaining ternary positive electrode precursor Ni (OH)2@Ni0.8Co0.05Mn0.15(OH)2。
The SEM image of the precursor obtained in the comparative example is shown in FIG. 4, the particle surface has no cracks, the particle size is 3-7 μm, and the morphology of the primary particles is different from that of the precursor in example 1.
Mixing a precursor material with LiOH in a ratio of 1: 1.05, and sintering at 830 ℃ for 10 hours to obtain the cathode material.
Comparative example 4
Comparative example 4 differs from example 1 only in that: cobalt sulfate solution is added in the first stage coprecipitation reaction, the second stage coprecipitation reaction and the third stage coprecipitation reaction, and the flow rate of the cobalt sulfate solution is kept consistent; finally obtaining the ternary anode precursor with the chemical formula of Ni0.95Co0.05(OH)2@Ni0.8Co0.05Mn0.15(OH)2。
Mixing a precursor material with LiOH in a ratio of 1: 1.05, and sintering at 830 ℃ for 10 hours to obtain the cathode material.
The positive electrode materials obtained in example 1 and comparative examples 1 to 4 were assembled into button cells in the same manner as button cells were assembled conventionally in the art. The cycling performance of the button cell batteries was tested, and the first discharge gram capacities of the batteries of the positive electrode materials of example 1 and comparative examples 1 to 3 were 202, 185.4, 194 and 186.5189.6 mAh/g at 2.75-4.6V and 1C, respectively, as shown in FIG. 5. The circulation is performed for 100 circles at 1C, the capacities are 190.9, 143.1, 140.6 and 142.8165.8 mAh/g respectively, and the capacity retention rates are 94.5%, 77.2%, 72.5%, 76.6% and 87.4% respectively; the result proves that the cycle performance of the battery of the cathode material obtained by the invention is greatly improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The precursor material is characterized by comprising an inner core, an intermediate layer and a shell, wherein the inner core and the intermediate layer are both cobalt-doped nickel hydroxide, the shell is nickel-cobalt-manganese hydroxide, the content of nickel in the inner core, the content of nickel in the intermediate layer and the content of cobalt in the shell are consistent, the content of cobalt in the inner core, the content of cobalt in the intermediate layer and the content of cobalt in the shell are inconsistent, and the content of cobalt in the intermediate layer is higher than the content of cobalt in the inner core.
2. The precursor material of the three-layer structure according to claim 1, wherein the particle size of the inner core of the precursor material is 1/4-1/3 of the particle size of the precursor material; the size of particles formed by the inner core and the middle layer of the precursor material is 1/2-2/3 of the size of the particles of the precursor material.
3. The precursor material of three-layer structure according to claim 1 or 2, wherein the precursor material has a nickel content of not less than 60 mol%, a cobalt content of not more than 10 mol% and a manganese content of not more than 30 mol%.
4. A preparation method of a precursor material with a three-layer structure is characterized by comprising the following steps:
step S1, preparing a nickel salt solution, a manganese salt solution and a cobalt salt solution; preparing a precipitator solution and a complexing agent solution;
step S2, preparing a reaction kettle bottom liquid;
step S3, adding a nickel salt solution, a cobalt salt solution, a precipitator solution and a complexing agent solution into the bottom liquid of the reaction kettle in a parallel flow manner to perform a one-stage coprecipitation reaction until the particle size D50 of the reaction slurry is 1/4-1/3 of the target particle size D50 value of the precursor material;
step S4, after the first-stage coprecipitation reaction is finished, adding a nickel salt solution, a cobalt salt solution, a precipitator solution and a complexing agent solution in a parallel flow manner to perform a second-stage coprecipitation reaction until the particle size D50 of the reaction slurry is 1/2-2/3 of the target particle size D50 value of the precursor material;
step S5, after the two-stage coprecipitation reaction is finished, adding a nickel salt solution, a cobalt salt solution, a manganese salt solution, a precipitator solution and a complexing agent solution in a parallel flow manner to carry out the three-stage coprecipitation reaction until the granularity D50 of the reaction slurry reaches the target granularity D50 value of the precursor material, and stopping the reaction;
step S6, carrying out solid-liquid separation on the reaction slurry to obtain a solid phase, washing and drying the solid phase to obtain a precursor material with a three-layer structure;
wherein, the total molar weight of the nickel element added into the reaction kettle in the steps S3, S4 and S5 is kept consistent, and the total molar weight of the cobalt element added into the reaction kettle is different; the total molar amount of the cobalt element added in the step S4 is greater than the total molar amount of the cobalt element added in the step S3; and controlling the pH value of a reaction system in the coprecipitation reaction process of the steps S3, S4 and S5 to be 10-12.5 and the ammonia concentration to be 6-10 g/L.
5. The preparation method according to claim 4, wherein the concentration of nickel in the nickel salt solution is 4 to 8 mol/L; the manganese concentration of the manganese salt solution is 3-6 mol/L; the concentration of cobalt in the cobalt salt solution is 1-5 mol/L.
6. The method of claim 4, wherein the coprecipitation reactions of the steps S3, S4 and S5 are performed for the same time, the flow rates of the nickel salt solutions are kept consistent, and the flow rates of the cobalt salt solutions are different; the flow rate of the cobalt salt solution in step S4 is greater than the flow rate of the cobalt salt solution in step S3.
7. The preparation method according to claim 4, wherein the precipitant is NaOH, and the concentration of the precipitant solution is 4-8 mol/L; the complexing agent solution is an ammonia water solution, and the concentration of the complexing agent solution is 3-6 mol/L.
8. The method according to claim 4, wherein the reaction kettle bottom solution has a pH of 10 to 12.5 and an ammonia concentration of 6 to 10 g/L.
9. The method of claim 4, wherein the precursor material has a target particle size D50 value of 3 to 7 μm.
10. A positive electrode material, characterized by being obtained by lithium-mixed sintering of the precursor material having a three-layer structure according to any one of claims 1 to 3 or the precursor material having a three-layer structure prepared by the preparation method according to any one of claims 4 to 9.
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| CN115215389A (en) * | 2022-09-05 | 2022-10-21 | 中南大学 | Composite modified precursor, positive electrode material and preparation method of composite modified precursor |
| CN115403074A (en) * | 2022-09-26 | 2022-11-29 | 湘潭大学 | High-nickel cobalt lithium manganate precursor and preparation method thereof |
| WO2023193826A1 (en) * | 2022-06-30 | 2023-10-12 | 北京当升材料科技股份有限公司 | Positive electrode material, preparation method therefor, and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023193826A1 (en) * | 2022-06-30 | 2023-10-12 | 北京当升材料科技股份有限公司 | Positive electrode material, preparation method therefor, and application thereof |
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| CN115215389B (en) * | 2022-09-05 | 2023-04-07 | 中南大学 | Composite modified precursor, positive electrode material and preparation method of composite modified precursor |
| CN115403074A (en) * | 2022-09-26 | 2022-11-29 | 湘潭大学 | High-nickel cobalt lithium manganate precursor and preparation method thereof |
| CN115403074B (en) * | 2022-09-26 | 2024-05-17 | 湘潭大学 | High-nickel type nickel cobalt lithium manganate precursor and preparation method thereof |
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| CN114583141B (en) | 2022-08-23 |
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