CN112002878A - Preparation method of ternary gradient material with manganese-rich surface layer - Google Patents
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Abstract
The invention discloses a preparation method of a ternary gradient material rich in manganese on the surface layer, which adopts a method of sequential precipitation to synthesize a precursor of a ternary cathode material rich in manganese on the surface layer, the process can control the appearance, the particle size, the sphericity and the particle dispersibility of a core-precursor, the ternary cathode material is obtained by adopting a secondary sintering method, and a shell with the concentration gradient of the manganese-rich surface layer can provide smooth transition of lithium ions and has higher specific capacity, better cycle performance and better thermal stability. The method can control the shape and the particle size of the material, is simple and controllable, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of new energy material preparation, and particularly relates to a preparation method of a ternary gradient material with a manganese-rich surface layer.
Background
As is well known, in the emerging high and new technology of the 2l century, the new energy technology is the first time to come, and the battery industry, as an important component in the technical field of new energy, occupies a great position in the global development of science and technology and economy. In the current battery industry, lithium ion batteries are more and more favored by consumers. The lithium ion battery has the advantages of high specific capacity, high energy density, high charging and discharging efficiency, good safety performance, long cycle life and the like. Electronic products in production and life of people are as small as watches, mobile phones, notebook computers and cameras and as large as electric bicycles and electric automobiles, and used batteries are lithium ion batteries or are evolved from the lithium ion batteries, so that the lithium ion battery has excellent market advantages and application prospects.
The anode material is an important component of the lithium ion battery and a key factor for restricting the energy density of the battery. The lithium ion battery anode material which is industrialized at present is LiCoO2The process is mature, the comprehensive performance is good, but the price is high, the toxicity is high, the safety performance is poor, and particularly, the material is unstable when overcharged, reacts with electrolyte and the like.
LiFePO4And LiMn2O4Materials as LiCoO2The substitute material of (2) can be produced at the same time. LiFePO4The high-performance lithium ion battery has excellent thermal stability and cycle performance, but the actual specific capacity is low (less than 150 mAh/g), the working voltage is low, the electronic conductivity is low, the rate capability is poor, and the improvement of the energy density of the battery is limited. LiMn2O4The cost is low, the safety is good, but the cycle performance, particularly the high-temperature cycle performance, is poor, the structure is unstable, and the ginger-Taylor effect occurs to cause the capacity to be sharply attenuated.
At present, the ternary cathode material nickel-cobalt-manganese (aluminum) oxide system has the advantages of low cost, high specific capacity, high voltage plateau and the like, and is concerned. However, the gelation of the electrode membrane is serious due to the nickel enrichment of the surface of the high-nickel ternary material, so that the performance is influenced by the deterioration of the material. And the low-nickel ternary material is more stable than a high-nickel ternary material and has better cycle performance. The electrochemical reaction is generated at the interface of electrode electrolyte, and the condition of material interface has very important influence on the performance, so the invention designs a concentration gradient material, namely a core-shell structure, and adopts a high-capacity high-nickel material as a core and a manganese-based material with a stable structure in a high lithium removal state as a shell. The shell with the manganese-rich surface layer concentration gradient can provide smooth transition of lithium ions, and has higher specific capacity and better cycle performance and thermal stability.
The conventional high-nickel ternary positive electrode material precursor is usually synthesized by adopting a coprecipitation method, ammonia water is used as a complexing agent, and sodium hydroxide is used as a precipitator, so that pure hydroxide precipitate is obtained. The ternary gradient material with rich manganese on the surface is prepared by mixing a low nickel solution and a high nickel solution by a method of sequential precipitation to form a ternary material precursor with concentration gradient, and coating a layer of ternary material with low nickel content on the surface of the material during sintering, so that the aims of avoiding gelation and improving the cycle performance and the stability performance of the material are fulfilled.
Disclosure of Invention
The invention aims to provide a preparation method of a ternary gradient material with a manganese-rich surface layer, which is used for improving the rate capability, the cycle performance and the stability of a ternary cathode material.
In order to achieve the above purpose, the solution of the invention is:
1) melting one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt into water, and adding one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt to form a high-nickel-concentration solution A;
2) melting one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt into water, and adding one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt to form a low-nickel-concentration solution B;
3) adding the low-nickel concentration solution into the high-nickel concentration solution at a certain rotating speed, stirring continuously, and adding the uniformly mixed metal ion solution into the reaction kettle at a certain rotating speed;
4) preparing ammonia water solution with a certain concentration, and marking the ammonia water solution as solution C, and preparing NaOH solution with a certain concentration, and marking the NaOH solution as solution D;
5) adding the solution C into the reaction kettle at a certain rotating speed; in the subsequent reaction process, the pH value of the system is adjusted to a fixed value, and the pH value is automatically controlled by the system through the addition of NaOH;
6) after the reaction is carried out for a certain time, taking out the gradient precursor solution for washing and suction filtration, and then drying at a certain temperature;
7) grinding and mixing the precursor and LiOH uniformly according to a certain proportion, carrying out secondary sintering in an oxygen atmosphere, presintering at low temperature, and then carrying out heat treatment in a high-temperature oxygen atmosphere to finally obtain the manganese-enriched ternary gradient material on the surface layer.
The nickel salt, iron salt, chromium salt, cobalt salt, magnesium salt, aluminum salt, zinc salt and manganese salt are one or more of sulfate, nitrate and chloride, the concentration of the high nickel metal salt solution is 1.0-4.0 mol/L, the concentration of the low nickel metal salt solution is 1.0-4.0 mol/L, the content of high nickel is 60-80%, and the content of low nickel is 20-30%.
The concentration of the ammonia water solution is 1-4 mol/L, and the concentration of the NaOH solution is 4-8 mol/L.
The synthesis process parameters are metal salt solution, alkaline aqueous solution and settling agent solution, the metal salt solution, the alkaline aqueous solution and the settling agent solution are continuously input into a vortex reaction kettle by a metering pump, and the PH value is controlled to be 11.0-12.5; the precipitation temperature is 50-90 ℃;
the stirring speed of the reaction kettle is 100-500 rpm, and the coprecipitation reaction time is 15-48 hours.
The mixing ratio of LiOH and the precursor is 1.01-1.1, the pre-sintering temperature is 400-550 ℃, the pre-sintering time is 3-5h, the high-temperature sintering temperature is 800-900 ℃, and the sintering time is 10-20 h.
The ternary cathode material adopts a high-capacity high-nickel material as a core and a manganese-based material with a stable structure in a high lithium removal state as a shell to form a concentration gradient material, namely the core-shell structure material, wherein the content of manganese on a section is increased from 12.857% to 17.227%, and the content of nickel on the section is decreased from 70.176% to 66.787%.
The ternary positive electrode material is spherical, D50 is 2-20 mu m, and tap density is more than or equal to 2.30 g/cm 3.
The invention has the advantages that: in a reaction kettle, a sequential precipitation technology is adopted to synthesize a ternary cathode material precursor with a manganese-rich NCM concentration gradient on the surface layer, the process can control the appearance, the particle size, the sphericity and the particle dispersibility of a core-precursor, the ternary cathode material is obtained by adopting a secondary sintering method, and a shell with the manganese-rich surface layer concentration gradient can provide smooth transition of lithium ions and has higher specific capacity, better cycle performance and better thermal stability.
The ternary cathode material disclosed by the invention has excellent stability, can improve the cycle stability of the ternary cathode material, and is beneficial to the industrialization process of power batteries. The method can control the shape and the particle size of the material, is simple and controllable, and is suitable for industrial production.
Drawings
FIG. 1 is a flow chart of a precursor preparation method in example 1 of the present invention.
Fig. 2 is a cross-sectional element distribution diagram of the NCM811 concentration gradient ternary cathode material provided in example 1 of the present invention.
FIG. 3 is a scanning electron microscope image of a ternary cathode material having a concentration gradient of NCM811 according to example 1 of the present invention.
Detailed Description
Example 1
Mixing NiSO4，CoSO4，Mn2(SO4)3According to the molar ratio of Ni: co: mn = 8: 1:1 proportion preparing nickel-cobalt-manganese mixed aqueous solution with the concentration of 1.5 mol/L, preparing 1.5 mol/L NCM111 metal ion solution, preparing 1.8mol/L ammonia water solution, preparing 4.0mol/L sodium hydroxide solution, adding the 111 solution into the 811 solution at the speed of 400 rpm, stirring continuously, and mixing uniformlyThe homogeneous metal ion solution was added to the reaction vessel at a rate of 800 rpm, while the aqueous ammonia solution was added at a rate of 800 rpm. In the subsequent reaction process, the pH value of the system is adjusted to 11.2, and the pH value is automatically controlled by the system through the addition of NaOH. After the reaction is continued for 25 hours, the gradient precursor solution is taken out for washing and suction filtration, and then the solution is dried at the temperature of 80 ℃. Grinding and uniformly mixing the precursor and excess LiOH according to the ratio of 1:1.08, presintering at 550 ℃ for 4 h, and then performing heat treatment at 820 ℃ for 12 h in an oxygen atmosphere to obtain the manganese-enriched ternary gradient material on the surface of the product.
Table 1 shows the element contents of the NCM811 concentration gradient ternary cathode material provided in example 1 of the present invention.
| r(μm) | Ni% | Co% | Mn% |
| 0 | 70.176 | 16.967 | 12.857 |
| 1.5 | 70.945 | 14.529 | 14.517 |
| 2.5 | 72.203 | 14.188 | 13.609 |
| 3.5 | 72.264 | 12.625 | 15.111 |
| 4.2 | 70.232 | 15.468 | 14.299 |
| 4.5 | 70.052 | 13.316 | 16.632 |
| 5.0 | 69.176 | 16.348 | 14.475 |
| 5.5 | 66.860 | 16.884 | 16.255 |
| 6.0 | 66.787 | 15.986 | 17.227 |
Example 2
Mixing NiSO4，CoSO4，Mn2(SO4)3According to the molar ratio of Ni: co: mn = 8: 1:1 proportion preparing nickel-cobalt-manganese mixed water solution with the concentration of 1.5 mol/L and preparing 1.5 mol/L NCM111 metal ion solution, preparing ammonia water solution with the concentration of 1.8mol/L, preparing sodium hydroxide solution with the concentration of 4.0mol/L, adding 111 solution into 811 solution at the speed of 400 rpm, stirring continuously, adding the uniformly mixed metal ion solution into a reaction kettle at the speed of 800 rpm, and simultaneously adding the ammonia water solution at the speed of 800 rpm. In the subsequent reaction process, the pH value of the system is adjusted to 11.2, and the pH value is automatically controlled by the system through the addition of NaOH. After the reaction is continued for 15 hours, the gradient precursor solution is taken out for washing and suction filtration, and then the solution is dried at the temperature of 80 ℃. Grinding and uniformly mixing the precursor and excess LiOH according to the ratio of 1:1.08, presintering at 550 ℃ for 4 h, and then performing heat treatment at 820 ℃ for 12 h in an oxygen atmosphere to obtain the manganese-enriched ternary gradient material on the surface of the product.
Example 3
Mixing NiSO4，CoSO4，Mn2(SO4)3According to the molar ratio of Ni: co: mn = 8: 1:1 proportion preparing nickel-cobalt-manganese mixed aqueous solution, the concentration is 1.5 mol/L, simultaneously preparing 1.5 mol/L NCM111 metal ion solution, preparing 1.8mol/L ammonia water solution, preparing 4.0mol/L sodium hydroxide solution, adding the 111 solution into the 811 solution at the speed of 400 rpm, stirring continuously, adding the uniformly mixed metal ion solution into a reaction kettle at the speed of 800 rpm, and simultaneously adding the ammonia water solution at the speed of 800 rpm. In the subsequent reaction process, the pH value of the system is adjusted to 11.2, and the pH value is automatically controlled by the system through the addition of NaOH. After the reaction is continued for 25 hours, the gradient precursor solution is taken out for washing and suction filtration, and then the solution is dried at the temperature of 80 ℃. Grinding and uniformly mixing the precursor and excess LiOH according to the ratio of 1:1.08, presintering at 550 ℃ for 4 h, and then performing heat treatment at 820 ℃ for 12 h in an oxygen atmosphere to obtain the manganese-enriched ternary gradient material on the surface of the product.
Example 4
Mixing NiSO4，CoSO4，Mn2(SO4)3According to the molar ratio of Ni: co: mn = 8: 1:1 proportion preparing nickel-cobalt-manganese mixed aqueous solution with the concentration of 1.5 mol/L, and preparing 1.5 mol/L NCM111 metal ion solution with the concentration of 1.8mol/LAnd (2) preparing an ammonia water solution, namely preparing a sodium hydroxide solution with the concentration of 4.0mol/L, adding the 111 solution into the 811 solution at the speed of 400 rpm, stirring continuously, adding the uniformly mixed metal ion solution into the reaction kettle at the speed of 800 rpm, and simultaneously adding the ammonia water solution at the speed of 800 rpm. In the subsequent reaction process, the pH value of the system is adjusted to 11.2, and the pH value is automatically controlled by the system through the addition of NaOH. And after the reaction is continued for 48 hours, taking out the gradient precursor solution, washing, carrying out suction filtration, and then drying at the temperature of 80 ℃. Grinding and uniformly mixing the precursor and excess LiOH according to the ratio of 1:1.08, presintering at 550 ℃ for 4 h, and then performing heat treatment at 820 ℃ for 12 h in an oxygen atmosphere to obtain the manganese-enriched ternary gradient material on the surface of the product.
Claims (8)
1. A surface manganese-rich ternary gradient material is characterized in that: the ternary positive electrode material precursor is a concentration gradient ternary material precursor rich in manganese on the surface layer, and is microscopically in a microsphere shape assembled by nano wires, the ternary positive electrode material is a concentration gradient ternary positive electrode material rich in manganese on the surface layer, and is microscopically in a microsphere shape assembled by nano particles.
2. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: comprises the following steps of (a) carrying out,
1) melting one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt into water, and adding one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt to form a high-nickel-concentration solution A;
2) melting one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt into water, and adding one or more than two of soluble nickel salt, soluble ferric salt, soluble zinc salt, soluble manganese salt, soluble cobalt salt, soluble magnesium salt, soluble aluminum salt and soluble chromium salt to form a low-nickel-concentration solution B;
3) adding the low-nickel concentration solution into the high-nickel concentration solution at a certain rotating speed, stirring continuously, and adding the uniformly mixed metal ion solution into the reaction kettle at a certain rotating speed;
4) preparing ammonia water solution with a certain concentration, and marking the ammonia water solution as solution C, and preparing NaOH solution with a certain concentration, and marking the NaOH solution as solution D;
5) adding the solution C into the reaction kettle at a certain rotating speed; in the subsequent reaction process, the pH value of the system is adjusted to a fixed value, and the pH value is automatically controlled by the system through the addition of NaOH;
6) after the reaction is carried out for a certain time, taking out the gradient precursor solution for washing and suction filtration, and then drying at a certain temperature;
7) grinding and mixing the precursor and LiOH uniformly according to a certain proportion, carrying out secondary sintering in an oxygen atmosphere, presintering at low temperature, and then carrying out heat treatment in a high-temperature oxygen atmosphere to finally obtain the manganese-enriched ternary gradient material on the surface layer.
3. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein:
the nickel salt, iron salt, chromium salt, cobalt salt, magnesium salt, aluminum salt, zinc salt and manganese salt are one or more of sulfate, nitrate and chloride, the concentration of the high nickel metal salt solution is 1.0-4.0 mol/L, the concentration of the low nickel metal salt solution is 1.0-4.0 mol/L, the content of high nickel is 60-80%, and the content of low nickel is 20-30%.
4. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: the concentration of the ammonia water solution is 1-4 mol/L, and the concentration of the NaOH solution is 4-8 mol/L.
5. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: the synthesis process parameters are metal salt solution, alkaline aqueous solution and settling agent solution, the metal salt solution, the alkaline aqueous solution and the settling agent solution are continuously input into a vortex reaction kettle by a metering pump, and the PH value is controlled to be 11.0-12.5; the precipitation temperature is 50-90 ℃;
the method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: the stirring speed of the reaction kettle is 100-500 rpm, and the coprecipitation reaction time is 15-48 hours.
6. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: the mixing ratio of LiOH and the precursor is 1.01-1.1, the pre-sintering temperature is 400-550 ℃, the pre-sintering time is 3-5h, the high-temperature sintering temperature is 800-900 ℃, and the sintering time is 10-20 h.
7. The method for preparing the surface manganese-rich ternary gradient material of claim 1, wherein: the ternary cathode material adopts a high-capacity high-nickel material as a core and a manganese-based material with a stable structure in a high lithium removal state as a shell to form a concentration gradient material, namely the core-shell structure material, wherein the content of manganese on a section is increased from 12.857% to 17.227%, and the content of nickel on the section is decreased from 70.176% to 66.787%.
8. The method for preparing a precursor of a ternary cathode material having an LTH structure as defined in claim 1, wherein: the ternary positive electrode material is spherical-like, D50 is 2-20 mu m, and tap density is more than or equal to 2.30 g/cm3。
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