CN112133904A - High-nickel ternary cathode material of lithium ion battery and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-nickel ternary cathode material of a lithium ion battery and a preparation method thereof, wherein the preparation method comprises the following steps: s1, uniformly mixing the ternary precursor with lithium hydroxide, and sintering in an atmosphere furnace to obtain a product S1; s2, mixing S1 with water according to the weight ratio of 1:1-2, washing, adding 0.2-2 wt% of corrosion inhibitor, washing for 0.1-2h at the rotation speed of 200-; s3, mixing the S2 with an oxide with the weight percent of less than 1%, and then carrying out secondary sintering in an atmosphere furnace to obtain a product S3. The invention can avoid the damage to the matrix material, reduce the mixed arrangement degree of lithium and nickel, form a film on the surface layer of the matrix, and generate a fast ion conductor layer in the process of secondary sintering to prevent the electrolyte from corroding the anode material, thereby being beneficial to obtaining the anode material with high cycle performance and high capacity.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a high-nickel ternary anode material for a lithium ion battery and a preparation method thereof.
Background
Since sony corporation introduced the commercialization of lithium ion batteries in 1991, the lithium ion battery technology has been rapidly developed in the aspects of 3C, power vehicles, electric tools, energy storage, etc., and it is only counted that the global shipment of lithium ion power vehicles in 2019 is 220 thousands, and the battery loading is 115.2 GW. The global shipment of the ternary material as the anode material is more than 34 ten thousand tons, wherein the shipment of the Chinese ternary material is about 19 ten thousand tons, and accounts for 56 percent; the high-nickel ternary alloy has the advantage of high specific capacity, the gram capacity is more than 200mAh/g, and due to the high capacity ratio, the high safety is applied to the field of power automobiles on a large scale, and particularly is widely applied to new energy vehicles with high endurance mileage.
However, in general, the molar ratio of Li/Me is greater than 1 in the design of the raw material proportioning process for preparing the high-nickel ternary material, so that partial lithium salt exists on the surface of the lithium ion high-nickel ternary positive electrode material, and therefore, the content of the lithium salt on the surface of the material is often required to be controlled in the process of large-scale mass production, otherwise, a large amount of gas is generated in the process of side reaction between an active substance and an electrolyte when the prepared battery is used, and the battery is bulged, and has great potential safety hazard. In the process of preparing the high-nickel ternary material, because the amount of carbonate on the surface is controlled, a washing process is generally carried out to remove the redundant carbonate on the surface of the positive electrode material.
For example, chinese patent document CN108023078A, patent No. CN201711242826.9, patent name: the patent document mentions that a base material is mixed with a detergent, then dried and then coated with a coating agent.
For example, journal article Xu Shiguo etc. the effects of washing on LiNi0.83Co0.12Mn0.05O2cathode materials, Solid State Ionics 2019,334,110-0.83Co0.12Mn0.05O2Influence of the cathode material, solid-state ionization 2019,334,110-115) mentions that the substrate material has side reactions, oxide and gas phase generation during the water washing process, and has influence on the microstructure and performance of the substrate material.
In summary, the prior art employs washing to reduce the content of surface carbonate in the process of processing the high nickel ternary material, but as mentioned in the above documents, the method is also accompanied by side reactions, which damage the matrix material, increase the degree of lithium-nickel mixing, and adversely affect the capacity and cycle performance of the battery in the subsequent battery preparation process.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a high-nickel ternary cathode material for a lithium ion battery and a method for preparing the same, which can avoid damage to a substrate material, reduce the degree of lithium-nickel mixing, and form a film on the surface of the substrate, so that a fast ion conductor layer can be generated during a secondary sintering process, thereby preventing the corrosion of the electrolyte to the cathode material, and facilitating obtaining of a high-cycle performance and high-capacity cathode material.
The adopted technical scheme is as follows:
the invention relates to a preparation method of a high-nickel ternary cathode material of a lithium ion battery, which comprises the following steps of:
s1. ternary precursor NixCoyMnz(OH)2Wherein x is more than or equal to 0.8, x + y + Z is 1, the molar ratio of Li to Me is 1-1.1, and Me is the sum of Ni, Co and Mn; uniformly mixing the ternary precursor with lithium hydroxide, and performing primary sintering in an atmosphere furnace, wherein the sintering temperature is 750-850 ℃, the sintering time is 1-15h, and the atmosphere is oxygen, so that a product obtained after the primary sintering is S1;
s2, mixing S1 with water according to the weight ratio of 1:1-2, washing, adding 0.2-2 wt% of corrosion inhibitor, drying at the temperature of 110-;
s3, mixing the S2 with an oxide with the weight percent below 1 percent, and then carrying out secondary sintering in an atmosphere furnace, wherein the sintering temperature is 300-650 ℃, and the sintering time is 1-5h, so as to obtain a product S3, namely the high-nickel ternary cathode material of the lithium ion battery.
Preferably, in step S2, the corrosion inhibitor is one or more of sodium tungstate, ammonium tungstate, and sodium borate.
Preferably, in step S3, the oxide is one or both of aluminum oxide and boron oxide.
Preferably, in the step S2, the rotation speed is 500-1000r/min, and the product S2 is obtained by drying the product at 120 ℃ for 6-12h after being dried by a centrifugal machine.
The invention relates to a high-nickel ternary cathode material for a lithium ion battery, which is prepared by the preparation method in any scheme.
The invention has the beneficial effects that:
the invention mainly adds a proper amount of corrosion inhibitor when the washing process for reducing the residual lithium on the surface is carried out on the high-nickel ternary solution, reduces the side reaction in the washing process, forms a layer of protective film, reduces the mixed discharging of lithium and nickel, and generates a fast ion conductor layer in the process of secondary burning to prevent the electrolyte from corroding the anode material, thereby being beneficial to obtaining the anode material with high cycle performance and high capacity. The corrosion inhibitor is mainly and preferably one or more of tungstate and borate, and the content is 0.2-2 wt%; preferably ammonium tungstate, sodium borate or several. The corrosion inhibitor has the main functions that ions in the corrosion inhibitor are coated on the surface of positive material particles in the washing process of the positive material to prevent water from reacting with the material, and a proper amount of tungstate and borate can react with lithium salt on the surface of the material to generate a fast ion conductor without other impurity phases in the secondary sintering process.
Therefore, the invention can avoid the damage to the matrix material, reduce the mixed arrangement degree of lithium and nickel, form a film on the surface layer of the matrix, generate a fast ion conductor layer in the secondary sintering process, prevent the electrolyte from corroding the anode material, and is beneficial to obtaining the anode material with high cycle performance and high capacity.
For the resulting high nickel ternary positive electrode materials, e.g. LiNi0.82Co0.12Mn0.06O2The capacity of the high-efficiency high-. .
Drawings
The following brief description of the drawings is provided:
figure 1 is the XRD pattern of the S3 sample of example 1. The ordinate intensity in the figure is intensity.
Fig. 2 is an XRD pattern of the sample of S3 in comparative example 1. The ordinate intensity in the figure is intensity.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the use and purpose of these exemplary embodiments are merely to exemplify the present invention, and do not set forth any limitation on the actual scope of the present invention in any form, and the scope of the present invention is not limited thereto.
Example 1
A preparation method of a high-nickel ternary cathode material of a lithium ion battery comprises the following steps:
selecting a commercial ternary precursor Ni0.82Co0.12Mn0.06(OH)2Uniformly mixing the precursor with lithium hydroxide according to the Li/Me molar ratio of 1.1, wherein Me is Ni + Co + Mn, and performing primary sintering in an atmosphere furnace at 800 ℃ for 10 hours in the presence of oxygen to obtain a product obtained after the primary sintering, namely S1;
mixing S1 with water according to the weight ratio of 1:2, washing, adding 0.5 wt% of ammonium tungstate, washing for 0.5h at the rotating speed of 500r/min, drying at 120 ℃ for 6h after spin-drying by a centrifugal machine to obtain a product S2;
mixing S2 with 0.2 wt% of alumina and 0.3 wt% of boron oxide, and then carrying out secondary sintering in an atmosphere furnace, wherein the sintering temperature is 350 ℃, and the sintering time is 5 hours, so as to obtain a product S3, namely the high-nickel ternary cathode material for the lithium ion battery.
Microstructure analysis of S3 is carried out as shown in FIG. 1, an XRD spectrum shows that a S3 sample belongs to a hexagonal system, has a typical alpha-NaFeO 2 layered structure, a space group is R-3m, a diffraction peak is sharp, high crystallinity is achieved, and cell parameters obtained by Topas refinement software refinement are shown in Table 1.
TABLE 1
| Sample (I) | Cell parameter a (nm) | Cell parameter c | c/a | Lithium-nickel mixed bar |
| EXAMPLE 1 sample S3 | 0.28709 | 1.42000 | 4.946 | 0.025 |
| Comparative example 1 sample S3 | 0.28708 | 1.41955 | 4.945 | 0.027 |
Half-cells were prepared using S3, as per w (ternary material sample): w (conductive carbon): w (pvdf) 80: 10:10, preparing positive electrode slurry of the button test battery, using flat and clean aluminum foil as a positive electrode current collector of the battery, using a flat and clean lithium sheet (stored in an argon glove box) as a negative electrode, and using LiPF with 1.0mol/L electrolyte6(PC: EC: DMC: 10: 30: 60, volume ratio). Assembling the CR2430 button cell must be completed in an argon-filled glove box, and H in the glove box2O and O2Mass fraction is less than 10-7. After the button cell is assembled, the button cell is kept still in the glove box for 60min, and then the charge and discharge properties of the button cell are tested on a LANCET 2001 cell test system under the test conditions that the charge and discharge current is 0.1C (20mA) at normal temperature and the voltage interval is 2.5-4.25V. And carrying out electrochemical performance test on the half-cell. The test results are shown in table 1.
Comparative example 1
A preparation method of a high-nickel ternary cathode material of a lithium ion battery comprises the following steps:
selecting a commercial ternary precursor Ni0.82Co0.12Mn0.06(OH)2Uniformly mixing the precursor with lithium hydroxide according to the Li/Me molar ratio of 1.1, wherein Me is Ni + Co + Mn, and performing primary sintering in an atmosphere furnace at 800 ℃ for 10 hours in the presence of oxygen to obtain a product obtained after the primary sintering, namely S1; mixing S1 with water according to a ratio of 1:2, washing for 0.5h at a rotation speed of 500r/min, spin-drying with a centrifuge, and drying at 120 ℃ for 6h to obtain a product S2;
and mixing the S2 with 0.2 wt% of alumina and 0.3 wt% of boron oxide, and then carrying out secondary sintering in an atmosphere furnace, wherein the sintering temperature is 350 ℃, and the sintering time is 5 hours, so as to obtain a product S3, namely the high-nickel ternary cathode material.
Microstructural analysis of S3 As shown in FIG. 2, the sample S3 was in the hexagonal system as shown by XRD patternHaving a typical alpha-NaFeO2The layered structure has a space group of R-3m, a sharp diffraction peak and high crystallinity, and the cell parameters obtained by Topas refinement software refinement are shown in Table 1.
As can be seen from Table 1, the c/a value after washing in water is smaller than that after washing in corrosion inhibitor, and the Li-Ni mixing value is larger.
Half-cells were prepared using S3, as per w (ternary material sample): w (conductive carbon): w (pvdf) 80: 10:10 by weight, button test battery positive electrode slurry was prepared, flat and clean aluminum foil was used as a battery positive electrode current collector, a flat and clean surface lithium sheet was used for a negative electrode (stored in an argon glove box), and the electrolyte was LiPF6 (PC: EC: DMC ═ 10: 30: 60, volume ratio) at 1.0 mol/L. Assembling the CR2430 button cell must be completed in an argon-filled glove box, and H in the glove box2O and O2Mass fraction is less than 10-7. After the button cell is assembled, the button cell is kept still in the glove box for 60min, and then the charge and discharge properties of the button cell are tested on a LANCET 2001 cell test system under the test conditions that the charge and discharge current is 0.1C (20mA) at normal temperature and the voltage interval is 2.5-4.25V.
And carrying out electrochemical performance test on the half-cell. The test results are shown in table 2.
As can be seen from table 2, when the substrate material is washed during the preparation of the high-nickel ternary cathode material, the addition of the corrosion inhibitor is helpful for improving the electrochemical performance, which is related to the low lithium-nickel mixed-row in the XRD test.
TABLE 2
Example 2
A preparation method of a high-nickel ternary cathode material of a lithium ion battery comprises the following steps:
selecting a commercial ternary precursor Ni0.82Co0.12Mn0.06(OH)2According to the molar ratio of Li/Me of 1.07, wherein Me is Ni + Co + Mn, the precursor is uniformly mixed with lithium hydroxide, and primary sintering is carried out in an atmosphere furnace at the sintering temperature of 820 ℃ for the sintering timeThe atmosphere is oxygen for 12 hours, and the obtained product after primary sintering is S1;
mixing S1 with water according to the weight ratio of 1:1.5, washing, adding a corrosion inhibitor as shown in Table 2, washing for 2h at the rotating speed of 700r/min, drying by a centrifugal machine, and drying at 120 ℃ for 8h to obtain a product S2;
and (3) uniformly mixing S2 with 0.3 wt% of alumina and 0.45 wt% of boron oxide, and then carrying out secondary sintering in an atmosphere furnace, wherein the sintering temperature is 320 ℃, and the sintering time is 4 hours, so as to obtain a product S3, namely the high-nickel ternary cathode material.
Half-cells were prepared using S3, as per w (ternary material sample): w (conductive carbon): w (pvdf) 80: 10:10, preparing positive electrode slurry of the button test battery, using flat and clean aluminum foil as a positive electrode current collector of the battery, using a flat and clean lithium sheet (stored in an argon glove box) as a negative electrode, and using LiPF with 1.0mol/L electrolyte6(PC: EC: DMC: 10: 30: 60, volume ratio). Assembling the CR2430 button cell must be completed in an argon-filled glove box, and H in the glove box2O and O2Mass fraction is less than 10-7. After the button cell is assembled, the button cell is kept still in the glove box for 60min, and then the charge and discharge properties of the button cell are tested on a LANCET 2001 cell test system under the test conditions that the charge and discharge current is 0.1C (20mA) at normal temperature and the voltage interval is 2.5-4.25V.
And carrying out electrochemical performance test on the half-cell. The test results are shown in table 3.
It can be seen from table 3 that the electrochemical performance of the corrosion inhibitor added in the washing process is better than that of the sample washed directly with water, which reduces the side reaction during washing, avoids the damage to the matrix material, reduces the degree of lithium-nickel mixed-discharging, and forms a film on the surface of the matrix, which can generate a fast ion conductor layer in the process of secondary sintering, and hinders the electrolyte from corroding the anode material. When the amount of the additive is large, the electrochemical performance is lowered as in examples 2 to 5, which may cause an excessive amount of the additive, and the rapid ion conductor layer may not be formed completely, thereby affecting the transport of lithium ions.
TABLE 3
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (5)
1. A preparation method of a high-nickel ternary cathode material of a lithium ion battery is characterized by comprising the following steps:
s1. ternary precursor NixCoyMnz(OH)2Wherein x is more than or equal to 0.8, x + y + Z is 1, the molar ratio of Li to Me is 1-1.1, and Me is the sum of Ni, Co and Mn; uniformly mixing the ternary precursor with lithium hydroxide, and performing primary sintering in an atmosphere furnace, wherein the sintering temperature is 750-850 ℃, the sintering time is 1-15h, and the atmosphere is oxygen, so that a product obtained after the primary sintering is S1;
s2, mixing S1 with water according to the weight ratio of 1:1-2, washing, adding 0.2-2 wt% of corrosion inhibitor, drying at the temperature of 110-;
s3, mixing the S2 with an oxide with the weight percent below 1 percent, and then carrying out secondary sintering in an atmosphere furnace, wherein the sintering temperature is 300-650 ℃, and the sintering time is 1-5h, so as to obtain a product S3, namely the high-nickel ternary cathode material of the lithium ion battery.
2. The method for preparing the high-nickel ternary cathode material for the lithium ion battery according to claim 1, wherein in step S2, the corrosion inhibitor is one or more of sodium tungstate, ammonium tungstate and sodium borate.
3. The method for preparing the high-nickel ternary cathode material for the lithium ion battery according to claim 1, wherein in step S3, the oxide is one or both of alumina and boron oxide.
4. The method for preparing the high-nickel ternary cathode material for the lithium ion battery as claimed in claim 1, wherein in the step S2, the rotation speed is 500-1000r/min, and the product S2 is obtained by drying the material at 120 ℃ for 6-12h after being dried by a centrifuge.
5. A high-nickel ternary cathode material for a lithium ion battery, which is characterized by being prepared by the preparation method of any one of claims 1 to 4.
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