CN110112385B - Method for improving stability and rate performance of ternary cathode material - Google Patents

Method for improving stability and rate performance of ternary cathode material Download PDF

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CN110112385B
CN110112385B CN201910336371.XA CN201910336371A CN110112385B CN 110112385 B CN110112385 B CN 110112385B CN 201910336371 A CN201910336371 A CN 201910336371A CN 110112385 B CN110112385 B CN 110112385B
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汤昊
谢天
谭龙
孙润光
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Nanchang University
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
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    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
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    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for improving the stability and rate capability of a ternary cathode material. The preparation method comprises the following steps: the chemical formula is LiNixCo(1‑x‑y)MnyO2(x + y is more than 0 and less than 1) ternary positive electrode material and a certain proportion of LiPF (chemical formula of LiPF)6、LiAsF6、LiBF4Adding one of the additives, uniformly mixing, adding a solvent to prepare a rheological body mixture, drying at 50-80 ℃ for 3-6 h to obtain a precursor, calcining the precursor at 300-800 ℃ under a certain atmosphere for 1-20 h to obtain the precursor with the chemical formula of Li (Ni)xCoyMn(1‑x‑y))(1‑γ)MγO2‑F(x + y is 0 < 1, gamma is 0 < 0.1, 0 < 0.6, M is P, As or B). The layered lithium transition metal oxide positive electrode material disclosed by the invention has high specific capacity, good safety performance and excellent cycle and rate performance, and is suitable for lithium ion power batteries.

Description

Method for improving stability and rate performance of ternary cathode material
Technical Field
The invention belongs to the technical field of lithium ion battery electrode materials, and particularly relates to a method for improving the stability and rate capability of a ternary cathode material.
Background
Lithium ion batteries are widely used in various fields because of their high energy density, long service life, stable operating voltage, and low self-discharge rate. At this stage, research efforts on lithium ion batteries have focused on developing power batteries with high mass/volume energy density to meet the needs of electric vehicles. The choice of the positive electrode material is particularly important, among all factors that determine the energy density of a lithium ion battery. Currently, the industrialized anode materials mainly comprise layered lithium transition metal oxides, spinel lithium manganate and olivine lithium iron phosphate. Among them, the layered lithium transition metal oxide has great potential in realizing high energy density of a lithium ion battery, and thus becomes a key research object of researchers.
At present, in order to improve the energy density of the layered lithium transition metal oxide and simultaneously consider the cycle and rate performance of the layered lithium transition metal oxide, the corresponding layered lithium transition metal oxide needs to be subjected to surface coating or ion doping. The surface coating technology is adopted, so that the electrode material and the electrolyte can be prevented from reacting, the phase change of the material is prevented, and the stability of the material is improved; and the adoption of the ion doping technology can stabilize the material structure, improve the conductivity, reduce the impedance and polarization effect and the like.
Common ion doping includes: doping of metal ions, e.g. Mg2+、Al3+、Ti4+、V5+、Sc3+、Y3+、Nb5+、In3+、Sn4+、Ce4+、Eu3+、Gd3+、Er3+、Ta4+、Ge4+、W6+One or more of (patent application No.: CN 201811268765.2); doping with anions, e.g. F-(patent application No.: CN 201611190763.2); ③ Co-doping of anions and cations, like Ti4+And F-The product Li (Ni) is obtained0.4Co0.2Mn0.4)0.95Ti0.05O1.95F0.05(patent application No.: CN 201310264936.0). According to the reported results, the electrochemical performance of the doped material is effectively improved by an ion doping technology, for example, in the Chinese patent application CN201510843893.0, a method for mixing a layered nickel-cobalt-manganese ternary material and a fluorine-containing compound to obtain a fluorine-doped anode material is disclosed, the capacity of a lithium ion battery can reach 205mAh/g for the first time under the condition of low-current discharge by the modification method, and the capacity retention rate is 93.1% after 80 cycles, namely the electrochemical performance of the doped material is superior to that of the undoped material. Nevertheless, the ion doping technology for layered lithium transition metal oxide at present cannot meet the requirement of high energy density for power batteries on electric vehicles, i.e. there is still great space for improvement and difficulty in synthesizing safe and high-performance layered lithium transition metal oxide.
Disclosure of Invention
In view of the above prior art, the technical problem to be solved by the present invention is to provide a method for synthesizing a layered lithium transition metal oxide positive electrode material with high specific capacity, safer use, and better cycle performance and rate capability.
In order to solve the technical problems, the invention provides a method for improving the stability and rate capability of a ternary cathode material, which comprises the following steps:
(1) the chemical formula is LiNixCo(1-x-y)MnyO2(x is more than 0 and y is less than 1) ternary positive electrode material and a certain proportion of LiPF6、LiAsF6、LiBF4Uniformly mixing one of the added auxiliary agents to obtain a mixture A;
(2) adding a certain amount of lubricating agent into the mixture A prepared in the step (1) to prepare a rheological body mixture, and drying the mixture at the temperature of between 50 and 80 ℃ for 3 to 6 hours to obtain a precursor;
(3) putting the precursor prepared in the step (2) in a certain atmosphere, and calcining the precursor for 1 to 20 hours at the temperature of between 300 and 800 ℃ to obtain the precursor with the chemical formula of Li (Ni)xCoyMn(1-x-y))(1-γ)MγO2-FThe ternary positive electrode material of (1), wherein x + y is more than 0 and less than 1, gamma is more than 0 and less than or equal to 0.1, 0 and less than or equal to 0.6, and M is P, As or B.
More preferably, the lubricating agent in step (2) is one or more of water, absolute ethyl alcohol, isopropyl alcohol and ethylene glycol, preferably ethyl alcohol and isopropyl alcohol.
Preferably, the atmosphere in step (3) is one of air, oxygen, argon and nitrogen, and preferably air.
More preferably, the mass of the additive in the step (1) is LiNixCoyMn(1-x-y)O20.2-20% of the ternary cathode material, preferably 1.0-5.0%.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention selects low melting point and easy combination of decomposition products and LiNixCoyMn(1-x-y)O2The reaction is carried out, and ions are dopedThe additive entering the material crystal lattice realizes the ion doping of different nonmetals at the transition metal position and the oxygen position of the layered lithium transition metal oxide anode material for the first time, thereby obtaining the anode material with greatly improved rate capability and cycle performance, and further being applied to a lithium ion power battery.
2. The ion doping technology adopted by the invention has the advantages of simple doping process, high repeatability and easy industrialization.
Drawings
Fig. 1 is a high-resolution X-ray photoelectron spectrum of fluorine (a) and phosphorus (b) in the ternary positive electrode material obtained in example 1 of the present invention.
FIG. 2 is X-ray diffraction patterns of the ternary positive electrode material (3% doping amount ratio) obtained in example 2 of the present invention and a control (0% doping amount ratio).
Detailed Description
The invention will be further described with reference to the drawings and preferred embodiments.
Example 1:
weighing 2.73g of ternary cathode material LiNi according to the mass ratio of 91: 90.6Co0.2Mn0.2O2(LNCM622) and 0.27g LiPF at a concentration of 1mol/L6Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 80 ℃ to obtain a precursor; finally, calcining the precursor at 500 ℃ for 10h to obtain F, P codoped ternary cathode material Li (Ni)0.6Co0.2Mn0.2)0.991P0.009O1.946F0.054。
Adding the ternary cathode material prepared in the embodiment, conductive carbon black and PVDF into a certain amount of NMP according to the mass ratio of 8: 1, and mixing and stirring to obtain a slurry; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 1, which indicates that the F, P co-doped ternary cathode material has better performance than the undoped sample and the reported fluorine-doped sample.
The ternary cathode material prepared in this example was subjected to X-ray photoelectron spectroscopy (XPS) analysis, and the results are shown in fig. 1. As can be seen from the figure, P, F elements are present in the ternary cathode material, indicating that P, F elements have been successfully incorporated.
Example 2:
weighing 2.91g of ternary cathode material LNCM622 and 0.09g of LiPF with the concentration of 1mol/L according to the mass ratio of 97: 36Uniformly mixing the solution; then adding 3mL of isopropanol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 80 ℃ to obtain a precursor; finally, calcining the precursor at 550 ℃ for 8h to obtain F, P co-doped ternary cathode material Li (Ni)0.6Co0.2Mn0.2)0.997P0.003O1.982F0.018。
Adding the ternary cathode material prepared in the embodiment, conductive carbon black and PVDF into a certain amount of NMP according to the mass ratio of 8: 1, and mixing and stirring to obtain a slurry; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 1, which indicates that the F, P co-doped ternary cathode material has better performance than the undoped sample and the reported fluorine-doped sample.
The ternary cathode material prepared in this example (doping amount ratio of 3%) and the control sample (doping amount ratio of 0%) were subjected to XRD characterization, and the results are shown in fig. 2. As can be seen from the figure, the ternary cathode material prepared by the embodiment belongs to a hexagonal system and has alpha-NaFeO2The layered structure of (1) and no other hetero-peaks appear in the figure, indicating that no new phase is formed by doping.
Example 3:
weighing 2.94g of ternary cathode material LNCM622 and 0.06g of LiBF with the concentration of 1mol/L according to the mass ratio of 98: 24Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 70 ℃ to obtain a precursor; finally will be beforeCalcining the precursor at 500 ℃ for 8h to obtain F, B co-doped ternary cathode material Li (Ni)0.6Co0.2Mn0.2)0.998B0.002O1.992F0.008。
The ternary positive electrode material prepared in the embodiment, conductive carbon black and PVDF are added with a certain amount of NMP to be mixed and stirred into slurry according to the mass ratio of 8: 1; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 1, which indicates that the F, B co-doped ternary cathode material has better performance than the undoped sample and the reported fluorine-doped sample.
Example 4:
weighing 2.82g of ternary cathode material LiNi according to the mass ratio of 94: 60.5Co0.2Mn0.3O2(LNCM523) and 0.18g LiPF at a concentration of 1mol/L6Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 70 ℃ to obtain a precursor; finally, the precursor is placed at 500 ℃ to be calcined for 6h, and F, P co-doped ternary cathode material Li (Ni) is obtained0.5Co0.2Mn0.3)0.994P0.006O1.964F0.036。
Adding the ternary cathode material prepared in the embodiment, conductive carbon black and PVDF into a certain amount of NMP according to the mass ratio of 8: 1, and mixing and stirring to obtain a slurry; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 2, which indicates that the F, P co-doped ternary cathode material has better performance than the undoped sample and the disclosed fluorine-doped sample.
Example 5:
weighing 2.88g of ternary cathode material LNCM523 and 0.12g of LiBF with the concentration of 1mol/L according to the mass ratio of 96: 44Uniformly mixing the solution; then 3mL of absolute ethyl alcohol is added and magnetically stirred at normal temperatureStirring for 4h to obtain a rheological fluid mixture; then drying the mixture at 80 ℃ to obtain a precursor; finally, calcining the precursor at 500 ℃ for 8h to obtain F, B co-doped ternary cathode material Li (Ni)0.5Co0.2Mn0.3)0.994B0.006O1.976F0.024。
Adding the ternary cathode material prepared in the embodiment, conductive carbon black and PVDF into a certain amount of NMP according to the mass ratio of 8: 1, and mixing and stirring to obtain a slurry; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 2, which indicates that the F, B co-doped ternary cathode material has better performance than the undoped sample and the disclosed fluorine-doped sample.
Example 6:
weighing 2.91g of ternary cathode material LiNi according to the mass ratio of 97: 31/3Co1/3Mn1/3O2(LNCM333) and 0.09g LiPF at a concentration of 1mol/L6Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 70 ℃ to obtain a precursor; finally, calcining the precursor at 500 ℃ for 10h to obtain F, P codoped ternary cathode material Li (Ni)1/3Co1/3Mn1/3)0.997P0.003O1.982F0.018。
Adding the ternary cathode material prepared in the embodiment, conductive carbon black and PVDF into a certain amount of NMP according to the mass ratio of 8: 1, and mixing and stirring to obtain a slurry; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 3, which indicates that the F, P co-doped ternary cathode material has better performance than the undoped sample and the disclosed fluorine-doped sample.
Example 7:
weighing 2.82g of ternary cathode material LiNi according to the mass ratio of 94: 60.8Co0.1Mn0.1O2(LNCM811) and 0.18g LiBF at a concentration of 1mol/L4Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 80 ℃ to obtain a precursor; finally, calcining the precursor at 500 ℃ for 8h to obtain F, B co-doped ternary cathode material Li (Ni)0.8Co0.1Mn0.1)0.994B0.006O1.976F0.024。
The ternary positive electrode material prepared in the embodiment, conductive carbon black and PVDF are added with a certain amount of NMP to be mixed and stirred into slurry according to the mass ratio of 8: 1; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 4, which indicates that the F, B co-doped ternary cathode material has better performance than the undoped sample and the reported fluorine-doped sample.
Example 8:
2.82g of ternary cathode material LNCM811 and 0.18g of LiAsF with the concentration of 1mol/L are weighed according to the mass ratio of 94: 66Uniformly mixing the solution; then adding 3mL of absolute ethyl alcohol and magnetically stirring for 4h at normal temperature to obtain a rheological body mixture; then drying the mixture at 80 ℃ to obtain a precursor; finally, the precursor is placed at 500 ℃ to be calcined for 6h, and F, As co-doped ternary cathode material Li (Ni) is obtained0.6Co0.2Mn0.2)0.994As0.006O1.964F0.036。
The ternary positive electrode material prepared in the embodiment, conductive carbon black and PVDF are added with a certain amount of NMP to be mixed and stirred into slurry according to the mass ratio of 8: 1; then uniformly coating the aluminum foil on the surface of an aluminum foil, and drying for 1h at 80 ℃; then putting the mixture into a vacuum drying oven to dry for 10 hours at the temperature of 120 ℃; and finally, slicing to prepare the button cell for electrochemical test. The test results are shown in table 4, which indicates that the F, As co-doped ternary cathode material has better performance than the undoped sample and the reported fluorine-doped sample.
TABLE 1 measurement of the charge and discharge performance of the LNCM622 doped material and the comparative samples in the examples
Figure BDA0002037986990000071
The reference: p.yue, Z.Wang, X.Li et al.Electrochimica Acta 95(2013)112-118.
TABLE 2 measurement of the charge and discharge performance of the LNCM523 doped material and the comparative samples in each example
Figure BDA0002037986990000072
The comparison patent: CN201611190763.2
TABLE 3 measurement of the charge and discharge performance of the LNCM333 doped material and each comparative sample in the examples
Figure BDA0002037986990000081
The comparison patent: CN201611190763.2
TABLE 4 measurement of the charge and discharge performance of the LNCM811 doped material and the comparative samples in the examples
Figure BDA0002037986990000082
The reference: p.yue, Z.Wang, J.Wang et al.powder Technology 237(2013)623-626.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (4)

1. A method for improving the stability and rate capability of a ternary cathode material is characterized by comprising the following steps:
(1) the chemical formula is LiNixCoyMn(1-x-y)O2(0 < x + y < 1) and LiPF (lithium ion power factor) as a ternary positive electrode material in a certain proportion6、LiAsF6、LiBF4Uniformly mixing one of the added auxiliary agents to obtain a mixture A;
(2) adding a certain amount of lubricating agent into the mixture A prepared in the step (1) to prepare a rheological body mixture, and drying the mixture at the temperature of between 50 and 80 ℃ for 3 to 6 hours to obtain a precursor;
(3) putting the precursor prepared in the step (2) in a certain atmosphere, and calcining the precursor for 1 to 20 hours at the temperature of between 300 and 800 ℃ to obtain the precursor with the chemical formula of Li (Ni)xCoyMn(1-x-y))(1-γ)MγO2-FThe ternary positive electrode material is characterized in that 0 < x + y < 1, 0 < gamma < 0.1, 0 < 0.6, and M < P, As or B.
2. The method for improving the stability and rate capability of the ternary cathode material according to claim 1, wherein the method comprises the following steps: the lubricating agent in the step (2) is one or more of water, absolute ethyl alcohol, isopropanol and ethylene glycol.
3. The method for improving the stability and rate capability of the ternary cathode material according to claim 1, wherein the method comprises the following steps: and (3) the atmosphere in the step is one of air, oxygen, argon and nitrogen.
4. The method for improving the stability and rate capability of the ternary cathode material according to any one of claims 1 to 3, wherein: the additive in the step (1) is a ternary positive electrode material LiNixCoyMn(1-x-y)O20.2-20% of the mass.
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