CN108199037B - Nickel-cobalt lithium aluminate cathode material mixed with anions and cations and preparation method thereof - Google Patents
Nickel-cobalt lithium aluminate cathode material mixed with anions and cations and preparation method thereof Download PDFInfo
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- 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
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- 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
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Abstract
The invention is suitable for the technical field of lithium batteries, and provides a nickel cobalt lithium aluminate anode material mixed and doped with anions and cations and a preparation method thereof, wherein the method comprises the steps of firstly adopting a pre-sintering method of spraying a sodium bicarbonate solution and an F solution, pre-sintering a nickel cobalt lithium aluminate NCA precursor into a porous honeycomb-like spherical pre-sintering precursor, then preparing Mg and Nb sources into a solution according to a proportion, mixing the solution with the pre-sintering precursor under a water system condition, effectively introducing the Mg and Nb solution into the interior of an anode material substrate through honeycomb-shaped holes, then spraying an F ion regulator solution when a high-speed mixer is used for mixing and lithium supplement, fully and uniformly mixing the materials, and finally sintering at a high temperature to crystallize a finished product to obtain the nickel cobalt lithium aluminate anode material mixed and doped with anions; among the positive electrode materials, Nb4+ can reduce cation mixing, Mg3+ can reduce polarization and enhance electrochemical performance, therefore Mg3+/Nb4The negative ion doping F can fix oxygen, reduce oxygen precipitation, stabilize material structure and improve circulation capacity.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a nickel cobalt lithium aluminate anode material mixed with anions and cations and a preparation method thereof.
Background
The nickel cobalt lithium aluminate ternary positive electrode material is widely applied to the fields of IT products and new energy automobiles due to higher energy density, but the simple nickel cobalt lithium aluminate (L NCA) has poor structural stability, and the nickel cobalt lithium aluminate has higher nickel content, so that cation mixed discharge is easy to occur, and Ni2+, L i + occupy space between each other, preventing L i + from transmitting and destroying the crystal structure of the material, and L i + has poor transmission capability between grain boundaries, which causes great harm to the cycle life and capacity of the material.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a nickel cobalt lithium aluminate cathode material doped with mixed anions and cations and a preparation method thereof, and aims to solve the technical problems of poor cycle life and capacity of the existing nickel cobalt lithium aluminate ternary cathode material.
On one hand, the preparation method of the anion and cation mixed doped nickel cobalt lithium aluminate cathode material comprises the following steps:
s1, pre-sintering step:
weighing a nickel-cobalt lithium aluminate precursor, spraying a certain amount of sodium bicarbonate solution and F solution, uniformly mixing, transferring into a sintering furnace, performing low-temperature presintering, rapidly heating, and performing high-temperature presintering for a period of time to obtain a porous presintering precursor;
s2, cation doping step:
preparing and mixing Nb solution and Mg solution with certain concentration, weighing the porous presintering precursor, pouring the presintering precursor into the Nb and Mg mixed solution under the condition of stirring and heating for a period of time, and uniformly mixing to obtain a standby sample;
s3, drying:
drying the standby sample to obtain Nb and Mg doped precursor raw materials;
s4, mixing materials and anion doping:
weighing the Nb-Mg doped precursor raw materials, adding a lithium source according to a certain lithium proportion, putting the Nb-Mg doped precursor raw materials and the lithium source into a high-speed mixer together for mixing, and spraying a certain amount of F ion regulator solution while mixing;
s5, sintering:
and putting the mixed sample into a sintering kiln, setting the sintering temperature and the sintering time, introducing gas, sieving the sintered sample to remove iron, and thus obtaining the anion and cation mixed doped nickel cobalt lithium aluminate cathode material.
On the other hand, the anion and cation mixed doped lithium nickel cobalt aluminate cathode material is prepared by the method, and the chemical formula of the component is L ixNi1-a-b-c-dCoaAlbMgcNbdO2-yFyWherein x is more than or equal to 0.85 and less than or equal to 1.2, a is more than or equal to 0 and less than or equal to 0.15, b is more than or equal to 0 and less than or equal to 0.03, c is more than or equal to 0.001 and less than or equal to 0.003, d is more than or equal to 0.001 and less than or equal to 0.0003, and y is more than or equal to 0.001 and less.
The invention has the beneficial effects that: according to the preparation method, firstly, a pre-sintering method of spraying a sodium bicarbonate solution and an F solution is adopted, a nickel-cobalt lithium aluminate NCA precursor is pre-sintered into a porous honeycomb-shaped quasi-spherical pre-sintering precursor, then Mg and Nb sources are prepared into a solution according to a proportion, and after the solution is mixed with the pre-sintering precursor under a water system condition, the Mg and Nb solution is effectively introduced into the inner part of a base material of the positive electrode material through honeycomb-shaped holes, then an F ion regulator solution is sprayed when a high-speed mixer is used for mixing and lithium supplementing, so that the materials are fully and uniformly mixed, and finally, the high-temperature sintering is carried out, so that a finished product is crystallized, and the anion-cation mixed and; among the positive electrode materials, Nb4+ can reduce cation mixing, Mg3+ can reduce polarization and enhance electrochemical performance, therefore Mg3+/Nb4The electrochemical reaction and valence change do not occur in the charging process, the crystal structure can be stabilized, oxygen can be fixed through doping of F negative ions, oxygen precipitation is reduced, and the material structure is stabilizedAnd the circulation capacity is improved.
Drawings
FIG. 1 is a flow chart of a preparation method of a cathode and anode mixed doped nickel cobalt lithium aluminate cathode material of the invention;
FIG. 2 is an electron micrograph of a pre-sintered precursor according to an embodiment of the present invention;
FIG. 3 is an electron microscope image of Mg, Nb and F ion mixed doped lithium nickel cobalt aluminate cathode material obtained in the example of the invention;
fig. 4 is a graph comparing the electrical properties of lithium batteries manufactured in examples of the present invention and comparative examples.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the preparation method of the anion and cation mixed doped nickel cobalt lithium aluminate anode material provided by the invention comprises the following steps:
s1, pre-sintering step: weighing a nickel-cobalt lithium aluminate precursor, spraying a certain amount of sodium bicarbonate solution and F solution, uniformly mixing, transferring into a sintering furnace, performing low-temperature presintering, rapidly heating, and performing high-temperature presintering for a period of time to obtain a porous presintering precursor.
The sodium bicarbonate solution accounts for 5-10% of the mass percentage concentration, the spraying amount accounts for 1-10% of the total mass of the nickel cobalt lithium aluminate precursor, the F solution accounts for 0.2-1.5% of the mass percentage concentration, the F solution accounts for 1-5% of the total mass of the nickel cobalt lithium aluminate precursor, and the F solution is NH4F, NaF and MgF2One of (1); the low-temperature presintering temperature of the sintering furnace is 300 ℃, the time is 2-5h, then the temperature is rapidly raised according to 5-10 ℃/min, and the high-temperature presintering is carried out after the temperature is raised to 600-.
S2, cation doping step: preparing and mixing Nb solution and Mg solution with certain concentration, weighing the porous presintering precursor, pouring the presintering precursor into the Nb and Mg mixed solution under the condition of stirring and heating for a period of time, and uniformly mixing to obtain a standby sample.
The mass percentage concentration of the Nb solution and the Mg solution is 0.05-3%, and the mass ratio of the presintering precursor to the Nb-Mg mixed solution is 1: (5-20), stirring for 1-4h at the temperature of 40-80 ℃, wherein the Nb solution is one or more of niobium nitrate, niobic acid, lithium niobate, niobium fluoride and niobium sulfate, and the Mg solution is one or more of magnesium nitrate, magnesium oxalate, magnesium chloride and magnesium sulfate.
S3, drying: and drying the standby sample to obtain Nb and Mg doped precursor raw materials.
The method comprises the following steps of adopting a rotary evaporation drying process, placing the standby sample into a rotary evaporator, carrying out rotary reduced pressure distillation, setting the temperature of the rotary evaporator at 60-90 ℃ and the rotation time at 2-6h, and completely evaporating water to obtain a material, namely the Nb-Mg doped precursor raw material.
S4, mixing materials and anion doping: weighing the Nb-Mg doped precursor raw materials, adding a lithium source according to a certain lithium proportion, putting the mixture into a high-speed mixer for mixing, and spraying a certain amount of F ion regulator solution while mixing.
The mass percent concentration of the F ion regulator solution is greater than that of the F solution in the step S1, and the mass percent concentration of the F ion regulator solution is 1-10%, and the F ion regulator solution is NH4F、NaF、MgF2Wherein the lithium source is one or more of lithium hydroxide monohydrate, lithium carbonate and lithium chloride, the lithium proportion of L i/Me is 1.0-1.2, Me is the total molar weight of nickel, cobalt, aluminum, manganese and niobium, the mixing time is 2-10min, and the rotating speed is 500-1400 rpm.
S5, sintering: and putting the mixed sample into a sintering kiln, setting the sintering temperature and the sintering time, introducing gas, sieving the sintered sample to remove iron, and thus obtaining the anion and cation mixed doped nickel cobalt lithium aluminate cathode material. The sintering temperature is 500-800 ℃, the sintering time is 10-25h, and the introduced gas is air or oxygen.
Finally obtainThe component of the nickel cobalt lithium aluminate anode material mixed with the anions and the cations is nickel cobalt lithium aluminate, the shape of the nickel cobalt lithium aluminate is similar to a spherical shape, and the chemical formula of the component can be L ixNi1-a-b-c-dCoaAlbMgcNbdO2-yFyExpressed that x is more than or equal to 0.85 and less than or equal to 1.2, a is more than or equal to 0 and less than or equal to 0.15, b is more than or equal to 0 and less than or equal to 0.03, c is more than or equal to 0.001 and less than or equal to 0.003, d is more than or equal to 0.001 and less than or equal to 0.0003, and y is more than or equal to 0.001.
By doping a proper amount of mixed cations of Mg3+ and Nb4+ and F anions, the cation mixing discharge can be effectively reduced through the cation doping of Mg + Nb, and oxygen can be fixed through the anion doping of F, so that the oxygen precipitation is reduced, the material structure is stabilized, and the cycle capacity is improved.
The effect of the product is verified by the following specific examples and comparative examples:
example (b):
1) 100g of nickel cobalt lithium aluminate precursor is weighed and sprayed with 5% sodium bicarbonate solution and 0.2% NH4And (4) uniformly mixing the solution F, and then transferring the solution F into a sintering furnace for pre-sintering. The spraying amount of the baking soda solution is 5% of the mass ratio of the nickel-cobalt lithium aluminate precursor, the spraying amount of the F solution accounts for 2% of the total mass of the nickel-cobalt lithium aluminate precursor, the sintering temperature is 300 ℃ for 2 hours, then the temperature is rapidly increased to 600 ℃ at the speed of 5 ℃/min for 10 hours, and the hole-shaped presintering precursor is obtained.
2) Weighing 100g of pre-sintered precursor which is already in a hole shape, adding the pre-sintered precursor into 1 percent of NbCl under the condition of stirring and heating5Solution and 2% MgCl2And mixing the solution uniformly to obtain a standby sample. The mass ratio of the presintering precursor to the Mg-Nb mixed solution is 1:10, the stirring temperature is 40 ℃, and the stirring time is 1 h.
3) And (3) placing the doped standby sample into a rotary evaporator, setting the temperature of the rotary evaporator at 80 ℃ and the rotation time at 2h, carrying out rotary reduced pressure distillation, and completely evaporating water to obtain the material, namely the Nb-Mg doped precursor raw material.
4) Weighing 100g of Nb-Mg doped precursor raw material, adding lithium hydroxide according to L i/Me of 1.03, putting the two raw materials into a high-speed mixer, and spraying NH with the concentration of 4 percent at the same time4Solution F, then mixed for 10min at 1000 rpm.
5) And putting the mixed sample into a sintering kiln, sintering at the temperature of 750 ℃ for 20h, introducing oxygen, sieving the sintered sample to remove iron, and thus obtaining the anion and cation mixed doped nickel cobalt lithium aluminate cathode material.
Comparative example:
weighing 100g of nickel cobalt lithium aluminate precursor, adding lithium hydroxide according to L i/Me of 1.03, putting the two raw materials into a high-speed mixer, putting the mixed sample into a sintering kiln, sintering at the temperature of 600 ℃ for 12h, introducing oxygen, obtaining the sintered sample, and sieving to remove iron to obtain the common lithium aluminate cathode material.
The button cell is assembled by taking the positive electrode materials prepared in the examples and the comparative examples as positive electrode active materials and taking a lithium sheet as a negative electrode. The composition of the positive electrode sheet is m (active material): m (acetylene black): and m (PVDF) is 80:12:8, a blue test system is adopted for testing, the charge-discharge voltage is 2.75-4.3V, and the cycle performance is tested in the normal temperature environment. The relationship between the number of charge and discharge cycles and the capacity retention rate is shown in fig. 4. After 50 cycles, the retention rate of the lithium battery prepared from the positive electrode material of the example is 97.2%, and the retention rate of the lithium battery prepared from the positive electrode material of the comparative example is 95.3%. Therefore, the cathode and anode mixed doped nickel cobalt lithium aluminate anode material has better electrical property than the common nickel cobalt lithium aluminate anode material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A preparation method of a cathode and anode mixed doped nickel cobalt lithium aluminate cathode material is characterized by comprising the following steps:
s1, pre-sintering step:
weighing a nickel-cobalt lithium aluminate precursor, spraying a certain amount of sodium bicarbonate solution and F solution, uniformly mixing, transferring into a sintering furnace, performing low-temperature presintering, rapidly heating, and performing high-temperature presintering for a period of time to obtain a porous presintering precursor;
s2, cation doping step:
preparing and mixing Nb solution and Mg solution with certain concentration, weighing the porous presintering precursor, pouring the presintering precursor into the Nb and Mg mixed solution under the condition of stirring and heating for a period of time, and uniformly mixing to obtain a standby sample;
s3, drying:
drying the standby sample to obtain Nb and Mg doped precursor raw materials;
s4, mixing materials and anion doping:
weighing the Nb-Mg doped precursor raw materials, adding a lithium source according to a certain lithium proportion, putting the Nb-Mg doped precursor raw materials and the lithium source into a high-speed mixer together for mixing, and spraying a certain amount of F ion regulator solution while mixing;
s5, sintering:
putting the mixed sample into a sintering kiln, setting the sintering temperature and the sintering time, introducing gas, sieving the sintered sample to remove iron to obtain the anion and cation mixed doped nickel cobalt lithium aluminate cathode material;
in step S1, the baking soda solution has a mass percentage concentration of 5% to 10%, the baking soda solution is sprayed in an amount of 1% to 10% of the total mass of the nickel cobalt lithium aluminate precursor, the F solution has a mass percentage concentration of 0.2% to 1.5%, the F solution is 1% to 5% of the total mass of the nickel cobalt lithium aluminate precursor, and the F solution is one of NH4F, NaF, and MgF 2; the low-temperature presintering temperature of the sintering furnace is 300 ℃, the time is 2-5h, then the temperature is rapidly raised according to 5-10 ℃/min, and the high-temperature presintering is carried out after the temperature is raised to 600-; in step S2, the mass percentage concentrations of the Nb solution and the Mg solution are both 0.05 to 3%, and the mass ratio of the pre-sintering precursor to the Nb and Mg mixed solution is 1: (5-20), the stirring temperature is 40-80 ℃, the stirring time is 1-4h,
the method comprises the steps of S1, wherein the mass percentage concentration of an F ion regulator solution in the step S4 is larger than that of the F solution in the step S1, the mass percentage concentration of the F ion regulator solution is 1-10%, the mass percentage concentration of the F ion regulator solution is one of NH4F, NaF and MgF2, a lithium source used is one or more of lithium hydroxide monohydrate, lithium carbonate and lithium chloride, the lithium proportion L i/Me is 1.0-1.2, the mixing time is 2-10min, and the rotating speed is 500-1400 rpm.
2. The method for preparing the anion and cation mixed doped lithium nickel cobalt aluminate anode material of claim 1, wherein step S3 adopts a rotary evaporation drying process, the spare sample is placed in a rotary evaporator, rotary reduced pressure distillation is carried out, and the material obtained after water evaporation is completed is the Nb and Mg doped precursor raw material.
3. The method for preparing the anion and cation mixed doped nickel cobalt lithium aluminate anode material as claimed in claim 2, wherein the temperature of the rotary evaporator is set to 60-90 ℃ and the rotation time is 2-6 h.
4. The method as claimed in claim 1, wherein the sintering temperature in step S5 is 500-800 ℃, the sintering time is 10-25h, and the introduced gas is air or oxygen.
5. A mixed anion and cation doped lithium nickel cobalt aluminate cathode material, wherein the mixed anion and cobalt lithium aluminate cathode material is prepared by the method of any one of claims 1 to 4.
6. The hybrid anion and cation doped nickel cobalt lithium aluminate cathode material of claim 5, wherein the composition formula of the hybrid anion and cobalt lithium aluminate cathode material is L ixNi1-a-b-c-dCoaAlbMgcNbdO2-yFyWherein x is more than or equal to 0.85 and less than or equal to 1.2, a is more than 0 and less than or equal to 0.15, b is more than 0 and less than or equal to 0.03, c is more than or equal to 0.001 and less than or equal to 0.003, d is more than or equal to 0.001 and less than or equal to 0.0003, and y is more than or equal to 0.001 and less than or equal to 0..
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| CN111233042B (en) * | 2020-01-16 | 2022-03-11 | 阜阳师范大学 | Lithium manganate positive electrode material precursor, lithium manganate positive electrode material and preparation method thereof |
| CN112701271A (en) * | 2020-12-28 | 2021-04-23 | 格林美（无锡）能源材料有限公司 | Element doping method based on ternary precursor positive electrode material |
| CN113178565B (en) * | 2021-03-29 | 2023-06-16 | 广东邦普循环科技有限公司 | Mixing process for preparing high-nickel anode material and application thereof |
| CN114914436B (en) * | 2022-02-10 | 2024-06-04 | 中国第一汽车股份有限公司 | High-nickel ternary positive electrode material and preparation method thereof |
| CN116169280B (en) * | 2023-03-07 | 2024-07-16 | 北京工业大学 | High-entropy compound for positive electrode of aluminum ion battery and preparation method thereof |
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| CN105470454A (en) * | 2014-09-03 | 2016-04-06 | 中国科学院宁波材料技术与工程研究所 | Modified lithium ion battery positive electrode material and preparation method therefor |
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Effective date of registration: 20211224 Address after: 448000 No. 8 Yingbin Avenue, Duodao District, Jingmen City, Hubei Province (greenmei new energy) Patentee after: Greenmei (Hubei) new energy materials Co.,Ltd. Address before: No.214142, xinshuofang Road, Wuxi City, Jiangsu Province Patentee before: GEM (WUXI) ENERGY MATERIAL Co.,Ltd. Patentee before: JINGMEN GEM Co.,Ltd. Patentee before: GEM Co.,Ltd. |
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