CN112310373A - Preparation method of ternary cathode material of lithium ion battery - Google Patents

Preparation method of ternary cathode material of lithium ion battery Download PDF

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CN112310373A
CN112310373A CN202011188186.XA CN202011188186A CN112310373A CN 112310373 A CN112310373 A CN 112310373A CN 202011188186 A CN202011188186 A CN 202011188186A CN 112310373 A CN112310373 A CN 112310373A
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ternary
coated
precursor
cqds
lithium ion
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CN112310373B (en
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汪宇
郑刚
刘汉康
林浩
张迎霞
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • H01M4/52—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
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a ternary cathode material of a lithium ion battery, which comprises the following steps of adopting a solvothermal method to prepare a ternary precursor NixCoyMnz(OH)2Growing CQDs on the surface of (x + y + z ═ 1) in situ, mixing the ternary precursor coated with the CQDs on the surface with an aluminum salt solution for reaction to obtain a ternary precursor double-coated on the surface, and finally adding a lithium source for mixing and sintering to obtain the ternary cathode material double-coated on the surface. The ternary cathode material prepared by the invention has good electronic conductivity and can effectively reduce the corrosion of HF to transition metalThereby improving the multiplying power and the cycle performance of the ternary lithium ion battery.

Description

Preparation method of ternary cathode material of lithium ion battery
Technical Field
The invention relates to the technical field of battery manufacturing, in particular to a preparation method of a ternary cathode material of a lithium ion battery.
Background
With the increasingly prominent problems of energy crisis, environmental pollution and the like, the development of sustainable new energy becomes an urgent need to build a low-carbon society. The lithium ion battery is a novel high-energy green battery, wherein the nickel-cobalt-manganese ternary material is considered as a material with great development prospect due to the advantages of high specific capacity, long cycle, good thermal stability and the like. However, the nickel-cobalt-manganese ternary material generally has some problems to be solved. Firstly, the rate capability is to be further improved; secondly, the method comprises the following steps: due to the corrosion of hydrogen fluoride generated by the decomposition of the electrolyte, transition metals of nickel, cobalt and manganese in the ternary material can be dissolved into the electrolyte from the electrode to form surface structure collapse, and the cycle performance is poor.
The surface coating technology can effectively inhibit the corrosion of electrolyte to transition metal, but the traditional surface single coating technology can effectively relieve the dissolution of metal ions, reduce the corrosion of HF to active substances and improve the cycle performance of the battery, but has no effect on the improvement of the rate capability of the battery or reduces the original conductivity performance of the ternary material to a certain extent. Therefore, while the interface reaction is reduced, the electronic conductivity of the coating substance must be considered at the same time, so that the rate and the cycle performance of the ternary material can be better improved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a ternary cathode material of a lithium ion battery.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a ternary anode material of a lithium ion battery comprises the following steps,
adopts a solvothermal method to prepare Ni in a ternary precursorxCoyMnz(OH)2Growing CQDs on the surface of (x + y + z ═ 1) in situ, mixing the ternary precursor coated with CQDs on the surface with aluminum salt solution for reaction to obtain ternary precursor with double-coated surface, and finally obtaining the ternary precursor with double-coated surfaceAnd then adding a lithium source, mixing and sintering to obtain the ternary cathode material with the double-coated surface.
Further, the solvent thermal method comprises the following specific steps: mixing ethylene glycol (CH)2OH)2And placing the precursor and the ternary precursor in a beaker according to the mass ratio of 1-2:4-6, continuously stirring for 1-3h, transferring the uniformly mixed solution into a reaction kettle, heating to 240 ℃ for 160-.
Further, the preparation steps of the surface double-coated ternary precursor are as follows: adding a ternary precursor with the surface coated with CQDs into deionized water, and adding Al2(SO4)3Adding into deionized water, reacting to obtain slurry, aging for 1-3 hr, washing, and drying to obtain surface double-coated CQDs and Al2O3The ternary precursor of (2).
Further, the mass ratio of the ternary precursor of the surface-coated CQDs to the deionized water is 1: 50-100.
Further, the surface is double coated with CQDs and Al2O3Al in the ternary precursor2O3The coating layer accounts for 1-10% by mass.
Further, the lithium source and the ternary precursor NixCoyMnz(OH)2In a molar ratio of 1.02-1.07: 1.
Further, the sintering is to perform the sintering in a sintering furnace at 400-800 ℃ for 4-6h, and oxygen is introduced into the furnace during the sintering.
Compared with the prior art, the invention has the beneficial technical effects that:
the CQDs can passivate the crystal boundary defects of the ternary material and reduce the sensitivity of the surface of the ternary material to moisture and carbon dioxide, so that the alkali content of the surface of the ternary material is reduced;
in addition, the CQDs also have excellent conductivity, and can improve the transmission efficiency of electrons and lithium ions, thereby improving the rate capability of the ternary material;
in addition, Al is used2O3The corrosion of electrolyte to the anode material in the charge-discharge process can be further relieved by using the electrolyte as a coating outer layer, so that the cycle stability of the ternary material is improved.
The ternary cathode material prepared by the invention has good electronic conductivity and can effectively reduce the corrosion of HF to transition metal, thereby improving the multiplying power and the cycle performance of the ternary lithium ion battery.
Drawings
FIG. 1 is a scanning electron microscope image of a double-coated ternary positive electrode material of example 2 under different times in the present invention;
FIG. 2 is a graph showing the power multiplication performance of the batteries prepared in example 2 and comparative example 1 according to the present invention;
fig. 3 is a graph showing high-temperature cycle characteristics of the batteries manufactured in example 2 and comparative example 1 according to the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The preparation method of the ternary cathode material of the lithium ion battery is specifically described as follows:
the preparation method of the ternary anode material of the lithium ion battery comprises the following steps,
(1) mixing ethylene glycol (CH)2OH)2Putting the ternary precursor and the ternary precursor into a beaker according to the mass ratio of 1-2:4-6, wherein the ternary positive electrode material is a nickel-cobalt-manganese ternary positive electrode material, and the molecular formula is LiNixCoyMnzO2Wherein x is more than or equal to 0 and less than 1, y is more than or equal to 0 and less than 1, z is more than or equal to 0 and less than 1, and x + y + z is 1; continuously stirring for 1-3h, transferring the uniformly mixed solution into a reaction kettle, heating to 240 ℃ for 160-;
(2) the surface is double-coatedThe preparation steps of the ternary precursor are as follows: adding a ternary precursor with the surface coated with CQDs into deionized water, and adding Al2(SO4)3Adding into deionized water, reacting to obtain slurry, aging for 1-3 hr, washing, and drying to obtain surface double-coated CQDs and Al2O3The surface of the prepared ternary precursor is doubly coated with CQDs and Al2O3Al in the ternary precursor2O3The coating layer occupies the surface and is coated with CQDs and Al2O3The mass portion of the ternary precursor is 1-10%;
(3) finally, adding a lithium source, mixing and sintering, wherein the lithium source and the ternary precursor Ni are mixedxCoyMnz(OH)2The molar ratio of the carbon-based ternary positive electrode material to the inorganic oxide is 1.02-1.07:1, the sintering is carried out for 4-6h in a sintering furnace with the temperature of 400-800 ℃, oxygen is introduced into the furnace during sintering, the material obtained by sintering is mechanically crushed, and the surface of the material is subjected to sieving and demagnetizing, thus obtaining the ternary positive electrode material with double coatings.
Example 1
A preparation method of a ternary cathode material of a lithium ion battery comprises the following steps:
the method comprises the following steps: synthesizing a precursor of a ternary material with the surface coated with CQDs: 30ml of ethylene glycol (CH)2OH)2With 80mg of ternary precursor Ni0.6Co0.2Mn0.2(OH)2Placing in a 100ml beaker, continuously stirring for 3h, transferring the uniformly mixed solution into a reaction kettle, heating to 200 ℃, and preserving heat for 5 h; after cooling to room temperature, centrifuging and washing, and placing the precipitate in an oven at 100 ℃ for vacuum drying for 6h to obtain a precursor of the ternary material with the surface coated with CQDs;
step two: surface double coating (CQDs and Al)2O3) Synthesizing the ternary material precursor: adding the precursor of the ternary material with the surface coated with the CQDs in the step one into deionized water, wherein the mass ratio of the precursor of the ternary material with the surface coated with the CQDs to the deionized water is 1: 50; 100mmol of aluminum source Al2(SO4)3Adding into deionized water, reacting, aging for 3 hr, and washing with pure waterUntil the pH value of the washing water is lower than 8, drying to obtain the surface double-coated CQDs and Al2O3The ternary precursor of (2);
step three: surface double coating (CQDs and Al)2O3) The synthesis of the ternary cathode material: according to the molar ratio of the total amount of nickel, cobalt and manganese to lithium of 1:1.05, the surface is doubly coated with CQDs and Al2O3Mixing the ternary precursor with a lithium source, then feeding the mixed material into a 600 ℃ sintering furnace for calcining for 5 hours, and introducing oxygen into the furnace during sintering; and finally, mechanically crushing the sintered material, and sieving and demagnetizing to obtain the ternary cathode material with double-coated surfaces.
Example 2
A preparation method of a ternary cathode material of a lithium ion battery comprises the following steps:
the method comprises the following steps: synthesizing a precursor of a ternary material with the surface coated with CQDs: 30ml of ethylene glycol (CH)2OH)2With and 100mg of a ternary precursor Ni0.6Co0.2Mn0.2(OH)2Placing in a 100ml beaker, continuously stirring for 3h, transferring the uniformly mixed solution into a reaction kettle, heating to 200 ℃, and preserving heat for 5 h; after cooling to room temperature, centrifuging and washing, and putting the precipitate into a drying oven at 100 ℃ for vacuum drying for 6 hours to obtain a precursor of the ternary material with the surface coated with CQDs;
step two: surface double coating (CQDs and Al)2O3) Adding the ternary material precursor coated with CQDs on the surface in the step one into deionized water, wherein the mass ratio of the precursor to the deionized water is 1: 50; then 100mmol of aluminum source Al2(SO4)3Adding deionized water, fully reacting, aging the obtained slurry for 3 hours, washing with pure water after aging until the pH value of washing water is lower than 8, and drying to obtain a ternary precursor with the surface double-coated with CQDs and Al2O 3;
step three: surface double coating (CQDs and Al)2O3) The synthesis of the ternary cathode material: according to the molar ratio of the total amount of nickel, cobalt and manganese to lithium of 1:1.05, the surface is doubly coated with CQDs and Al2O3Before the third element ofMixing the driver with a lithium source, then feeding the mixed material into a 600 ℃ sintering furnace to be calcined for 5 hours, and introducing oxygen into the furnace during sintering; and finally, mechanically crushing the sintered material, and sieving and demagnetizing to obtain the ternary cathode material with double-coated surfaces. Fig. 1 is a scanning electron microscope image of the ternary cathode material under different magnifications, and it can be seen from the image that the coating is uniformly distributed on the surface of the ternary material.
Example 3
A preparation method of a ternary cathode material of a lithium ion battery comprises the following steps:
the method comprises the following steps: synthesizing a precursor of a ternary material with the surface coated with CQDs: 30ml of ethylene glycol (CH)2OH)2And 120mg of a ternary precursor Ni0.6Co0.2Mn0.2(OH)2Placing in a 100ml beaker, continuously stirring for 3h, transferring the uniformly mixed solution into a reaction kettle, heating to 200 ℃, and preserving heat for 5 h; after cooling to room temperature, centrifuging and washing, and placing the precipitate in an oven at 100 ℃ for vacuum drying for 6h to obtain a precursor of the ternary material with the surface coated with CQDs;
step two: surface double coating (CQDs and Al)2O3) Synthesizing the ternary material precursor: adding the precursor of the ternary material with the surface coated with the CQDs in the step one into deionized water, wherein the mass ratio of the precursor to the deionized water is 1: 50; then 100mmol of aluminum source Al2(SO4)3Adding deionized water, fully reacting, aging the obtained slurry for 3 hours, washing with pure water after aging until the pH value of the washing water is lower than 8, and drying to obtain CQDs and Al with double-coated surfaces2O3The ternary precursor of (2);
step three: surface double coating (CQDs and Al)2O3) Synthesis of ternary cathode material
According to the molar ratio of the total amount of nickel, cobalt and manganese to lithium of 1:1.05, the surface is doubly coated with CQDs and Al2O3Mixing the ternary precursor with a lithium source, then feeding the mixed material into a 600 ℃ sintering furnace for calcining for 5 hours, and introducing oxygen into the furnace during sintering; finally, the material obtained by sintering is mechanically crushed and sieved and removedAnd (4) carrying out magnetism to obtain the ternary cathode material with the surface double-coated.
Comparative example 1 ternary positive electrode material without coating.
Corresponding ternary lithium ion batteries are respectively prepared by using the example 2 and the comparative example 1, and the materials, the using amounts and the battery preparation methods of the two groups of lithium ion batteries except the anode material are the same. The following are the results of testing the performance of the batteries of example 2 and comparative example 1:
1. and (3) battery rate performance test:
the specific test method comprises the following steps: the batteries of comparative example 1 and example 2 were charged from 2.8V to 4.2V at a constant current of 1C, and the constant voltage charge of 4.2V was maintained, with a cutoff current of 0.05C; and then discharging to 2.8V at 1C/2C/3C respectively, sequentially recording the discharge capacity retention rate under different multiplying factors, and in the set of experiments, two battery cells are taken for testing in both the example 2 and the comparative example 1, and the test results are shown in the table 1 and the figure 2.
TABLE 1
Figure BDA0002752012010000051
As can be seen from table 1 and fig. 2, the capacity retention rate of the battery of example 2 is significantly better than that of the battery of comparative example 1 under the high-rate discharge, and the capacity retention rate of example 2 still reaches more than 91% when the battery is discharged at 3C rate; therefore, the rate performance of the battery is remarkably improved when the double-coated modified ternary cathode material prepared by the method is applied to the lithium ion battery.
2. Testing the high-temperature cycle performance of the battery:
the specific test method comprises the following steps: the batteries of example 2 and comparative example 1 were charged at a constant current of 1C from 2.8V to 4.2V, and were charged at a constant voltage of 4.2V, and were stopped at a current of 0.05C, and then discharged at a constant current of 1C to 2.8V, and the batteries were cyclically charged and discharged for 1000 weeks in this step, and in this set of experiments, two cells were additionally used for the tests in both example 2 and comparative example 1, and the test results are shown in table 2 and fig. 3.
TABLE 2
Figure BDA0002752012010000052
Figure BDA0002752012010000061
As can be seen from table 2 and fig. 3, the capacity retention rate of the battery of comparative example 1 is less than 80.00% for about 600 weeks of the current cycle; the high-temperature cycle life of the battery in the embodiment 2 can be more than 800 weeks, so that the high-temperature cycle performance of the battery is improved by applying the double-coated modified ternary cathode material prepared by the invention to the lithium ion battery.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. A preparation method of a ternary anode material of a lithium ion battery is characterized by comprising the following steps,
adopts a solvothermal method to prepare Ni in a ternary precursorxCoyMnz(OH)2Growing CQDs on the surface of (x + y + z ═ 1) in situ, mixing the ternary precursor coated with the CQDs on the surface with an aluminum salt solution for reaction to obtain a ternary precursor double-coated on the surface, and finally adding a lithium source for mixing and sintering to obtain the ternary cathode material double-coated on the surface.
2. The preparation method of the ternary cathode material of the lithium ion battery according to claim 1, wherein the solvent thermal method comprises the following specific steps: mixing ethylene glycol (CH)2OH)2Placing the ternary precursor and the precursor in a beaker according to the mass ratio of 1-2:4-6, continuously stirring for 1-3h, transferring the uniformly mixed solution into a reaction kettle, heating to 160-fold sand 240 ℃, preserving heat for 4-6h, and cooling to the temperature of 160-fold sand 240 DEG CCentrifuging and washing the precipitate at room temperature, and drying the precipitate at the temperature of 100-120 ℃ in vacuum for 4-8h to obtain the precursor of the ternary material with the surface coated with CQDs.
3. The preparation method of the ternary cathode material for the lithium ion battery according to claim 1, wherein the preparation steps of the surface double-coated ternary precursor are as follows: adding a ternary precursor with the surface coated with CQDs into deionized water, and adding Al2(SO4)3Adding into deionized water, reacting to obtain slurry, aging for 1-3 hr, washing, and drying to obtain surface double-coated CQDs and Al2O3The ternary precursor of (2).
4. The preparation method of the ternary cathode material for the lithium ion battery according to claim 3, wherein the mass ratio of the ternary precursor of the surface-coated CQDs to the deionized water is 1: 50-100.
5. The method for preparing the ternary cathode material of the lithium ion battery as claimed in claim 3, wherein the surface is doubly coated with CQDs and Al2O3Al in the ternary precursor2O3The coating layer accounts for 1-10% by mass.
6. The method of claim 1, wherein the lithium source and the ternary precursor Ni are selected from the group consisting of lithium ion battery ternary cathode materials and lithium ion battery ternary cathode materialsxCoyMnz(OH)2In a molar ratio of 1.02-1.07: 1.
7. The method for preparing the ternary cathode material of the lithium ion battery as claimed in claim 1, wherein the sintering is performed by calcining for 4-6h in a sintering furnace at 400-800 ℃, and oxygen is introduced into the furnace during sintering.
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