CN108878825B - Surface-coated positive electrode material and preparation method thereof - Google Patents
Surface-coated positive electrode material and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention is applicable to the technical field of lithium battery anode materials, and provides a surface-coated anode material and a preparation method thereofbLamZrnO12The method not only improves the cycle performance and the rate capability of the material, but also coats the anode material in the washing process, simplifies the wet coating process of the prior medium-high nickel material, utilizes a spray drying method for drying, improves the drying efficiency, and greatly reduces the ion concentration in the washing water, thereby reducing the processing difficulty, utilizes a rotary kiln for coating and secondary burning, also improves the equipment productivity, reduces the usage amount of saggars, reduces the energy consumption of the secondary burning, simultaneously has more uniform sintering material, and ensures that the surface after sintering is uniformly coated with LibLamZrnO12The nickel cobalt lithium manganate anode material has better comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of lithium battery anode materials, and particularly relates to a surface-coated anode material and a preparation method thereof.
Background
In order to relieve the increasingly serious energy crisis and environmental pollutionIn addition, a series of policies are issued in all countries in the world to promote the upgrading of fuel vehicles to electric vehicles. The requirement of electric automobiles on high energy density of batteries promotes the rapid development of high-nickel ternary materials. The overall energy density of the ternary material is improved with the increase of the nickel content, but the structural stability of the material is reduced due to the reduction of the contents of cobalt, manganese/aluminum and the like. Meanwhile, the surface of the high nickel material has high residual alkali (LiOH, Li)2CO3) The characteristics of the electrolyte also cause the occurrence of gel when the anode material is mixed with slurry in the process of preparing the lithium ion battery, thereby causing the problem of difficult preparation of a pole piece, and the residual alkali can react with the electrolyte in the use process of the battery to generate gas, thereby causing the battery failure and seriously affecting the safety performance of the battery. Aiming at the defects of poor structural stability and high residual alkali of the existing high nickel material, the existing common solution is to add the processes of washing, filtering, coating, secondary sintering and the like to the production process of the high nickel material so as to strengthen and improve the cycle performance, rate capability, safety performance and the like of the high nickel. However, these additional steps increase the production cost, and further, the residual heavy metal-containing wastewater or solvent which has not completely reacted is troublesome for the subsequent recovery work.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a surface-coated positive electrode material and a method for preparing the same, which aims to simplify the conventional preparation process of a high-nickel positive electrode material and improve the cycle performance and rate capability of the material by using residual alkali on the surface of the material.
In one aspect, the surface-coated cathode material and the preparation method thereof comprise the following steps:
step S1, dissolving a certain mass of zirconium acetate and lanthanum acetate in deionized water, and then uniformly mixing the nickel cobalt lithium manganate positive electrode material and the deionized water in a constant-temperature water bath according to a certain metering ratio to obtain positive electrode material slurry containing zirconium acetate, lanthanum acetate and LiOH;
s2, slowly adding ammonia water and acetic acid into the positive electrode material slurry obtained in the step S1, continuously stirring in the adding process, adjusting the pH value of the slurry to 8-10, continuously stirring after the pH value of the slurry is adjusted, and performing hydrolysis reaction on zirconium acetate in the stirring process to obtain nano zirconium and lanthanum hydroxide and slurry of the nickel cobalt lithium manganate positive electrode material;
step S3, transferring the slurry obtained in the step S2 to spray drying equipment for drying treatment to obtain powder of the nickel cobalt lithium manganate positive electrode material mixed with a trace amount of LiOH, zirconium hydroxide and lanthanum hydroxide;
step S4, the powder obtained in the step S3 is burnt in a rotary kiln, the atmosphere of air or oxygen is kept, and the nano-grade zirconium hydroxide and lanthanum hydroxide react with residual LiOH on the surface of the anode material to generate Li in the burning processbLamZrnO12To obtain the Li with uniform surface coatingbLamZrnO12The positive electrode material of (1).
On the other hand, the surface-coated cathode material inner layer is a nickel cobalt lithium manganate cathode material LiaNixCoyMn1-x- yO2Wherein a is more than or equal to 0.9 and less than or equal to 1.2, x is more than or equal to 0.6, y is more than 0 and less than or equal to 0.3, and the outer layer is LibLamZrnO12And (4) coating.
The invention has the beneficial effects that: the invention provides a surface-coated positive electrode material and a preparation method thereof, and Li is coated on the outer layer of a nickel cobalt lithium manganate positive electrode materialbLamZrnO12The method not only improves the cycle performance and the rate capability of the material, but also coats the anode material in the washing process, simplifies the wet coating process of the prior medium-high nickel material, utilizes a spray drying method for drying, improves the drying efficiency, and greatly reduces the ion concentration in the washing water, thereby reducing the processing difficulty, utilizes a rotary kiln for coating and secondary burning, also improves the equipment productivity, reduces the usage amount of saggars, reduces the energy consumption of the secondary burning, simultaneously has more uniform sintering material, and ensures that the surface after sintering is uniformly coated with LibLamZrnO12The nickel cobalt lithium manganate anode material has better comprehensive performance.
Drawings
FIG. 1 is a view showing Li cladding in example 1 of the present inventionbLamZrnO12Lithium nickel cobalt manganese oxide positive electrode material and comparative example 1The volume retention rate of the lithium battery with the nickel cobalt lithium manganate positive electrode material is compared with the figure.
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.
The surface-coated positive electrode material and the preparation method thereof provided by the invention comprise the following steps:
step S1, dissolving a certain mass of zirconium acetate and lanthanum acetate in deionized water, and then uniformly mixing the nickel cobalt lithium manganate positive electrode material and the deionized water in a constant-temperature water bath according to a certain metering ratio to obtain positive electrode material slurry containing zirconium acetate, lanthanum acetate and LiOH;
in the step, the total amount of lithium left on the surface of the nickel cobalt lithium manganate positive electrode material is 1.0-3.5 mol%, the mass of zirconium acetate is 300-2000 ppm of the total mass of the nickel cobalt lithium manganate positive electrode material, the mass of lanthanum acetate is 800-4500 ppm of the total mass of the nickel cobalt lithium manganate positive electrode material, the mass ratio of the nickel cobalt lithium manganate positive electrode material to deionized water is 1: 0.7-1: 3, and the temperature of a constant-temperature water bath is 25-65 ℃.
S2, slowly adding ammonia water and acetic acid into the positive electrode material slurry obtained in the step S1, continuously stirring in the adding process, adjusting the pH value of the slurry to 8-10, continuously stirring after the pH value of the slurry is adjusted, and performing hydrolysis reaction on zirconium acetate in the stirring process to obtain nano zirconium and lanthanum hydroxide and slurry of the nickel cobalt lithium manganate positive electrode material;
in the step, the stirring speed is 300-800 r/min, and the stirring time after the pH of the slurry is adjusted to 8-10 is 0.5-3.0 h.
Step S3, transferring the slurry obtained in the step S2 to spray drying equipment for drying treatment to obtain powder of the nickel cobalt lithium manganate positive electrode material mixed with a trace amount of LiOH, zirconium hydroxide and lanthanum hydroxide;
in this step, the inlet temperature of the spray drying equipment is controlled at 250 ℃ of 200-.
Step S4, the powder obtained in the step S3 is burnt in a rotary kiln, the atmosphere of air or oxygen is kept, and the nano-grade zirconium hydroxide and lanthanum hydroxide react with residual LiOH on the surface of the anode material to generate Li in the burning processbLamZrnO12To obtain the Li with uniform surface coatingbLamZrnO12The positive electrode material of (1).
In the step, the firing temperature in the rotary kiln is 400-.
The inner layer of the finally prepared surface-coated positive electrode material is a nickel cobalt lithium manganate positive electrode material LiaNixCoyMn1-x-yO2Wherein a is more than or equal to 0.9 and less than or equal to 1.2, x is more than or equal to 0.6, y is more than 0 and less than or equal to 0.3, and the outer layer is LibLamZrnO12And (4) coating.
According to the invention, in the process of preparing the nickel cobalt lithium manganate cathode material, zirconium hydroxide and lanthanum hydroxide are added to carry out solid-phase reaction with residual LiOH on the surface of the material, so that residual alkali on the surface of the material is reduced, the processability of the material in the subsequent battery manufacturing process is improved, and Li is generated by reactionbLamZrnO12The coating is coated on the surface of the material, so that the corrosion of the electrolyte to the material is weakened, and the structural stability of the material is improved, so that the cycle performance of the material is improved, and the coating has higher ionic conductivity and improves the rate capability of the material; the anode material is coated in the water washing process, so that the wet coating process of the conventional medium-high nickel material is simplified, the spray drying method is used for drying, the drying efficiency is improved, and the ion concentration in the washing water is greatly reduced, so that the treatment difficulty is reduced; in addition, the invention uses the rotary kiln to coat the secondary sintering, thereby not only improving the productivity of the equipment, reducing the using amount of the saggars and the energy consumption of the secondary sintering, but also ensuring that the sintered surface is uniformly coated with LibLamZrnO12The nickel cobalt lithium manganate anode material has better comprehensive performance.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
Example 1:
1) weighing 100g of nickel cobalt lithium manganate positive electrode material, 0.3g of zirconium acetate and 0.7g of lanthanum acetate, dissolving the zirconium acetate and the lanthanum acetate in 100g of deionized water, and then uniformly mixing the nickel cobalt lithium manganate positive electrode material and the deionized water in a constant-temperature water bath to obtain positive electrode material slurry containing zirconium acetate, lanthanum acetate and LiOH.
2) And (2) slowly adding ammonia water and acetic acid into the positive electrode material slurry obtained in the step (1), continuously stirring at the stirring speed of 500r/min in the adding process, adjusting the pH of the slurry to 8-10, continuously stirring for 1h after the pH is adjusted, and carrying out hydrolysis reaction on zirconium acetate in the stirring process to obtain slurry mixed with the nano zirconium and lanthanum hydroxide and the nickel cobalt lithium manganate positive electrode material.
3) And (4) transferring the slurry obtained in the step (S2) to spray drying equipment for drying treatment, wherein the inlet temperature of the spray drying equipment is controlled at 210 ℃, the outlet temperature of the spray drying equipment is controlled at 120 ℃, and powder of the nickel cobalt lithium manganate positive electrode material mixed with trace LiOH, zirconium hydroxide and lanthanum hydroxide is obtained.
4) Putting the powder obtained in the step S3 into a rotary kiln, keeping the atmosphere of air or oxygen, firing for 6h at 550 ℃, and reacting the nano-grade zirconium hydroxide and lanthanum hydroxide with residual LiOH on the surface of the positive electrode material to generate Li in the firing processbLamZrnO12To obtain the Li with uniform surface coatingbLamZrnO12The nickel cobalt lithium manganate anode material.
Comparative example 1:
the lithium nickel cobalt manganese oxide cathode material obtained in the step 1 of the embodiment 1 is taken.
The positive electrode material obtained in example 1 was a material in which the surface was uniformly coated with LibLamZrnO12The nickel cobalt lithium manganate positive electrode material of comparative example 1 is an uncoated nickel cobalt lithium manganate positive electrode material, after the positive electrode materials of example 1 and comparative example 1 are made into batteries for charging (at the moment, the electrode plate is fully contacted with electrolyte), the positive electrode plate is taken out, and the batteries are charged to 4.3V at constant current, and the constant current charging current is 1And 2C, carrying out discharge capacity test under the condition that the constant current discharge current is 1C. The test result is shown in fig. 1, the discharge capacity of the nickel cobalt lithium manganate positive electrode material coated by the hydroxide of zirconium and lanthanum in example 1 prepared by the method of the present invention starts to decrease significantly when the number of cyclic charge and discharge is 20, while the discharge capacity of the nickel cobalt lithium manganate positive electrode material coated by the hydroxide of zirconium and lanthanum in example 1 prepared by the method of the present invention decreases by less than 5mAh/g when the number of cyclic charge and discharge reaches 50, which indicates that the positive electrode material prepared by the method of the present invention has excellent cycle performance; in addition, the discharge capacity of the cathode material prepared by the method is obviously superior to that of the uncoated nickel cobalt lithium manganate cathode material. Therefore, the nickel cobalt lithium manganate positive electrode material coated by the hydroxide of zirconium and lanthanum not only improves the structure stability of the material and the cycle performance of the material, but also improves the rate capability of the material because the coating zirconium and lanthanum have higher ionic conductivity.
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 surface-coated cathode material is characterized by comprising the following steps:
step S1, dissolving a certain mass of zirconium acetate and lanthanum acetate in deionized water, and then uniformly mixing the nickel cobalt lithium manganate positive electrode material and the deionized water in a constant-temperature water bath according to a certain metering ratio to obtain positive electrode material slurry containing zirconium acetate, lanthanum acetate and LiOH, wherein residual alkali LiOH remains on the surface of the nickel cobalt lithium manganate positive electrode material;
s2, slowly adding ammonia water and acetic acid into the positive electrode material slurry obtained in the step S1, continuously stirring in the adding process, adjusting the pH value of the slurry to 8-10, continuously stirring after the pH value of the slurry is adjusted, and performing hydrolysis reaction on zirconium acetate in the stirring process to obtain nano zirconium and lanthanum hydroxide and slurry of the nickel cobalt lithium manganate positive electrode material;
step S3, transferring the slurry obtained in the step S2 to spray drying equipment for drying treatment to obtain powder of the nickel cobalt lithium manganate positive electrode material mixed with a trace amount of LiOH, zirconium hydroxide and lanthanum hydroxide;
step S4, the powder obtained in the step S3 is burnt in a rotary kiln, the atmosphere of air or oxygen is kept, and the nano-grade zirconium hydroxide and lanthanum hydroxide react with residual LiOH on the surface of the anode material to generate Li in the burning processbLamZrnO12To obtain the Li with uniform surface coatingbLamZrnO12The positive electrode material of (1).
2. The method of claim 1, wherein in step S1, the total amount of lithium remaining on the surface of the lithium nickel cobalt manganese oxide positive electrode material is 1.0 mol% to 3.5 mol%, the mass of zirconium in zirconium acetate is 300 ppm to 2000ppm of the total mass of the lithium nickel cobalt manganese oxide positive electrode material, the mass of lanthanum in lanthanum acetate is 800 ppm to 4500ppm of the total mass of the lithium nickel cobalt manganese oxide positive electrode material, the mass ratio of the lithium nickel cobalt manganese oxide positive electrode material to deionized water is 1:0.7 to 1:3, and the temperature of the constant temperature water bath is 25 ℃ to 65 ℃.
3. The method of claim 1, wherein in step S2, the stirring speed is 300-800 r/min, and the stirring time after the pH of the slurry is adjusted to 8-10 is 0.5-3.0 h.
4. The method as claimed in claim 1, wherein in step S3, the inlet temperature of the spray drying device is controlled at 250 ℃ and the outlet temperature is controlled at 130 ℃ and 200 ℃.
5. The method as claimed in claim 1, wherein in step S4, the firing temperature in the rotary kiln is 400-600 ℃, and the firing time is 5-12 h.
6. A surface-coated positive electrode material, characterized in that the surface-coated positive electrode material is prepared by the method according to any one of claims 1 to 5The inner layer of the cathode material coated on the surface is a nickel cobalt lithium manganate cathode material LiaNixCoyMn1-x-yO2Wherein a is more than or equal to 0.9 and less than or equal to 1.2, x is more than or equal to 0.6, y is more than 0 and less than or equal to 0.3, and the outer layer is LibLamZrnO12And (4) coating.
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| CN110767899B (en) * | 2019-10-24 | 2021-06-29 | 厦门厦钨新能源材料股份有限公司 | Preparation method of composite anode material of lithium ion battery |
| CN112366295A (en) * | 2020-09-04 | 2021-02-12 | 万向一二三股份公司 | Spherical ternary composite cathode material of lithium ion battery and preparation method thereof |
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