CN108878828B - Carbon-coated high-nickel ternary cathode material and preparation method thereof - Google Patents
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Abstract
The invention provides a carbon-coated high-nickel ternary cathode material and a preparation method thereof, belonging to the technical field of lithium battery cathode materials. The carbon-coated high-nickel ternary cathode material comprises the high-nickel ternary cathode material and a coating layer, wherein the coating layer is made of carbon, and the molar ratio of nickel, cobalt and manganese elements in the high-nickel ternary cathode material is 0.7:0.2: 0.25.
Description
Technical Field
The invention belongs to the technical field of lithium battery anode materials, and relates to a carbon-coated high-nickel ternary anode material and a preparation method thereof.
Background
Currently, the types of cathode materials which are commercially produced on a large scale are limited, such as lithium iron phosphate, ternary lithium cobaltate and the like. Among them, the ternary lithium battery is regarded by enterprises due to higher energy density and relatively lower production cost. However, for many years, due to the simple design concept of the ternary cathode material, the types of the materials are limited, 523, 622 and 811 are popular materials for large-scale commercial application, and due to the reversible capacity of the 523 and 622 ternary cathode materials, the increasing capacity requirement of the power battery of the electric automobile can not be met. 811 is high in nickel content, strong in alkalinity of the material, and easy to absorb water, and the positive electrode binder PVDF is easy to agglomerate, so that the processing performance is influenced, and even the production cannot be carried out. Therefore, the development of ternary materials has encountered bottlenecks.
Some functionalized coating materials can further improve the cycle performance and rate capability of the material. Carbon coating is an important means for improving the conductivity of the material, and has the advantages of low cost, environmental friendliness and the like, so that the carbon coating gradually becomes an important strategy for modifying the anode material. Various carbon coating means such as lithium iron phosphate have been widely used in the market.
The carbon coating of the conventional method is also very limited in the improvement and improvement of the performance. The reason is that in the ordinary carbon coating method, in the carbonization process, an ordinary carbon source forms reducing gas such as CO or H2 having reducing property, and the reducing gas has a certain influence on the ternary positive electrode material to a large extent. So that the valence states of various metals are changed, and the lattice structure is degenerated.
Disclosure of Invention
The first purpose of the invention is to provide a carbon-coated high-nickel ternary cathode material, and the second purpose of the invention is to provide a preparation method of the carbon-coated high-nickel ternary cathode material.
The first object of the present invention can be achieved by the following technical solutions: the carbon-coated high-nickel ternary cathode material is characterized by comprising a high-nickel ternary cathode material and a coating layer, wherein the coating layer is made of carbon, and the molar ratio of nickel, cobalt and manganese elements in the high-nickel ternary cathode material is 0.7:0.2: 0.25.
The second object of the present invention can be achieved by the following technical solutions: a preparation method of a carbon-coated high-nickel ternary cathode material is characterized by comprising the following steps of:
(1) dissolving nickel sulfate, cobalt sulfate and manganese sulfate in a molar ratio of 0.7:0.2:0.25 in a solvent to remove O2In deionized water;
(2) conveying the metal salt solution and the sodium hydroxide solution in the step (1) into a reaction kettle according to the flow rate of 1:1.15, and introducing ammonia water; controlling the pH value of the whole reaction system to be 11.5, controlling the stirring speed of the reaction kettle to be 580r/min, and controlling the temperature of the reaction slurry to be 65 ℃;
(3) filtering, washing and drying the slurry reacted in the step (2) at 120 ℃ to obtain a high-nickel ternary precursor;
(4) uniformly mixing the precursor in the step (3) and lithium carbonate in a mixer according to the mol ratio of 1: 0.53;
(5) putting the uniformly mixed material in the step (4) into a sagger and pushing the sagger into a kiln, reacting at the temperature of 785 ℃ for 18 hours, introducing O2 in the whole process, and obtaining a target product after the reaction is finished;
(6) adding the target product obtained in the step (5) and a precursor of silicon dioxide into a solvent, uniformly stirring, heating to 20-80 ℃, reacting for 2-7 h, evaporating the solvent to dryness, and finally calcining at 200-700 ℃ for 2-8 h to obtain a silicon dioxide-coated high-nickel ternary cathode material;
(7) mixing and dispersing the high-nickel ternary cathode material coated with the silicon dioxide and the carbon source obtained in the step (6) into a solvent according to the mass ratio of 1% -10%, stirring for reaction to obtain a suspension, washing and filtering the suspension to form a filter cake, drying, and calcining for 1-20 h at 100-1000 ℃ in air, nitrogen or argon to obtain the high-nickel ternary cathode material coated with the silicon dioxide and the carbon;
(8) and (4) soaking the silicon dioxide and carbon double-coated high-nickel ternary cathode material in the step (7) in an alkaline solution to obtain a carbon-coated high-nickel ternary cathode material.
Preferably, the precursor in step (6) is one or more of silica particles, silicon tetrachloride, ethyl orthosilicate and diphenyldibromo (silyl) silane.
Preferably, the solvent in step (6) is one or more of water, methanol, ethanol, isopropanol and ethylene glycol.
Preferably, the mass percentage of the silicon dioxide in the silicon dioxide-coated high-nickel ternary cathode material in the step (6) is 0.5-2 wt%.
Preferably, the carbon source in step (7) comprises an organic polymer material, a saccharide substance, and dopamine.
Preferably, the solvent of step (7) is one or more of water, ethanol, ethylene glycol, dichloromethane, methanol and isopropanol.
Preferably, the alkaline solution in step (8) is one or more of sodium hydroxide, potassium hydroxide, ammonia water, sodium bicarbonate and sodium carbonate.
Preferably, the concentration of the alkaline solution in the step (8) is 0.1mol/L-2 mol/L.
The invention has the beneficial effects that:
1. the traditional ternary cathode material is designed by the idea that the molar ratio sum of nickel, cobalt and manganese is 1, and the high-nickel cathode material is prepared by the principle that the molar ratio of elements such as lithium (+ 1), nickel (+ 2), cobalt (+ 3) and manganese (+ 4) in the ternary material meets the material electric neutrality, so that the novel high-nickel ternary cathode material LiNi0.7Co0.2Mn0.25O2 is prepared.
2. According to the method for preparing the carbon-coated high-nickel ternary cathode material, silicon dioxide is used as an intermediate protective layer, a carbon source is prevented from releasing reducing gas to reduce a main body material in a high-temperature carbonization process, and the formed carbon coating layer can more obviously show excellent conductivity of conductive carbon, so that the large-current charge and discharge capacity of a battery is improved, and the rate capability is improved.
3. The carbon-coated high-nickel ternary cathode material has good material cycling stability and rate capability.
4. The method provided by the embodiment of the invention is simple in preparation process, low in cost and suitable for industrial production.
Drawings
FIG. 1 is a scanning electron microscope image of an uncoated high-nickel ternary positive electrode material.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1 preparation of a high nickel ternary cathode material
Dissolving nickel sulfate, cobalt sulfate and manganese sulfate in deionized water with O2 removed according to the molar ratio of 0.7:0.2: 0.25; conveying a metal salt solution and a sodium hydroxide solution into a reaction kettle according to the flow rate of 1:1.15, and introducing ammonia water; controlling the pH value of the whole reaction system to be 11.5, controlling the stirring speed of the reaction kettle to be 580r/min, and controlling the temperature of the reaction slurry to be 65 ℃; filtering the reacted slurry, washing, and drying at 120 ℃ to obtain a high-nickel ternary precursor; uniformly mixing the high-nickel ternary precursor and lithium carbonate in a proportion of 1:0.53 mol in a mixer; putting the uniformly mixed materials into a sagger and pushing the sagger into a kiln, reacting at the temperature of 785 ℃ for 18 hours, introducing O2 in the whole process, and obtaining the target product after the reaction is finished.
Example 2 one of the preparations of carbon-coated high-nickel ternary cathode materials
1. Mixing the prepared high-nickel ternary cathode material and tetraethoxysilane (converted into silicon dioxide) in an ethanol phase according to the mass ratio of 1:0.01, stirring for 3 hours at 60 ℃, dropwise adding a certain amount of deionized water according to a stoichiometric ratio, reacting for 3 hours at 800r/min, heating to 100 ℃ to release all solvents, scraping powder, placing in air at 500 ℃ to sinter for 5 hours, and then cooling to obtain the silicon dioxide coated high-nickel ternary cathode material.
2. Adding the silicon dioxide coated high-nickel ternary cathode material into a 5% glucose aqueous solution, heating, stirring, evaporating to dryness, and sintering in a tubular furnace at 800 ℃ in a nitrogen atmosphere for 3 hours to obtain the silicon dioxide and carbon double-coated high-nickel ternary cathode material.
3. And (3) soaking the high-nickel ternary anode material double-coated with silicon dioxide and carbon in 0.5mol/L NaOH solution for 1h, etching to obtain a pure carbon-coated material, and then filtering and drying to finish the preparation of the carbon-coated anode material.
Example 3 preparation of carbon-coated high-nickel ternary cathode Material
1. Mixing the prepared high-nickel ternary cathode material and silicon tetrachloride (converted into silicon dioxide) in a mass ratio of 1:0.005 in an ethanol phase, stirring at 20 ℃ for 7 hours, dropwise adding a certain amount of deionized water according to a stoichiometric ratio, reacting at 800r/min for 3 hours, heating to 100 ℃ to completely dissolve all the solvent, scraping the powder, juxtaposing, sintering in air at 200 ℃ for 8 hours, and cooling to obtain the silicon dioxide-coated high-nickel ternary cathode material.
2. Adding the silicon dioxide coated high-nickel ternary cathode material into 1% glucose aqueous solution, heating and stirring, evaporating to dryness, then placing into a tubular furnace, sintering at 100 ℃ for 20h in the atmosphere of nitrogen, and obtaining the silicon dioxide and carbon double-coated high-nickel ternary cathode material.
3. And (3) soaking the material in the high-nickel ternary anode material double-coated with silicon dioxide and carbon in 0.1mol/L ammonia water solution for 1h, etching to obtain a pure carbon-coated material, and then filtering and drying to finish the preparation of the carbon-coated anode material.
EXAMPLE 4 preparation of carbon-coated high-nickel ternary cathode Material III
1. Mixing the prepared high-nickel ternary cathode material and silicon dioxide particles in a methanol phase according to a mass ratio of 1:0.02, stirring for 2h at 80 ℃, dropwise adding a certain amount of deionized water according to a stoichiometric ratio, reacting for 3h at 800r/min, heating to 100 ℃ to complete all solvents, scraping powder, placing in air at 700 ℃ to sinter for 2h, and then cooling to obtain the silicon dioxide coated high-nickel ternary cathode material.
2. Adding the silicon dioxide coated high-nickel ternary cathode material into 10% glucose aqueous solution, heating and stirring, evaporating to dryness, then placing into a tubular furnace, sintering for 1h at 1000 ℃ in the atmosphere of nitrogen, and double-coating the silicon dioxide and carbon high-nickel ternary cathode material.
3. And (3) soaking the silicon dioxide and carbon double-coated high-nickel ternary cathode material in 2mol/L KOH solution for 1h, etching to obtain a pure carbon-coated material, and then filtering and drying to finish the preparation of the carbon-coated cathode material.
Comparative example 1
A prepared high-nickel ternary positive electrode material is added into a 10% glucose aqueous solution, heated, stirred and evaporated to dryness. Then the mixture is put into a tube furnace and sintered for 3 hours at 800 ℃ under the atmosphere of nitrogen. And obtaining the carbon-coated high-nickel ternary cathode material.
Comparative example 2
Adding a common nickel-cobalt-manganese ternary cathode material (Li (Ni5Co2Mn3) O2) into a 10% glucose aqueous solution, heating, stirring, and evaporating to dryness. Then the mixture is put into a tube furnace and sintered for 3 hours at 800 ℃ under the atmosphere of nitrogen. And obtaining the carbon-coated nickel-cobalt-manganese ternary cathode material.
Performance testing
The battery assembling method comprises the following steps: the positive electrode material powders in examples 1 to 4 and comparative example 1 were mixed with conductive carbon black super p and a binder polyvinylidene fluoride (PVDF) at a mass ratio of 85: 10: 5, grinding by hand to be uniform. Adding a certain amount of 1-methyl-2-pyrrolidone (NMP), and uniformly stirring by using a homogenizer. Then, blade coating was carried out with a flat coater, and the blade coating thickness was set to 0.02mm (before drying). Drying at 80 deg.C for five hours, and vacuum oven drying at 100 deg.C overnight. And cutting the electrode plates into electrode plates with the diameter of 11.7mm, and then putting the electrode plates into an argon box to assemble the batteries in sequence. And standing for one day after the assembly is finished, and testing.
The test method comprises the following steps: the battery is tested on a blue 5V-5mA or 5V-10mA battery test system, and the test method is to carry out charge and discharge experiments on an electrochemical window of 2.8-4.3V based on the current density of 1C-180 mA/g; and the charge and discharge cycles are completed under different multiplying factors of 0.2C, 0.5C, 1C, 2C and 5C.
Results of the experiment
The batteries of examples 1 to 4 and comparative example 1 were tested for discharge capacity (unit: mAh/g) at 0.5C rate in a voltage range of 4.3V, and the test results are shown in Table 1:
the batteries of examples 1 to 4 and comparative example 1 were tested for discharge capacity (unit: mAh/g) at a rate of 0.2C, 0.5C, 1C, 2C, 5C, respectively, and were cycled again at 0.2C after rate cycling, and the specific discharge capacity results are shown in Table 2:
the specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (8)
1. A preparation method of a carbon-coated high-nickel ternary cathode material is characterized by comprising the following steps of:
(1) dissolving nickel sulfate, cobalt sulfate and manganese sulfate in a molar ratio of 0.7:0.2:0.25 in a solvent to remove O2In deionized water;
(2) conveying the metal salt solution and the sodium hydroxide solution in the step (1) into a reaction kettle according to the flow rate of 1:1.15, and introducing ammonia water; controlling the pH value of the whole reaction system to be 11.5, controlling the stirring speed of the reaction kettle to be 580r/min, and controlling the temperature of the reaction slurry to be 65 ℃;
(3) filtering, washing and drying the slurry reacted in the step (2) at 120 ℃ to obtain a high-nickel ternary precursor;
(4) uniformly mixing the precursor in the step (3) and lithium carbonate in a mixer according to the mol ratio of 1: 0.53;
(5) putting the uniformly mixed materials in the step (4) into a sagger and pushing the sagger into a kiln, reacting at the temperature of 785 ℃ for 18 hours, and introducing O in the whole process2(iii) reaction junctionBundling to obtain a target product;
(6) adding the target product obtained in the step (5) and a precursor of silicon dioxide into a solvent, uniformly stirring, heating to 20-80 ℃, reacting for 2-7 h, evaporating the solvent to dryness, and finally calcining at 200-700 ℃ for 2-8 h to obtain a silicon dioxide-coated high-nickel ternary cathode material;
(7) mixing and dispersing the high-nickel ternary cathode material coated with the silicon dioxide and the carbon source obtained in the step (6) into a solvent according to the mass ratio of 1% -10%, stirring for reaction to obtain a suspension, washing and filtering the suspension to form a filter cake, drying, and calcining for 1-20 h at 100-1000 ℃ in air, nitrogen or argon to obtain the high-nickel ternary cathode material coated with the silicon dioxide and the carbon;
(8) and (4) soaking the silicon dioxide and carbon double-coated high-nickel ternary cathode material in the step (7) in an alkaline solution to obtain a carbon-coated high-nickel ternary cathode material.
2. The method for preparing the carbon-coated high-nickel ternary cathode material as claimed in claim 1, wherein the precursor in the step (6) is one or more of silica particles, silicon tetrachloride, ethyl orthosilicate and diphenyldibromo (silyl) silane.
3. The method for preparing the carbon-coated high-nickel ternary cathode material as claimed in claim 1, wherein the solvent in the step (6) is one or more of water, methanol, ethanol, isopropanol and ethylene glycol.
4. The method for preparing the carbon-coated high-nickel ternary cathode material according to claim 1, wherein the mass percentage of the silicon dioxide in the silicon dioxide-coated high-nickel ternary cathode material in the step (6) is 0.5-2 wt%.
5. The method for preparing a carbon-coated high-nickel ternary cathode material as claimed in claim 1, wherein the carbon source in step (7) comprises an organic polymer material, a saccharide substance or dopamine.
6. The method for preparing the carbon-coated high-nickel ternary cathode material according to claim 1, wherein the solvent in the step (7) is one or more of water, ethanol, ethylene glycol, dichloromethane, methanol and isopropanol.
7. The method for preparing the carbon-coated high-nickel ternary cathode material as claimed in claim 1, wherein the alkaline solution in the step (8) is one or more of sodium hydroxide, potassium hydroxide, ammonia water, sodium bicarbonate and sodium carbonate.
8. The method for preparing the carbon-coated high-nickel ternary cathode material as claimed in claim 1, wherein the concentration of the alkaline solution in the step (8) is 0.1mol/L-2 mol/L.
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| CN109728279A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The surface treatment method and product and battery of a kind of nickelic tertiary cathode material |
| CN110504425A (en) * | 2019-08-16 | 2019-11-26 | 安徽师范大学 | A kind of yolk shell structure sulfur granules/polypyrrole conductive hydrogel composite material and preparation method thereof and lithium-sulphur cell positive electrode and battery |
| CN111217408B (en) * | 2020-01-16 | 2022-08-12 | 东莞东阳光科研发有限公司 | High-nickel anode material and preparation method and application thereof |
| CN113140713B (en) * | 2020-01-20 | 2022-07-26 | 中国科学院金属研究所 | LiFePO 4 /C-coated ternary cathode material and preparation method and application thereof |
| CN113889624B (en) * | 2020-07-02 | 2023-09-29 | 中国石油化工股份有限公司 | Carbon-coated ternary positive electrode material, and preparation method and application thereof |
| CN112151781A (en) * | 2020-09-24 | 2020-12-29 | 贵州梅岭电源有限公司 | Rapid composite coating modification method for lithium battery positive electrode material |
| CN114005970B (en) * | 2021-10-12 | 2023-06-02 | 合肥国轩高科动力能源有限公司 | Carbon/conductive polymer coated ternary positive electrode material and preparation method thereof |
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