CN111029550A - Surface modification method of high-nickel cathode material of lithium ion battery - Google Patents
Surface modification method of high-nickel cathode material of lithium ion battery Download PDFInfo
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- CN111029550A CN111029550A CN201911316698.7A CN201911316698A CN111029550A CN 111029550 A CN111029550 A CN 111029550A CN 201911316698 A CN201911316698 A CN 201911316698A CN 111029550 A CN111029550 A CN 111029550A
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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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Abstract
The invention discloses a surface modification method of a high-nickel anode material of a lithium ion battery, which comprises the following steps of mixing the high-nickel anode material with deionized water, and stirring to form slurry; then, under the condition of stirring, simultaneously adding an acidic solution and a precipitator solution into the slurry, and maintaining the pH of the reaction system to be 10.0-12.0 for reaction; then carrying out solid-liquid separation on the slurry obtained after the reaction, drying the obtained solid, and sieving to obtain an unfired high-nickel cathode material with a coating layer on the surface; and finally, heating the high-nickel anode material with the coating layer on the surface to 300-700 ℃ in an oxygen atmosphere, preserving the heat for 3-12 h, and then cooling to room temperature to obtain the surface-modified high-nickel anode material. The method effectively improves the processing performance in the battery preparation process, simplifies the preparation process, saves the production cost and improves the cycling stability of the material.
Description
Technical Field
The invention relates to the technical field of high-nickel anode materials of lithium ion batteries, relates to reduction of residual Li on the surface of a high-nickel anode material or formation of a lithium-containing coating layer, and particularly relates to a surface modification method of a high-nickel anode material of a lithium ion battery.
Background
Lithium ion batteries have been successfully applied to various electronic devices and equipment due to their advantages of high energy density, long service life, no pollution, etc. After the commercial application of lithium ion batteries for nearly 30 years, the positive electrode material still is one of the key factors restricting the development of the overall performance of the batteries. The high nickel anode material of the lithium ion battery becomes a hotspot of the current industrialization due to low raw material price, high capacity, simple preparation process and the like. However, the nickel content of the material is high, the material is sensitive to moisture, and lithium hydroxide and lithium carbonate are easily generated on the surface, so that the residual lithium on the surface of the material is too high, and the problems of poor processing performance, serious capacity loss, poor cycle stability, serious gas expansion and the like in the battery preparation process are caused, thereby restricting the commercialization process of the high-nickel cathode material. Therefore, it is important to perform surface modification treatment on the high nickel positive electrode material.
Disclosure of Invention
The invention provides a surface modification method of a high-nickel anode material of a lithium ion battery, which aims to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a surface modification method of a high-nickel cathode material of a lithium ion battery comprises the following steps:
(1) mixing the high-nickel anode material with deionized water, and stirring to obtain slurry;
(2) adding an acidic solution or simultaneously adding the acidic solution and a precipitator solution into the slurry obtained in the step (1) under the condition of stirring, and maintaining the pH value of a reaction system to be 10.0-12.0 for reaction;
(3) carrying out solid-liquid separation on the slurry obtained after the reaction in the step (2), drying the obtained solid, and sieving to obtain an unfired high-nickel cathode material with a coating layer on the surface;
(4) heating the high-nickel anode material with the coating layer on the surface to 300-700 ℃ in an oxygen atmosphere, preserving the heat for 3-12 h, and then cooling to room temperature to obtain the surface-modified high-nickel anode material.
Further, the mass of the deionized water in the step (1) is 0.5-10 times of that of the high-nickel cathode material.
Further, the chemical formula of the high-nickel cathode material in the step (1) is LiNixM1-xO2Wherein x is more than or equal to 0.8, and M is one or more of Co, Mn and Al.
Further, the acid solution in the step (2) is one of oxalic acid solution, acetic acid solution, boric acid solution, silicic acid solution and phosphoric acid solution, and the concentration of the acid solution is 0.01-0.1 mol/L.
Further, the precipitator in the step (2) is at least one of soluble nitrate, chloride, acetate and acetate of B, Mg, Al, Si, Co, Ni, Ti, Zn, Cr, Zr, Mo, Y, V, Ga, Ge, Sc, Nb, Sn, Te, La or W, and the concentration of the solution of the precipitator is less than 0.05 mol/L.
Furthermore, the mass of the cation in the precipitant solution in the step (2) is 300-3000 ppm.
Further, the reaction temperature in the step (2) is 20-40 ℃, and the stirring time is 5-60 min.
Further, in the step (3), the drying temperature is 120 ℃, and the drying time is 4-12 h.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a method for modifying the surface of a high-nickel anode material of a lithium ion battery, which utilizes OH in residual alkali on the surface of the high-nickel anode material-And CO3 2-And weak acid radicals and cations added in the solution form precipitates to coat the surfaces of the particles, so that the alkali amount on the surfaces of the materials is reduced, and the generated precipitates coat the surfaces of the particles. The process combines the water washing process and the coating process into a one-step method for modification, and directly achieves the effects of reducing alkali and coating simultaneously in the water washing process; the coating agent can be uniformly distributed on the surfaces of the material particles by adopting wet coating; the complex process of coating after washing and drying is avoided, the preparation efficiency is greatly improved, the requirement on equipment is low, the cost is relatively low, and the method is suitable for industrial production.
Drawings
Fig. 1 is an X-ray powder diffraction contrast chart of the surface-modified high nickel cathode material in example 1 of the present invention and the non-surface-modified high nickel cathode material in comparative example 1.
Fig. 2 is a scanning electron microscope image of the surface-modified high-nickel cathode material in example 2 of the present invention.
Fig. 3 is a schematic diagram showing the comparison of the cycle performance of the surface-modified high nickel cathode material in example 3 of the present invention and the non-surface-modified high nickel cathode material in comparative example 3.
Detailed Description
Embodiments of the invention are described in further detail below:
a surface modification method for a high-nickel cathode material of a lithium ion battery comprises the following steps:
(1) mixing a certain amount of high-nickel anode material with 50-1000 wt% of deionized water, stirring to form slurry, and placing the slurry into a kettle;
(2) under the condition of stirring, adding an acid solution into the kettle by using a peristaltic pump or simultaneously adding the acid solution and a precipitator solution, maintaining the pH of a reaction system within the range of 10.0-12.0, and stirring for 5-60 min at the reaction temperature of 20-40 ℃;
wherein the acid solution is one of oxalic acid solution, acetic acid solution, boric acid solution, silicic acid solution and phosphoric acid solution, and the concentration of the acid solution is 0.01-0.1 mol/L; the precipitator is at least one of soluble nitrate, chloride, acetate and acetate of B, Mg, Al, Si, Co, Ni, Ti, Zn, Cr, Zr, Mo, Y, V, Ga, Ge, Sc, Nb, Sn, Te, La or W, and the concentration of the solution of the precipitator is less than 0.05 mol/L.
(3) And carrying out solid-liquid separation on the obtained slurry, drying the obtained solid for 4-16 h at 120 ℃, and sieving to obtain the high-nickel cathode material with the coating layer on the surface.
(4) And (3) heating the material obtained in the step (3) to 300-700 ℃ in an oxygen atmosphere, preserving heat for 3-12 hours, and then cooling to room temperature to obtain the surface-modified high-nickel anode material, wherein the weight of the surface modification substances in the surface-modified high-nickel anode material accounts for less than 5% of the total weight.
The present invention is described in further detail below with reference to examples:
according to the method, the acid solution and the precipitant solution are used for reducing the residual alkali amount on the surface of the high-nickel anode material and simultaneously forming the coating layer to modify the surface, and the weak acid solution and the cation solution are specifically used for treating the residual alkali on the surface of the high-nickel anode material and forming the coating layer.
Example 1
A certain amount of boric acid was dissolved to obtain 20L of a solution of 0.01 mol/L. 1000g of LiNi0.8Co0.1Mn0.1O2Stirring the mixture and 500g of deionized water to form slurry, placing the slurry in a reaction kettle, simultaneously dropwise adding a boric acid solution into the kettle at the flow rate of 20mL/min by a metering pump, controlling the pH of a reaction system to be 12 under the condition of keeping stirring at the reaction temperature of 25 ℃, and after stirring for 60min, performing solid-liquid separation on the obtained material in the reaction kettle by a centrifugal machine to obtain solid, and drying the solid for 8 hours at the temperature of 120 ℃. And (3) preserving the heat of the materials at 300 ℃ for 12h in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the surface-modified high-nickel cathode material.
Comparative example 1
1000g of LiNi0.8Co0.1Mn0.1O2And (3) preserving the heat for 2h at 700 ℃ in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the target cathode material.
Example 1 and comparative example 1 Performance test
By adopting the high-nickel cathode material with the surface modified in the embodiment 1 of the invention and the high-nickel cathode material in the comparative example 1, the X-ray powder diffraction analysis is respectively carried out on the high-nickel cathode material with the step size of 0.02 degrees, and the scanning angle 2 theta is 0-80 degrees, so that as can be seen from the figure 1, compared with the high-nickel cathode material without adopting the surface modification in the comparative example 1, the high-nickel cathode material after being modified in the embodiment 1 of the invention still maintains α -NaFeO2A layer-shaped structure. It was thus determined that the surface modification did not change the crystal structure of the material.
Example 2
20L of oxalic acid solution with the concentration of 0.1mol/L is prepared. 2000g of LiNi0.83Co0.11Mn0.04Al0.02O2Stirred with 4000g of deionized water to form slurry, and the slurry is placed in a reaction kettle to prepare 160ml of 0.05mol/L zinc acetate solution. Under the state of keeping stirring, dripping oxalic acid solution into the kettle at the flow rate of 10ml/min by a metering pump, dripping zinc acetate solution into the kettle at the flow rate of 20ml/min, controlling the pH of a reaction system to be 10.0 after the dripping of the zinc acetate solution is finished, continuing stirring for 30min, and stopping the reaction. And (3) performing solid-liquid separation on the material obtained in the reaction kettle by using a centrifugal machine to obtain solid, and drying the solid at 120 ℃ for 16 h. And (3) preserving the heat of the materials at 700 ℃ for 3h in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the surface-modified high-nickel cathode material.
Comparative example 2
2000g of LiNi0.83Co0.11Mn0.04Al0.02O2And (3) preserving the heat for 3h at 700 ℃ in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the target cathode material.
Example 2 and comparative example 2 Performance testing
The surface characteristics of the sample are tested at 5kV by adopting the surface modified high-nickel cathode material in the embodiment 2 of the invention. It can be seen that the coating exists on the surface of the surface-modified high-nickel cathode material in example 2, and the particles of the coating are fine and uniformly distributed. Therefore, the modification method can be confirmed to be capable of effectively modifying the surface of the material.
Example 3
A certain amount of oxalic acid dihydrate is dissolved to obtain 20L of 0.1mol/L solution. 500g of LiNi0.91Co0.06Al0.03O2Stirred with 5000g of deionized water to form slurry, and the slurry is placed in a reaction kettle. Weighing 58.3g of cobalt nitrate hexahydrate and 96.2g of magnesium nitrate hexahydrate, adding the weighed materials into 200ml of deionized water to prepare a mixed solution of the cobalt nitrate and the magnesium nitrate, dropwise adding an oxalic acid solution into the kettle at the flow rate of 8ml/min through a metering pump, adding the mixed solution of the cobalt nitrate and the magnesium nitrate into the kettle at the flow rate of 10ml/min under the condition of keeping stirring, controlling the pH value of a reaction system to be 10.5 after the dropwise addition of the mixed solution is finished, continuously stirring for 1min, and stopping the reaction. And (3) carrying out solid-liquid separation on the materials obtained in the reaction kettle by using a centrifugal machine to obtain solids, and drying the solids at 120 ℃ for 4 hours. And (3) preserving the heat of the materials for 6h at 500 ℃ in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the surface-modified high-nickel cathode material.
Comparative example 3
1000g of LiNi0.91Co0.06Al0.03O2And (3) preserving the heat for 6h at 500 ℃ in an oxygen atmosphere, naturally cooling, and crushing and screening to obtain the target cathode material.
Example 3 and comparative example 3 Performance test
By adopting the surface modified high-nickel anode material in the embodiment 3 and the high-nickel anode material in the comparative example 3, the CR2025 button cell is assembled respectively, and the charging and discharging cycle tests are carried out respectively under 3.0-4.3V and 1C, so that the comparative schematic diagram of the cycle performance curve shown in FIG. 3 is obtained. Compared with the high-nickel cathode material which is not subjected to surface modification in the comparative example 3, the high-nickel cathode material subjected to surface modification in the example 3 has higher discharge capacity and cycle stability in the cycle process. Therefore, the surface modification can improve the cycling stability of the high-nickel cathode material in the charging and discharging processes.
Claims (8)
1. A surface modification method of a high-nickel cathode material of a lithium ion battery is characterized by comprising the following steps:
(1) mixing the high-nickel anode material with deionized water, and stirring to obtain slurry;
(2) adding an acidic solution or simultaneously adding the acidic solution and a precipitator solution into the slurry obtained in the step (1) under the condition of stirring, and maintaining the pH value of a reaction system to be 10.0-12.0 for reaction;
(3) carrying out solid-liquid separation on the slurry obtained after the reaction in the step (2), drying the obtained solid, and sieving to obtain an unfired high-nickel cathode material with a coating layer on the surface;
(4) heating the high-nickel anode material with the coating layer on the surface to 300-700 ℃ in an oxygen atmosphere, preserving the heat for 3-12 h, and then cooling to room temperature to obtain the surface-modified high-nickel anode material.
2. The surface modification method of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the mass of the deionized water in the step (1) is 0.5 to 10 times of the mass of the high-nickel cathode material.
3. The method for modifying the surface of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the chemical formula of the high-nickel cathode material in the step (1) is LiNixM1-xO2Wherein x is more than or equal to 0.8, and M is one or more of Co, Mn and Al.
4. The surface modification method of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the acidic solution in the step (2) is one of oxalic acid solution, acetic acid solution, boric acid solution, silicic acid solution and phosphoric acid solution, and the concentration of the acidic solution is 0.01-0.1 mol/L.
5. The surface modification method of the lithium ion battery high-nickel cathode material according to claim 1, characterized in that the precipitant in the step (2) is at least one of soluble nitrate, chloride, acetate and acetate of B, Mg, Al, Si, Co, Ni, Ti, Zn, Cr, Zr, Mo, Y, V, Ga, Ge, Sc, Nb, Sn, Te, La or W, and the concentration of the precipitant solution is less than 0.05 mol/L.
6. The surface modification method of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the mass of the cations in the precipitant solution in the step (2) is 300-3000 ppm.
7. The surface modification method of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the reaction temperature in the step (2) is 20-40 ℃, and the stirring time is 5-60 min.
8. The surface modification method of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein the drying temperature in the step (3) is 120 ℃, and the drying time is 4-12 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112086679A (en) * | 2020-09-30 | 2020-12-15 | 合肥国轩高科动力能源有限公司 | High-nickel ternary material, surface modification method and lithium ion battery |
| CN114023950A (en) * | 2021-09-30 | 2022-02-08 | 北京大学 | Surface-stable amorphous passivation layer coated lithium ion battery positive electrode material and preparation method thereof |
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| CN109768254A (en) * | 2019-01-15 | 2019-05-17 | 合肥国轩高科动力能源有限公司 | Modified low nickelic tertiary cathode material of residual alkali type and the preparation method and application thereof |
| CN110436531A (en) * | 2019-06-20 | 2019-11-12 | 浙江美都海创锂电科技有限公司 | High Ni-monocrystal tertiary cathode material of low surface residual alkali and preparation method thereof |
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| CN105280885A (en) * | 2014-07-15 | 2016-01-27 | 北京当升材料科技股份有限公司 | Preparation method for high-nickel material surface coating layer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112086679A (en) * | 2020-09-30 | 2020-12-15 | 合肥国轩高科动力能源有限公司 | High-nickel ternary material, surface modification method and lithium ion battery |
| CN114023950A (en) * | 2021-09-30 | 2022-02-08 | 北京大学 | Surface-stable amorphous passivation layer coated lithium ion battery positive electrode material and preparation method thereof |
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Application publication date: 20200417 |