CN111446445A - Plasma treatment method for nickel-based lithium ion positive electrode material precursor - Google Patents
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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 discloses a plasma processing method of a nickel-based lithium ion anode material precursor, belonging to the technical field of lithium ion batteries and comprising the following steps of: placing the dried nickel-based precursor into a plasma generator, introducing mixed gas containing oxygen, and reacting under the conditions of frequency of 10-50MHz and power of 100-; the intermediate and lithium salt are mixed by a dry method or a wet method, and the nickel-based lithium ion anode material is prepared by sintering; the invention adopts oxygen-based plasma to treat the precursor of the nickel-based lithium ion anode material, and can efficiently treat Ni2+Oxidation to Ni3+The method reduces the degree of ion mixing in the material, increases the regularity of the material structure, obtains the lithium ion battery anode material with high capacity, high cycle and high multiplying power, and has simple and efficient method and easy large-scale application.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a plasma treatment method for a precursor of a nickel-based lithium ion positive electrode material.
Background
The nickel-based anode material of the lithium ion battery has high specific energy density, so the nickel-based anode material is widely applied to the fields of portable electronic products and new energy power batteries. The performance of the nickel-based anode material is greatly influenced by the precursor, and the content of nickel in the precursor is increasedPlus, Ni2+Difficult to oxidize into Ni3+And Ni3+Is easy to be reduced into Ni at the temperature higher than 600 DEG C2+Due to Ni2+And L i+Close ionic radii, Ni2+Has stronger migration capability and is easy to occupy the lithium position to generate L i+/Ni2+The phenomenon inhibits the transmission of lithium ions, increases the mixed lithium-nickel discharge of the high-nickel anode material and seriously reduces the lithium storage capacity and the cycling stability of the high-nickel anode material.
In order to solve the problem, a patent (CN102074679A) discloses a method for preparing spherical aluminum-doped lithium nickel cobalt oxide of a lithium ion battery anode material by combining liquid phase oxidation and control of crystal phase, which synthesizes a high-concentration spherical hydroxyl nickel cobalt aluminum oxide precursor through a control process, mixes the precursor with a lithium source, and then calcines the mixture for 10 to 24 hours at the temperature of 500-. However, the method introduces an oxidant in the coprecipitation process, so that anions are embedded between precursor layers and are difficult to wash away, and finally, the ionic rearrangement degree of the material is increased and the electrochemistry is reduced.
The patent (CN108511746A) discloses a preparation method of a preoxidized and modified high-nickel ternary cathode material, which comprises the steps of mixing a precursor with nitrate and a solvent, drying and presintering to obtain the preoxidized precursor, reducing the lithium-nickel mixed-discharging degree in the layered structure of the high-nickel ternary cathode material, and improving the first efficiency, capacity and cycle performance of the high-nickel ternary cathode material. However, this process is complicated, involves nitrates and remains after the treatment.
Therefore, it is still necessary to research how to effectively and simply reduce the degree of lithium-nickel mixing and thus improve the performance of the nickel-based lithium ion positive electrode material.
Disclosure of Invention
In order to solve the problems, the invention discloses a plasma treatment method for a nickel-based lithium ion positive electrode material precursor, which is used for treating the nickel-based precursor by adopting oxygen-based plasma to obtain a high-performance lithium ion battery positive electrode material, and the method is simple, efficient and easy to apply on a large scale.
A plasma processing method of a nickel-based lithium ion anode material precursor comprises the following steps:
s1, placing the dried nickel-based precursor into a plasma generator, introducing a mixed gas containing oxygen, and reacting under the conditions of frequency of 10-50MHz and power of 100 and 500W to obtain an intermediate;
s2: and (3) mixing the S1 intermediate with lithium salt by a dry method or a wet method, and sintering to obtain the nickel-based lithium ion cathode material.
Preferably, the S1 reaction time is 1-30 min.
Preferably, the S1 plasma generator is a plasma cleaning gun, a plasma cleaning tank, a plasma enhanced CVD furnace or a stirrer or fluidized bed containing a plasma generator.
Preferably, the S1 mixed gas is air and O2Mixed with Ar, O2And N2Mixing, O2With Ar and N2The three are mixed, and the volume fraction of oxygen in the mixed gas is 10-70%.
Preferably, the S1 nickel-based precursor is Ni (OH)2、NixCoyMn1-x-y(OH)2、NixCoyAl1-x-y(OH)2、NiCO3、NixCoyMn1-x-yCO3Or NixCoyAl1-x-yCO3。
Preferably, the molar ratio of the intermediate to the lithium salt is 1:1.01 to 1.15.
Preferably, the S2 lithium salt is L iOH, L i2CO3、LiF、LiCl、LiNO3Or lithium acetate.
Preferably, the dry mixing of S2 is grinding, ball milling or stirring mixing.
Preferably, the solvent in the S2 wet mixing is ethanol, acetone, isopropanol or methanol.
Preferably, the sintering conditions of S2 are as follows: under the condition of oxygen-enriched sintering atmosphere, keeping the temperature at 400-800 ℃ for 2-20 h and keeping the temperature at 650-600 ℃ for 10-20h, and cooling to room temperature; wherein the heating rate is 1-15 ℃/min, and the cooling rate is 1-20 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
according to the method for processing the nickel-based lithium ion positive electrode material precursor, the nickel-based precursor is processed by adopting oxygen-based plasma, so that the nickel-based lithium ion battery positive electrode material with high capacity, high cycle and high multiplying power is obtained, and the method is simple, efficient and easy to apply on a large scale; the mechanism of the treatment method is that the plasma is in a state of existence of a fourth substance except gas, liquid and solid, is generally generated by glow discharge, contains a plurality of high-activity particles, and is used for treating a nickel-based precursor to easily treat Ni2+Oxidation to Ni3+Reduction of Ni in the material2+The degree of lithium-nickel mixed arrangement caused by ions increases the regularity of the material structure, thereby improving the performance of the nickel-based lithium ion anode material.
Drawings
Fig. 1 is XRD spectra of the nickel-based lithium ion positive electrode materials prepared in example 1 and comparative example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all the existing methods unless otherwise specified; the raw materials and reagents are commercially available, unless otherwise specified.
Example 1
A plasma processing method of a nickel-based lithium ion anode material precursor comprises the following steps:
mixing Ni0.8Co0.1Mn0.1(OH)2Placing the powder in a plasma cleaning box, introducing dry air with the radio frequency of 10MHz and the power of 100W, and treating for 1 min; treated Ni0.8Co0.1Mn0.1(OH)2Grinding and mixing with L iOH according to the molar ratio of 1:1.01, heating at the speed of 1 ℃/min, respectively preserving heat for 5h and 12h at the temperature of 400 ℃ and 750 ℃, then cooling to room temperature at the speed of 20 ℃/min, grinding to obtain the nickel-based lithium ion anodeA material.
80mg of the positive electrode material, 10mg of PVDF and 10mg of conductive carbon black are prepared into slurry, the slurry is coated on an aluminum foil by the height surface of 250 mu m of a scraper, and the aluminum foil is dried to form the positive electrode plate. And stamping the positive plate into a pole piece with the diameter of 12mm, and preparing the button cell for electrochemical test.
Example 2
A plasma processing method of a nickel-based lithium ion anode material precursor comprises the following steps:
10g of Ni0.8Co0.15Al0.05(OH)2Placing the powder in a plasma enhanced CVD furnace, and introducing O2the/Ar is mixed gas of 7:3, and the plasma generator is switched on, the frequency of the radio frequency source is 14MHz, the power is 300W, and the processing time is 20 min; will be treated with Ni0.8Co0.15Al0.05(OH)2And performing wet mixing with L iF by using ethanol as a solvent in a ratio of 1:1.05, heating at a speed of 15 ℃/min, respectively preserving heat at 400 ℃ and 750 ℃ for 5h and 12h, then cooling to room temperature at 1 ℃/min, and grinding to obtain the nickel-based lithium ion cathode material.
80mg of the positive electrode material, 10mg of PVDF and 10mg of conductive carbon black are prepared into slurry, the slurry is coated on an aluminum foil by the height surface of 250 mu m of a scraper, and the aluminum foil is dried to form the positive electrode plate. And stamping the positive plate into a pole piece with the diameter of 12mm, and preparing the pole piece into a button cell for electrochemical test.
Example 3
A plasma processing method of a nickel-based lithium ion anode material precursor comprises the following steps:
10g of Ni0.8Co0.1Mn0.1(OH)2Placing the powder in a plasma rotary furnace, and introducing O2/N2The radio frequency is 20MHz, the power is 500W, and the processing time is 30 min; treated Ni0.8Co0.1Mn0.1(OH)2And L iNO3Stirring and mixing at a ratio of 1:1.07, heating at a speed of 3 ℃/min, respectively keeping the temperature at 600 ℃ and 800 ℃ for 2h and 10h, then cooling to room temperature at 3 ℃/min, and grinding to obtain the nickel-based lithium ion anodeA material.
160mg of the positive electrode material, 20mg of PVDF and 20mg of acetylene black are prepared into slurry, the slurry is coated on an aluminum foil by a 250-micrometer height surface of a scraper, and the aluminum foil is dried to form a positive electrode plate. And stamping the positive plate into a pole piece with the diameter of 12mm, and preparing the pole piece into a button cell for electrochemical test.
Example 4
A plasma processing method of a nickel-based lithium ion anode material precursor comprises the following steps:
mixing 10g of Ni (OH)2Placing the plasma gun under the conditions that the radio frequency of the plasma is 50MHz, the power is 300W, and introducing O2/Ar/N2The processing time is 30min when the ratio is 1:4: 5; mixing the treated Ni (OH)2And L iNO3And performing wet mixing by using acetone as a solvent according to the ratio of 1:1.15, heating at the speed of 10 ℃/min, respectively preserving heat at 470 ℃ and 650 ℃ for 2h and 20h, then cooling to room temperature at the speed of 3 ℃/min, and grinding to obtain the nickel-based lithium ion cathode material.
160mg of the positive electrode material, 20mg of PVDF and 20mg of acetylene black are prepared into slurry, the slurry is coated on an aluminum foil by a 250-micrometer height surface of a scraper, and the aluminum foil is dried to form a positive electrode plate. And stamping the positive plate into a pole piece with the diameter of 12mm, and preparing the pole piece into a button cell for electrochemical test.
Comparative example 1
Mixing Ni0.8Co0.1Mn0.1(OH)2Grinding and mixing the powder and L iOH according to a ratio of 1:1.05, respectively preserving heat for 5h and 12h at 400 ℃ and 750 ℃ at a heating rate of 5 ℃/min under an oxygen atmosphere, then cooling to room temperature at 3 ℃/min, grinding to obtain a nickel-based lithium ion positive electrode material, preparing 80mg of the positive electrode material, 10mg of PVDF and 10mg of conductive carbon black into slurry, coating the slurry on an aluminum foil by using a height surface of 250 mu m of a scraper, drying to obtain a positive electrode plate, punching the positive electrode plate into a pole piece with a diameter of 12mm, and preparing the pole piece into a button cell for electrochemical test.
First, XRD examination was performed on the positive electrode materials obtained in example 1 and comparative example 1, and the results are shown in FIG. 1. As can be seen from FIG. 1, the positive electrode materials obtained in example 1 and comparative example 1 were α -NaFeO2Structure, XRDThe I (003)/I (104) in the formula can reflect the ion-mixing degree, the peak intensity ratio of the two materials is 1.64 (example 1) and 1.40 (comparative example 1), and the plasma-treated material has a better layered structure and the ion-mixing degree is reduced.
Electrochemical tests were performed on the button cells prepared in examples 1 to 4 and comparative example 1, and the results are shown in table 1:
table 1 button cell performance test results in examples 1-4 and comparative example 1
As can be seen from table 1, after the precursors of the nickel-based lithium ion positive electrode materials of examples 1 to 4 are subjected to plasma treatment, the prepared positive electrode material undergoes 300 cycles, the cycle retention rate is significantly improved, and compared with comparative example 1, the cycle retention rate is improved by 59.2% to 74.7%, the first discharge capacity is improved by 1% to 6.4%, the rate capability is improved by 130% to 143%, and the first coulombic efficiency is improved by 2.61% to 4.7%; the nickel-based lithium ion positive electrode material prepared by processing the precursor by the method is proved to have obviously improved performance because the plasma is in a fourth substance existing state except gas, liquid and solid states, is usually generated by glow discharge, contains various high-activity particles and is easy to remove Ni2+Oxidation to Ni3+The ion mixing and discharging phenomenon in the anode material is inhibited, and the regularity of the material structure is increased, so that the high-capacity, high-cycle and high-rate lithium ion battery anode material is obtained; the method is simple, efficient and easy for large-scale application.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (10)
1. A plasma processing method for a nickel-based lithium ion anode material precursor is characterized by comprising the following steps:
s1, placing the dried nickel-based precursor into a plasma generator, introducing a mixed gas containing oxygen, and reacting under the conditions of frequency of 10-50MHz and power of 100 and 500W to obtain an intermediate;
s2: and (3) mixing the S1 intermediate with lithium salt by a dry method or a wet method, and sintering to obtain the nickel-based lithium ion cathode material.
2. The plasma treatment method of the nickel-based lithium ion positive electrode material precursor according to claim 1, wherein the reaction time of S1 is 1-30 min.
3. The plasma treatment method of the nickel-based lithium-ion positive electrode material precursor according to claim 1, wherein the S1 plasma generator is a plasma cleaning gun, a plasma cleaning tank, a plasma enhanced CVD furnace, or a stirrer or a fluidized bed containing the plasma generator.
4. The plasma processing method of the nickel-based lithium ion positive electrode material precursor according to claim 1, wherein the S1 mixed gas is air and O2Mixed with Ar, O2And N2Mixing, O2With Ar and N2The three are mixed, and the volume fraction of oxygen in the mixed gas is 10-70%.
5. The plasma processing method of the nickel-based lithium ion positive electrode material precursor according to claim 1, wherein the S1 nickel-based precursor is Ni (OH)2、NixCoyMn1-x-y(OH)2、NixCoyAl1-x-y(OH)2、NiCO3、NixCoyMn1-x-yCO3Or NixCoyAl1-x-yCO3。
6. The plasma treatment method of the nickel-based lithium ion positive electrode material precursor according to claim 1, wherein the molar ratio of the intermediate to the lithium salt is 1:1.01 to 1.15.
7. The plasma treatment method of the nickel-based lithium-ion positive electrode material precursor according to claim 1, wherein the S2 lithium salt is L iOH, L i2CO3、LiF、LiCl、LiNO3Or lithium acetate.
8. The plasma processing method of the nickel-based lithium ion positive electrode material precursor according to claim 1, wherein the dry mixing of S2 is grinding, ball milling or stirring mixing.
9. The plasma processing method of the nickel-based lithium-ion positive electrode material precursor according to claim 1, wherein the solvent in the S2 wet mixing is ethanol, acetone, isopropanol or methanol.
10. The plasma processing method of the nickel-based lithium-ion positive electrode material precursor according to claim 1, wherein the sintering conditions of S2 are as follows: under the condition of oxygen-enriched sintering atmosphere, keeping the temperature at 400-800 ℃ for 2-20 h and keeping the temperature at 650-600 ℃ for 10-20h, and cooling to room temperature; wherein the heating rate is 1-15 ℃/min, and the cooling rate is 1-20 ℃/min.
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Cited By (5)
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| CN113186560A (en) * | 2021-03-30 | 2021-07-30 | 广州费舍尔人工智能技术有限公司 | Ni-rich alloy3+Nickel cobaltate modified carbon ball electrode catalyst |
| CN113363468A (en) * | 2021-06-24 | 2021-09-07 | 西北工业大学 | Modified hard carbon and modification method and application thereof |
| CN113422040A (en) * | 2021-07-02 | 2021-09-21 | 青岛多元锂业有限公司 | Preparation method of medium-high nickel ternary material subjected to pre-oxidation treatment of precursor and lithium salt |
| WO2023202951A1 (en) * | 2022-04-22 | 2023-10-26 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for producing nickel-rich cathode active material and method for producing cathode electrode |
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| CN112563486B (en) * | 2020-12-25 | 2022-08-26 | 昆明理工大学 | Method and device for rapidly preparing doped ternary lithium ion battery anode material by using oxygen thermal plasma |
| CN113186560A (en) * | 2021-03-30 | 2021-07-30 | 广州费舍尔人工智能技术有限公司 | Ni-rich alloy3+Nickel cobaltate modified carbon ball electrode catalyst |
| CN113363468A (en) * | 2021-06-24 | 2021-09-07 | 西北工业大学 | Modified hard carbon and modification method and application thereof |
| CN113422040A (en) * | 2021-07-02 | 2021-09-21 | 青岛多元锂业有限公司 | Preparation method of medium-high nickel ternary material subjected to pre-oxidation treatment of precursor and lithium salt |
| WO2023202951A1 (en) * | 2022-04-22 | 2023-10-26 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for producing nickel-rich cathode active material and method for producing cathode electrode |
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