CN110767899B - Preparation method of composite anode material of lithium ion battery - Google Patents
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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 provides a preparation method of a composite anode material of a lithium ion battery, which comprises the following steps: simultaneously putting the metal salt solution and the alkali solution into a reaction kettle for coprecipitation reaction; overflowing the reacted feed liquid into an aging tank for aging; pumping the aged finished feed liquid into a high-temperature coating machine for solid-liquid separation to obtain dry precursor particles; controlling the rotation speed of the high-temperature covering machine to keep the precursor particles at a certain material dispersion degree; pumping doped coating liquid into the high-temperature coating machine to react to obtain a lithium-containing composite anode material precursor, wherein the doped coating liquid comprises a lithium source and a doped substance; and conveying the lithium-containing composite anode material precursor to a rotary kiln for sintering to obtain the composite anode material. By adopting the preparation method, the product performance is improved while the automatic production is realized.
Description
Technical Field
The invention relates to the technical field of lithium ion battery composite anode materials, in particular to a preparation method of a lithium ion battery composite anode.
Background
The lithium ion battery composite anode material has the advantages of high specific capacity, long cycle life, good portability and the like, and is widely applied to the fields of digital products, electric tools, energy storage power supplies, new energy vehicles and the like. With the rapid development of new energy vehicle industry, the demand of power lithium ion batteries is also rapidly increasing. Meanwhile, with the improvement of the standard of new energy vehicles, the requirements on the lithium ion battery composite anode material are increasingly improved.
Chinese patent CN102522526B provides a device and a process for producing a positive electrode or a negative electrode material of a converter type lithium battery, which utilizes a fluidized mixing device to physically mix raw materials and additives, and then produces the positive electrode or the negative electrode material of the lithium battery through a converter high-temperature reaction. However, this method can only realize an automated operation, and it cannot improve the performance of the product.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide the preparation method of the lithium ion battery composite positive electrode material, which can realize stable and efficient productivity and improve the product performance.
The invention provides a preparation method of a composite anode material of a lithium ion battery, which comprises the following steps: simultaneously putting the metal salt solution and the alkali solution into a reaction kettle for coprecipitation reaction; overflowing the reacted feed liquid into an aging tank for aging; pumping the aged finished feed liquid into a high-temperature coating machine for solid-liquid separation to obtain dry precursor particles; controlling the rotation speed of the high-temperature covering machine to keep the precursor particles at a certain material dispersion degree; pumping doped coating liquid into the high-temperature coating machine to react to obtain a lithium-containing composite anode material precursor, wherein the doped coating liquid comprises a lithium source and a doped substance; and conveying the lithium-containing composite anode material precursor to a rotary kiln for sintering to obtain the composite anode material.
In the preparation method of the composite anode material of the lithium ion battery, the whole process flow is continuous and automatic control can be realized through the reaction kettle, the ageing tank, the high-temperature coating machine and the rotary kiln which are sequentially communicated; and the coating solution containing the lithium source and the doping material is introduced into the high-temperature coating machine, and element doping and coating are directly carried out on the precursor to obtain the multi-element precursor containing lithium, so that the element doping effect is obtained, and the product performance is further improved.
Drawings
FIG. 1 is a graph showing voltage-first discharge capacity curves of batteries made of the positive electrode materials obtained in examples 1 to 3 and comparative example.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the embodiments in the drawings, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of a composite anode material of a lithium ion battery, which comprises the following steps:
s1: and simultaneously putting the metal salt solution and the alkali solution into a reaction kettle for coprecipitation reaction.
Preferably, the metal salt includes at least one of a nickel salt, a cobalt salt, a manganese salt, an aluminum salt, a zirconium salt, and a tungsten salt. The nickel salt, the cobalt salt, the manganese salt, the aluminum salt, the zirconium salt and the tungsten salt are at least one of sulfate, chloride, acetate, nitrate and oxalate.
The alkali solution is an aqueous solution containing a precipitator and a complexing agent. Preferably, the precipitant includes at least one of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, and potassium carbonate. The complexing agent comprises at least one of ammonia water, oxalic acid, citric acid and ethylene diamine tetraacetic acid.
In step S1, the pH value, the stirring speed, the reaction time, and the solid content of the slurry of the reaction system need to be controlled according to the production process requirements, so that the reacted feed liquid can reach the predetermined index.
It is understood that the following steps are also included before step S1: and adding high-purity salt-free water into the preparation tank, adding metal salt, and fully stirring to obtain a metal salt solution.
Preferably, the metal salt includes nickel salt, cobalt salt and manganese salt. Specifically, nickel salt, cobalt salt and manganese salt with the weight corresponding to the required mole ratio of nickel, cobalt and manganese are added into high-purity salt-free water with the preset volume, and the metal salt solution is obtained by uniformly stirring.
Preferably, the configuration tank is communicated with the reaction kettle, and the metal salt solution can be automatically pumped into the reaction kettle.
S2: and overflowing the reacted feed liquid into an aging tank for aging. And (4) promoting the crystal grains of the precipitate to grow to a proper crystal form through aging treatment.
Preferably, the ageing tank is communicated with the reaction kettle. When the liquid level of the feed liquid in the reaction kettle reaches an overflow port, a valve of the overflow port of the reaction kettle is opened, and the feed liquid is automatically discharged into the ageing tank.
S3: and pumping the aged finished product feed liquid into a high-temperature coating machine for solid-liquid separation to obtain dry precursor particles.
Specifically, the aged finished product feed liquid is fed into a high-temperature coating machine, the reaction temperature of the high-temperature coating machine is adjusted, and the finished product feed liquid is stirred, so that liquid in the finished product feed liquid is evaporated to perform solid-liquid separation, and dry precursor particles are obtained.
Preferably, the high-temperature coating machine is communicated with the ageing tank, and the aged finished material liquid can be automatically pumped into the high-temperature coating machine.
S4: and controlling the rotation speed of the high-temperature coating machine to keep the precursor particles at a certain material dispersion degree.
S5: and pumping the doped coating liquid into the high-temperature coating machine for reaction to obtain a lithium-containing composite anode material precursor, wherein the doped coating liquid comprises a lithium source and a doped substance.
Specifically, the doped cladding liquid is pumped into the high-temperature cladding machine at a preset flow rate, so that the doped cladding liquid and the precursor particles can be in full contact reaction.
Preferably, the lithium source includes at least one of lithium hydroxide, lithium carbonate, lithium oxide, lithium acetate, and lithium oxalate. The doping material comprises at least one of aluminum oxide, aluminum hydroxide, aluminum oxyhydroxide, lanthanum oxide, niobium pentoxide, zirconium oxide, titanium oxide, lithium carbonate, lithium hydroxide, calcium carbonate, magnesium oxide, strontium oxide and yttrium oxide.
Preferably, the chemical formula of the lithium-containing composite cathode material precursor is as follows: nixCoyMnz(OH)2Wherein x + y + z is 1, x is more than or equal to 0.15 and less than or equal to 0.95, y is more than or equal to 0 and less than or equal to 0.5, and z is more than or equal to 0 and less than or equal to 0.5. The granularity range of the lithium-containing composite anode material precursor is 3-20 um.
S6: and conveying the lithium-containing composite anode material precursor to a rotary kiln for sintering to obtain the composite anode material. The sintering temperature is 200-900 ℃. The sintering atmosphere is air atmosphere, oxygen atmosphere or air-oxygen mixed atmosphere.
Preferably, the rotary kiln is communicated with the high-temperature covering machine through a pipeline, and the lithium-containing composite anode material precursor can be automatically conveyed into the rotary kiln through airflow.
S7: and conveying the composite anode material to a high-speed mixer, and adding the additive into the high-speed mixer for mixing to obtain the additive-coated composite anode material.
The surface of the composite cathode material is coated with a proper additive, so that the composite cathode material with better performance (such as safety, cyclicity and the like) can be obtained.
Preferably, the composite cathode material and the additive are simultaneously added into the high-speed mixer for mixing. Specifically, the high-speed mixer comprises a mixing bin, a first bin and a second bin, the composite anode material is conveyed to the first bin, the additive is thrown into the second bin, and the composite anode material and the additive enter the mixing bin to be mixed at the same time.
Preferably, the high-speed mixer is communicated with the sintering furnace through a pipeline.
S8: and conveying the composite cathode material coated by the additive to a sintering furnace for sintering.
Specifically, the composite cathode material coated with the additive is conveyed to a charging device, the charging device charges the composite cathode material coated with the additive into a sagger, and the sagger is placed into a sintering furnace for sintering. And after sintering, packaging and warehousing the finished product.
Preferably, the charging equipment is communicated with the high-speed mixer through a pipeline, and the materials mixed in the high-speed mixer can be automatically conveyed to the charging equipment.
Further, the following steps are also included between steps S6 and S7: and conveying the composite anode material to a screening device for screening, and scattering agglomerated particles of the material.
According to the preparation method of the composite anode material of the lithium ion battery, provided by the invention, the composite anode material coated by the additive is filled into a sagger and enters a sintering furnace for sintering through a configuration groove, a reaction kettle, an ageing groove, a high-temperature coating machine, a rotary kiln and a charging device which are sequentially communicated, so that the composite anode material can be packaged, the whole process flow is continuous, and automatic control can be realized; and the coating solution containing the lithium source and the doping material is introduced into the high-temperature coating machine, and element doping and coating are directly carried out on the precursor to obtain the multi-element precursor containing lithium, so that the element doping effect is obtained, and the product performance is further improved.
The present invention will be specifically described below by way of examples and comparative examples.
Example 1
Putting nickel salt, cobalt salt and manganese salt into a configuration tank filled with high-purity brine-free water with a preset volume according to the weight of the nickel salt, the cobalt salt and the manganese salt with the molar ratio of 6:2:2, and uniformly stirring to obtain a mixed metal salt solution. And (3) putting the prepared mixed metal salt solution into a reaction kettle, introducing a proper amount of sodium hydroxide solution and ammonia water according to the production process requirements, and adjusting the pH value to 11.5. And overflowing the material liquid reaching the preset index into an aging tank for aging.
Pumping the aged finished product feed liquid into a high-temperature coating machine, adjusting the reaction temperature of the high-temperature coating machine to 130 ℃, and controlling the high-temperature coating machine to stir the finished product feed liquid in the high-temperature coating machine for 0.5 h; adjusting the rotation speed of the high-temperature coating machine to 150 revolutions per minute for 0.5h, and reducing the reaction temperature of the high-temperature coating machine to 60 ℃; introducing an additive solution containing Zr and Li into the high-temperature coating machine for reaction to obtain a precursor material of the lithium-containing composite positive electrode material.
And conveying the lithium-containing composite anode material precursor material to a rotary kiln from a discharge hole of the high-temperature covering machine, and rapidly sintering at 920 ℃ to obtain the composite anode material. Conveying the sintered composite anode material into a screening device through a pipeline, and mechanically crushing the agglomerated particles of the material to obtain the zirconium-coated anode material with the median particle size of 3 um.
Conveying the zirconium-coated anode material to a first bin of a high-speed mixer, adding a required additive A into a second bin of the high-speed mixer, and controlling the zirconium-coated anode material and the additive A to simultaneously enter a mixing bin of the high-speed mixer and be uniformly mixed; the mixed materials are conveyed to a charging device through a pipeline, are loaded in a sagger of 3kg and enter a sintering furnace for sintering, and the sintering temperature is 300 ℃. And packaging and warehousing the sintered finished product.
Example 2
Putting nickel salt, cobalt salt and manganese salt into a configuration tank filled with high-purity brine-free water with a preset volume according to the weight of the nickel salt, the cobalt salt and the manganese salt with the molar ratio of 6:2:2, and uniformly stirring to obtain a mixed metal salt solution. And (3) putting the prepared mixed metal salt solution into a reaction kettle, introducing a proper amount of sodium hydroxide solution and ammonia water according to the production process requirements, and adjusting the pH value to 11.5. And overflowing the material liquid reaching the preset index into an aging tank for aging.
Pumping the aged finished product feed liquid into a high-temperature coating machine, adjusting the reaction temperature of the high-temperature coating machine to 130 ℃, and controlling the high-temperature coating machine to stir the finished product feed liquid in the high-temperature coating machine for 0.5 h; adjusting the rotation speed of the high-temperature coating machine to 150 revolutions per minute for 0.5h, and reducing the reaction temperature of the high-temperature coating machine to 60 ℃; and introducing an additive solution containing Ti and Li into the high-temperature coating machine for reaction to obtain the precursor material of the lithium-containing composite positive electrode material.
And conveying the lithium-containing composite anode material precursor material to a rotary kiln from a discharge hole of the high-temperature covering machine, and rapidly sintering at 920 ℃ to obtain the composite anode material. Conveying the sintered composite anode material into a screening device through a pipeline, and mechanically crushing the agglomerated particles of the material to obtain the titanium-coated anode material with the median particle size of 3 um.
Conveying the zirconium-coated anode material to a first bin of a high-speed mixer, adding a required additive A into a second bin of the high-speed mixer, and controlling the titanium-coated anode material and the additive A to simultaneously enter a mixing bin of the high-speed mixer and be uniformly mixed; the mixed materials are conveyed to a charging device through a pipeline, are loaded in a sagger of 3kg and enter a sintering furnace for sintering, and the sintering temperature is 300 ℃. And packaging and warehousing the sintered finished product.
Example 3
Putting nickel salt, cobalt salt and manganese salt into a configuration tank filled with high-purity brine-free water with a preset volume according to the weight of the nickel salt, the cobalt salt and the manganese salt with the molar ratio of 6:2:2, and uniformly stirring to obtain a mixed metal salt solution. And (3) putting the prepared mixed metal salt solution into a reaction kettle, introducing a proper amount of sodium hydroxide solution and ammonia water according to the production process requirements, and adjusting the pH value to 11.5. And overflowing the material liquid reaching the preset index into an aging tank for aging.
Pumping the aged finished product feed liquid into a high-temperature coating machine, adjusting the reaction temperature of the high-temperature coating machine to 130 ℃, and controlling the high-temperature coating machine to stir the finished product feed liquid in the high-temperature coating machine for 0.5 h; adjusting the rotation speed of the high-temperature coating machine to 150 revolutions per minute for 0.5h, and reducing the reaction temperature of the high-temperature coating machine to 60 ℃; and introducing an additive solution containing Al and Li into the high-temperature coating machine for reaction to obtain a precursor material of the lithium-containing composite positive electrode material.
And conveying the lithium-containing composite anode material precursor material to a rotary kiln from a discharge hole of the high-temperature covering machine, and rapidly sintering at 920 ℃ to obtain the composite anode material. Conveying the sintered composite anode material into a screening device through a pipeline, and mechanically crushing the agglomerated particles of the material to obtain the aluminum-coated anode material with the median particle size of 3 um.
Conveying the zirconium-coated anode material to a first bin of a high-speed mixer, adding a required additive A into a second bin of the high-speed mixer, and controlling the aluminum-coated anode material and the additive A to simultaneously enter a mixing bin of the high-speed mixer and be uniformly mixed; the mixed materials are conveyed to a charging device through a pipeline, are loaded in a sagger of 3kg and enter a sintering furnace for sintering, and the sintering temperature is 300 ℃. And packaging and warehousing the sintered finished product.
Comparative example
Putting nickel salt, cobalt salt and manganese salt into a configuration tank filled with high-purity brine-free water with a preset volume according to the weight of the nickel salt, the cobalt salt and the manganese salt with the molar ratio of 6:2:2, and uniformly stirring to obtain a mixed metal salt solution. And (3) putting the prepared mixed metal salt solution into a reaction kettle, introducing a proper amount of sodium hydroxide solution and ammonia water according to the production process requirements, and adjusting the pH value to 11.5. And overflowing the material liquid reaching the preset index into an aging tank for aging.
Pumping the aged finished product feed liquid into a high-temperature coating machine, adjusting the reaction temperature of the high-temperature coating machine to 130 ℃, and controlling the high-temperature coating machine to stir the finished product feed liquid in the high-temperature coating machine for 0.5 h; adjusting the rotation speed of the high-temperature coating machine to 150 revolutions per minute for 0.5h, and reducing the reaction temperature of the high-temperature coating machine to 60 ℃; and introducing the additive solution containing Li into the high-temperature coating machine for reaction to obtain the precursor material of the lithium-containing composite positive electrode material.
And conveying the lithium-containing composite anode material precursor material to a rotary kiln from a discharge hole of the high-temperature covering machine, and rapidly sintering at 920 ℃ to obtain the composite anode material. Conveying the sintered composite anode material into a screening device through a pipeline, and mechanically crushing the agglomerated particles of the material to obtain the uncoated anode material with the median particle size of 3 um.
Conveying the zirconium-coated anode material to a first bin of a high-speed mixer, adding a required additive A into a second bin of the high-speed mixer, and controlling the uncoated anode material and the additive A to simultaneously enter a mixing bin of the high-speed mixer and be uniformly mixed; the mixed materials are conveyed to a charging device through a pipeline, are loaded in a sagger of 3kg and enter a sintering furnace for sintering, and the sintering temperature is 300 ℃. And packaging and warehousing the sintered finished product.
After the positive electrode materials obtained in examples 1-3 and comparative example were made into batteries, the electrochemical properties related to the batteries were tested by a button cell tester. Table 1 shows the results of testing the electrochemical properties 0.1C first discharge capacity, first efficiency and storage property of the batteries made of the positive electrode materials obtained in examples 1 to 3 and comparative example. FIG. 1 is a graph showing voltage-first discharge capacity curves of batteries made of the positive electrode materials obtained in examples 1 to 3 and comparative example.
TABLE 1 Primary discharge Capacity, Primary efficiency and storage Performance
The test results show that the positive electrode materials coated with the dopant in the embodiments 1 to 3 of the present invention have better first discharge capacity, first efficiency and storage performance than the positive electrode materials not coated with the dopant in a comparative ratio.
It can be seen from fig. 1 that the positive electrode materials of examples 1 to 3 of the present invention, which were coated with the dopant, have better voltage-first discharge capacity performance than the positive electrode material of comparative example, which was not coated with the dopant.
In addition, other modifications within the spirit of the invention will occur to those skilled in the art, and it is understood that such modifications are included within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a lithium ion battery composite anode material is characterized in that the lithium ion battery composite anode material is produced by a reaction kettle, an ageing tank, a high-temperature coating machine and a rotary kiln which are sequentially communicated, and the preparation method of the lithium ion battery composite anode material comprises the following steps:
simultaneously putting the metal salt solution and the alkali solution into a reaction kettle for coprecipitation reaction;
when the liquid level of the feed liquid in the reaction kettle reaches an overflow port, opening a valve of the overflow port of the reaction kettle, and automatically overflowing the reacted feed liquid into an aging tank for aging;
automatically pumping the aged finished product feed liquid into a high-temperature coating machine, adjusting the reaction temperature of the high-temperature coating machine to 130 ℃, controlling the high-temperature coating machine to stir the finished product feed liquid for 0.5h, adjusting the rotation speed of the high-temperature coating machine to 150 rpm for 0.5h, reducing the reaction temperature of the high-temperature coating machine to 60 ℃,
pumping doped coating liquid into the high-temperature coating machine to react to obtain a lithium-containing composite anode material precursor, wherein the doped coating liquid comprises a lithium source and a doped substance;
the rotary kiln is communicated with the high-temperature covering machine through a pipeline, and the lithium-containing composite anode material precursor is automatically conveyed into the rotary kiln through airflow to be sintered to obtain the composite anode material.
2. The method of claim 1, wherein the metal salt comprises at least one of a nickel salt, a cobalt salt, a manganese salt, an aluminum salt, a zirconium salt, and a tungsten salt, and wherein the nickel salt, the cobalt salt, the manganese salt, the aluminum salt, the zirconium salt, and the tungsten salt is at least one of a sulfate, a chloride, an acetate, a nitrate, and an oxalate.
3. The method for preparing the composite positive electrode material of the lithium ion battery according to claim 2, wherein the chemical formula of the precursor of the lithium-containing composite positive electrode material is as follows: nixCoyMnz(OH)2Wherein x + y + z is 1, x is more than or equal to 0.15 and less than or equal to 0.95, y is more than or equal to 0 and less than or equal to 0.5, and z is more than or equal to 0 and less than or equal to 0.5, and the particle size range of the precursor of the lithium-containing composite cathode material is 3-20 um.
4. The method of claim 1, wherein the alkaline solution is an aqueous solution comprising a precipitant and a complexing agent.
5. The method for preparing the composite positive electrode material of the lithium ion battery according to claim 1, wherein the sintering temperature of the precursor of the lithium-containing composite positive electrode material in the rotary kiln is 200 ℃ to 900 ℃.
6. The method of claim 1, wherein the dopant material comprises at least one of aluminum oxide, aluminum hydroxide, aluminum oxyhydroxide, lanthanum oxide, niobium pentoxide, zirconium oxide, titanium oxide, lithium carbonate, lithium hydroxide, calcium carbonate, magnesium oxide, strontium oxide, and yttrium oxide.
7. The method for preparing the composite positive electrode material of the lithium ion battery according to claim 1, further comprising the steps of: adding water and metal salt into a preparation tank, and fully stirring to obtain the metal salt solution.
8. The method for preparing the composite positive electrode material of the lithium ion battery according to claim 1, further comprising the steps of: and conveying the composite anode material to a high-speed mixer, and adding the additive into the high-speed mixer for mixing to obtain the additive-coated composite anode material.
9. The method for preparing the composite positive electrode material of the lithium ion battery according to claim 8, further comprising the steps of: and conveying the composite cathode material coated by the additive to a sintering furnace for sintering.
10. The method of claim 1, further comprising the steps of, between the step of sintering to obtain the composite positive electrode material and the step of mixing to obtain the additive coated composite positive electrode material: and conveying the composite cathode material to a screening device for screening.
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| CN104701534A (en) * | 2015-03-31 | 2015-06-10 | 南通瑞翔新材料有限公司 | High-energy-density Ni-Co-based lithium ion positive electrode material and preparation method thereof |
| CN105206828A (en) * | 2015-09-08 | 2015-12-30 | 虞志远 | Nickel and cobalt-based lithium-ion cathode material and preparation method thereof |
| CN106654210B (en) * | 2016-12-22 | 2018-07-10 | 广州朝锂新能源科技有限公司 | A kind of nickelic positive electrode of high temperature long circulating lithium ion battery and preparation method thereof |
| CN106938844A (en) * | 2017-04-21 | 2017-07-11 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of the individual particle artificial plumbago negative pole material of high power capacity low bulk |
| CN107565121B (en) * | 2017-07-17 | 2020-07-10 | 江西南氏锂电新材料有限公司 | Preparation method of modified positive electrode material of lithium battery |
| CN108899480A (en) * | 2018-05-24 | 2018-11-27 | 中国科学院青岛生物能源与过程研究所 | A kind of long circulation life height ratio capacity nickel cobalt aluminium positive electrode and preparation method thereof |
| CN108878825B (en) * | 2018-06-26 | 2021-05-25 | 格林美（无锡）能源材料有限公司 | Surface-coated positive electrode material and preparation method thereof |
| CN108807949A (en) * | 2018-08-07 | 2018-11-13 | 浙江美都海创锂电科技有限公司 | A kind of preparation method of high nickel lithium manganate cathode material |
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