CN110010873B - Preparation method of mixed anode slurry - Google Patents

Preparation method of mixed anode slurry Download PDF

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CN110010873B
CN110010873B CN201910280567.1A CN201910280567A CN110010873B CN 110010873 B CN110010873 B CN 110010873B CN 201910280567 A CN201910280567 A CN 201910280567A CN 110010873 B CN110010873 B CN 110010873B
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active material
slurry
graphitized carbon
stirring
vacuum
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CN110010873A (en
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王钢
邹勇兰
孙刘云
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Jiangxi DBK Corporation Co.,Ltd.
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Jiangxi Dbk Corp Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a preparation method of mixed anode slurry, the mixed anode slurry comprises a first active material, a second active material and graphitized carbon nanofibers, the average particle size of the first active material is 90-110nm, the average particle size of the second active material is 0.5-2 μm, the length of the graphitized carbon nanofibers is 10-50 μm, and the mass percentage of each component meets the following condition, the first active material/(the first active material + the second active material) is 22.5-24.5%, and the graphitized carbon nanofibers/(the first active material + the second active material) is more than 8%. The inventors found that when the three components are within the above-mentioned parameter ranges, the stability of the resulting slurry is greatly improved, the storage property is enhanced, and the uniformly dispersed mixed positive electrode slurry can be rapidly and effectively obtained by the mixing method of the present invention.

Description

Preparation method of mixed anode slurry
Technical Field
The invention relates to the technical field of lithium ion battery production, in particular to a preparation method of mixed anode slurry.
Background
The power battery has the advantages of high energy density, high power, environmental protection and the like, and is commonly used in the field of electric vehicles. The mixed anode is adopted by the anode of the current power battery mostly, the mixed anode is a mixed anode material of a ternary material and a lithium iron phosphate material generally, the ternary material has high energy density, high working voltage, high safety of the lithium iron phosphate and good cycle performance, the mixed use of the ternary material and the lithium iron phosphate can bring more positive influence to the multiplying power performance and the cycle life of the power battery, but the conductivity of the lithium iron phosphate is poor, so that the particle size of the lithium iron phosphate is extremely large relative to the particle size difference of the ternary material, and the particles with various particle sizes exist in the slurry, so that great difficulty is brought to the mixing process, the dispersion is not uniform easily, the particle size difference is large, the sedimentation phenomenon is obvious, and the coating quality is influenced.
Disclosure of Invention
The inventor discovers through research that when the particle size and mass ratio of the lithium iron phosphate particles to the ternary material particles are within a specific range, a stable mixed fluid phase can be formed, the stability is greatly improved, and the carbon nanofibers are added to form a network in the slurry, so that the stability of the slurry is further improved. Meanwhile, the specific charging sequence adopted by the invention is beneficial to the dispersibility of various components, shortens the mixing time and improves the stability of the slurry.
On the basis, the invention provides a preparation method of mixed positive electrode slurry, the mixed positive electrode slurry comprises a first active material, a second active material and graphitized carbon nanofibers, the average particle size of the first active material is 90-110nm, the average particle size of the second active material is 0.5-2 μm, the length of the graphitized carbon nanofibers is 10-50 μm, and the mass percentage of each component meets the following condition that the first active material/(the first active material + the second active material) is 22.5-24.5%, and the graphitized carbon nanofibers/(the first active material + the second active material) is more than 8%. The inventors found that when the three components are within the above parameter ranges, the stability of the prepared slurry is greatly improved, the storage property is enhanced, and the uniformly dispersed mixed cathode slurry can be rapidly and effectively obtained by the preparation method of the present invention.
The specific scheme is as follows:
a preparation method of mixed anode slurry comprises a first active material, a second active material and graphitized carbon nanofibers, wherein the average particle size of the first active material is 95-110nm, the average particle size of the second active material is 1.8-2.1 μm, the average length of the graphitized carbon nanofibers is 35-50 μm, and the mass percentages of the components meet the following conditions, the first active material/(the first active material + the second active material) is 22.5-24.5%, and the graphitized carbon nanofibers/(the first active material + the second active material) is more than 8%, and specifically comprises the following steps:
1) sequentially adding a solvent, a binder and graphitized carbon nanofibers into a first vacuum stirring kettle, and stirring in vacuum to obtain a first slurry;
2) sequentially adding a solvent, a binder and a second active material into a second vacuum stirring kettle, and stirring in vacuum to obtain a second slurry;
3) and adding the first slurry into the second slurry according to the proportion of the components, stirring in vacuum, then adding the first active material, stirring in vacuum, adding a solvent to adjust the solid-liquid ratio, and stirring in vacuum to obtain the mixed anode slurry.
Further wherein the mass percent first active material/(first active material + second active material) is substantially equal to 23.5%.
Further, the graphitized carbon nanofiber/(the first active material + the second active material) is less than 12%.
Further, the graphitized carbon nanofibers have a length of 40 μm.
Further, the first active material is selected from lithium iron phosphate or modified lithium iron phosphate; the second active material is selected from lithium nickel cobalt manganese oxide or modified lithium nickel cobalt manganese oxide.
Further, wherein the mass ratio in the mixed slurry, the first and second active materials: graphitized carbon nanofiber: the binder is 100:8-12: 4-6.
The invention has the following beneficial effects:
1) when the particle size and mass ratio of the lithium iron phosphate particles to the ternary material particles are within a specific range, a stable mixed fluid phase can be formed, and the stability is greatly improved;
2) the carbon nanofiber is added to form a network in the slurry, so that the stability of the slurry is further improved;
3) according to the invention, the carbon nanofibers and the ternary material are respectively mixed, so that the dispersion of the carbon nanofibers and the ternary material is facilitated, the particle size of the lithium iron phosphate is too small, and if the lithium iron phosphate is directly dispersed in a solution, the lithium iron phosphate is easy to agglomerate, so that the dispersion difficulty is increased;
4) the invention has the advantages of simple material mixing process, less time consumption, high stability of the prepared slurry and good storage performance.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
1) Sequentially adding NMP, PVDF and graphitized carbon nanofibers with the average length of 35 mu m into a first vacuum stirring kettle, and stirring for 4 hours in vacuum to obtain first slurry;
2) sequentially adding NMP, PVDF and nickel cobalt lithium manganate (333 type) with the average particle size of 1.8 mu m into a second vacuum stirring kettle, and stirring for 6 hours in vacuum to obtain second slurry;
3) adding the first slurry into the second slurry according to a ratio, stirring for 3 hours in vacuum, then adding lithium iron phosphate with the average particle size of 95nm according to the ratio, stirring for 6 hours in vacuum, adding NMP to adjust the solid-to-liquid ratio to be 58%, stirring for 1 hour in vacuum to obtain mixed anode slurry, wherein the mass ratio of each component in the mixed slurry, lithium iron phosphate and nickel cobalt lithium manganate: graphitized carbon nanofiber: PVDF 100:8: 4; the content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 22.5 percent.
Example 2
1) Sequentially adding NMP, PVDF and graphitized carbon nanofibers with the average length of 50 mu m into a first vacuum stirring kettle, and stirring for 4 hours in vacuum to obtain first slurry;
2) sequentially adding NMP, PVDF and nickel cobalt lithium manganate (333 type) with the average particle size of 2.1 mu m into a second vacuum stirring kettle, and stirring for 6 hours in vacuum to obtain second slurry;
3) adding the first slurry into the second slurry according to a ratio, stirring for 3 hours in vacuum, then adding lithium iron phosphate with the average particle size of 110nm according to the ratio, stirring for 6 hours in vacuum, adding NMP to adjust the solid-to-liquid ratio to be 58%, stirring for 1 hour in vacuum to obtain mixed anode slurry, wherein the mass ratio of each component in the mixed slurry, lithium iron phosphate and nickel cobalt lithium manganate: graphitized carbon nanofiber: PVDF 100:12: 6; the content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 24.5 percent.
Example 3
1) Sequentially adding NMP, PVDF and graphitized carbon nanofibers with the average length of 40 mu m into a first vacuum stirring kettle, and stirring for 4 hours in vacuum to obtain first slurry;
2) sequentially adding NMP, PVDF and nickel cobalt lithium manganate (333 type) with the average particle size of 2 mu m into a second vacuum stirring kettle, and stirring for 6 hours in vacuum to obtain second slurry;
3) adding the first slurry into the second slurry according to a ratio, stirring for 3 hours in vacuum, then adding lithium iron phosphate with the average particle size of 100nm according to the ratio, stirring for 6 hours in vacuum, adding NMP to adjust the solid-to-liquid ratio to be 58%, stirring for 1 hour in vacuum to obtain mixed anode slurry, wherein the mass ratio of each component in the mixed slurry, lithium iron phosphate and nickel cobalt lithium manganate: graphitized carbon nanofiber: PVDF 100:10: 5; 23.5 percent of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide.
Example 4
1) Sequentially adding NMP, PVDF and graphitized carbon nanofibers with the average length of 40 mu m into a first vacuum stirring kettle, and stirring for 2 hours in vacuum to obtain first slurry;
2) sequentially adding NMP, PVDF and nickel cobalt lithium manganate (333 type) with the average particle size of 2 mu m into a second vacuum stirring kettle, and stirring for 4 hours in vacuum to obtain second slurry;
3) adding the first slurry into the second slurry according to a ratio, stirring for 1h in vacuum, then adding lithium iron phosphate with the average particle size of 100nm according to the ratio, stirring for 4h in vacuum, adding NMP to adjust the solid-to-liquid ratio to be 58%, stirring for 1h in vacuum to obtain mixed anode slurry, wherein the mass ratio of each component in the mixed slurry, lithium iron phosphate and nickel cobalt lithium manganate: graphitized carbon nanofiber: PVDF 100:10: 5; the content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 23 percent.
Comparative example 1
Lithium iron phosphate having an average particle size of 50nm and nickel cobalt lithium manganate having an average particle size of 3 μm were provided, and the other parameters were the same as in example 3.
Comparative example 2
The content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 30%, and other parameters are the same as those in example 3.
Comparative example 3
The content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 15%, and other parameters are the same as those in example 3.
Comparative example 4
Providing nickel cobalt lithium manganate with the average particle size of 2 microns, lithium iron phosphate with the average particle size of 100nm, sequentially adding NMP, PVDF and graphitized carbon nanofibers with the average length of 40 microns in a vacuum stirring kettle, stirring for 6 hours in vacuum, adding lithium nickel manganese cobalt and lithium iron phosphate according to the proportion, stirring for 8 hours in vacuum, adding NMP to adjust the solid-to-liquid ratio to be 58%, stirring for 1 hour in vacuum, and obtaining mixed anode slurry, wherein the mass ratio of each component in the mixed slurry, the lithium iron phosphate and the nickel cobalt lithium manganate: graphitized carbon nanofiber: PVDF 100:10: 5; the content of lithium iron phosphate/lithium iron phosphate and lithium nickel cobalt manganese oxide is 23 percent.
Test and results
The viscosity of the slurry is measured, and then the slurry is placed for 6 hours, 12 hours and 24 hours, and then the solid content of the slurry at the position 5cm below the top layer is measured, the data are shown in table 1, as can be seen from the comparison between examples 1-4 and comparative examples 1-3, although the viscosity after mixing is similar, the dispersibility of the invention is better, the viscosity is slightly higher under the condition of the same binder, and the more obvious, the slurry prepared by the invention has better storage stability, wherein the component content and the particle size range of the two active materials have great influence on the stability of the slurry; as can be seen from the comparison between example 4 and comparative example 4, the mixing time of example 4 is only 10 hours, while the mixing time of comparative example 4 is 15 hours, but the dispersion degree of the active materials is still not as good as that of example 4, and the viscosity is lower under the condition of the same binder content, so that the mixing method of the invention has a very positive effect on improving the dispersion degree of the slurry and shortening the pulping time.
TABLE 1
Viscosity (mPa. s) 6h 12h 24h
Example 1 4250 55.6％ 52.8％ 49.6％
Example 2 4380 56.4％ 53.6％ 50.1％
Example 3 4310 56.6％ 54.1％ 51.7％
Example 4 4290 56.2％ 54.4％ 50.5％
Comparative example 1 4260 51.3％ 48.4％ 44.8％
Comparative example 2 4340 50.4％ 47.5％ 43.6％
Comparative example 3 4280 49.7％ 46.5％ 43.2％
Comparative example 4 3980 53.6％ 51.4％ 48.5％
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.

Claims (2)

1. A method for preparing mixed anode slurry, wherein the mixed anode slurry comprises a first active material, a second active material and graphitized carbon nanofibers, and is characterized in that: the average particle size of the first active material is 95-110nm, the average particle size of the second active material is 1.8-2.1 μm, the average length of the graphitized carbon nanofiber is 35-50 μm, and the mass percentages of the components meet the following conditions, wherein the mass percentage of the first active material/(the first active material + the second active material) is 23.5%, the mass percentage of the graphitized carbon nanofiber/(the first active material + the second active material) is more than 8%, and the first active material is selected from lithium iron phosphate or modified lithium iron phosphate; the second active material is selected from lithium nickel cobalt manganese oxide or modified lithium nickel cobalt manganese oxide, and the method specifically comprises the following steps:
1) sequentially adding a solvent, a binder and graphitized carbon nanofibers into a first vacuum stirring kettle, and stirring in vacuum to obtain a first slurry;
2) sequentially adding a solvent, a binder and a second active material into a second vacuum stirring kettle, and stirring in vacuum to obtain a second slurry;
3) adding the first slurry into the second slurry according to the proportion of the components, carrying out vacuum stirring, then adding the first active material, carrying out vacuum stirring, adding a solvent to adjust the solid-liquid ratio, and carrying out vacuum stirring to obtain the mixed anode slurry, wherein the mass ratio of the mixed anode slurry, the first active material and the second active material: graphitized carbon nanofibers: the binder is 100:8-12: 4-6.
2. The method of claim 1, the graphitized carbon nanofibers having a length of 40 μ ι η.
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CN110416496B (en) * 2019-08-05 2020-12-11 泰州纳新新能源科技有限公司 Cathode slurry and preparation method of cathode
CN111430694A (en) * 2020-04-09 2020-07-17 盛蕾 Mixing method of composite anode slurry
EP4258383A1 (en) * 2022-02-23 2023-10-11 Contemporary Amperex Technology Co., Limited Positive electrode sheet, secondary battery, battery module, battery pack, electric device, and method for balancing internal voltage difference of battery

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