CN110034276B - Mixing and pulping method of anode material - Google Patents
Mixing and pulping method of anode material Download PDFInfo
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- CN110034276B CN110034276B CN201910358463.8A CN201910358463A CN110034276B CN 110034276 B CN110034276 B CN 110034276B CN 201910358463 A CN201910358463 A CN 201910358463A CN 110034276 B CN110034276 B CN 110034276B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
- B01F23/511—Methods thereof characterised by the composition of the liquids or solids
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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
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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
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- H—ELECTRICITY
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- 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
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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
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- 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
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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
- 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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a mixed material pulping method of a positive electrode material, wherein the positive electrode material comprises a first active material and a second active material, and the first active material is selected from lithium cobaltate or modified lithium cobaltate; the second active material is selected from lithium nickel manganese cobaltate or modified lithium nickel manganese cobaltate. The first active material includes first particles having an average particle diameter of 80 to 200nm and second particles having an average particle diameter of 1.2 to 1.5 μm; the second active material has an average particle diameter of 2 to 2.5 μm; wherein the total mass of the first particles, the second particles and the second active material is 100%, the first particles account for 8-12%, the second particles account for 20-25%, and the second active material accounts for 65-70%; according to the invention, the first particles, the second particles and the second active material are respectively pulped and then mixed in batches, and the obtained slurry has high stability and good coating performance.
Description
Technical Field
The invention relates to the technical field of lithium ion battery production, in particular to a mixing and pulping method of a positive electrode material.
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 existing electric vehicle battery generally adopts a positive electrode blended by lithium cobaltate and a ternary material, and because the particle diameters of the lithium cobaltate and the ternary material are different, the coating performance of slurry is poor, and cracks are easy to occur in the drying process.
Disclosure of Invention
The inventors have found through studies that when the particle diameter of a particle having a specific content in lithium cobaltate is in a specific range, a stable rheological phase can be formed with the slurry, and the stability of the slurry is greatly improved.
On the basis, the invention provides a mixed material pulping method of a positive electrode material, wherein the positive electrode material comprises a first active material and a second active material, and the first active material comprises first particles with the average particle size of 80-200nm and second particles with the average particle size of 1.2-1.5 mu m; the second active material has an average particle diameter of 2 to 2.5 μm; wherein the total mass of the first particles, the second particles and the second active material is 100%, the first particles account for 8-12%, the second particles account for 20-25%, and the second active material accounts for 65-70%; according to the invention, the first particles, the second particles and the second active material are respectively pulped and then mixed in batches, and the obtained slurry has high stability and good coating performance. The first active material is selected from lithium cobaltate or modified lithium cobaltate; the second active material is selected from lithium nickel manganese cobaltate or modified lithium nickel manganese cobaltate.
The specific scheme is as follows:
a mixed material pulping method of a positive electrode material comprises a first active material and a second active material, wherein the first active material comprises first particles with the average particle size of 80-200nm and second particles with the average particle size of 1.2-1.5 mu m; the second active material has an average particle diameter of 2 to 2.5 μm; wherein, according to the total mass of the first particles, the second particles and the second active material in the anode slurry as 100 percent, the first particles account for 8-12 percent, the second particles account for 20-25 percent and the second active material accounts for 65-70 percent, and the method specifically comprises the following steps:
1) sequentially adding the binder and the conductive agent into the solvent, stirring, adding the first particles, and stirring to obtain a first slurry;
2) sequentially adding the binder and the conductive agent into the solvent, stirring, adding the second particles, and stirring to obtain a second slurry;
3) sequentially adding the binder and the conductive agent into the solvent, stirring, adding the second active substance, and stirring to obtain a third slurry;
4) and according to the proportion of the first particles, the second particles and the second active material in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring, then adding the second slurry into the mixed slurry while stirring, adding a solvent to adjust the solid content, and stirring to obtain the anode slurry.
Further, the first active material is selected from lithium cobaltate or modified lithium cobaltate; the second active material is selected from lithium nickel manganese cobaltate or modified lithium nickel manganese cobaltate.
Further, the solid content of the positive electrode slurry is 56-58%.
Further, the solid content of the first slurry is 62-65%, the solid content of the second slurry is 60-62%, and the solid content of the third slurry is 58-60%.
Further, the first particles have an average particle diameter of 80 to 120 nm.
Furthermore, the proportion of the positive electrode active material, the binder and the conductive agent in the positive electrode slurry is 100:6-7: 4-5.
Further, the method specifically comprises the following steps:
1) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding first particles, and stirring for 8h to obtain first slurry, wherein the ratio of the first particles, PVDF and conductive carbon black is 100:6-7: 4-5;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding second particles, and stirring for 6h to obtain a second slurry, wherein the ratio of the second particles, PVDF and conductive carbon black is 100:6-7: 4-5;
3) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding a second active material, and stirring for 4h to obtain a third slurry, wherein the ratio of the second active material to the PVDF to the conductive carbon black is 100:6-7: 4-5;
4) according to the proportion of the first particles, the second particles and the second active material in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content, and stirring for 4 hours to obtain the anode slurry.
The invention has the following beneficial effects:
1) when the particle size of particles with specific content in the lithium cobaltate is in a specific range, a stable rheological phase can be formed with the slurry, and the stability of the slurry is greatly improved;
2) the three active substances with different particle sizes are respectively mixed, so that the dispersion of various materials is facilitated, and the solid solution amount of the slurry is adjusted according to the particle sizes of different materials, so that the stability of the slurry is increased;
3) the inventor finds that the addition sequence of the three kinds of slurry is favorable for mutual dispersion of the three kinds of slurry, avoids settlement and is favorable for quickly forming stable slurry;
4) the mixing process is simple, and the prepared slurry has good stability.
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. In the following examples, the first active material was lithium cobaltate; the second active material is lithium nickel manganese cobaltate (Ni: Mn: Co is 8:1:1)
Example 1
1) Adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate A with the average particle size of 80nm, and stirring for 8h to obtain first slurry, wherein the proportion of the lithium cobaltate, the PVDF and the conductive carbon black is 100:6:4, and the solid content is 62%;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate B with the average particle size of 1.2 mu m, and stirring for 6h to obtain a second slurry, wherein the ratio of the lithium cobaltate to the PVDF to the conductive carbon black is 100:6:4, and the solid content is 60%;
3) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium nickel manganese cobalt oxide with the average particle size of 2 mu m, and stirring for 4h to obtain a third slurry, wherein the proportion of the lithium nickel manganese cobalt oxide, the PVDF and the conductive carbon black is 100:6:4, and the solid content is 58%;
4) according to the proportion that lithium cobaltate A accounts for 8%, lithium cobaltate B accounts for 25% and lithium nickel manganese cobaltate accounts for 67% in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content to 58%, and stirring for 4 hours to obtain the anode slurry.
Example 2
1) Adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate A with the average particle size of 200nm, and stirring for 8h to obtain first slurry, wherein the proportion of the lithium cobaltate, the PVDF and the conductive carbon black is 100:7:5, and the solid content is 65%;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate B with the average particle size of 1.5 mu m, and stirring for 6h to obtain a second slurry, wherein the ratio of the lithium cobaltate to the PVDF to the conductive carbon black is 100:7:5, and the solid content is 62%;
3) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium nickel manganese cobaltate with the average particle size of 2.5 mu m, and stirring for 4h to obtain a third slurry, wherein the ratio of the lithium nickel manganese cobaltate to the PVDF to the conductive carbon black is 100:7:5, and the solid content is 60%;
4) according to the proportion that lithium cobaltate A accounts for 12%, lithium cobaltate B accounts for 20% and lithium nickel manganese cobaltate accounts for 68% in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content to 58%, and stirring for 4 hours to obtain the anode slurry.
Example 3
1) Adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate A with the average particle size of 80nm, and stirring for 8h to obtain first slurry, wherein the proportion of the lithium cobaltate, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 63%;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate B with the average particle size of 1.4 mu m, and stirring for 6h to obtain a second slurry, wherein the ratio of the lithium cobaltate to the PVDF to the conductive carbon black is 100:6:5, and the solid content is 61%;
3) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium nickel manganese cobaltate with the average particle size of 2.2 mu m, and stirring for 4h to obtain a third slurry, wherein the proportion of the lithium nickel manganese cobaltate, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 60%;
4) according to the proportion that lithium cobaltate A accounts for 10%, lithium cobaltate B accounts for 25% and lithium nickel manganese cobaltate accounts for 65% in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content to 58%, and stirring for 4 hours to obtain the anode slurry.
Example 4
1) Adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate A with the average particle size of 120nm, and stirring for 8h to obtain first slurry, wherein the proportion of the lithium cobaltate, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 64%;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate B with the average particle size of 1.4 mu m, and stirring for 6h to obtain a second slurry, wherein the ratio of the lithium cobaltate to the PVDF to the conductive carbon black is 100:6:5, and the solid content is 62%;
3) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium nickel manganese cobaltate with the average particle size of 2.5 mu m, and stirring for 4h to obtain a third slurry, wherein the proportion of the lithium nickel manganese cobaltate, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 60%;
4) according to the proportion that lithium cobaltate A accounts for 10%, lithium cobaltate B accounts for 20% and lithium nickel manganese cobaltate accounts for 70% in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content to 58%, and stirring for 4 hours to obtain the anode slurry.
Comparative example 1
Lithium cobaltate a having an average particle diameter of 500nm was provided, and the other parameters were the same as in example 4.
Comparative example 2
Lithium cobaltate a having an average particle diameter of 30nm was provided, and the other parameters were the same as in example 4.
Comparative example 3
The positive electrode slurry contained 20% of lithium cobaltate a, 10% of lithium cobaltate B and 70% of lithium nickel manganese cobaltate, and the other parameters were the same as in example 4.
Comparative example 4
The positive electrode slurry contained 5% of lithium cobaltate a, 25% of lithium cobaltate B and 70% of lithium nickel manganese cobaltate, and the other parameters were the same as in example 4.
Test and results
The viscosity of the slurry was measured and then the solid content of the slurry 5cm below the top layer was measured after standing at room temperature for 6h, 12h, 18h, the data are shown in table 1, the viscosity after mixing was almost similar as seen from the comparison of examples 1-4 and comparative examples 1-4, but the particle size range and content range of lithium cobaltate a affected the stability of the slurry, and the longer the standing time, the more obvious the chromatography phenomenon and the worse the stability of the slurry.
TABLE 1
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 (1)
1. A mixed material pulping method of a positive electrode material comprises lithium cobaltate and nickel manganese lithium cobaltate, wherein the lithium cobaltate comprises lithium cobaltate A with the average particle size of 120nm and lithium cobaltate B with the average particle size of 1.4 mu m; the average particle size of the lithium nickel manganese cobaltate is 2.5 mu m; the method comprises the following steps of according to the total mass of lithium cobaltate A, lithium cobaltate B and lithium nickel manganese cobaltate as a reference value of 100%, wherein the total mass of the lithium cobaltate A, the lithium cobaltate B and the lithium nickel manganese cobaltate accounts for 10%, the total mass of the lithium cobaltate B and the lithium nickel manganese cobaltate accounts for 20%, and the total mass of the lithium nickel manganese cobaltate accounts for 70%, wherein:
1) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate A with the average particle size of 120nm, and stirring for 8h to obtain first slurry, wherein the proportion of the lithium cobaltate A, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 64%;
2) adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium cobaltate B with the average particle size of 1.4 mu m, and stirring for 6h to obtain a second slurry, wherein the ratio of the lithium cobaltate B to the PVDF to the conductive carbon black is 100:6:5, and the solid content is 62%;
3) and adding PVDF into NMP, stirring for 2h, adding conductive carbon black, stirring for 4h, adding lithium nickel manganese cobaltate with the average particle size of 2.5 mu m, wherein the ratio of Ni: mn: the molar ratio of Co is 8:1:1, stirring is carried out for 4 hours, and a third slurry is obtained, wherein the proportion of the lithium nickel manganese cobaltate, the PVDF and the conductive carbon black is 100:6:5, and the solid content is 60%;
4) according to the proportion that lithium cobaltate A accounts for 10%, lithium cobaltate B accounts for 20% and lithium nickel manganese cobaltate accounts for 70% in the anode slurry, stirring the third slurry while slowly adding the first slurry into the third slurry, continuously stirring for 4 hours, then adding the second slurry into the mixed slurry while stirring, adding NMP to adjust the solid content to 58%, and stirring for 4 hours to obtain the anode slurry.
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| CN110581256B (en) * | 2019-10-17 | 2020-12-18 | 泰州纳新新能源科技有限公司 | Preparation method of lithium iron phosphate anode |
| CN111276757B (en) * | 2020-02-19 | 2021-01-05 | 苏州睿邦工业设计有限公司 | Preparation method of power type lithium ion battery |
| CN111313085B (en) * | 2020-04-13 | 2021-07-06 | 东方醒狮储能电池有限公司 | Preparation method of lithium ion battery anode |
| CN111933913A (en) * | 2020-08-18 | 2020-11-13 | 苏州精诚智造智能科技有限公司 | Preparation method for anode |
| CN111864179B (en) * | 2020-09-03 | 2021-10-22 | 东莞维科电池有限公司 | Positive pole piece and preparation method thereof, lithium ion battery containing positive pole piece and application of lithium ion battery |
| CN115989598A (en) | 2020-09-10 | 2023-04-18 | 宁德时代新能源科技股份有限公司 | Electrode active composition, preparation method thereof, electrode, battery and device |
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