CN111883736A - Preparation method of lithium ion battery anode slurry - Google Patents
Preparation method of lithium ion battery anode slurry Download PDFInfo
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- CN111883736A CN111883736A CN202010510599.9A CN202010510599A CN111883736A CN 111883736 A CN111883736 A CN 111883736A CN 202010510599 A CN202010510599 A CN 202010510599A CN 111883736 A CN111883736 A CN 111883736A
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- 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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- 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
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
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- 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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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of lithium ion battery anode slurry, which comprises the following steps: s1, adding the conductive agent into the dispersing agent, and stirring and dispersing to obtain a conductive agent dispersion liquid with the solid content of 0.5-3%; s2, dissolving the adhesive in a solvent to obtain an adhesive solution with solid content of 5-9%; s3, adding the adhesive solution into the conductive agent dispersion liquid, pre-stirring, and then stirring fully to obtain mixed slurry; s4, adding the positive electrode active material into the mixed slurry, pre-stirring, and then fully stirring to obtain a positive electrode slurry with a solid content of 58-65%; step S1 and step S2 are performed simultaneously, step S1 is performed first and then step S2 is performed, or step S2 is performed first and then step S1 is performed. Compared with the prior art, the preparation method is high in preparation efficiency, and the prepared anode slurry is uniform in dispersion and good in stability, and is beneficial to improving the overall performance of the lithium ion battery.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of lithium ion battery anode slurry.
Background
Lithium ion batteries have been gaining great attention in consumer electronics and power products because of their advantages of high operating voltage, high energy density, long cycle life, safety, environmental protection, and the like. The lithium ion battery mainly comprises a positive plate, a negative plate, an isolating membrane, electrolyte and the like, wherein the preparation of the positive plate needs to be carried out through the processes of preparation, coating, rolling and the like of positive slurry, and when the positive electrode of the lithium ion battery is prepared, the uniformity and the stability of the positive slurry have considerable influence on the performance of the lithium ion battery.
In the preparation process of the positive electrode slurry, it is necessary to disperse the active material, the conductive agent, the binder, and the solvent. In the prior art, the preparation methods of the anode slurry are more, and the current main dispersing methods include the following methods:
1) uniformly mixing the conductive agent, the solvent and the binder dry powder, and then adding the active substance and the solvent and stirring to prepare the required anode slurry. In the method, the oil absorption value of the conductive agent is far greater than that of the active substance, so that the surface of the active substance is difficult to wet, and the stability of the slurry is poor.
2) And uniformly mixing the active substance and the binder dry powder, and then adding the conductive agent and the solvent and stirring to prepare the required anode slurry. The method has the advantages that the surface area of the added conductive agent is large, so that the conductive agent adsorbs a large amount of solvent to be agglomerated, and the slurry has poor stability and is easy to settle.
3) Mixing active substance, conductive agent and binder, adding solvent, controlling solid content and making the slurry be in ultrahigh viscosity, and uniformly stirring. Because the surface appearance of a plurality of active substances is irregular, particularly, the surfaces of large particles present depressions with different degrees, the depressions easily cause the aggregation of the conductive agent and the binder powder when dry powder is mixed, the binder on the surface of the aggregated part of the powder is dissolved after the solvent is added, the powder is extruded to be more compact under the condition of ultrahigh-viscosity stirring, the conductive agent and the binder in the depressions cannot be wetted and dissolved by the solvent, and the prepared slurry is uneven in dispersion and large in viscosity rebound under the standing state.
In view of the above, it is necessary to provide a new method for preparing a positive electrode slurry of a lithium ion battery.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the preparation method of the lithium ion battery anode slurry is provided, the preparation efficiency is high, the prepared anode slurry is uniform in dispersion and good in stability, and the overall performance of the lithium ion battery is favorably improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of lithium ion battery anode slurry comprises the following steps:
s1, adding the conductive agent into the dispersing agent, and stirring and dispersing to obtain a conductive agent dispersion liquid with the solid content of 0.5-3%;
s2, dissolving the adhesive in a solvent to obtain an adhesive solution with solid content of 5-9%;
s3, adding the adhesive solution into the conductive agent dispersion liquid, and stirring the mixture in advance and then stirring the mixture fully to obtain mixed slurry;
s4, adding the positive electrode active material into the mixed slurry, pre-stirring, and then fully stirring to obtain a positive electrode slurry with a solid content of 58-65%;
step S1 and step S2 are performed simultaneously, step S1 is performed first and then step S2 is performed, or step S2 is performed first and then step S1 is performed.
In step S1, stirring and dispersing are performed at a revolution speed of 25 to 40r/min and a rotation speed of 300 to 800r/min for 3 to 10 min.
In step S3, pre-stirring is performed at a revolution speed of 25 to 40r/min and a rotation speed of 300 to 800r/min for 3 to 8 min. Firstly, stirring at a low speed is adopted, so that most of the conductive agent is firstly contacted and dispersed with the adhesive, and the conductive agent is prevented from self-agglomerating.
In step S3, the positive electrode slurry of the lithium ion battery is fully stirred at a revolution speed of 25-40 r/min and a rotation speed of 1000-1500 r/min for 60 min. When the conductive agent and the adhesive are fully contacted and dispersed, the high-speed self-rotation is adopted to optimize the dispersion effect.
In step S4, pre-stirring is performed at a revolution speed of 25 to 40r/min and a rotation speed of 300 to 800r/min for 3 to 8 min. Firstly, stirring at a low speed is adopted, so that most of the conductive agent is firstly contacted and dispersed with the positive active material, and the conductive agent is prevented from self-agglomerating.
In step S4, the positive electrode slurry of the lithium ion battery is fully stirred at a revolution speed of 25-40 r/min and a rotation speed of 1200-1800 r/min for 240 min. When the conductive agent and the positive active material are fully contacted and dispersed, the high-speed self-rotation is adopted to optimize the dispersion effect.
In the anode slurry, the total weight of an anode active material, a conductive agent and a binder is 100 parts, and the anode active material is 97-98.5 parts, the conductive agent is 0.1-1.5 parts and the binder is 0.5-1.5 parts.
As an improvement of the preparation method of the lithium ion battery anode slurry, the conductive agent comprises at least one of conductive carbon black, conductive graphite, carbon nano tubes, carbon fibers and graphene, and the dispersing agent is N-methyl pyrrolidone.
As an improvement of the preparation method of the lithium ion battery anode slurry, the adhesive comprises polyvinylidene fluoride, and the solvent is N-methyl pyrrolidone.
As an improvement of the preparation method of the lithium ion battery anode slurry, the anode active material comprises a ternary anode material and lithium manganate which are mechanically mixed in any proportion.
Compared with the prior art, the beneficial effects of the invention include but are not limited to:
1) the conductive agent is dispersed firstly, the conductive agent is prevented from participating in subsequent stirring in an agglomeration state, and in the subsequent mixing process, a mode of pre-stirring and full-force stirring is adopted, the pre-stirring can ensure that most of the conductive agent, the adhesive and the positive active material are fully contacted and dispersed, the self-agglomeration of the conductive agent is prevented, and the full-force stirring optimizes the dispersion effect under the condition of full-contact dispersion, so that the conductive agent of the positive slurry prepared by the invention has good dispersion uniformity, no obvious agglomeration phenomenon, better stability and contribution to improving the overall performance of the battery.
2) According to the invention, the binder solution and the positive active material are added at one time, so that the production process is simplified, the stirring and mixing time is shortened, the productivity is further improved, and the stirring efficiency is effectively improved while the slurry is uniformly distributed.
Drawings
Fig. 1 is an SEM image of a positive electrode sheet made using the positive electrode slurry obtained in example 1.
Fig. 2 is an SEM image of a positive electrode sheet made using the positive electrode slurry obtained in comparative example 4.
Fig. 3 is a graph comparing the viscosity change curves of the positive electrode pastes prepared in example 1 and comparative example 4.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and the accompanying drawings, but the embodiments of the invention are not limited thereto.
Example 1
The embodiment provides a preparation method of lithium ion battery anode slurry, which comprises the following steps:
s1, adding the conductive agent into the dispersing agent, and stirring and dispersing at a revolution speed of 25-40 r/min and a rotation speed of 300-800 r/min for 3-10 min to obtain a conductive agent dispersion liquid with a solid content of 0.5-3%;
s2, dissolving the adhesive in a solvent to obtain an adhesive solution with solid content of 5-9%;
s3, adding the adhesive solution into the conductive agent dispersion liquid, pre-stirring at a revolution speed of 25-40 r/min and a rotation speed of 300-800 r/min for 3-8 min, and then fully stirring at a revolution speed of 25-40 r/min and a rotation speed of 1000-1500 r/min for 60min to obtain mixed slurry;
s4, adding the positive electrode active material into the mixed slurry, pre-stirring at a revolution speed of 25-40 r/min and a rotation speed of 300-800 r/min for 3-8 min, and fully stirring at a revolution speed of 25-40 r/min and a rotation speed of 1200-1800 r/min for 240min to obtain a positive electrode slurry with a solid content of 58-65%;
step S1 and step S2 are performed simultaneously, step S1 is performed first and then step S2 is performed, or step S2 is performed first and then step S1 is performed.
In the positive electrode slurry, the total weight of the positive electrode active material, the conductive agent and the binder is 100 parts, and the positive electrode active material is 97-98.5 parts, the conductive agent is 0.1-1.5 parts and the binder is 0.5-1.5 parts.
In this embodiment, the conductive agent includes at least one of conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene, and the dispersant is N-methylpyrrolidone. The adhesive comprises polyvinylidene fluoride and the solvent is N-methyl pyrrolidone. The positive electrode active material includes a ternary positive electrode material and lithium manganate mechanically mixed at a mass ratio of 2: 8.
Example 2
The embodiment provides a preparation method of a lithium ion battery anode slurry, which is different from the embodiment 1 in that: the positive electrode active material includes a ternary positive electrode material and lithium manganate mechanically mixed at a mass ratio of 1: 1.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 1
The embodiment provides a preparation method of a lithium ion battery anode slurry, which is different from the embodiment 1 in that: in step S3, the adhesive solution is added to the conductive agent dispersion without pre-stirring, and the mixture is directly stirred at a revolution speed of 25 to 40r/min and a rotation speed of 1000 to 1500r/min for 60min to obtain a mixed slurry.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 2
The embodiment provides a preparation method of a lithium ion battery anode slurry, which is different from the embodiment 1 in that: in step S4, the positive electrode active material is added into the mixed slurry, and the positive electrode active material is directly stirred at a revolution speed of 25-40 r/min and a rotation speed of 1200-1800 r/min for 240min without pre-stirring, so as to obtain a positive electrode slurry with a solid content of 58-65%.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 3
The embodiment provides a preparation method of a lithium ion battery anode slurry, which is different from the embodiment 1 in that: in step S3, adding the adhesive solution into the conductive agent dispersion liquid, and directly carrying out full-force stirring at a revolution speed of 25-40 r/min and a rotation speed of 1000-1500 r/min for 60min without pre-stirring to obtain mixed slurry; in step S4, the positive electrode active material is added into the mixed slurry, and the positive electrode active material is directly stirred at a revolution speed of 25-40 r/min and a rotation speed of 1200-1800 r/min for 240min without pre-stirring, so as to obtain a positive electrode slurry with a solid content of 58-65%.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 4
The comparative example provides a preparation method of a lithium ion battery anode slurry, which comprises the following steps:
s1, taking 97-98.5 parts of the positive active material, 0.1-1.5 parts of the conductive agent and 0.5-1.5 parts of the binder according to 100 parts of the total weight, and uniformly mixing the positive active material, the conductive agent and the binder to obtain a mixed dry material;
and S2, adding a solvent into the mixed dry material, and uniformly stirring to obtain the anode slurry.
Performance testing
1) The positive electrode slurry prepared in example 1 and comparative example 4 was coated on a positive electrode current collector to prepare a positive electrode sheet, and SEM characterization was performed on the positive electrode sheet, and the results are shown in fig. 1 and fig. 2, respectively.
2) The positive electrode pastes prepared in examples 1 to 2 and comparative examples 1 to 4 were subjected to viscosity tests at regular intervals, and the results are shown in table 1, wherein the viscosity change curves of example 1 and comparative example 4 are shown in fig. 3.
TABLE 1 test results
As can be seen from comparison between fig. 1 and fig. 2, the positive plate made of the positive slurry prepared by the preparation method of the present invention has good conductive carbon dispersion uniformity and no obvious agglomeration, while the positive plate made of the positive slurry prepared by the preparation method of comparative example 4 has obvious agglomeration and uneven dispersion. Therefore, the preparation method can greatly improve the problem of uneven dispersion of the conductive carbon in the positive electrode slurry.
As can be seen from the test data in table 1 and the comparative graph of the curve in fig. 3, the positive electrode slurry prepared by the preparation method of the present invention has small viscosity change, is more stable in the overall state, and can better maintain the original dispersion state of the positive electrode slurry. Therefore, the preparation method can greatly improve the stability of the positive electrode slurry.
In conclusion, the preparation method of the invention can improve the stability of uneven dispersion and poor stability of the anode slurry, and the uniformity and stability of the anode slurry have non-negligible influence on the performance of the lithium ion battery, so that the overall performance of the lithium ion battery is improved.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. The preparation method of the lithium ion battery anode slurry is characterized by comprising the following steps:
s1, adding the conductive agent into the dispersing agent, and stirring and dispersing to obtain a conductive agent dispersion liquid with the solid content of 0.5-3%;
s2, dissolving the adhesive in a solvent to obtain an adhesive solution with solid content of 5-9%;
s3, adding the adhesive solution into the conductive agent dispersion liquid, and stirring the mixture in advance and then stirring the mixture fully to obtain mixed slurry;
s4, adding the positive electrode active material into the mixed slurry, pre-stirring, and then fully stirring to obtain a positive electrode slurry with a solid content of 58-65%;
step S1 and step S2 are performed simultaneously, step S1 is performed first and then step S2 is performed, or step S2 is performed first and then step S1 is performed.
2. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in step S1, stirring and dispersing are carried out at a revolution speed of 25-40 r/min and a rotation speed of 300-800 r/min for 3-10 min.
3. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in step S3, pre-stirring is performed at a revolution speed of 25 to 40r/min and a rotation speed of 300 to 800r/min for 3 to 8 min.
4. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in step S3, stirring is carried out with full force at a revolution speed of 25-40 r/min and a rotation speed of 1000-1500 r/min for 60 min.
5. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in step S4, pre-stirring is performed at a revolution speed of 25 to 40r/min and a rotation speed of 300 to 800r/min for 3 to 8 min.
6. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in step S4, stirring is carried out at a revolution speed of 25-40 r/min and a rotation speed of 1200-1800 r/min for 240 min.
7. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: in the positive electrode slurry, the total weight of the positive electrode active material, the conductive agent and the binder is 100 parts, and the positive electrode active material is 97-98.5 parts, the conductive agent is 0.1-1.5 parts and the binder is 0.5-1.5 parts.
8. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: the conductive agent comprises at least one of conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers and graphene, and the dispersing agent is N-methylpyrrolidone.
9. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: the adhesive comprises polyvinylidene fluoride, and the solvent is N-methyl pyrrolidone.
10. The method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein: the positive active material comprises a ternary positive material and lithium manganate which are mechanically mixed in any proportion.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112331835A (en) * | 2020-11-12 | 2021-02-05 | 河北零点新能源科技有限公司 | Hybrid process for improving low-temperature performance of lithium battery |
| CN112635715A (en) * | 2020-12-18 | 2021-04-09 | 湖北亿纬动力有限公司 | Lithium ion battery anode slurry, and homogenizing method and application thereof |
| CN112687863A (en) * | 2020-12-25 | 2021-04-20 | 惠州亿纬锂能股份有限公司 | Lithium-sulfur battery positive electrode slurry, homogenizing method and application thereof |
| CN112701240A (en) * | 2020-12-29 | 2021-04-23 | 湖北亿纬动力有限公司 | Preparation method of positive electrode slurry and positive electrode slurry |
| CN112768638A (en) * | 2021-01-15 | 2021-05-07 | 厦门海辰新能源科技有限公司 | Water-based positive electrode slurry and preparation method thereof |
| CN113991106A (en) * | 2021-09-14 | 2022-01-28 | 惠州锂威新能源科技有限公司 | Dry preparation method of negative electrode slurry |
| CN114400303A (en) * | 2021-11-25 | 2022-04-26 | 四川英能基科技有限公司 | Positive electrode slurry for sodium ion battery, application and preparation process |
| CN115090142A (en) * | 2022-07-22 | 2022-09-23 | 郑州中科新兴产业技术研究院 | A kind of lithium-sulfur battery cathode material, slurry and homogenization method thereof |
| CN115642227A (en) * | 2022-11-02 | 2023-01-24 | 楚能新能源股份有限公司 | Lithium ion battery anode slurry, preparation method thereof and lithium ion battery |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112331835A (en) * | 2020-11-12 | 2021-02-05 | 河北零点新能源科技有限公司 | Hybrid process for improving low-temperature performance of lithium battery |
| CN112635715A (en) * | 2020-12-18 | 2021-04-09 | 湖北亿纬动力有限公司 | Lithium ion battery anode slurry, and homogenizing method and application thereof |
| CN112687863A (en) * | 2020-12-25 | 2021-04-20 | 惠州亿纬锂能股份有限公司 | Lithium-sulfur battery positive electrode slurry, homogenizing method and application thereof |
| CN112701240A (en) * | 2020-12-29 | 2021-04-23 | 湖北亿纬动力有限公司 | Preparation method of positive electrode slurry and positive electrode slurry |
| CN112768638A (en) * | 2021-01-15 | 2021-05-07 | 厦门海辰新能源科技有限公司 | Water-based positive electrode slurry and preparation method thereof |
| CN112768638B (en) * | 2021-01-15 | 2022-02-22 | 厦门海辰新能源科技有限公司 | Water-based positive electrode slurry and preparation method thereof |
| CN113991106A (en) * | 2021-09-14 | 2022-01-28 | 惠州锂威新能源科技有限公司 | Dry preparation method of negative electrode slurry |
| CN114400303A (en) * | 2021-11-25 | 2022-04-26 | 四川英能基科技有限公司 | Positive electrode slurry for sodium ion battery, application and preparation process |
| CN115090142A (en) * | 2022-07-22 | 2022-09-23 | 郑州中科新兴产业技术研究院 | A kind of lithium-sulfur battery cathode material, slurry and homogenization method thereof |
| CN115090142B (en) * | 2022-07-22 | 2023-03-10 | 郑州中科新兴产业技术研究院 | A lithium-sulfur battery positive electrode material, slurry and homogenization method thereof |
| CN115642227A (en) * | 2022-11-02 | 2023-01-24 | 楚能新能源股份有限公司 | Lithium ion battery anode slurry, preparation method thereof and lithium ion battery |
| CN115642227B (en) * | 2022-11-02 | 2023-11-14 | 楚能新能源股份有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery |
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