CN115020633A - Battery negative plate preparation method, battery negative plate and battery thereof - Google Patents
Battery negative plate preparation method, battery negative plate and battery thereof Download PDFInfo
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- CN115020633A CN115020633A CN202210597610.9A CN202210597610A CN115020633A CN 115020633 A CN115020633 A CN 115020633A CN 202210597610 A CN202210597610 A CN 202210597610A CN 115020633 A CN115020633 A CN 115020633A
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- negative electrode
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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
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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
-
- 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
- H01M4/139—Processes of manufacture
-
- 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
- H01M2004/027—Negative 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a battery negative plate preparation method, a battery negative plate and a battery thereof. The preparation method of the battery negative plate comprises the following steps: preparing a negative electrode slurry, wherein the negative electrode slurry comprises carboxyl carboxymethyl cellulose; laying the negative electrode slurry on a current collector and drying; compacting the dried negative electrode slurry to obtain a negative electrode sheet; and heating the negative plate at a high temperature to carbonize the carboxyl carboxymethyl cellulose in the negative plate. According to the invention, the impedance is further reduced without further improving the proportion of the active material of the negative plate and reducing the proportion of the thickening agent carboxyl carboxymethyl cellulose, the binder modified acrylate and the like, but the compacted and dried negative plate is heated at high temperature to carbonize the carboxyl carboxymethyl cellulose, and the original non-conductive carboxyl carboxymethyl cellulose is converted into conductive carbon, so that the impedance of the negative plate is further reduced, the normal preparation process and performance of the negative plate can be ensured, and a series of problems caused by the low proportion of the thickening agent and the binder can be avoided.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a battery negative plate preparation method, a battery negative plate and a battery thereof.
Background
A lithium ion battery is a secondary battery (rechargeable battery) that mainly operates by movement of lithium ions between a positive electrode and a negative electrode. During charging and discharging, Li + is inserted and extracted back and forth between two electrodes: during charging, Li + is extracted from the positive electrode and is inserted into the negative electrode through the electrolyte, and the negative electrode is in a lithium-rich state; the opposite is true during discharge.
The negative plate of the lithium ion battery comprises a modified active material, a carboxyl carboxymethyl cellulose lithium (CMC-Li) thickening agent, a modified acrylate binder and the like. At present, the impedance of the negative electrode sheet is generally reduced by increasing the proportion of an active material and reducing the proportion of a thickener carboxyl carboxymethyl cellulose (CMC), a binder modified acrylate and the like. However, the active material ratio has been raised to the limit at present, and the ratio of the carboxylmethyl cellulose and the modified acrylate has been lowered to the limit. Under the condition of ensuring the normal preparation process and performance of the negative plate, the difficulty of further reducing the impedance of the negative plate is more and more high.
Disclosure of Invention
The invention aims to provide a preparation method of a battery negative plate, the battery negative plate and a battery thereof, which can further reduce the impedance of the negative plate under the condition of ensuring the normal preparation process and performance of the negative plate.
The invention discloses a preparation method of a battery negative plate, which comprises the following steps:
preparing a negative electrode slurry, wherein the negative electrode slurry comprises carboxyl carboxymethyl cellulose;
laying the negative electrode slurry on a current collector and drying;
compacting the dried negative electrode slurry to obtain a negative electrode sheet;
and heating the negative plate at a high temperature to carbonize the carboxyl carboxymethyl cellulose in the negative plate.
Optionally, the step of heating the negative electrode plate at a high temperature specifically includes: heating the negative plate at a high temperature of 500-700 ℃.
Optionally, the step of heating the negative electrode plate at a high temperature specifically includes: heating the negative plate at a high temperature of 550 ℃.
Optionally, the step of heating the negative electrode plate at a high temperature specifically includes: and (3) vacuumizing and baking the negative plate for 2-3 hours at 500-700 ℃.
Optionally, the preparation method further comprises the steps of: and introducing inert gas to prevent the current collector from being oxidized.
Optionally, the surface density of the anode slurry laid on the current collector is 50-150 g/m 2 。
Optionally, the compacted density of the negative electrode slurry is 1.5-1.8 g/cm 3 。
The invention also discloses a battery negative plate prepared by the preparation method.
The invention also discloses a battery, which comprises the battery negative plate.
According to the preparation method of the battery negative plate, carboxyl carboxymethyl cellulose (CMC) is added into the negative slurry to serve as a thickening agent, so that the normal configuration and the laying of the negative slurry on a current collector are ensured. After the negative plate is obtained by compacting and drying, the negative plate is heated at high temperature, so that the carboxyl carboxymethyl cellulose in the negative plate is carbonized. The carbonized carboxyl carboxymethyl cellulose is changed into conductive carbon from original non-conduction, electrons can be conducted, the effect similar to that of an active material is achieved, the content of conductive components can be increased, and simultaneously the components (original non-carbonized CMC) with non-conduction but rising resistance values can be reduced, so that the impedance of a negative plate is reduced, the energy density of the battery is improved, and the comprehensive performance of the battery is obviously improved. Therefore, according to the technical scheme provided by the invention, the proportion of the active materials of the negative plate is not further improved, and the proportion of the thickening agent carboxyl carboxymethyl cellulose, the binder modified acrylate and the like is reduced to further reduce the impedance, but the compacted and dried negative plate is subjected to high-temperature heating to carbonize the carboxyl carboxymethyl cellulose, and the original non-conductive carboxyl carboxymethyl cellulose is converted into conductive carbon, so that the impedance of the negative plate is further reduced, the normal preparation process and the battery performance of the negative plate can be ensured, and a series of problems caused by the excessively low proportion of the thickening agent and the binder can be avoided.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a graph showing the results of resistivity tests of comparative and experimental groups of the present invention.
Detailed Description
It is to be understood that the terminology, the specific structural and functional details disclosed herein are for the purpose of describing particular embodiments only, and are representative, but that the present invention may be embodied in many alternate forms and should not be construed as limited to only the embodiments set forth herein.
In the field of lithium battery technology, in order to reduce the impedance of a negative electrode sheet, the proportion of an active material is generally increased, and the proportion of a thickener such as carboxy carboxymethyl cellulose (CMC) or a binder-modified acrylate is generally decreased. At present, the proportion of active materials is improved to the limit, which reaches about 98.5 percent, and the improvement space is not large. The ratio of the carboxyl carboxymethyl cellulose to the modified acrylic ester is reduced to the limit, the ratio of the thickener carboxyl carboxymethyl cellulose is reduced to about 0.6 percent, and if the dosage is reduced, the processing stability of the negative electrode slurry is poor, which is represented by poor filtering performance of the slurry, slurry sedimentation and filter element blockage. The percentage of the modified acrylate of the binder is reduced to about 0.9 percent, and if the amount of the modified acrylate of the binder is reduced, the stripping force of the negative plate is poor, which is expressed as stripping and powder falling of the negative plate.
Therefore, in order to further reduce the impedance of the negative plate under the condition of ensuring the normal preparation process and performance of the negative plate, the invention provides a preparation method of the battery negative plate.
The invention is described in detail below with reference to the figures and alternative embodiments.
As an embodiment of the invention, a method for preparing a battery negative plate is disclosed, which comprises the following steps:
preparing a negative electrode slurry, wherein the negative electrode slurry comprises carboxyl carboxymethyl cellulose;
laying the negative electrode slurry on a current collector and drying;
compacting the dried negative electrode slurry to obtain a negative electrode sheet;
and heating the negative plate at a high temperature to carbonize the carboxyl carboxymethyl cellulose in the negative plate.
According to the preparation method of the battery negative plate, carboxyl carboxymethyl cellulose (CMC) is added into the negative slurry to serve as a thickening agent, so that the normal configuration and the laying of the negative slurry on a current collector are ensured. After the negative plate is obtained by compacting and drying, the negative plate is heated at high temperature, so that the carboxyl carboxymethyl cellulose in the negative plate is carbonized. The carbonized carboxyl carboxymethyl cellulose is changed into conductive carbon from original non-conduction, electrons can be conducted, the effect similar to that of an active material is achieved, the content of conductive components can be increased, and simultaneously the components (original non-carbonized CMC) with non-conduction but rising resistance values can be reduced, so that the impedance of a negative plate is reduced, the energy density of the battery is improved, and the comprehensive performance of the battery is obviously improved.
Therefore, according to the technical scheme provided by the invention, the proportion of the active material of the negative plate is not further improved, and the proportion of the thickening agent carboxyl carboxymethyl cellulose, the binder modified acrylate and the like is reduced to further reduce the impedance, but the compacted and dried negative plate is heated at high temperature to carbonize the carboxyl carboxymethyl cellulose, so that the original non-conductive carboxyl carboxymethyl cellulose is converted into conductive carbon, further reduction of the impedance of the negative plate is realized, the normal preparation process and performance of the negative plate can be guaranteed, and series problems caused by too low proportion of the thickening agent and the binder can be avoided.
It should be emphasized that, in the conventional process, the carboxylmethyl cellulose serves as a thickener of the negative electrode slurry, and plays a role in thickening at the slurry preparation stage, so as to ensure that the negative electrode slurry has a required viscosity so as to be laid on a current collector for drying and forming. The conventional carboxycarboxymethyl cellulose serves to maintain the shape of the electrode only at the initial stage of the process. In such inherent recognition, those skilled in the art have a technical prejudice that "the thickener has little influence on the performance of the negative electrode sheet, and the main component affecting the impedance of the negative electrode sheet is the active material". Therefore, the current practice of reducing the impedance of the negative electrode sheet is to increase the proportion of the active material as much as possible and to reduce the proportion of the thickener and the binder. Under the influence of this technical prejudice, it is difficult for those skilled in the art to further reduce the impedance of the negative electrode sheet as analyzed above.
The technical scheme of the invention overcomes the technical prejudice, does not continuously research and improve the active material, but focuses on the improvement on the original abandoned thickener carboxymethyl cellulose, and carbonizes the carboxymethyl cellulose to ensure that the carboxymethyl cellulose has conductivity, thereby solving the technical problem that the impedance value is difficult to further reduce.
Specifically, the step of heating the negative electrode plate at a high temperature specifically includes: heating the negative plate at a high temperature of 500-700 ℃. The carbonization temperature of the carboxyl carboxymethyl cellulose is about 490 ℃, so in the scheme, the negative plate is heated at a high temperature of 500-700 ℃ to ensure the carbonization of the carboxyl carboxymethyl cellulose.
Specifically, the step of heating the negative electrode plate at a high temperature specifically includes: heating the negative plate at a high temperature of 550 ℃. As shown in fig. 1, the preferred high-temperature heating temperature is 550 ℃, and the improvement effect of increasing the temperature is not significant.
Specifically, the step of heating the negative electrode plate at a high temperature specifically includes: and (3) vacuumizing and baking the negative plate for 2-3 hours at 500-700 ℃. The vacuum baking can prevent the current collector from being oxidized, and the baking of the negative plate for 2-3 hours can ensure that the carboxyl carboxymethyl cellulose is fully carbonized. Specifically, the current collector may be a copper foil or the like.
Specifically, the preparation method further comprises the steps of: and introducing inert gas to prevent the current collector from being oxidized. The inert gas is introduced to further ensure that the current collector is not oxidized.
Specifically, the negative plate can be placed into a muffle furnace or other high-temperature adding equipment, vacuum-baked at 500-700 ℃ for 2-3 h, and then inert gas is introduced for protection.
Specifically, the surface density of the negative electrode slurry paved on the current collector is 50-150 g/m 2 . Specifically, the compacted density of the negative electrode slurry is 1.5-1.8 g/cm 3 。
The embodiment also discloses a battery negative plate prepared by the preparation method.
The embodiment also discloses a battery, which comprises the battery negative plate.
The technical effects of the technical solution of the present invention are better demonstrated by the following experimental examples and comparative examples.
Comparison group
Preparing a negative plate: preparing cathode slurry according to a conventional process; the negative electrode slurry is mixed according to the proportion of 100g/m 2 Coating the copper foil with surface density, drying, and compacting to obtain a compact density of 1.6g/cm 3 Rolling to obtain a negative plate;
preparing a positive plate: preparing a positive plate by adopting a conventional process;
preparing a battery: and (3) winding the prepared negative plate, the positive plate and the isolating membrane by a winding process, and matching with an electrolyte to prepare the lithium ion battery.
The comparison group is prepared by common batteries without high-temperature heating and carbonizing of carboxyl carboxymethyl cellulose on the negative plate. This comparative group prepared 6 lithium ion batteries as parallel groups according to the above procedure. And respectively testing the resistivity of each lithium ion battery.
Experimental group (550 ℃ C.)
Preparing a negative plate: preparing cathode slurry according to a conventional process; adding 100g/m of negative electrode slurry 2 Coating the copper foil with surface density, drying, and compacting to obtain a compact density of 1.6g/cm 3 Rolling to obtain a negative plate;
putting the negative plate into a muffle furnace, baking for 2.5h at 550 ℃ in vacuum, and protecting the copper foil from being oxidized under the protection of inert gas;
preparing a positive plate: preparing a positive plate by adopting a conventional process;
preparing a battery: and (3) winding the prepared negative plate, the positive plate and the isolating membrane by a winding process, and matching with an electrolyte to prepare the lithium ion battery.
The experimental group prepared 6 lithium ion batteries as parallel groups according to the above procedure. And respectively testing the resistivity of each lithium ion battery.
Experiment group (700 ℃ C.)
Preparing a negative plate: preparing cathode slurry according to a conventional process; adding 100g/m of negative electrode slurry 2 Coating the copper foil with surface density, drying, and compacting to obtain a compact density of 1.6g/cm 3 Rolling to obtain a negative plate;
placing the negative plate into a muffle furnace, and baking for 2.5 hours at 700 ℃ in vacuum, wherein the copper foil is prevented from being oxidized under the protection of inert gas;
preparing a positive plate: preparing a positive plate by adopting a conventional process;
preparing a battery: and (3) winding the prepared negative plate, the positive plate and the isolating membrane by a winding process, and matching with an electrolyte to prepare the lithium ion battery.
The experimental group prepared 6 lithium ion batteries as parallel groups according to the above procedure. And respectively testing the resistivity of each lithium ion battery.
Results of the experiment
As shown in fig. 1, the resistivity of the 6 parallel groups of the common batteries of the comparative group in which the carboxyl carboxymethyl cellulose was not carbonized by heating the negative electrode sheet at a high temperature was about 275 to 285(m Ω cm); the resistivity of the cells of the experimental group (550 ℃) and of the 6 parallel groups of the experimental group (700 ℃) was 130(m Ω cm). Therefore, the impedance of the negative plate can be directly reduced from about 280(m omega cm) to about 130(m omega cm), the impedance value is only half of the original impedance value and is only about 0.46 times of the original impedance value (130/280), the impedance value is directly reduced by a large half, the reduction is obvious, the effect is obvious, and the unexpected technical effect is obtained.
It should be noted that, the limitations of the steps involved in the present disclosure are not considered to limit the order of the steps without affecting the implementation of the specific embodiments, and the steps written in the foregoing may be executed first, or executed later, or even executed simultaneously, and as long as the present disclosure can be implemented, all should be considered to belong to the protection scope of the present disclosure.
The foregoing is a further detailed description of the invention in connection with specific alternative embodiments and is not intended to limit the invention to the specific embodiments described herein. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (9)
1. A preparation method of a battery negative plate is characterized by comprising the following steps:
preparing a negative electrode slurry, wherein the negative electrode slurry comprises carboxyl carboxymethyl cellulose;
laying the negative electrode slurry on a current collector and drying;
compacting the dried negative electrode slurry to obtain a negative electrode sheet;
and heating the negative plate at a high temperature to carbonize the carboxyl carboxymethyl cellulose in the negative plate.
2. The method for preparing the negative electrode plate of the battery according to claim 1, wherein the step of heating the negative electrode plate at a high temperature specifically comprises:
heating the negative plate at a high temperature of 500-700 ℃.
3. The preparation method of the negative electrode plate of the battery according to claim 2, wherein the step of heating the negative electrode plate at a high temperature specifically comprises:
heating the negative plate at a high temperature of 550 ℃.
4. The method for preparing the negative electrode plate of the battery according to claim 2, wherein the step of heating the negative electrode plate at a high temperature specifically comprises:
and (3) vacuumizing and baking the negative plate for 2-3 hours at 500-700 ℃.
5. The method for preparing the negative electrode sheet for the battery according to claim 2, further comprising the steps of:
and introducing inert gas to prevent the current collector from being oxidized.
6. The preparation method of the negative plate for the battery according to claim 1, wherein the surface density of the negative slurry laid on the current collector is 50-150 g/m 2 。
7. The preparation method of the negative electrode sheet for the battery according to claim 1, wherein the compacted density of the negative electrode slurry is 1.5-1.8 g/cm 3 。
8. A battery negative electrode sheet characterized by being produced by the production method according to any one of claims 1 to 7.
9. A battery comprising the negative electrode sheet of claim 8.
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| CN108886148A (en) * | 2016-03-30 | 2018-11-23 | 住友精化株式会社 | Non-aqueous electrolyte secondary battery electrode adhesive, electrode for nonaqueous electrolyte secondary battery mixture, electrode for nonaqueous electrolyte secondary battery, non-aqueous electrolyte secondary battery and electrical equipment |
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- 2022-05-30 CN CN202210597610.9A patent/CN115020633A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101069304A (en) * | 2004-12-10 | 2007-11-07 | 松下电器产业株式会社 | Lithium ion secondary battery and method for producing negative electrode therefor |
| JP2007080733A (en) * | 2005-09-15 | 2007-03-29 | Sharp Corp | Non-aqueous power storage device |
| CN102270759A (en) * | 2010-06-03 | 2011-12-07 | 索尼公司 | Cathode, lithium ion secondary battery, electric power tool and electrical vehicle |
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| CN108886148A (en) * | 2016-03-30 | 2018-11-23 | 住友精化株式会社 | Non-aqueous electrolyte secondary battery electrode adhesive, electrode for nonaqueous electrolyte secondary battery mixture, electrode for nonaqueous electrolyte secondary battery, non-aqueous electrolyte secondary battery and electrical equipment |
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