CN112103475A - Method for preparing lithium battery electrode by using supercritical current collector and electrode - Google Patents
Method for preparing lithium battery electrode by using supercritical current collector and electrode Download PDFInfo
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- CN112103475A CN112103475A CN202011008214.5A CN202011008214A CN112103475A CN 112103475 A CN112103475 A CN 112103475A CN 202011008214 A CN202011008214 A CN 202011008214A CN 112103475 A CN112103475 A CN 112103475A
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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
- H01M4/139—Processes of manufacture
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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
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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
- H01M4/04—Processes of manufacture in general
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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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
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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
- 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
Abstract
The invention relates to a method for preparing a lithium battery electrode by using a supercritical current collector and an electrode; the method comprises the following steps: putting the electrode material, the conductive agent and the adhesive into a high-pressure reaction kettle according to a required proportion; adding supercritical CO into a high-pressure reaction kettle2Stirring the fluid for 1 to 20 hours in a high-temperature and high-pressure closed environment with the temperature of between 100 and 150 ℃ and the pressure of between 1 and 20MPa, and carrying out reaction in the supercritical CO2Under the action of the fluid, the electrode material, the conductive agent and the adhesive form an electrode system which is uniformly distributed; carrying out pressure relief after the stirring is finished, wherein the pressure relief process is carried outSaid supercritical CO2Conversion of fluids to gaseous CO2Discharging the high-pressure reaction kettle; and after the pressure relief is finished, drying and hot-pressing the product in the high-pressure reaction kettle to obtain the lithium battery electrode.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a method for preparing a lithium battery electrode by using a supercritical current collector and the electrode.
Background
Due to rapid development of modern socioeconomic and science and technology, the performance of the traditional lithium ion battery can not meet the current energy requirement. The fields of rapidly developing electric automobiles, intelligent consumer electronics and the like all urgently need lithium ion batteries with higher energy density, long cycle life, low cost and high safety.
At present, in the aspects of positive and negative electrodes, the requirement on material capacity is higher and higher, and meanwhile, higher requirements on the stability and consistency of positive and negative electrode plates are also provided. At present, the research and development of various domestic enterprises and research units is mainly focused on the development of NCM811/NCA/LiCoO2the/LRM is a positive electrode and a high-capacity silicon-based material is a negative electrode such as SiO and nano silicon, and the materials are hopeful to realize a lithium ion battery with high energy density, but the cycle performance and the cycle life can be improved by optimizing the processing technology on the premise of controlling the production cost.
Currently, lithium ion battery electrodes are prepared by coating a mixed slurry of active material, conductive agent, binder, and solvent on a current collector, followed by drying the mixed slurry by exposure to one or more environments including, but not limited to, air convection, heating, reduced pressure, thermal radiation, and the like. Drying in a combination of steps tends to result in a more uniform distribution of binder and conductive carbon material, which reduces electrode polarization and exhibits better cycling performance.
However, during the preparation of the electrode containing the solvent, the process parameters (temperature, gas flow, pressure, heat radiation, etc.) significantly affect the microstructure of the final electrode, and the drying process parameters, such as high temperature, change resulting in an increase in the drying rate, the binder accumulating near the evaporation surface and depleting near the current collector. Uneven distribution of the binder causes a decrease in the adhesion between the electrode and the current collector, an increase in the resistance, and a decrease in the capacity.
In addition to the influence on the electrochemical performance caused by solvent volatilization, in the preparation of the positive and negative electrodes, the used solvent is usually a toxic solvent containing an organic solvent, so that the manufacturing cost is high, and meanwhile, the environmental pollution and damage are easily caused.
Disclosure of Invention
The embodiment of the invention provides a method for preparing a lithium battery electrode by using a supercritical current collector and the electrode. The electrode pole piece is obtained by using supercritical fluid to replace the conventional volatile solvent to carry out the slurry mixing process of the electrode material and combining with a dry electrode preparation method.
In a first aspect, an embodiment of the present invention provides a method for preparing an electrode of a lithium battery by using a supercritical current collector, where the method includes:
putting the electrode material, the conductive agent and the adhesive into a high-pressure reaction kettle according to a required proportion;
adding supercritical CO into a high-pressure reaction kettle2Stirring the fluid for 1 to 20 hours in a high-temperature and high-pressure closed environment with the temperature of between 100 and 150 ℃ and the pressure of between 1 and 20MPa, and carrying out reaction in the supercritical CO2Under the action of the fluid, the electrode material, the conductive agent and the adhesive form an electrode system which is uniformly distributed;
carrying out pressure relief after the stirring is finished, wherein in the pressure relief process, the supercritical CO2Conversion of fluids to gaseous CO2Discharging the high-pressure reaction kettle;
and after the pressure relief is finished, drying and hot-pressing the product in the high-pressure reaction kettle to obtain the lithium battery electrode.
Preferably, the hot pressing is to directly hot press the dried product or hot press the dried product onto a current collector.
Preferably, the electrode material includes any one of a positive electrode material or a negative electrode material;
the positive electrode material comprises one or a combination of nickel cobalt lithium manganate, lithium iron phosphate, lithium cobaltate, lithium manganate and lithium nickelate;
the negative electrode material comprises one or a combination of several of nano silicon, silica, silicon carbon, graphite, soft carbon and hard carbon;
the conductive agent comprises one or a combination of more of conductive carbon black, carbon fiber, conductive graphite and carbon nano tube;
the adhesive comprises one or a combination of styrene butadiene rubber, sodium carboxymethylcellulose, polyphenolic acids, polyacrylonitrile and sodium alginate.
Preferably, the stirring speed of the stirring is as follows: 100rmp-2000 rpm.
In a second aspect, an embodiment of the present invention provides a lithium battery electrode prepared by using the method for preparing a lithium battery electrode using a supercritical current collector according to the first aspect.
In a third aspect, an embodiment of the present invention provides a lithium battery, including the lithium battery electrode described in the second aspect.
Preferably, the lithium battery includes any one of a liquid lithium ion battery, a mixed solid-liquid metal lithium battery, an all-solid lithium ion battery, and an all-solid metal lithium battery.
The method for preparing the lithium battery electrode by using the supercritical current collector provided by the embodiment of the invention uses supercritical CO2The fluid replaces the conventional traditional volatile solvent to carry out the slurry mixing process of the electrode material, so that the problem that the traditional volatile solvent can cause the migration of the adhesive in the heating and removing process is effectively solved, and the problem that the traditional volatile solvent can cause the migration of the inner adhesive to the side close to the surface layer along with the drying of the surface layer solvent in the heating and removing process and the gradual diffusion of the inner layer solvent to the surface layer can cause the migration of the inner layer adhesive to the side close to the surface layer along with the solvent, thereby affecting the electrochemical performance of the battery is also avoided. Certainly, the adverse factors that the traditional volatile organic solvent is easy to generate waste water and waste gas, damage the environment and harm the human health are avoided.
The method for preparing the lithium battery electrode by using the supercritical current collector provided by the invention creates a novel dry pulping process, can reduce the cost and pollution and reduce the introduction of impurities, and can be suitable for all positive and negative electrode systems because the system does not contain water. The preparation method can ensure that the adhesive is uniformly distributed in the whole electrode system, effectively enhances the bonding performance of the electrode material and the current collector, the cycle performance, the storage life and the rate performance of the battery, and effectively reduces the resistance.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
Fig. 1 is a flowchart of a method for preparing a lithium battery electrode using a supercritical current collector according to an embodiment of the present invention;
FIG. 2 is a graph comparing the 100-cycle performance at 0.1C for the cells of example 1 and comparative example 1 provided in the examples of the present invention;
fig. 3 is a graph comparing the rate charge and discharge performance at 0.2C, 1C, 2C, 3C, 5C, 7C, and 10C for the batteries of example 1 and comparative example 1 provided in the present invention.
Detailed Description
The invention is further illustrated by the following figures and specific examples, but it should be understood that these examples are for the purpose of illustration only and are not to be construed as in any way limiting the present invention, i.e., as in no way limiting its scope.
The embodiment of the invention provides a method for preparing a lithium battery electrode by using a supercritical current collector, which mainly comprises the following steps as shown in figure 1:
wherein the electrode material comprises any one of a positive electrode material or a negative electrode material;
the positive electrode material comprises one or a combination of nickel cobalt lithium manganate, lithium iron phosphate, lithium cobaltate, lithium manganate and lithium nickelate;
the cathode material comprises one or a combination of several of nano silicon, silica, silicon carbon, graphite, soft carbon and hard carbon;
the conductive agent comprises one or a combination of more of conductive carbon black, carbon fiber, conductive graphite and carbon nano tube;
the adhesive comprises one or more of styrene butadiene rubber, sodium carboxymethylcellulose, polyphenolic acids, polyacrylonitrile and sodium alginate.
specifically, the stirring rate of the stirring was 100rmp-2000 rpm.
and step 140, drying and hot-pressing the product in the high-pressure reaction kettle after pressure relief is finished, so as to obtain the lithium battery electrode.
Specifically, the hot pressing is to directly hot press the dried product, or hot press the dried product onto the current collector. The current collector can be selected from current collectors conventionally used at present.
The lithium battery electrode prepared by the method can be used as a lithium battery electrode, and particularly can be used in battery systems such as a liquid lithium ion battery, a mixed solid-liquid metal lithium battery, an all-solid lithium ion battery, an all-solid metal lithium battery and the like.
Compared with the prior art, the method for preparing the lithium battery electrode by using the supercritical current collector provided by the embodiment of the invention has the following advantages:
1. using supercritical CO2The fluid replaces the conventional volatile solvent and is prepared from supercritical CO2In the process of changing into a gaseous state, the solid binder does not migrate along with the diffusion of the solvent, so that the binder can be uniformly dispersed in the whole electrode system;
2. the adhesive is uniformly distributed in the whole electrode system, so that the adhesive property of the electrode and the current collector is improved;
3. the internal resistance of the lithium battery electrode is reduced, and the corresponding rate performance is improved;
4. no organic solvent is volatilized in the system, so that the method is green and safe;
5. using supercritical CO2Fluid replaces the traditional solvent, the system has no moisture, and the high specific energy anode material can be suitable for water intolerance。
The lithium battery electrode material prepared by the preparation method has good cycle stability, storage life, high-temperature performance, safety performance and rate capability.
In order to better understand the technical solutions provided by the present invention, the following description respectively describes specific processes for preparing an electrode of a lithium battery by applying the method provided by the above embodiments of the present invention, and a method for applying the same to a lithium battery and battery characteristics.
Example 1
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 120 ℃ and 20MPa, mixing a graphite negative electrode material, conductive carbon black, styrene butadiene rubber and sodium carboxymethyl cellulose (CMC) according to a mass ratio of 90: 5: 2.5: 2.5 putting the mixture into a high-pressure reaction kettle, and adding high-pressure supercritical CO into the high-pressure reaction kettle2And (3) continuously stirring a closed system of the high-pressure reaction kettle for 20 hours at the rotating speed of 1500rpm under the environment of 120 ℃ and 20MPa, then decompressing, and carrying out hot pressing on the obtained material after drying to obtain the negative pole piece.
To facilitate the description of the characteristics of the material obtained by the preparation method of the present invention, comparative example 1 was also prepared for comparison by the following method:
comparative example 1
Dispersing a certain proportion of CMC adhesive into water, then adding a graphite negative electrode material and conductive carbon black, uniformly stirring, and finally adding styrene butadiene rubber to form negative electrode slurry, wherein the specific components are as follows: the mass ratio of the graphite negative electrode material to the conductive carbon black to the styrene butadiene rubber to the CMC is 90: 5: 2.5: 2.5. and (3) coating the negative electrode slurry, and then drying in a forced air drying oven at 80 ℃ to obtain the electrode for comparison.
The negative pole piece using the supercritical fluid carbon dioxide as the solvent in example 1 and the negative pole piece of the traditional wet mixing method in comparative example 1 are respectively subjected to peeling test comparison (see table 1), and the sheet resistance measured by a four-probe method at 30 ℃ is compared (see table 2).
Electrode preparation method | Peel strength (N/cm) | Peel force (N) |
Supercritical fluid preparation | 0.0075 | 0.1869 |
Preparation by wet method | 0.0072 | 0.1790 |
TABLE 1
Electrode preparation method | Surface resistance (m omega) |
Supercritical fluid preparation | 5.87 |
Preparation by wet method | 6.32 |
TABLE 2
Therefore, the electrode prepared by the supercritical current collector provided by the embodiment of the invention is superior to the electrode prepared by the traditional wet method in the performance of bonding capacity, and has smaller area resistance, thereby being beneficial to the reduction of the internal resistance of the electrode.
Button cells were prepared for performance comparison in example 1 and comparative example 1, respectively. Wherein Celgard2300 type diaphragm is adopted, metal lithium is used as a counter electrode, Ethylene Carbonate (EC)/dimethyl carbonate (DMC) +1M LiPF6Is an electrolyte. Through tests, the cycle performance of the electrode prepared by the method of the embodiment at 0.1 ℃ for 100 weeks is improved by 69 percent (see figure 2) compared with that of the electrode prepared by the traditional heating drying method, and the multiplying power charging and discharging performance is also improved (see figure 3).
Example 2
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 115 ℃ and 15MPa, mixing a silicon-oxygen negative electrode material, conductive carbon black, styrene-butadiene rubber and CMC in a mass ratio of 88: 6: 3: 3, putting the mixture into a high-pressure reaction kettle, and adding high-pressure supercritical CO into the high-pressure reaction kettle2And (3) continuously stirring the sealed system of the high-pressure reaction kettle for 10 hours at the rotating speed of 1200rpm under the environment of 115 ℃ and 15MPa, then decompressing, and carrying out hot pressing after drying to obtain the negative pole piece.
Example 3
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 110 ℃ and 10MPa, mixing the nano silicon negative electrode material, the conductive carbon black, the styrene-butadiene rubber and the CMC in a mass ratio of 80: 10: 5: 5, placing the mixture into a high-pressure reaction kettle, and adding high-pressure supercritical CO into the high-pressure reaction kettle2And (3) continuously stirring the closed system of the high-pressure reaction kettle for 5 hours at the rotating speed of 2000rpm under the environment of 110 ℃ and 10MPa, then decompressing, and carrying out hot pressing after drying to obtain the negative pole piece.
Example 4
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 110 ℃ and 10MPa, mixing lithium cobaltate, conductive carbon black and polyvinylidene fluoride (PVDF) according to the mass ratio of 80: 10: 10 put under high pressureA reaction kettle, high-pressure supercritical CO is added into the high-pressure reaction kettle2And (3) continuously stirring the closed system of the high-pressure reaction kettle for 15 hours at the rotating speed of 200rpm under the environment of 110 ℃ and 10MPa, then decompressing, and carrying out hot pressing after drying to obtain the positive pole piece.
Example 5
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 120 ℃ and 20MPa, mixing lithium manganate, conductive carbon black and PVDF according to the mass ratio of 80: 10: 10 putting the mixture into a high-pressure reaction kettle, and adding high-pressure supercritical CO into the high-pressure reaction kettle2And (3) continuously stirring the closed system of the high-pressure reaction kettle for 1 hour at the rotating speed of 1200rpm under the environment of 120 ℃ and 20MPa, then decompressing, and carrying out hot pressing after drying to obtain the positive pole piece.
Example 6
The embodiment provides a method for preparing a lithium battery electrode by using a supercritical current collector, which comprises the following steps:
under the conditions of 120 ℃ and 20MPa, mixing nickel cobalt lithium manganate, conductive carbon black and PVDF according to the mass ratio of 70: 15: 15 is put into a high-pressure reaction kettle, and high-pressure supercritical CO is added into the high-pressure reaction kettle2And (3) continuously stirring the closed system of the high-pressure reaction kettle for 20 hours at the rotating speed of 800rpm under the environment of 120 ℃ and 20MPa by using a fluid, then decompressing, and carrying out hot pressing after drying to obtain the positive pole piece.
The invention provides a special dry method for manufacturing a high specific energy electrode by using supercritical CO2The fluid replaces the conventional traditional volatile solvent to carry out the slurry mixing process of the electrode material, so that the problem that the traditional volatile solvent can cause the migration of the adhesive in the heating and removing process is effectively solved, and the problem that the traditional volatile solvent can cause the migration of the inner adhesive to the side close to the surface layer along with the drying of the surface layer solvent in the heating and removing process and the gradual diffusion of the inner layer solvent to the surface layer can cause the migration of the inner layer adhesive to the side close to the surface layer along with the solvent, thereby affecting the electrochemical performance of the battery is also avoided. Certainly, the method also avoids the problems that the traditional volatile organic solvent is easy to generate waste water and gas and damage the environment,adverse factors harmful to human health.
The method for preparing the lithium battery electrode by using the supercritical current collector provided by the invention creates a novel dry pulping process, can reduce the cost and pollution and reduce the introduction of impurities, and can be suitable for all positive and negative electrode systems because the system does not contain water. The preparation method can ensure that the adhesive is uniformly distributed in the whole electrode system, effectively enhances the bonding performance of the electrode material and the current collector, the cycle performance, the storage life and the rate performance of the battery, and effectively reduces the resistance.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method of making a lithium battery electrode using a supercritical current collector, the method comprising:
putting the electrode material, the conductive agent and the adhesive into a high-pressure reaction kettle according to a required proportion;
adding supercritical CO into a high-pressure reaction kettle2Stirring the fluid for 1 to 20 hours in a high-temperature and high-pressure closed environment with the temperature of between 100 and 150 ℃ and the pressure of between 1 and 20MPa, and carrying out reaction in the supercritical CO2Under the action of the fluid, the electrode material, the conductive agent and the adhesive form an electrode system which is uniformly distributed;
carrying out pressure relief after the stirring is finished, wherein in the pressure relief process, the supercritical CO2Conversion of fluids to gaseous CO2Discharging the high-pressure reaction kettle;
and after the pressure relief is finished, drying and hot-pressing the product in the high-pressure reaction kettle to obtain the lithium battery electrode.
2. The method of claim 1, wherein the hot pressing is direct hot pressing of the dried product or hot pressing onto a current collector.
3. The method of claim 1, wherein the electrode material comprises any one of a positive electrode material or a negative electrode material;
the positive electrode material comprises one or a combination of nickel cobalt lithium manganate, lithium iron phosphate, lithium cobaltate, lithium manganate and lithium nickelate;
the negative electrode material comprises one or a combination of several of nano silicon, silica, silicon carbon, graphite, soft carbon and hard carbon;
the conductive agent comprises one or a combination of more of conductive carbon black, carbon fiber, conductive graphite and carbon nano tube;
the adhesive comprises one or a combination of styrene butadiene rubber, sodium carboxymethylcellulose, polyphenolic acids, polyacrylonitrile and sodium alginate.
4. The method of claim 1, wherein the agitation is at an agitation rate of: 100rmp-2000 rpm.
5. A lithium battery electrode prepared by the method for preparing a lithium battery electrode using a supercritical current collector as claimed in any one of claims 1 to 4.
6. A lithium battery comprising the lithium battery electrode as claimed in claim 4.
7. The lithium battery of claim 6, wherein the lithium battery comprises any one of a liquid lithium ion battery, a hybrid solid-liquid lithium metal battery, an all solid state lithium ion battery, and an all solid state lithium metal battery.
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CN113611815A (en) * | 2021-08-05 | 2021-11-05 | 南京航空航天大学 | Dry mixing method of battery electrode material and preparation method of battery electrode plate |
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Application publication date: 20201218 |