CN112259741A - Current collector and preparation method and application thereof - Google Patents
Current collector and preparation method and application thereof Download PDFInfo
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- CN112259741A CN112259741A CN202011042988.XA CN202011042988A CN112259741A CN 112259741 A CN112259741 A CN 112259741A CN 202011042988 A CN202011042988 A CN 202011042988A CN 112259741 A CN112259741 A CN 112259741A
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- current collector
- black phosphorus
- dispersion liquid
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/22—Servicing or operating apparatus or multistep processes
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
-
- 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
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/80—Porous plates, e.g. sintered carriers
- H01M4/808—Foamed, spongy materials
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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 current collector and a preparation method and application thereof. The current collector comprises a three-dimensional metal framework and a black phosphorus layer, wherein the black phosphorus layer covers the whole outer surface of the three-dimensional metal framework. The preparation method comprises the following steps: adding magnesium salt into the black phosphorus dispersion liquid to form mixed dispersion liquid; and taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, and placing the negative electrode and the positive electrode in the mixed dispersion liquid for electrophoretic deposition to obtain the current collector. The invention also provides application of the current collector in preparation of a lithium negative electrode. The current collector has excellent cycle performance when used as a lithium negative electrode current collectorRing stability at a current density of 1mA cm‑2Capacity of 1mAh cm‑2The coulombic efficiency is kept above 95% for 200 times of lower circulation.
Description
Technical Field
The invention relates to the field of current collectors, in particular to a current collector and a preparation method and application thereof.
Background
At present, most of three-dimensional current collectors are modified by selectively modifying metal nanoparticles to form alloys or lithium-philic materials such as metal nitrides and oxides, the current collectors modified by lithium-philic sites induce uniform nucleation of lithium metal, however, after initial selective nucleation is performed on a substrate, an effective strategy is still lacked to induce the lateral growth of the lithium metal along the surface of the substrate, and a more stable lithium metal cathode without dendrites is difficult to obtain, so that the cycle stability of the lithium metal cathode is poor.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the current collector has poor circulation stability, and the coulomb efficiency is reduced after multiple cycles.
In order to solve the technical problems, the invention provides a current collector and a preparation method and application thereof.
The invention provides a current collector which comprises a three-dimensional metal framework and a black phosphorus layer, wherein the black phosphorus layer covers the whole outer surface of the three-dimensional metal framework.
Further, the three-dimensional metal framework is foamed copper, foamed nickel, foamed aluminum or metal mesh.
Further, the particle size of the black phosphorus in the black phosphorus layer is 50nm-30 μm.
The invention also provides a preparation method of the current collector, which comprises the following steps:
adding magnesium salt into the black phosphorus dispersion liquid to form mixed dispersion liquid;
and taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, and placing the negative electrode and the positive electrode in the mixed dispersion liquid for electrophoretic deposition to obtain the current collector.
Further, the magnesium salt is magnesium nitrate and/or magnesium chloride.
Further, the conductive substrate is conductive glass.
Further, the mass fraction of the black phosphorus in the mixed dispersion liquid is 0.05-5%.
Further, the mass fraction of the magnesium salt in the mixed dispersion is 1% -20%.
Further, the voltage of the electrophoretic deposition is a direct current constant voltage of 15-150V, and the time of the electrophoretic deposition is 10-60 minutes.
Further, the black phosphorus dispersion liquid is prepared by dispersing black phosphorus powder in a solvent, followed by ultrasonic pulverization.
In addition, the invention also provides an application of the current collector or the current collector prepared by the preparation method in the preparation of a lithium metal negative electrode.
Compared with the prior art, the invention has the advantages that: the current collector comprises a three-dimensional metal framework and black phosphorus, the whole outer surface of the three-dimensional metal framework is covered with the black phosphorus, the black phosphorus not only has strong lithium affinity, but also has an extremely low edge [100 ]]The potential barrier of crystal face ion migration has high lithium ion selective transmission characteristics, and can effectively inhibit dendritic crystal growth; in addition, the three-dimensional conductive framework is used as a framework material of lithium metal, so that the volume expansion of the lithium negative electrode can be reduced, and the current collector has excellent cycle stability when being used as a lithium negative electrode current collector and has the current density of 1 mA-cm-2Capacity of 1mAh cm-2The coulombic efficiency is kept above 95% for 200 times of lower circulation.
Drawings
The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, and in which:
fig. 1 is a schematic structural diagram of a current collector prepared in example 1 of the present invention;
fig. 2 is a schematic view of an apparatus for preparing a current collector according to the present invention;
fig. 3 is a schematic structural view of the copper foam used in example 1 of the present invention (left drawing) and the prepared current collector (right drawing);
fig. 4 is a raman spectrum of the current collector prepared in example 1 of the present invention;
fig. 5 is a coulombic efficiency graph of the current collector and the copper foam prepared in example 1 of the present invention.
Fig. 6 is a coulombic efficiency graph of the current collector prepared in example 1 of the present invention.
Description of reference numerals: 1. a three-dimensional metal skeleton; 2. and a black phosphorus layer.
Detailed Description
The specific embodiment provides a current collector, which comprises a three-dimensional metal framework 1 and a black phosphorus layer 2, wherein the black phosphorus layer 2 covers the whole outer surface of the three-dimensional metal framework 1; wherein the three-dimensional metal framework is foamed copper, foamed nickel, foamed aluminum or metal mesh; the particle size of the black phosphorus in the black phosphorus layer is 50nm-30 mu m.
The specific embodiment further comprises a preparation method of the current collector, which comprises the following steps:
adding magnesium salt into the black phosphorus dispersion liquid to form mixed dispersion liquid; wherein the magnesium salt is magnesium nitrate and/or magnesium chloride;
taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, placing the negative electrode and the positive electrode in the mixed dispersion liquid, and performing direct current constant voltage electrophoretic deposition for 10-60 minutes at 15-150V to obtain the current collector; the conductive substrate is conductive glass; further, the conductive glass is FTO conductive glass.
Wherein the mass fraction of the black phosphorus in the mixed dispersion liquid is 0.05-5%; the mass fraction of the magnesium salt in the mixed dispersion liquid is 1-20%; the black phosphorus dispersion liquid is prepared by dispersing black phosphorus powder in a solvent and then carrying out ultrasonic crushing for 5-60 minutes; the solvent is isopropanol and/or ethanol.
The specific embodiment further comprises the application of the current collector or the current collector prepared by the preparation method in the preparation of a lithium metal negative electrode.
The following detailed description of the preferred embodiments of the present invention is provided in connection with the accompanying drawings, which form a part hereof, and which together with the embodiments of the invention serve to explain the principles of the invention and not to limit the scope thereof. Both copper foam and black phosphorus were purchased from the market in the examples described below.
Example 1
The embodiment provides a method for preparing a current collector, which includes:
1) cutting 1mm thick foam copper into 5 × 8cm, sequentially placing in acetone, ethanol, hydrochloric acid, and deionized water, ultrasonically cleaning for 15min, and drying;
2) putting commercial black phosphorus crystals in a glove box in an argon atmosphere in a dark place, and grinding the black phosphorus in the dark place in the glove box; dispersing the ground black phosphorus crystals into isopropanol, and taking out the black phosphorus crystals from a glove box; ultrasonically crushing the isopropanol dispersed with the black phosphorus powder by using a cell crusher to form black phosphorus dispersion liquid, wherein the particle size of black phosphorus in the black phosphorus dispersion liquid is 50nm-10 mu m; adding magnesium nitrate into the black phosphorus dispersion liquid as an ionic conductivity improver, carrying out ultrasonic dispersion in an ultrasonic cleaning machine for 20 minutes, and storing under a dark condition to obtain a mixed dispersion liquid for electrophoretic deposition; the mass fraction of the black phosphorus in the mixed dispersion liquid is 5%, and the mass fraction of the magnesium nitrate is 15%.
3) And (3) putting the mixed dispersion liquid into a beaker, taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, putting the negative electrode and the positive electrode into the beaker filled with the mixed dispersion liquid, performing electrophoretic deposition to prepare the current collector, performing electrophoretic deposition at a constant voltage of 30V for 30min, drying with nitrogen, and drying at 45 ℃ for 2h to obtain the current collector.
Material characterization test: and performing SEM, Raman and other tests on the current collector. As shown in fig. 3, the surface of the copper foam itself is smooth as seen from the left, and after the treatment by the method, the black phosphorus nanosheet is uniformly attached to the copper foam as seen from the right. As shown in fig. 4, further illustrated in conjunction with raman spectroscopy are deposited black phosphorus nanoplates on copper foam. The collector (BP @ Cu Foam or Cu Foam @ BP) and the copper Foam (Cu Foam) were subjected to a coulombic efficiency test at a current density of 3 mA-cm-2Capacity of 3mAh · cm-2The lower coulombic efficiency is shown in fig. 5, the coulombic efficiency of the copper foam is greatly reduced after 20 times of repeated operations, the manifold has higher coulombic efficiency after hundreds of repeated operations, and the coulombic efficiency can be stabilized to be more than 90% in the previous 90 times. At a current density of 1mA cm-2Capacity of 1mAh cm-2The lower coulombic efficiency is shown in fig. 6, and the coulombic efficiency is kept above 95% for 200 cycles.
The embodiment also includes an application of the current collector in the preparation of a lithium negative electrode, specifically as follows:
cutting the prepared current collector into a wafer with the diameter of 14mm, transferring the wafer to an argon atmosphere glove box with the water oxygen value less than 0.1ppm, assembling a battery with lithium metal, uniformly depositing the lithium metal on the current collector by using a blue test system to form a composite lithium cathode, and disassembling the battery in the glove box to take out the composite lithium cathode.
Example 2
The embodiment provides a method for preparing a current collector, which includes:
1) cutting 1mm thick foam copper into 5 × 8cm, sequentially placing in acetone, ethanol, hydrochloric acid, and deionized water, ultrasonically cleaning for 15min, and drying;
2) putting commercial black phosphorus crystals in a glove box in an argon atmosphere in a dark place, and grinding the black phosphorus in the dark place in the glove box; dispersing the ground black phosphorus crystals into isopropanol, and taking out the black phosphorus crystals from a glove box; ultrasonically crushing the isopropanol dispersed with the black phosphorus powder by using a cell crusher to form black phosphorus dispersion liquid, wherein the particle size of black phosphorus in the black phosphorus dispersion liquid is 50nm-30 mu m; adding magnesium nitrate into the black phosphorus dispersion liquid as an ionic conductivity improver, carrying out ultrasonic dispersion in an ultrasonic cleaning machine for 5 minutes, and storing under a dark condition to obtain a mixed dispersion liquid for electrophoretic deposition; the mass fraction of the black phosphorus in the mixed dispersion liquid is 1%, and the mass fraction of the magnesium nitrate is 20%.
3) And (3) putting the mixed dispersion liquid into a beaker, taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, putting the negative electrode and the positive electrode into the beaker filled with the mixed dispersion liquid, performing electrophoretic deposition to prepare the current collector, performing electrophoretic deposition at a constant voltage of 15V for 40min, drying with nitrogen, and drying at 45 ℃ for 2h to obtain the current collector.
The embodiment also includes an application of the current collector in the preparation of a lithium negative electrode, specifically as follows:
cutting the prepared current collector into a wafer with the diameter of 14mm, transferring the wafer to an argon atmosphere glove box with the water oxygen value less than 0.1ppm, assembling a battery with lithium metal, uniformly depositing the lithium metal on the current collector by using a blue test system to form a composite lithium cathode, and disassembling the battery in the glove box to take out the composite lithium cathode.
Example 3
The embodiment provides a method for preparing a current collector, which includes:
1) cutting 1mm thick foam copper into 5 × 8cm, sequentially placing in acetone, ethanol, hydrochloric acid, and deionized water, ultrasonically cleaning for 15min, and drying;
2) putting commercial black phosphorus crystals in a glove box in an argon atmosphere in a dark place, and grinding the black phosphorus in the dark place in the glove box; dispersing the ground black phosphorus crystals into isopropanol, and taking out the black phosphorus crystals from a glove box; ultrasonically crushing the isopropanol dispersed with the black phosphorus powder by using a cell crusher to form a dispersed black phosphorus dispersion liquid, wherein the particle size of black phosphorus in the black phosphorus dispersion liquid is 50nm-10 mu m; adding magnesium chloride serving as an ionic conductivity improver into the black phosphorus dispersion liquid, performing ultrasonic dispersion in an ultrasonic cleaning machine for 40 minutes, and storing under a dark condition to serve as a mixed dispersion liquid for electrophoretic deposition; the mass fraction of black phosphorus in the mixed dispersion liquid is 3%, and the mass fraction of magnesium nitrate is 15%.
3) And (3) putting the mixed dispersion liquid into a beaker, taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, putting the negative electrode and the positive electrode into the beaker filled with the mixed dispersion liquid, performing electrophoretic deposition to prepare the current collector, performing electrophoretic deposition at a constant voltage of 15V for 40min, drying with nitrogen, and drying at 45 ℃ for 2h to obtain the current collector.
The embodiment also includes an application of the current collector in the preparation of a lithium negative electrode, specifically as follows:
cutting the prepared current collector into a wafer with the diameter of 14mm, transferring the wafer to an argon atmosphere glove box with the water oxygen value less than 0.1ppm, assembling a battery with lithium metal, uniformly depositing the lithium metal on the current collector by using a blue test system to form a composite lithium cathode, and disassembling the battery in the glove box to take out the composite lithium cathode.
Example 4
The embodiment provides a method for preparing a current collector, which includes:
1) cutting foamed nickel with the thickness of 1mm into the size of 5 multiplied by 8cm, sequentially putting the cut foamed nickel into acetone, ethanol, hydrochloric acid and deionized water for ultrasonic cleaning for 15min, and drying for later use;
2) putting commercial black phosphorus crystals in a glove box in an argon atmosphere in a dark place, and grinding the black phosphorus in the dark place in the glove box; dispersing the ground black phosphorus crystals into isopropanol, and taking out the black phosphorus crystals from a glove box; ultrasonically crushing the isopropanol dispersed with the black phosphorus powder by using a cell crusher to form a dispersed black phosphorus dispersion liquid, wherein the particle size of black phosphorus in the black phosphorus dispersion liquid is 50nm-10 mu m; adding magnesium chloride serving as an ionic conductivity improver into the black phosphorus dispersion liquid, carrying out ultrasonic dispersion in an ultrasonic cleaning machine for 25 minutes, and storing under a dark condition to serve as a mixed dispersion liquid for electrophoretic deposition; the mass fraction of black phosphorus in the mixed dispersion liquid is 1%, and the mass fraction of magnesium nitrate is 1%.
3) And (3) putting the mixed dispersion liquid into a beaker, taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, putting the negative electrode and the positive electrode into the beaker filled with the mixed dispersion liquid, performing electrophoretic deposition to prepare the current collector, performing electrophoretic deposition at a constant voltage of 15V for 40min, drying with nitrogen, and drying at 45 ℃ for 2h to obtain the current collector.
The embodiment also includes an application of the current collector in the preparation of a lithium negative electrode, specifically as follows:
cutting the prepared current collector into a wafer with the diameter of 14mm, transferring the wafer to an argon atmosphere glove box with the water oxygen value less than 0.1ppm, assembling a battery with lithium metal, uniformly depositing the lithium metal on the current collector by using a blue test system to form a composite lithium cathode, and disassembling the battery in the glove box to take out the composite lithium cathode.
Example 5
This example is substantially identical to the method of example 1, with the only difference that: the three-dimensional metal framework is foamed aluminum.
Example 6
This example is substantially identical to the method of example 1, with the only difference that: the three-dimensional metal framework is a metal net.
Comparative example 1
A method of making a current collector, the method comprising:
1) cutting 1mm thick foam copper into 5 × 8cm, sequentially placing in acetone, ethanol, hydrochloric acid, and deionized water, ultrasonically cleaning for 15min, and drying;
2) putting commercial black phosphorus crystals in a glove box in an argon atmosphere in a dark place, and grinding the black phosphorus in the dark place in the glove box; dispersing the ground black phosphorus crystals into isopropanol, and taking out the black phosphorus crystals from a glove box; ultrasonically crushing the isopropanol dispersed with the black phosphorus powder by using a cell crusher to form black phosphorus dispersion liquid, wherein the particle size of black phosphorus in the black phosphorus dispersion liquid is 50nm-10 mu m, ultrasonically dispersing for 20 minutes in an ultrasonic cleaning machine, and storing under the condition of keeping out of the sun to be used as mixed dispersion liquid for electrophoretic deposition; the mass fraction of the black phosphorus in the mixed dispersion liquid is 5%, and the mass fraction of the magnesium nitrate is 15%.
The comparative example is tested by SEM, Raman and the like (not shown in the figure), and black phosphorus nanosheets are almost not formed on the foam copper, which shows that the magnesium salt influences the deposition effect of the black phosphorus.
Comparative example 2
A method of making a current collector, the method comprising:
1) cutting 1mm thick foam copper into 5 × 8cm, sequentially placing in acetone, ethanol, hydrochloric acid, and deionized water, ultrasonically cleaning for 15min, and drying;
2) placing graphene in a glove box in an argon atmosphere, and grinding the graphene in the glove box; dispersing the ground graphene into isopropanol, and taking out the graphene from a glove box; ultrasonically crushing the isopropanol dispersed with the graphene powder by using a cell crusher to form graphene dispersion liquid, wherein the particle size of graphene in the graphene dispersion liquid is 50nm-10 mu m, ultrasonically dispersing for 20 minutes in an ultrasonic cleaning machine, and storing under the condition of keeping out of the sun to obtain mixed dispersion liquid for electrophoretic deposition; the mass fraction of graphene in the mixed dispersion liquid is 5%, and the mass fraction of magnesium nitrate is 15%.
At a current density of 1mA cm-2Capacity of 1mAh cm-2And performing a coulombic efficiency test, wherein the coulombic efficiency of the current collector is about 90% at first, and the coulombic efficiency is sharply reduced after 90 times of circulation.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. The current collector is characterized by comprising a three-dimensional metal framework and a black phosphorus layer, wherein the black phosphorus layer covers the whole outer surface of the three-dimensional metal framework.
2. The current collector of claim 1, wherein the three-dimensional metal skeleton is copper foam, nickel foam, aluminum foam, or metal mesh.
3. The current collector of claim 1, wherein the black phosphorus in the black phosphorus layer has a particle size of 50nm to 30 μ ι η.
4. A method for preparing the current collector of any one of claims 1 to 3, comprising the steps of:
adding magnesium salt into the black phosphorus dispersion liquid to form mixed dispersion liquid;
and taking a three-dimensional metal framework as a negative electrode and a conductive substrate as a positive electrode, and placing the negative electrode and the positive electrode in the mixed dispersion liquid for electrophoretic deposition to obtain the current collector.
5. The method according to claim 4, wherein the magnesium salt is magnesium nitrate and/or magnesium chloride.
6. The method according to claim 4, wherein the mass fraction of the black phosphorus in the mixed dispersion is 0.05 to 5%.
7. The method according to claim 4, wherein the magnesium salt is present in the mixed dispersion at a mass fraction of 1% to 20%.
8. The method of claim 4, wherein the voltage of the electrophoretic deposition is a DC constant voltage of 15-150V, and the time of the electrophoretic deposition is 10-60 minutes.
9. The production method according to claim 4, wherein the black phosphorus dispersion liquid is produced by dispersing black phosphorus powder in a solvent, followed by ultrasonic pulverization.
10. Use of a current collector according to any one of claims 1 to 3 or a current collector obtained by the method according to any one of claims 4 to 9 for the preparation of a lithium metal negative electrode.
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Application publication date: 20210122 |
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