CN114242953A - Metallic lithium cathode and preparation method and application thereof - Google Patents
Metallic lithium cathode and preparation method and application thereof Download PDFInfo
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- CN114242953A CN114242953A CN202111581486.9A CN202111581486A CN114242953A CN 114242953 A CN114242953 A CN 114242953A CN 202111581486 A CN202111581486 A CN 202111581486A CN 114242953 A CN114242953 A CN 114242953A
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—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
- 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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- 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
- H01M4/1399—Processes of manufacture of electrodes based on electro-active polymers
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- 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
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Abstract
The invention discloses a metallic lithium cathode and a preparation method and application thereof, and the preparation method comprises the following steps: s1, dissolving a fluorine-containing or/and chlorine-containing high molecular compound in a solvent to obtain a reaction solution, wherein the solvent is a compound containing an amido group and/or an aldehyde group; and S2, uniformly coating the reaction solution on the surface of the lithium metal to react for 0.5-30min to obtain the lithium metal negative electrode with the passivation layer on the surface. The fluorine-chlorine-containing polymer and the metal lithium react rapidly under the action of the solvent to form a lithium fluoride or lithium chloride passivation layer on the surface of the metal lithium rapidly, so that the complete preparation process can be realized within 0.5min, and meanwhile, the unreacted polymer forms a wrapping protection effect on the outermost layer, so that the direct contact between the metal lithium and the electrolyte is effectively prevented, and the electrochemical performance of the lithium metal battery is improved.
Description
Technical Field
The invention relates to the technical field of lithium metal batteries, in particular to a lithium metal cathode and a preparation method and application thereof.
Background
In the process of charging and discharging of the lithium metal battery, lithium ion deposition is uneven, so that lithium dendrite is formed on the surface of a lithium metal negative electrode, the service efficiency and the service life of the battery are seriously influenced, and even the danger of short-circuit combustion and explosion is more serious. In the prior art, a layer of solid electrolyte interface film is constructed on the surface of metal lithium, so that the direct contact between the metal lithium and electrolyte is effectively prevented, the side reaction on the surface of the metal lithium is inhibited, and the growth of lithium dendrite can be slowed down. However, the artificially constructed SEI film has limited performance, and the preparation method is complex and high in cost, so that the method is not beneficial to industrial production.
Chinese patent CN113299887A discloses a method for preparing a lithium metal negative electrode, a lithium metal negative electrode and a lithium metal battery. The technical scheme is as follows: dissolving a first passivation substance and a second passivation substance in a solvent to obtain a passivation solution, wherein the first passivation substance is a polyalkyl compound, the number of carbon atoms in the polyalkyl compound is 10-20, and the second passivation substance is a halide salt; placing the metal lithium in a passivation solution to react for 0.1-24h to obtain a metal lithium cathode with a passivation layer on the surface; and cleaning the metal lithium cathode by adopting a solvent, and drying the cleaned metal lithium cathode in an inert environment to obtain the metal ion cathode. The first passivation may be a lithium polyalkylphosphate, a lithium polyalkylamine, a lithium polyalkylcarboxylate, a lithium polyalkylmercaptide, or a lithium polyalkylalkoxide. The halide salt may be an aluminum halide, a zinc halide, an indium halide, a bismuth halide, an arsenic halide, or a tin halide. The patent technology can form a passivation layer on the surface of the metal lithium, wherein the polyalkyl chain in the polyalkyl compound in the first passivation can play a role in blocking polysulfide, so that the polyalkyl lithium salt generated by the first passivation and the metal lithium can reject the polysulfide, and meanwhile, the halide salt in the second passivation can perform a displacement reaction with the metal lithium to obtain a lithium-based alloy which can be used as a lithium ion rapid transmission channel. However, the preparation process of the patent technology is complicated and limited by the process principle, the obtained lithium metal negative electrode is exposed, and a passivation layer is formed on the surface of the lithium metal negative electrode, which is not beneficial to the contact between the lithium metal negative electrode and a current collector.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the invention provides a lithium metal cathode and a preparation method and application thereof, the invention adopts fluorine and chlorine containing macromolecules as reactants, the fluorine and chlorine containing macromolecules react with lithium metal rapidly under the action of a solvent to form a lithium fluoride or lithium chloride passivation layer on the surface of the lithium metal rapidly, and simultaneously, unreacted macromolecules form a wrapping protection effect on the outermost layer, thereby effectively preventing the lithium metal from being in direct contact with electrolyte and improving the electrochemical performance of the lithium metal battery.
The technical scheme adopted by the invention is as follows: a preparation method of a lithium metal negative electrode comprises the following steps:
s1, dissolving a fluorine-containing or/and chlorine-containing high molecular compound in a solvent to obtain a reaction solution, wherein the solvent is a compound containing an amido group and/or an aldehyde group;
and S2, uniformly coating the reaction solution on the surface of the lithium metal to react for 0.5-30min to obtain the lithium metal negative electrode with the passivation layer on the surface.
In the invention, a fluorine-containing or/and chlorine-containing high molecular compound rapidly reacts with metal lithium under the synergistic action of a solvent to form a lithium fluoride passivation layer or a lithium chloride passivation layer, a small amount of unreacted substances form a wrapping protection effect on the outermost layer, and under the combined action, the electrochemical performance of the lithium metal battery is effectively improved.
The fluorine-containing or/and chlorine-containing polymer compound is one or two of vinylidene fluoride and polyvinyl chloride, and may be other fluorine-containing or/and chlorine-containing polymer compounds. The general molecular structure formula of the fluorine-containing and chlorine-containing substance related by the invention is shown as formula (1) and formula (2), and polyvinylidene fluoride or polyvinyl chloride is preferred.
In the invention, the solvent is a mixture of an amide compound and an aldehyde compound or/and a formamide compound. The specific solvents related to the invention are mainly divided into two types, one type is a mixture of an amide compound and an aldehyde compound, the molecular structural general formula of the specific solvents can be shown as a formula (3), the other type of the specific solvents is a formamide compound, and the molecular structural general formula of the specific solvents is shown as a formula (4):
in the present invention, the matching of the specific solvent and the fluorine-containing or/and chlorine-containing polymer compound is very important, which directly affects the performance of the passivation layer, and if the specific solvent is not selected in the manner of the present invention, it is difficult to obtain not only a passivation layer that meets the requirements but also a passivation layer structure, for example, when only a non-formamide compound is used as the solvent, it is difficult to form the passivation layer during the lithium metal treatment.
In the present invention, when the solvent is a formamide compound, the solvent is selected from one or more of N, N-dimethylformamide, N-diethylformamide, N-dipropylformamide, N-dibutylformamide and N, N-dipentylformamide.
In the present invention, when the solvent is a mixture of an amide compound and an aldehyde compound, the amide compound is selected from one or more of N, N-dimethylacetamide, N-dimethylpropionamide, N-diethylpropionamide, and N, N-diethylacetamide, and the aldehyde compound is selected from one or more of N-butyraldehyde, isobutyraldehyde, N-valeraldehyde, and isovaleraldehyde.
Further, when the fluorine-containing or chlorine-containing substance is vinylidene fluoride or polyvinyl chloride, the solvent is one or more of N, N-diethylformamide, a mixture of N, N-dimethylacetamide and N-butyraldehyde, a mixture of N, N-dimethylpropionamide and N-butyraldehyde, a mixture of N, N-dimethylacetamide and isobutyraldehyde, and N, N-dimethylformamide.
In the invention, when the fluorine-containing or chlorine-containing substance is polyvinylidene fluoride or polyvinyl chloride, the concentration of the polyvinylidene fluoride or polyvinyl chloride in the solvent needs to be moderate, and should not be too small or too large, when the dosage is too large, the reaction time is difficult to master, so that the thickness of the obtained passivation layer is difficult to control, and on the contrary, when the dosage is too small, the thickness and the performance of the obtained passivation layer are difficult to meet the requirements. In general, the reference concentration of the vinylidene fluoride or polyvinyl chloride in the solvent is 2 to 20 g/L.
Further, the passivation layer is lithium fluoride or/and lithium chloride.
Further, the thickness of the passivation layer is 50-1000 nm.
The invention also provides a lithium metal negative electrode prepared by the preparation method.
The invention also comprises a lithium metal battery which comprises the metal lithium negative electrode, wherein the metal lithium negative electrode is the metal lithium negative electrode.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, a specific solvent is matched with fluorine-and chlorine-containing macromolecules for use, and under the synergistic effect, the lithium fluoride or chlorine-containing macromolecules can rapidly react with metal lithium, so that a lithium fluoride or lithium chloride passivation layer is rapidly formed on the surface of the metal lithium, the complete preparation process can be realized within the shortest 0.5min, and then an unreacted substance is utilized to form a wrapping protection effect on the outermost layer, so that the direct contact between the metal lithium and an electrolyte is effectively prevented, the electrochemical performance of the lithium metal battery is improved, and the capacity retention rate of the lithium metal battery in the charge-discharge cycle process is obviously improved;
2. the preparation method has the advantages of simple process, low preparation cost, less process time consumption, easy control of the thickness of the passivation layer and the like, and is more suitable for industrial production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for preparing a metallic lithium anode with a passivation layer comprises the following steps:
s1, weighing 0.025g of polyvinylidene fluoride (fluorine-containing high molecular compound) and dissolving in 5mL of N, N-dimethylformamide solvent, and stirring and dissolving uniformly at 25 ℃ to obtain a reaction solution;
s2, flattening the metal lithium sheet, scanning the diaphragm adsorbing the reaction liquid on the surface of the metal lithium sheet at a constant speed, standing for 10min, and changing the liquid on the surface of the metal lithium sheet from colorless to colored liquid to obtain the metal lithium cathode with the passivation layer.
Example 2
Example 2 was the same as example 1 except that 0.1g of polyvinylidene fluoride was dissolved in 5ml of N, N-dimethylformamide solvent and the standing time was 0.5 min.
Example 3
Example 3 is the same as example 1 except that the standing time was 5 min.
Example 4
Example 4 is the same as example 1 except that polyvinylidene fluoride is replaced with polyvinyl chloride.
Example 5
Example 5 is the same as example 1 except that N, N-dimethylformamide is replaced with N, N-diethylformamide.
Example 6
Example 6 is the same as example 1 except that N, N-dimethylformamide was replaced with a mixture of N, N-dimethylacetamide and isobutyraldehyde.
Example 7
Example 7 is the same as example 1 except that N, N-dimethylformamide is replaced with a mixed solution of N, N-dimethylpropionamide and N-butyraldehyde.
Example 8
Example 8 is the same as example 1 except that N, N-dimethylformamide was replaced with a mixed solution of N, N-diethylacetamide and N-butyraldehyde.
Example 9
Example 9 is the same as example 6 except that polyvinylidene fluoride is replaced with polyvinyl chloride.
Example 10
Example 10 is the same as example 8 except that polyvinylidene fluoride is replaced with polyvinyl chloride.
Comparative example 1
Comparative example 1 is the same as example 1 except that N, N-dimethylformamide is replaced with N, N-dimethylacetamide.
Comparative example 2
Comparative example 2 is the same as example 1 except that N, N-dimethylformamide was replaced with N-butyraldehyde.
The thickness of the passivation layer on the surface of the lithium metal negative electrode of each of the above examples 1-10 and comparative examples 1-2 was tested, and the lithium metal negative electrode prepared by the above examples 1-10 and comparative examples 1-2 was used as the negative electrode of the test cell, and lithium iron phosphate was used as the positive electrode of the cell, and then a 2032 button cell was assembled by adding a proper amount of electrolyte to perform the electrochemical performance test. The test conditions were discharge to a capacity of 2.5V at a current density of 0.5C and then charge to 4.0V at the same current density, and the cycle was repeated until the cell failed. The coulombic efficiency test is a ratio of the capacity during charging to the capacity during discharging in the battery cycle stability test, and the test results are shown in table 1.
Table 1 shows the reaction conditions and electrochemical properties of assembled batteries of examples 1 to 10 and comparative examples 1 to 2
From the test results in table 1, the following conclusions can be drawn:
1. it can be seen from comparative examples 1 and 9 that when lithium metal sheets are treated with different polymeric compounds and different solvents, different passivation layers are formed with different thicknesses at the same treatment time, due to the different activities of the lithium sheets when the synergistic effects of the different polymeric compounds and different solvents react with each other.
2. It can be obtained by comparing examples 1 and 3 that the thickness of the passivation layer on the metallic lithium increases with time under different reaction time conditions, and the assembled battery capacity retention rate performance is optimal when the reaction time is 10 minutes.
3. It can be seen from comparing examples 1 and 2 that the assembled battery capacity retention rates are similar when the concentration of the reaction solution is increased and the reaction time is correspondingly shortened, thus illustrating that the processing time can be shortened by adjusting the concentration of the reactant, however, in the experimental process, it is found that the reaction time is more and more difficult to control as the concentration of the reactant is increased, so that the relationship between the concentration of the reactant and the reaction time needs to be balanced to make the whole reaction in a controllable range.
4. As can be seen from comparing examples 1, 5 and 8, when the solvent type is changed, the formed passivation layer has different thicknesses, which are mainly the structural differences of the passivation layer caused by the solvent effect, and the capacity retention rate rather tends to decrease with the increase of the passivation layer thickness, thereby indicating that the passivation layer thickness is not a determining factor of the capacity retention rate, and the increase of the passivation layer thickness does not necessarily increase the capacity retention rate of the battery.
5. By comparing examples 1 and 4, it can be obtained that the passivation layers formed by the polymer compounds respectively containing fluorine and chlorine are respectively lithium fluoride and lithium chloride, and the two different passivation layers have larger thickness difference, but the capacity retention rate is closer, and the technical effects are basically the same.
6. In comparison with example 1, the solvent of comparative example 1 contains only N, N-dimethylacetamide, and the solvent cannot react with metal lithium in cooperation with a polymer, and thus a passivation layer is not formed, and the battery capacity retention rate is at the worst 66.1%, thereby illustrating that when a formamide compound is used alone, since the formamide compound contains both amide and aldehyde groups, a passivation layer structure according with the expected performance can be obtained, whereas if an amide compound is used alone and a compound containing an aldehyde group is absent, a passivation layer structure is difficult to obtain, and finally a preparation process fails, and therefore, only when the solvent can contain both amide and aldehyde groups, a passivation layer having the expected performance can be ensured.
7. In comparison with example 1, the solvent of comparative example 2, which contains only n-butyraldehyde, can react with lithium metal to form a passivation layer of an alkyllithium compound, not a lithium chloride compound, and has a poor protective effect, thus demonstrating that, when the solvent contains only aldehyde groups and does not contain amide groups, although the passivation layer structure can be obtained, the property of the passivation layer is completely changed, so that the protection effect of the passivation layer on the metal lithium is obviously reduced, the technical effect claimed by the invention is difficult to achieve, therefore, the invention can effectively protect the lithium metal without forming a passivation layer, and the invention protects the lithium metal negative electrode by forming the lithium chloride or lithium fluoride passivation layer on the surface of the lithium metal, thereby obtaining excellent protection effect, however, when the passivation layer is not a lithium chloride or lithium fluoride passivation layer, it is difficult to ensure that the passivation layer can achieve the same or similar technical effects as the present application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of a lithium metal negative electrode is characterized by comprising the following steps:
s1, dissolving a fluorine-containing or/and chlorine-containing high molecular compound in a solvent to obtain a reaction solution, wherein the solvent is a compound containing an amido group and/or an aldehyde group;
and S2, uniformly coating the reaction solution on the surface of the lithium metal to react for 0.5-30min to obtain the lithium metal negative electrode with the passivation layer on the surface.
2. The method for preparing a lithium metal anode according to claim 1, wherein the fluorine-containing or/and chlorine-containing polymer compound is one or both of vinylidene fluoride and polyvinyl chloride.
3. The method of manufacturing a lithium metal anode according to claim 2, wherein the solvent is a mixture of an amide compound and an aldehyde compound or/and a formamide compound.
4. The method of claim 3, wherein when the solvent is a formamide compound, the solvent is one or more selected from the group consisting of N, N-dimethylformamide, N-diethylformamide, N-dipropylformamide, N-dibutylformamide, and N, N-dipentylcarboxamide.
5. The method of manufacturing a lithium metal anode according to claim 3, wherein when the solvent is a mixture of an amide compound selected from one or more of N, N-dimethylacetamide, N-dimethylpropionamide, N-diethylpropionamide, and N, N-diethylacetamide and an aldehyde compound selected from one or more of N-butyraldehyde, isobutyraldehyde, N-valeraldehyde, and isovaleraldehyde.
6. The method of preparing a lithium metal anode according to claim 1, wherein when the fluorine-or chlorine-containing substance is vinylidene fluoride or polyvinyl chloride, the solvent is one or more of N, N-diethylformamide, a mixture of N, N-dimethylacetamide and N-butyraldehyde, a mixture of N, N-dimethylpropionamide and N-butyraldehyde, a mixture of N, N-dimethylacetamide and isobutyraldehyde, and N, N-dimethylformamide.
7. The method of claim 6, wherein the passivation layer is lithium fluoride or/and lithium chloride.
8. The method of preparing a lithium metal anode of claim 7, wherein the passivation layer has a thickness of 50 to 1000 nm.
9. A lithium metal negative electrode produced by the production method according to any one of claims 1 to 8.
10. A lithium metal battery comprising a lithium metal anode, wherein the lithium metal anode is the lithium metal anode of claim 9.
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