CN111293316A - Negative pole piece, preparation method thereof and application thereof in solid-state battery - Google Patents
Negative pole piece, preparation method thereof and application thereof in solid-state battery Download PDFInfo
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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
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the 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
- 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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- 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
- 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
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Abstract
The invention discloses a negative pole piece, a preparation method thereof and application in a solid-state battery. The method comprises the following steps: and soaking the negative pole piece in an ester solution to obtain the negative pole piece containing the carbonate organic layer, wherein the ester solution comprises vinylene carbonate, and the negative pole piece comprises metal lithium. The method aims to solve the problem that in the prior art, a carbonate material can react with metal lithium under electrochemical induction to form loss, so that the surface of the metal lithium still has a certain deposition phenomenon. The film forming additive is an unsaturated carbide additive (vinylene carbonate), the vinylene carbonate has a lower reduction potential than that of a carbonate solvent, so that the vinylene carbonate is easier to reduce, a small amount of vinylene carbonate added into the ester solvent can play a better protection role on a carbonate protective layer, and is reduced in priority to the carbonate protective layer to form a complete carbonate protective layer.
Description
Technical Field
The invention belongs to the technical field of solid-state batteries, and particularly relates to a negative pole piece, a preparation method thereof and application thereof in a solid-state battery.
Background
The requirement on an energy storage system in the aspects of electric vehicles and power grid storage is continuously improved, so that the requirement on a high-capacity battery is increasingly urgent, and metallic lithium has theoretical capacity about ten times higher than graphite and has a very wide application prospect. In recent years, solid electrolytes are considered to be effective means for solving the problems of application of lithium metal because they are nonflammable, non-corrosive, non-volatile, and free from liquid leakage.
However, the solid electrolyte also has many practical application problems, for example, when the metallic lithium is applied to an all-solid system, a certain deposition phenomenon still exists on the surface of the metallic lithium, which has a certain adverse effect on the overall performance of the battery. Therefore, how to protect the metallic lithium negative electrode is also a technical problem to be solved by the solid electrolyte battery.
At present, the method for protecting the metal lithium cathode is a conventional method for adding a protective layer on the surface of lithium metal, and researches prove that the application of a carbonate protective layer on the surface of the metal lithium cathode has beneficial effects on improving the overall performances of the battery such as the first efficiency and the like; in previous studies, the applicant found that in solid-state batteries, even the carbonate material in the form of a protective layer reacts with metallic lithium under electrochemical induction to form losses, by the following mechanism:
therefore, the protective layer is slowly worn down with the lapse of the use time, so that the capacity retention rate of the battery is reduced; meanwhile, since the decomposition reaction of the protective layer is accompanied by the generation of a large amount of irreversible gas, the overall performance of the battery is also adversely affected. Therefore, how to ensure the integrity of the carbonate protective film is a technical problem which needs to be solved urgently.
CN108417774A discloses a negative electrode slurry mixing process with a pre-lithiation effect and a lithium battery, wherein under the environment condition that the dew point is-40 to-50 ℃, dry powder of a negative electrode active substance, a conductive agent and the like is uniformly stirred, then the conductive slurry is added, NMP is added twice and kneaded and uniformly mixed, and finally a metal lithium sheet and electrolyte containing a film-forming additive are added to disperse and pre-lithiate the negative electrode slurry. However, the method cannot only solve the problem of electrochemical consumption of carbonate solvents in an electrolyte environment, and does not relate to how to effectively solve the problem of surface deposition of the lithium metal.
Therefore, how to protect the integrity of the carbonate protective film in the lithium metal negative electrode is a technical problem which needs to be solved urgently in the solid electrolyte battery at present.
Disclosure of Invention
The method aims to solve the problem that in the prior art, a carbonate material can react with metallic lithium under electrochemical induction to form loss, so that the metallic lithium still has a certain deposition phenomenon on the surface when applied to an all-solid system. The invention aims to provide a negative pole piece, a preparation method thereof and application thereof in a solid-state battery. According to the invention, a small amount of vinylene carbonate is added into the ester solvent, so that a better protection effect on a carbonate protective layer can be achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of a negative pole piece, which comprises the following steps: and soaking the negative pole piece in an ester solution to obtain the negative pole piece containing the carbonate organic layer, wherein the ester solution comprises vinylene carbonate, and the negative pole piece comprises metal lithium.
The film forming additive is an unsaturated carbide additive (vinylene carbonate), the vinylene carbonate has a lower reduction potential than that of a carbonate solvent, so that the vinylene carbonate is easier to reduce, a small amount of vinylene carbonate added into the ester solvent can play a better protection role on a carbonate protective layer, and is reduced preferentially to the carbonate protective layer to form a complete SEI film.
Preferably, the negative electrode plate is a metal lithium plate or a metal lithium plate coated with a graphite layer, preferably a metal lithium plate coated with a graphite layer.
VC (vinylene carbonate) can reduce the activity of high active points on the graphite surface to form a surface film with a polymer structure.
Preferably, in the metal lithium sheet coated with the graphite layer, the thickness of the graphite layer is 5 to 100 μm, such as 10 μm, 20 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or 95 μm.
Preferably, in the metal lithium sheet coated with the graphite layer, the surface roughness of the graphite layer is 3-15 μm, such as 3 μm, 4 μm, 5 μm, 8 μm, 10 μm, 12 μm or 14 μm.
The appropriate roughness helps to improve the adhesion between the film layers, and on the other hand, if the roughness is too large, the thickness of the graphite layer has to be increased, so that the performance of the electrode plate is reduced.
The applicant proves that the integrity of the protective layer is favorable after the graphite layer is added, the interaction between VC and graphite ensures that a film layer formed between the protective layer and an electrode layer is more complete, and meanwhile, the adhesion between the protective layer and the graphite layer can be further improved by effectively processing the surface roughness of the graphite layer.
Preferably, in the lithium metal sheet coated with the graphite layer, the particle size of graphite is less than 400 meshes.
Preferably, the concentration of the solute in the ester solution is 0.5-10 mol/L, such as 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, 6mol/L, 7mol/L, 8mol/L or 9 mol/L.
Preferably, the concentration of the vinylene carbonate in the ester solution is 0.1-2 mol/L, such as 0.2mol/L, 0.5mol/L, 0.6mol/L, 0.8mol/L, 1mol/L, 1.2mol/L, 1.5mol/L, 1.6mol/L or 1.8 mol/L.
According to the invention, the structural integrity of the protective layer can be influenced by the excessive concentration of the vinylene carbonate in the selected ester solution; if the concentration is too low, the protective layer cannot be effectively protected.
Preferably, the solute in the ester solution comprises LiNO3、KNO3、NaNO3、LiPF2、LiPF6、LiClO4、KClO4、KPF6、LiBF4、LiClO4、LiBOB、LiDFOB、LiAsF6、LiSbF6、LiCF3SO3、LiN(SO2CF3)2、LiN(SO2C2F5)2、LiN(SO2CF3)2、LiN(SO2CF3)3、LiB(CF3)4Or LiBF3(C2F5) Any one or a combination of at least two of them, preferably LiNO3、LiPF6、LiBOB、LiCF3SO3、LiN(SO2CF3)2And LiBF3(C2F5) Any one or a combination of at least two of them.
Preferably, the solvent in the ester solution comprises any one or a combination of at least two of ethylene carbonate, propylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate.
Preferably, the negative electrode piece is immersed in the ester solution for 1 to 48 hours, such as 5 hours, 8 hours, 10 hours, 12 hours, 15 hours, 18 hours, 20 hours, 25 hours, 28 hours, 30 hours, 32 hours, 35 hours, 38 hours, 40 hours or 45 hours.
The soaking time is 1-48 h, the longer the soaking time is, the thicker the inorganic layer and the carbonate organic layer on the surface of the negative electrode are, and the preferable soaking time is 1-48 h for obtaining excellent electrochemical performance.
Preferably, after the negative electrode plate is immersed in the ester solution for soaking, a drying process is further included, and the drying process is preferably performed in a glove box.
Preferably, the drying temperature is 60 to 80 ℃, such as 62 ℃, 64 ℃, 65 ℃, 66 ℃, 68 ℃, 70 ℃, 72 ℃, 74 ℃, 75 ℃, 76 ℃ or 78 ℃.
The second purpose of the invention is to provide a negative pole piece, which is prepared by the method of the first purpose.
The third object of the present invention is to provide a solid-state battery, which comprises the second object of the negative electrode plate.
The present invention does not specifically limit the material composition of the positive electrode material and the electrolyte in the solid-state battery, and those skilled in the art can select the material composition according to actual conditions.
Compared with the prior art, the invention has the following beneficial effects:
aiming at the problem that the carbonate material existing as the protective layer still has loss under electrochemical induction, VC is used as an additive to form a film on the surface of the negative electrode so as to achieve the effect of forming a complete carbonate protective layer on the surface of the negative electrode; meanwhile, according to the characteristics of VC, the protection effect on the protective layer is improved by forming the specific graphite layer in the invention on the surface layer of the negative electrode.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
Ester solution described in this example: the solute is LiNO3And KNO3The mixed material is obtained by mixing according to the mass ratio of 1:1, the concentration of solute in the ester solution is 5mol/L, the solvent is dimethyl carbonate, and the concentration of vinylene carbonate is 1 mol/L;
(1) preparing a negative pole piece: soaking the lithium sheet in an ester solution for 24 hours, and drying at 70 ℃ in a glove box to obtain a negative electrode sheet containing a carbonate organic layer;
(2) preparing a positive pole piece: a positive electrode active material (lithium iron phosphate): conductive carbon black: mixing the PVDF binder at a mass ratio of 90:5:5, taking NMP as a solvent for slurry mixing, coating the mixture on an aluminum foil, and performing vacuum drying at 90 ℃ to obtain a positive pole piece;
(3) preparing an all-solid-state electrolyte battery: and assembling the positive pole piece, the negative pole piece and the solid electrolyte (lithium lanthanum zirconium oxygen) into a battery.
Example 2
The difference from example 1 is that a graphite layer having a surface roughness of 3 μm, a thickness of 20 μm and a graphite particle size of 500 mesh was formed on the surface of the lithium sheet.
Example 3
The difference from example 1 is that a graphite layer having a surface roughness of 20 μm, a thickness of 40 μm and a graphite particle size of 500 mesh was formed on the surface of the lithium sheet.
Example 4
The difference from example 1 is that a graphite layer having a surface roughness of 15 μm, a thickness of 20 μm and a graphite particle size of 500 mesh was formed on the surface of the lithium sheet.
Example 5
The difference from example 1 is that a graphite layer having a surface roughness of 25 μm, a thickness of 100 μm and a graphite particle size of 500 mesh was formed on the surface of the lithium sheet.
Comparative example 1
The difference from example 1 is that vinylene carbonate is not added.
Comparative example 2
The difference from example 1 is that vinylene carbonate is replaced by an equal amount of propylene sulfite.
And (3) performance testing:
the batteries obtained in the embodiments and the comparative examples are subjected to charge and discharge tests at 25 +/-2 ℃, the charge and discharge voltage is 2.75-4.25V, the current density is 0.1C, the first efficiency, the 10-circle capacity retention ratio, the 20-circle capacity retention ratio and the 30-circle capacity retention ratio are respectively tested, and the test results are shown in table 1:
TABLE 1
As can be seen from example 1, comparative example 1 and comparative example 2, not all film-forming additives are applicable to the solid-state battery system according to the present invention, and propylene sulfite and vinylene carbonate are conventional film-forming additives in the art, but the overall performance of the battery is not improved by propylene sulfite, but rather the battery performance is greatly degraded.
It can be confirmed that the addition of the graphite layer is advantageous for improving the overall performance of the battery, as compared with examples 1 and 2, and it is understood that the adjustment of the roughness of the graphite layer is advantageous for the performance of the battery, and the optimum technical effect can be achieved within the range selected by the present invention, as compared with examples 1 to 5.
The present invention is illustrated in detail by the examples described above, but the present invention is not limited to the details described above, i.e., it is not intended that the present invention be implemented by relying on the details described above. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a negative pole piece is characterized by comprising the following steps: and soaking the negative pole piece in an ester solution to obtain the negative pole piece containing the carbonate organic layer, wherein the ester solution comprises vinylene carbonate, and the negative pole piece comprises metal lithium.
2. The method according to claim 1, wherein the negative electrode sheet is a metallic lithium sheet or a metallic lithium sheet coated with a graphite layer, preferably a metallic lithium sheet coated with a graphite layer.
3. The method according to claim 1 or 2, wherein in the lithium metal sheet coated with a graphite layer, the thickness of the graphite layer is 5 to 100 μm;
preferably, in the metal lithium sheet coated with the graphite layer, the surface roughness of the graphite layer is 3-15 μm.
4. The method of any of claims 1-3, wherein the lithium metal sheet coated with graphite layers has a graphite particle size of less than 400 mesh.
5. The method according to any one of claims 1 to 4, wherein the concentration of the solute in the ester solution is 0.5 to 10 mol/L;
preferably, the concentration of the vinylene carbonate in the ester solution is 0.1-2 mol/L.
6. The method of any one of claims 1-5, wherein the solute in the ester solution comprises LiNO3、KNO3、NaNO3、LiPF2、LiPF6、LiClO4、KClO4、KPF6、LiBF4、LiClO4、LiBOB、LiDFOB、LiAsF6、LiSbF6、LiCF3SO3、LiN(SO2CF3)2、LiN(SO2C2F5)2、LiN(SO2CF3)2、LiN(SO2CF3)3、LiB(CF3)4Or LiBF3(C2F5) Any one or a combination of at least two of them, preferably LiNO3、LiPF6、LiBOB、LiCF3SO3、LiN(SO2CF3)2And LiBF3(C2F5) Any one or a combination of at least two of;
preferably, the solvent in the ester solution comprises any one or a combination of at least two of ethylene carbonate, propylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate.
7. The method according to any one of claims 1 to 6, wherein the negative electrode plate is immersed in the ester solution for 1 to 48 hours.
8. The method according to any one of claims 1 to 7, wherein after the negative electrode plate is immersed in the ester solution, a drying process is further included, preferably drying in a glove box;
preferably, the drying temperature is 60-80 ℃.
9. A negative electrode plate, characterized in that the negative electrode plate is prepared by the method of any one of claims 1 to 8.
10. A solid-state battery comprising the negative electrode tab of claim 9.
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| CN202010129564.0A CN111293316B (en) | 2020-02-28 | 2020-02-28 | Negative pole piece, preparation method thereof and application thereof in solid-state battery |
| CN202210261361.6A CN114583110B (en) | 2020-02-28 | 2020-02-28 | Negative electrode plate, preparation method thereof and application thereof in solid-state battery |
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| DE102022128066A1 (en) | 2022-10-24 | 2024-04-25 | Volkswagen Aktiengesellschaft | Electrode for a battery with temporary protective layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108468042A (en) * | 2018-03-23 | 2018-08-31 | 山东大学 | A kind of method that fluorinated ethylene carbonate handles lithium metal and its application in solid state battery |
| CN109273704A (en) * | 2017-07-18 | 2019-01-25 | 中国科学院上海硅酸盐研究所 | A kind of lithium anode and preparation method thereof with high-ratio surface protective layer |
| CN112042014A (en) * | 2018-09-27 | 2020-12-04 | 株式会社Lg化学 | Negative electrode for all-solid-state battery and method for producing same |
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| CN110970598A (en) * | 2019-12-23 | 2020-04-07 | 中航锂电技术研究院有限公司 | Composite negative electrode of lithium battery, preparation method thereof and lithium battery comprising negative electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109273704A (en) * | 2017-07-18 | 2019-01-25 | 中国科学院上海硅酸盐研究所 | A kind of lithium anode and preparation method thereof with high-ratio surface protective layer |
| CN108468042A (en) * | 2018-03-23 | 2018-08-31 | 山东大学 | A kind of method that fluorinated ethylene carbonate handles lithium metal and its application in solid state battery |
| CN112042014A (en) * | 2018-09-27 | 2020-12-04 | 株式会社Lg化学 | Negative electrode for all-solid-state battery and method for producing same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102022128066A1 (en) | 2022-10-24 | 2024-04-25 | Volkswagen Aktiengesellschaft | Electrode for a battery with temporary protective layer |
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| CN114583110B (en) | 2023-07-25 |
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