CN114188612A - All-solid-state battery and preparation method thereof - Google Patents
All-solid-state battery and preparation method thereof Download PDFInfo
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- CN114188612A CN114188612A CN202111462719.3A CN202111462719A CN114188612A CN 114188612 A CN114188612 A CN 114188612A CN 202111462719 A CN202111462719 A CN 202111462719A CN 114188612 A CN114188612 A CN 114188612A
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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
- H01M10/058—Construction or 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
- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses an all-solid-state battery and a preparation method thereof. The preparation method comprises the steps of firstly obtaining an inorganic solid electrolyte sheet by using a tabletting method, then assembling the inorganic solid electrolyte sheet and two electrodes into a sandwich structure by cold pressing and laminating, and soaking the assembled battery into an interface layer precursor solution to form a thin interface layer in situ. The method for preparing the interface layer in situ can ensure that the whole battery system is not separated, so that the electrolyte is fully fused with the surface of the pole piece, the interface compatibility of the pole piece and the electrolyte is improved, a continuous ion conduction channel is formed, the direct contact between a lithium cathode and the solid electrolyte is avoided, the electrochemical performance of the solid battery is improved, and the long-time circulation of the battery is ensured.
Description
Technical Field
The invention belongs to the technical field of new energy of all-solid-state batteries, and particularly relates to an all-solid-state battery and a preparation method thereof.
Background
With the development of new technologies, lithium ion batteries have been widely used in the fields of communication, power and digital products, secondary batteries with high safety and high energy density are the future development direction, and the conventional lithium ion batteries have certain safety problems due to the existence of liquid electrolyte. The Solid Electrolyte (SE) has the advantages of thermal stability, nonflammability, no leakage, no volatilization and the like, the solid battery greatly reduces the content of a solvent, has higher thermal runaway initial temperature, and greatly improves the stability and safety of the battery in the using process.
The solid electrolyte is a main material for research of domestic various institutes and enterprises, and mainly comprises an inorganic solid electrolyte and a polymer electrolyte. The polymer solid electrolyte has good flexibility, easy processing and other excellent performances, but has the defects of low conductivity, high operation temperature, low electrochemical window and the like, so that the application of the polymer electrolyte in a solid lithium battery is limited. The solid-state battery adopts the solid-state electrolyte, so that the problems of large interface resistance and poor interface compatibility exist, and in the circulating process of the solid-state battery, the solid-state electrolyte possibly generates an oxidation-reduction reaction with a lithium cathode, and a high-impedance interface phase is generated and accumulated between the cathode and the solid-state electrolyte to influence the lithium ion transmission. These problems seriously affect the rate performance of the solid-state battery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides an all-solid-state battery and a preparation method thereof, and solves the problems in the background art.
One of the technical schemes adopted by the invention for solving the technical problems is as follows: provided is a method for manufacturing an all-solid battery, including the steps of:
1) preparing an interface layer precursor solution:
uniformly mixing the lithium salt, the interface layer precursor and the solvent to obtain an interface layer precursor solution; the precursor of the interface layer is polyethylene carbonate, polypropylene carbonate or polybutylene carbonate;
2) preparing a sandwich structure:
tabletting to obtain inorganic solid electrolyte with thickness of 50 μm-3mm, and cold pressing and laminating with positive and negative electrodes to form sandwich structure;
3) assembling:
soaking the sandwich structure prepared in the step 2) in the interface layer precursor solution prepared in the step 1) for 0.1-2 h, drying the solvent in situ, and forming continuous interface layers among the layers of the sandwich structure to prepare the all-solid-state battery.
In a preferred embodiment of the present invention, the solvent is acetonitrile, N-dimethylformamide or tetrahydrofuran.
In a preferred embodiment of the present invention, the lithium salt is LiClO4LiTFSI, LiBOB, LiFSI or lidpob.
In a preferred embodiment of the present invention, the interfacial layer precursor content is 20-95 wt%.
In a preferred embodiment of the present invention, the concentration of the lithium salt in the interface layer precursor solution is 5-95 mol%.
In a preferred embodiment of the present invention, the inorganic solid electrolyte is at least one of an LGPS type inorganic solid electrolyte, a garnet type inorganic solid electrolyte, a perovskite type inorganic solid electrolyte, a LISICON type inorganic solid electrolyte, a digermorite type inorganic solid electrolyte, or an anti-perovskite type inorganic solid electrolyte.
In a preferred embodiment of the present invention, the inorganic solid electrolyte is Li10GeP2S12。
The second technical scheme adopted by the invention for solving the technical problems is as follows: the all-solid-state battery prepared by the method comprises a sandwich structure consisting of a positive electrode, an inorganic solid electrolyte and a negative electrode, wherein an interface layer is arranged on an interlayer interface of the sandwich structure.
In a preferred embodiment of the present invention, the interface layer is a gel polymer having viscosity; the thickness of the interface layer is 0.1-200 μm.
In a preferred embodiment of the present invention, the interface layer further covers the periphery of the battery with the sandwich structure.
Compared with the background technology, the technical scheme has the following advantages:
1. the assembled solid-state battery is soaked in the interface layer precursor to form the polymer interface layer in situ, so that the battery system is ensured not to be separated integrally, the direct contact between the lithium negative electrode and the solid-state electrolyte is avoided, the electrolyte is fully fused with the surface of the pole piece, the interface compatibility between the pole piece and the solid-state electrolyte is improved, a continuous ion conduction channel is formed, the direct contact between the lithium negative electrode and the solid-state electrolyte is avoided, the electrochemical performance of the solid-state battery is improved, and the cycle life and the electrochemical performance of the solid-state battery are improved;
2. the interface layer is a polymer formed in situ, is in a gel state, has good viscosity, can improve the contact between the solid electrolyte and the electrode, and effectively reduces the impedance.
Drawings
FIG. 1 is a schematic structural view of a lithium symmetric battery according to example 1; in the figure: 1-metallic lithium cathode, 2-interface layer, 3-inorganic solid electrolyte sheet, and 4-lithium metal anode.
FIG. 2 shows the concentration of 0.2mA/cm in an all-solid-state lithium symmetric cell containing an interface layer prepared in example 12Charge and discharge curves at current density.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following will describe the contents of the present invention in more detail by way of examples, but the scope of the present invention is not limited to these examples.
Example 1
(1) Preparing an interface layer precursor solution: in a glove box filled with argon, 1g of polyethylene carbonate (PEC) and lithium salt LiTFSI (mole fraction 60 mol%) were dissolved in 4mL of acetonitrile, and stirred to dissolve, obtaining a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
The all-solid-state lithium symmetric battery prepared in the embodiment comprises a sandwich structure consisting of a positive electrode 4, an inorganic solid electrolyte 3 and a negative electrode 1, wherein an interface layer 2 is arranged on an interlayer interface of the sandwich structure, and the interface layer 2 is a continuous gel-like polyethylene carbonate polymer. And the interface layer 2 is also wrapped at the periphery of the sandwich structure in a soaking mode and is connected with the interface layers 2 arranged among the layers, so that the lithium metal has good electrochemical stability and good capability of inhibiting the growth of lithium dendrites.
Example 2
(1) Preparing an interface layer precursor solution: in a glove box filled with argon, 1g of polyethylene carbonate (PEC) and lithium salt LiTFSI (mole fraction 80 mol%) were dissolved in 4mL of acetonitrile, and stirred to dissolve, obtaining a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
Example 3
(1) Preparing an interface layer precursor solution: in a glove box filled with argon, 1g of polyethylene carbonate (PEC) and lithium salt LiTFSI (mole fraction 100 mol%) were dissolved in 4mL of acetonitrile, and stirred to dissolve, obtaining a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
Example 4
(1) Preparing an interface layer precursor solution: in a glove box filled with argon, 1g of polypropylene carbonate (PPC) and lithium salt LiTFSI (mole fraction 60 mol%) are dissolved in 4mL of acetonitrile, and are stirred and dissolved to obtain a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
Example 5
(1) Preparing an interface layer precursor solution: dissolving 1g of polyethylene carbonate (PPC) and lithium salt LiTFSI (mole fraction 80 mol%) in 4mL of acetonitrile in a glove box filled with argon, and stirring to dissolve the mixture to obtain a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
Example 6
(1) Preparing an interface layer precursor solution: dissolving 1g of polyethylene carbonate (PPC) and lithium salt LiTFSI (mole fraction 100 mol%) in 4mL of acetonitrile in a glove box filled with argon, and stirring to dissolve the mixture to obtain a clear interface layer precursor solution;
(2) assembling the cell, 150mg Li10GeP2S12And (3) taking a sheet-shaped ceramic sheet as an electrolyte sheet, soaking the assembled electrolyte sheet and two electrodes into the interface layer precursor solution, and drying the solvent in a glove box at 85 ℃ to form an interface layer in situ.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of an all-solid-state battery is characterized by comprising the following steps: the method comprises the following steps:
1) preparing an interface layer precursor solution:
uniformly mixing the lithium salt, the interface layer precursor and the solvent to obtain an interface layer precursor solution; the precursor of the interface layer is polyethylene carbonate, polypropylene carbonate or polybutylene carbonate;
2) preparing a sandwich structure:
tabletting to obtain inorganic solid electrolyte with thickness of 50 μm-3mm, and cold pressing and laminating with positive and negative electrodes to form sandwich structure;
3) assembling:
soaking the sandwich structure prepared in the step 2) in the interface layer precursor solution prepared in the step 1) for 0.1-2 h, drying the solvent in situ, and forming continuous interface layers among the layers of the sandwich structure to prepare the all-solid-state battery.
2. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the solvent is acetonitrile, N-dimethylformamide or tetrahydrofuran.
3. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the lithium salt is LiClO4LiTFSI, LiBOB, LiFSI or lidpob.
4. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the content of the precursor of the interface layer is 20-95 wt%.
5. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the concentration of lithium salt in the interface layer precursor solution is 5-95 mol%.
6. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the inorganic solid electrolyte is at least one of LGPS type inorganic solid electrolyte, garnet type inorganic solid electrolyte, perovskite type inorganic solid electrolyte, LISICON type inorganic solid electrolyte, Geranite type inorganic solid electrolyte or anti-perovskite type inorganic solid electrolyte.
7. The method for manufacturing an all-solid battery according to claim 1, characterized in that: the inorganic solid electrolyte is Li10GeP2S12。
8. An all-solid battery prepared according to any one of claims 1 to 7, characterized in that: the electrolyte comprises a sandwich structure consisting of an anode, an inorganic solid electrolyte and a cathode, wherein an interface layer is arranged on an interlayer interface of the sandwich structure.
9. An all-solid battery according to claim 8, characterized in that: the interface layer is gel polymer with viscosity; the thickness of the interface layer is 0.1-200 μm.
10. An all-solid battery according to claim 8, characterized in that: the interface layer is also coated on the periphery of the battery with the sandwich structure.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115050964A (en) * | 2022-06-29 | 2022-09-13 | 北京航空航天大学 | Preparation method of solid electrolyte binder, binder and battery |
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| CN114188612B (en) | 2023-04-07 |
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