CN109286038B - Novel solid electrolyte and preparation method thereof - Google Patents
Novel solid electrolyte and preparation method thereof Download PDFInfo
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- CN109286038B CN109286038B CN201811135417.3A CN201811135417A CN109286038B CN 109286038 B CN109286038 B CN 109286038B CN 201811135417 A CN201811135417 A CN 201811135417A CN 109286038 B CN109286038 B CN 109286038B
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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
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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
- H01M10/058—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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
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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
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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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
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Abstract
The invention discloses a novel solid electrolyte, which comprises the following components: polyimide, lithium salt, ceramic powder, polyurethane and solvent; a preparation method of a novel solid electrolyte comprises the following preparation steps: adding polyimide into a solvent, and mechanically stirring uniformly; then adding lithium salt and uniformly stirring; step three: adding ceramic powder, stirring uniformly, adding polyurethane, and mechanically stirring uniformly; step four: after the glue solution is mechanically stirred uniformly, the glue solution is coated on two sides of the surface of the diaphragm by adopting curtain coating, and the novel solid electrolyte membrane can be obtained. Compared with the prior art, the invention achieves the technical effects that: the electrolyte membrane prepared by the method has greatly improved mechanical property and ionic conductivity.
Description
Technical Field
The invention relates to the technical field of flexible solid lithium ions, in particular to a novel solid electrolyte and a preparation method of the novel solid electrolyte.
Background
The lithium ion battery is widely applied to the fields of portable electronic equipment, transportation and the like, but the traditional lithium ion battery has huge potential safety hazard due to the use of organic liquid electrolyte. In recent years, solid-state batteries based on solid electrolytes have attracted much attention because of their advantages such as high energy density, longer cycle life, and better safety. The solid lithium ion battery mainly comprises three parts, namely a positive electrode material, a negative electrode material and a solid electrolyte, wherein the solid electrolyte is used as an important component and is researched and explored by vast researchers. Among a plurality of solid electrolytes, Li7La3Zr2O12(LLZO) with garnet structure is a solid electrolyte with good application prospect due to higher room temperature ionic conductivity, better thermal stability and good stability to metallic lithium cathode. However, when it is used in a solid-state battery, there is a large interface resistance at the interface between the electrode and the electrolyte, and the machinability of the ceramic material is poor.
Disclosure of Invention
The purpose of the invention is: aiming at the defects, a novel solid electrolyte and a preparation method thereof are provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a novel solid electrolyte is composed of the following components: the composite material comprises polyimide, lithium salt, ceramic powder, polyurethane and a solvent, wherein the mass parts of the components are as follows: 10-30 parts of polyimide, 10-30 parts of lithium salt, 5-10 parts of ceramic powder, 0.2-2 parts of polyurethane and 30-50 parts of solvent.
The lithium salt includes LiTFSI, LiClO4，LiBF4，LiPF6，LiAsF6。
The ceramic powder is one or two of lithium lanthanum titanium oxide powder, lithium lanthanum zirconium oxide powder and lithium lanthanum zirconium tantalum oxide.
The solvent is one of N-methyl pyrrolidone or deionized water.
A preparation method of a novel solid electrolyte comprises the following preparation steps:
the method comprises the following steps: taking 30-50 parts by mass of solvent, adding 10-30 parts by mass of polyimide into the solvent, and mechanically stirring the mixture uniformly;
step two: then adding 10-30 parts by mass of lithium salt and uniformly stirring;
step three: adding 5-10 parts by mass of ceramic powder, uniformly stirring, adding 0.2-2 parts by mass of polyurethane, and mechanically uniformly stirring;
step four: and after the glue solution is mechanically stirred uniformly, coating the glue solution on two sides of the surface of the diaphragm by adopting curtain coating, transferring the diaphragm to a vacuum oven at the temperature of 50-90 ℃, and drying for 4-12h to obtain the novel solid electrolyte membrane with the ionic conductivity reaching 8 x 10-4S/m at room temperature.
Compared with the prior art, the invention achieves the technical effects that: the electrolyte membrane prepared by the method has greatly improved mechanical property and ionic conductivity.
Drawings
FIG. 1 is a comparative graph of the results of the internal resistance test of the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples:
the first embodiment is as follows:
the invention relates to a novel solid electrolyte, which comprises the following components: the composite material comprises polyimide, lithium salt, ceramic powder, polyurethane and a solvent, wherein the mass parts of the components are as follows: 10 parts of polyimide, 10 parts of lithium salt, 5 parts of ceramic powder, 0.2 part of polyurethane and 30 parts of solvent.
The lithium salt is preferably LiClO4。
The ceramic powder is preferably lithium lanthanum zirconium tantalum oxygen.
The solvent is N-methyl pyrrolidone.
A preparation method of a novel solid electrolyte comprises the following preparation steps:
the method comprises the following steps: taking 30 parts by mass of N-methylpyrrolidone, adding 10 parts by mass of polyimide into the N-methylpyrrolidone, and mechanically stirring the mixture uniformly;
step two: then, 10 parts by mass of LiClO was added4Stirring uniformly;
step three: adding 5 parts by mass of lithium lanthanum zirconium tantalum oxygen, uniformly stirring, adding 0.2 part by mass of polyurethane, and mechanically uniformly stirring;
step four: and after the glue solution is mechanically stirred uniformly, coating the glue solution on two sides of the surface of the diaphragm by adopting a tape casting method, transferring the diaphragm to a vacuum oven at 70 ℃, and drying for 12 hours to obtain the novel solid electrolyte membrane with the ionic conductivity reaching 8 x 10-4S/m at room temperature.
Compared with the prior art, the invention achieves the technical effects that: the electrolyte membrane prepared by the method has greatly improved mechanical property and ionic conductivity.
Example two:
the invention relates to a novel solid electrolyte, which comprises the following components: the composite material comprises polyimide, lithium salt, ceramic powder, polyurethane and a solvent, wherein the mass parts of the components are as follows: 15 parts of polyimide, 15 parts of lithium salt, 10 parts of ceramic powder, 0.5 part of polyurethane and 40 parts of solvent.
The lithium salt is preferably LiBF4。
The ceramic powder is preferably lithium lanthanum zirconium oxygen powder.
The solvent is N-methyl pyrrolidone.
A preparation method of a novel solid electrolyte comprises the following preparation steps:
the method comprises the following steps: taking 40 parts by mass of N-methylpyrrolidone, adding 15 parts by mass of polyimide, and mechanically stirring uniformly;
step two: then 15 parts by mass of LiBF was added4Stirring uniformly;
step three: adding 10 parts by mass of lithium lanthanum zirconium oxygen powder, uniformly stirring, adding 0.5 part by mass of polyurethane, and mechanically uniformly stirring;
step four: and after the glue solution is mechanically stirred uniformly, coating the glue solution on two sides of the surface of the diaphragm by adopting curtain coating, transferring the diaphragm to a vacuum oven at 80 ℃, and drying for 8 hours to obtain the novel solid electrolyte membrane with the ionic conductivity reaching 8 x 10-4S/m at room temperature.
Compared with the prior art, the invention achieves the technical effects that: the electrolyte membrane prepared by the method has greatly improved mechanical property and ionic conductivity.
Example three:
the invention relates to a novel solid electrolyte, which comprises the following components: the composite material comprises polyimide, lithium salt, ceramic powder, polyurethane and a solvent, wherein the mass parts of the components are as follows: 20 parts of polyimide, 30 parts of lithium salt, 10 parts of ceramic powder, 1.5 parts of polyurethane and 50 parts of solvent.
The lithium salt is preferably LiAsF6。
The ceramic powder is preferably lithium lanthanum titanium oxide powder.
The solvent is deionized water.
A preparation method of a novel solid electrolyte comprises the following preparation steps:
the method comprises the following steps: taking 50 parts by mass of deionized water, adding 20 parts by mass of polyimide, and mechanically stirring uniformly;
step two: then, 30 parts by mass of LiAsF was added6Stirring uniformly;
step three: adding 10 parts by mass of lithium lanthanum titanium oxide powder, uniformly stirring, adding 1.5 parts by mass of polyurethane, and mechanically uniformly stirring;
step four: and after the glue solution is mechanically stirred uniformly, coating the glue solution on two sides of the surface of the diaphragm by adopting curtain coating, transferring the diaphragm to a vacuum oven at 90 ℃, and drying for 7 hours to obtain the novel solid electrolyte membrane with the ionic conductivity reaching 8 x 10-4S/m at room temperature.
Compared with the prior art, the invention achieves the technical effects that: the electrolyte membrane prepared by the method has greatly improved mechanical property and ionic conductivity.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (2)
1. Use of a solid electrolyte in a lithium ion battery, characterized in that: the solid electrolyte is composed of the following components: the composite material comprises polyimide, lithium salt, ceramic powder, polyurethane and a solvent, wherein the mass parts of the components are as follows: 10-30 parts of polyimide, 10-30 parts of lithium salt, 5-10 parts of ceramic powder, 0.2-2 parts of polyurethane and 30-50 parts of solvent;
the solid electrolyte is prepared by the following preparation method:
the method comprises the following steps: taking 30-50 parts by mass of solvent, adding 10-30 parts by mass of polyimide into the solvent, and mechanically stirring the mixture uniformly;
step two: then adding 10-30 parts by mass of lithium salt and uniformly stirring;
step three: adding 5-10 parts by mass of ceramic powder, uniformly stirring, adding 0.2-2 parts by mass of polyurethane, and mechanically uniformly stirring;
step four: after the glue solution is mechanically stirred uniformly, the glue solution is coated on two sides of the surface of the diaphragm by curtain coating, then the diaphragm is transferred to a vacuum oven with the temperature of 50-90 ℃ and dried for 4-12h, and the glue solution can be obtained at room temperatureThe ionic conductivity can reach (8-10) × 10-4An S/m solid electrolyte membrane;
the lithium salt includes LiTFSI, LiClO4，LiBF4，LiPF6，LiAsF6；
The ceramic powder is one or two of lithium lanthanum titanium oxide powder, lithium lanthanum zirconium oxide powder and lithium lanthanum zirconium tantalum oxide.
2. Use according to claim 1, characterized in that: the solvent is one of N-methyl pyrrolidone or deionized water.
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| CN111769320B (en) * | 2019-04-02 | 2021-08-13 | 深圳格林德能源集团有限公司 | Solid polymer electrolyte membrane and preparation method thereof |
| CN111354976A (en) * | 2020-03-16 | 2020-06-30 | 河南电池研究院有限公司 | A kind of preparation method of composite solid-state electrolyte and its application in solid-state lithium ion battery |
| CN112117488B (en) * | 2020-07-31 | 2021-11-02 | 华中科技大学 | Solid electrolyte, lithium metal negative electrode and preparation method thereof |
Citations (4)
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| CN103515649A (en) * | 2012-06-14 | 2014-01-15 | 东丽先端材料研究开发（中国）有限公司 | Organic/inorganic composite electrolyte and preparation method thereof |
| CN107346833A (en) * | 2017-08-30 | 2017-11-14 | 清陶（昆山）能源发展有限公司 | A kind of composite solid polymer electrolyte film and preparation method thereof |
| CN107681089A (en) * | 2016-08-02 | 2018-02-09 | 三星电子株式会社 | Composite membrane, the method for preparing the composite membrane and lithium-air battery and battery component including the composite membrane |
| CN108448169A (en) * | 2018-03-15 | 2018-08-24 | 清陶（昆山）能源发展有限公司 | A kind of inorganic-organic hybrid solid electrolyte membrane and its processing technology |
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| KR102452944B1 (en) * | 2015-05-12 | 2022-10-11 | 삼성전자주식회사 | Electrolyte composite, and negative electrode and lithium second battery including the electrolyte composite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103515649A (en) * | 2012-06-14 | 2014-01-15 | 东丽先端材料研究开发（中国）有限公司 | Organic/inorganic composite electrolyte and preparation method thereof |
| CN107681089A (en) * | 2016-08-02 | 2018-02-09 | 三星电子株式会社 | Composite membrane, the method for preparing the composite membrane and lithium-air battery and battery component including the composite membrane |
| CN107346833A (en) * | 2017-08-30 | 2017-11-14 | 清陶（昆山）能源发展有限公司 | A kind of composite solid polymer electrolyte film and preparation method thereof |
| CN108448169A (en) * | 2018-03-15 | 2018-08-24 | 清陶（昆山）能源发展有限公司 | A kind of inorganic-organic hybrid solid electrolyte membrane and its processing technology |
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