CN109286038A - A kind of New Solid electrolyte and preparation method thereof - Google Patents

A kind of New Solid electrolyte and preparation method thereof Download PDF

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Publication number
CN109286038A
CN109286038A CN201811135417.3A CN201811135417A CN109286038A CN 109286038 A CN109286038 A CN 109286038A CN 201811135417 A CN201811135417 A CN 201811135417A CN 109286038 A CN109286038 A CN 109286038A
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Prior art keywords
new solid
solid electrolyte
mass parts
parts
solvent
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CN201811135417.3A
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CN109286038B (en
Inventor
李峥
冯玉川
何泓材
李培养
杨帆
南策文
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Suzhou Qingtao New Energy S&T Co Ltd
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Suzhou Qingtao New Energy S&T Co Ltd
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 a kind of New Solid electrolyte, are made of following component: polyimides, lithium salts, ceramic powder, polyurethane and solvent；A kind of New Solid electrolyte preparation method, including following preparation step: taking solvent, wherein addition polymerization acid imide, and mechanical stirring is uniform；Then lithium salts is added to stir evenly；Step 3: adding ceramic powder after mixing evenly, adds polyurethane, and mechanical stirring is uniform；Step 4: it after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, can be obtained in New Solid dielectric film.Compared with prior art, the present invention is achieved has the technical effect that dielectric film mechanical performance and ionic conductivity prepared by the present invention have a distinct increment.

Description

A kind of New Solid electrolyte and preparation method thereof
Technical field
The present invention relates to flexible solid lithium-ion technology fields, more particularly to a kind of New Solid electrolyte, further relate to A kind of New Solid electrolyte preparation method.
Background technique
Lithium ion battery is in portable electronic device, and the fields such as communications and transportation have a wide range of applications, but traditional lithium Ion battery is due to using organic liquid electrolyte, and there is huge security risks.In recent years, based on solid electrolyte The advantages that energy density of solid state battery Yin Qigao, longer cycle life, preferable safety, causes the extensive pass of people Note.Solid lithium ion battery is mainly made of positive electrode, negative electrode material and solid electrolyte three parts, wherein solid state electrolysis Matter is as significant components always by numerous research workers' research and probe.In numerous solid electrolytes, garnet structure Li7La3Zr2O12 (LLZO) is because of its higher room-temperature ion conductance, preferable thermal stability and good to lithium anode Stability, be a kind of very promising solid electrolyte.But it is when being used for solid state battery, in electrode and electrolyte There are biggish interface resistances at interface, and the machining property of ceramic material is very poor.
Summary of the invention
The purpose of the present invention is: in view of the above deficiencies, provide a kind of New Solid electrolyte and preparation method thereof.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
A kind of New Solid electrolyte, is made of following component: polyimides, lithium salts, ceramic powder, polyurethane and Solvent, wherein the mass parts ratio of each component are as follows: 10-30 parts of polyimides, 10-30 parts of lithium salts, 5-10 parts of ceramic powder, poly- ammonia 0.2-2 parts of ester, 30-50 parts of solvent.
The lithium salts includes LiTFSI, LiClO4, LiBF4, LiPF6, LiAsF6。
The ceramic powder is Li-La-Ti oxygen powder, lithium lanthanum zirconium oxygen powder, it is a kind of in lithium lanthanum zirconium tantalum oxygen or two kinds.
The solvent is one of N-Methyl pyrrolidone or deionized water.
A kind of New Solid electrolyte preparation method, including following preparation step:
Step 1: taking the solvent of 30-50 mass parts, in the polyimides that 10-30 mass parts are wherein added, mechanical stirring Uniformly；
Step 2: and then the lithium salts of addition 10-30 mass parts stirs evenly；
Step 3: the ceramic powder for adding 5-10 mass parts after mixing evenly, adds the polyurethane of 0.2-2 mass parts, Mechanical stirring is uniform；
Step 4: it after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, is then transferred to 50-90 DEG C of vacuum drying oven, dry 4-12h, ionic conductivity at room temperature can be obtained, and to can reach (8-10) * 10-4S/m new Type solid electrolyte membrane.
Compared with prior art, the present invention is achieved has the technical effect that dielectric film mechanical performance prepared by the present invention And ionic conductivity has a distinct increment.
Detailed description of the invention
Fig. 1 is inner walkway comparative result figure of the invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments:
Embodiment one:
A kind of New Solid electrolyte of the invention, is made of following component: polyimides, ceramic powder, gathers lithium salts Urethane and solvent, wherein the mass parts ratio of each component are as follows: 10 parts of polyimides, 10 parts of lithium salts, 5 parts of ceramic powder, polyurethane 0.2 part, 30 parts of solvent.
The lithium salts is preferably LiClO4。
The ceramic powder is preferably lithium lanthanum zirconium tantalum oxygen.
The solvent is N-Methyl pyrrolidone.
A kind of New Solid electrolyte preparation method, including following preparation step:
Step 1: taking the N-Methyl pyrrolidone of 30 mass parts, mechanical in the polyimides that 10 mass parts are wherein added It stirs evenly；
Step 2: and then the LiClO of 10 mass parts is added4It stirs evenly；
Step 3: the lithium lanthanum zirconium tantalum oxygen for adding 5 mass parts after mixing evenly, adds the polyurethane of 0.2 mass parts, machine Tool stirs evenly；
Step 4: it after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, is then transferred to 70 DEG C of vacuum drying oven, dry 12h, ionic conductivity at room temperature, which can be obtained, can reach 8.5*10- 4S/m New Solid electricity Solve plasma membrane.
Compared with prior art, the present invention is achieved has the technical effect that dielectric film mechanical performance prepared by the present invention And ionic conductivity has a distinct increment.
Embodiment two:
A kind of New Solid electrolyte of the invention, is made of following component: polyimides, ceramic powder, gathers lithium salts Urethane and solvent, wherein the mass parts ratio of each component are as follows: 15 parts of polyimides, 15 parts of lithium salts, 10 parts of ceramic powder, poly- ammonia 0.5 part of ester, 40 parts of solvent.
The lithium salts is preferably LiBF4。
The ceramic powder is preferably lithium lanthanum zirconium oxygen powder.
The solvent is N-Methyl pyrrolidone.
A kind of New Solid electrolyte preparation method, including following preparation step:
Step 1: taking the N-Methyl pyrrolidone of 40 mass parts, mechanical in the polyimides that 15 mass parts are wherein added It stirs evenly；
Step 2: and then the LiBF of 15 mass parts is added4It stirs evenly；
Step 3: the lithium lanthanum zirconium oxygen powder for adding 10 mass parts after mixing evenly, adds the polyurethane of 0.5 mass parts, machine Tool stirs evenly；
Step 4: it after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, is then transferred to 80 DEG C of vacuum drying oven, dry 8h, ionic conductivity at room temperature, which can be obtained, can reach the electrolysis of 8*10- 4S/m New Solid Plasma membrane.
Compared with prior art, the present invention is achieved has the technical effect that dielectric film mechanical performance prepared by the present invention And ionic conductivity has a distinct increment.
Embodiment three:
A kind of New Solid electrolyte of the invention, is made of following component: polyimides, ceramic powder, gathers lithium salts Urethane and solvent, wherein the mass parts ratio of each component are as follows: 20 parts of polyimides, 30 parts of lithium salts, 10 parts of ceramic powder, poly- ammonia 1.5 parts of ester, 50 parts of solvent.
The lithium salts is preferably LiAsF6。
The ceramic powder is preferably Li-La-Ti oxygen powder.
The solvent is deionized water.
A kind of New Solid electrolyte preparation method, including following preparation step:
Step 1: taking the deionized water of 50 mass parts, and in the polyimides that 20 mass parts are wherein added, mechanical stirring is equal It is even；
Step 2: and then the LiAsF of 30 mass parts is added6It stirs evenly；
Step 3: the Li-La-Ti oxygen powder for adding 10 mass parts after mixing evenly, adds the polyurethane of 1.5 mass parts, machine Tool stirs evenly；
Step 4: it after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, is then transferred to 90 DEG C of vacuum drying oven, dry 7h, ionic conductivity at room temperature, which can be obtained, can reach the electrolysis of 10*10- 4S/m New Solid Plasma membrane.
Compared with prior art, the present invention is achieved has the technical effect that dielectric film mechanical performance prepared by the present invention And ionic conductivity has a distinct increment.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow be familiar with technique Personage cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to this hair Equivalent change or modification made by bright Spirit Essence, should be covered by the protection scope of the present invention.

Claims (5)

1. a kind of New Solid electrolyte, it is characterised in that: be made of following component: polyimides, ceramic powder, gathers lithium salts Urethane and solvent, wherein the mass parts ratio of each component are as follows: 10-30 parts of polyimides, 10-30 parts of lithium salts, ceramic powder 5-10 Part, 0.2-2 parts of polyurethane, 30-50 parts of solvent.
2. a kind of New Solid electrolyte according to claim 1, it is characterised in that: the lithium salts includes LiTFSI, LiClO4, LiBF4, LiPF6, LiAsF6。
3. a kind of New Solid electrolyte according to claim 1, it is characterised in that: the ceramic powder is Li-La-Ti oxygen Powder, lithium lanthanum zirconium oxygen powder, it is a kind of in lithium lanthanum zirconium tantalum oxygen or two kinds.
4. a kind of New Solid electrolyte according to claim 1, it is characterised in that: the solvent is N- crassitude One of ketone or deionized water.
5. a kind of New Solid electrolyte preparation method, it is characterised in that: including following preparation step:
Step 1: taking the solvent of 30-50 mass parts, and in the polyimides that 10-30 mass parts are wherein added, mechanical stirring is uniform；
Step 2: and then the lithium salts of addition 10-30 mass parts stirs evenly；
Step 3: the ceramic powder for adding 5-10 mass parts after mixing evenly, adds the polyurethane of 0.2-2 mass parts, mechanical It stirs evenly；
Step 4: after glue mechanical stirring is uniform, using cast coat in the two sides of membrane surface, it is then transferred to 50-90 DEG C vacuum drying oven, dry 4-12h, ionic conductivity at room temperature, which can be obtained, can reach (8-10) * 10-4S/m New Solid Dielectric film.
CN201811135417.3A 2018-09-28 2018-09-28 Novel solid electrolyte and preparation method thereof Active CN109286038B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111354976A (en) * 2020-03-16 2020-06-30 河南电池研究院有限公司 Preparation method of composite solid electrolyte and application of composite solid electrolyte in solid lithium ion battery
CN111769320A (en) * 2019-04-02 2020-10-13 深圳格林德能源集团有限公司 Solid polymer electrolyte membrane and preparation method thereof
CN112117488A (en) * 2020-07-31 2020-12-22 华中科技大学 Solid electrolyte, lithium metal negative electrode and preparation method thereof

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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
US20160336618A1 (en) * 2015-05-12 2016-11-17 Samsung Electronics Co., Ltd. Electrolyte composite and negative electrode and lithium second battery including the electrolyte composite
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20160336618A1 (en) * 2015-05-12 2016-11-17 Samsung Electronics Co., Ltd. Electrolyte composite and negative electrode and lithium second battery including the electrolyte composite
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111769320A (en) * 2019-04-02 2020-10-13 深圳格林德能源集团有限公司 Solid polymer electrolyte membrane and preparation method thereof
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 Preparation method of composite solid electrolyte and application of composite solid electrolyte in solid lithium ion battery
CN112117488A (en) * 2020-07-31 2020-12-22 华中科技大学 Solid electrolyte, lithium metal negative electrode and preparation method thereof

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