CN107369848A - A kind of composite electrolyte of sandwich structure and preparation method thereof - Google Patents
A kind of composite electrolyte of sandwich structure and preparation method thereof Download PDFInfo
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- CN107369848A CN107369848A CN201710574753.7A CN201710574753A CN107369848A CN 107369848 A CN107369848 A CN 107369848A CN 201710574753 A CN201710574753 A CN 201710574753A CN 107369848 A CN107369848 A CN 107369848A
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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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid 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
- 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
- H01M2300/0094—Composites in the form of layered products, e.g. coatings
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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
Abstract
The present invention relates to a kind of composite electrolyte of sandwich structure and preparation method thereof, which solve the technical problem that existing all solid state electrolyte interface performance is poor, electrical conductivity is low, it includes porous membrane and composite solid electrolyte material, porous membrane is fitted in the both sides of composite solid electrolyte material, porous membrane is made up of high molecular polymer, and porous membrane is adsorbed with liquid electrolyte.Invention also provides its preparation method.It the method can be widely used in the preparation field of electrolyte.
Description
Technical field
The present invention relates to lithium ion battery solid electrolyte field, relates in particular to a kind of compound electric of sandwich structure
Solve matter and preparation method thereof.
Background technology
With application of the lithium ion battery in energy storage field, the security of battery turns into focus of concern.It is big at present
Most lithium ion batteries all employ organic liquid electrolytes.The problem of organic liquid electrolytes are easily revealed, be inflammable, threatens electricity
The safety in pond.In order to solve this problem, solid electrolyte arises at the historic moment.Current solid electrolyte can be divided into polymer gel
Electrolyte, polymer all solid state electrolyte, inorganic solid electrolyte etc. are several.
Solid polyelectrolyte because in the absence of organic liquid electrolytes are inflammable, easily reveal the shortcomings that, and also have one
Fixed flexibility, so being increasingly becoming focus of concern.
Solid polyelectrolyte is because it is poor with the contact performance of electrode material, the relatively low (10-5s/ of electrical conductivity at room temperature
), cm there is certain limitation in actual use.People generally electrolyte is put under conditions of high temperature can just obtain compared with
Low interface impedance and higher lithium ion conductivity, the addition of heating element heater can make battery become very heavy.
In order to solve problem above, it is thus proposed that coat one layer of liquid electrolyte on all solid state electrolyte surface to improve material
The interface performance and electrical conductivity of material, but use the load capacity of the method liquid electrolyte of coating not high, can also there is liquid electric
Solve the danger of matter leakage.
The content of the invention
The present invention is exactly to solve the technical problem that existing all solid state electrolyte interface performance is poor, electrical conductivity is low, there is provided
A kind of composite electrolyte of sandwich structure and preparation method thereof.
Therefore, the present invention provides a kind of composite electrolyte of sandwich structure, it includes porous membrane and composite solid electricity
Material is solved, porous membrane is fitted in the both sides of composite solid electrolyte material, and porous membrane is made up of high molecular polymer, more
Hole film is adsorbed with liquid electrolyte.Porous membrane is fitted in the both sides of composite solid electrolyte by the present invention, passes through absorption one
Quantitative liquid electrolyte improves the interface performance and ionic conductivity of total electrolyte material.
Preferably, polymer be polyacrylonitrile (PAN), polymethyl methacrylate (PMMA), Kynoar (PVDF),
The one or more of polyethylene glycol oxide (PEO), bacteria cellulose (BC).
Preferably, solid electrolyte is inorganic solid electrolyte, organic solid-state electrolyte, one kind of inorganic nano-filler
It is or a variety of.
Preferably, inorganic solid electrolyte is the solid electrolyte of oxide system or the solid state electrolysis of sulfide systems
Matter；Liquid electrolyte is that lithium salts and organic solvent form, and lithium salts is lithium perchlorate, lithium hexafluoro phosphate, double fluoroform sulphonyl Asia
One or more among amine lithium；Organic solvent is ethylene carbonate, propene carbonate, the one or more of diethyl carbonate.
Preferably, the solid electrolyte of oxide system is LLTO, LATP, LLZO, LATP, LAGP one or more.
Preferably, solid electrolyte LGPS, LPS, LS-BS-LI of sulfide systems one or more.
Preferably, organic bath is polyacrylonitrile (PAN), polymethyl methacrylate (PMMA), Kynoar
(PVDF), the one or more of polyethylene glycol oxide (PEO).
Preferably, inorganic nano-filler is alundum (Al2O3) (Al203), silica (SiO2), lithium nitride (Li3N) it
It is one or more.
Present invention simultaneously provides a kind of preparation method of the composite electrolyte of sandwich structure, it comprises the following steps：(1)
Preferable polymer is put into container, a certain amount of solvent is added and is made into spinning solution, carry out electrostatic spinning, obtain porous thin
Film；(2) preferable organic solid-state electrolyte dissolution is added into a certain amount of acetonitrile and thereto preferable inoganic solids electricity
Xie Zhi, inorganic nano-filler one or more, are sufficiently stirred at room temperature, form homogeneous mixed solution；(3) by step (2)
In mixed solution be put into vacuumized in vacuum drying apparatus remove solution in bubble, then pour on processing release paper, be placed in flat board
30 DEG C of -50 DEG C of heating 1-2h on heater, 30 DEG C of -50 DEG C of heating 48h in vacuum drying chamber are subsequently placed in, obtain composite solid electricity
Solve matter film；(4) the composite solid electrolyte film both sides during the electrostatic spinning film in step (1) is pasted in step (3), and
With 100-500Pa pressure compaction, the composite electrolyte of sandwich structure is obtained.
Preferably, inorganic solid electrolyte or inorganic nano-filler account for the 5-20% of gross mass in step (2)；Gross mass is
The quality sum of organic solid-state electrolyte and inorganic solid electrolyte or inorganic nano-filler.
The present invention provides a kind of composite electrolyte of sandwich structure, its porous membrane prepared by electrostatic spinning and compound
Solid electrolyte material is formed.Porous membrane is made up of high molecular polymer, and porous membrane is fitted in composite solid by the present invention
The both sides of electrolyte, improve the interface performance and lithium ion conductance of all solid state electrolyte material by adsorbing a certain amount of electrolyte
Rate.Lithium ion conductivity highest can reach 3*10-3s/cm；The Ω of interface impedance 600, about full solid state polymer electrolyte interface
The 1/40 of impedance.
The solid polyelectrolyte of sandwich structure prepared by the present invention, there is shape and size designability；Have
It is preferably flexible.Preparation technology of the present invention is simple, environment-friendly, cost is cheap, easily realizes industrialized production and commercial applications.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is interface impedance schematic diagram of the present invention；
Fig. 3 is ionic conductivity schematic diagram of the present invention.
Specific embodiment
According to following embodiments, the present invention may be better understood.It is however, as it will be easily appreciated by one skilled in the art that real
Apply the content described by example and be merely to illustrate the present invention, without should be also without limitation on this hair described in claims
It is bright.
Embodiment 1
(1) by DMF and DMK according to mass ratio 1:1 is made into that mixed solution is standby, takes appropriate PVDF powder to be added to above-mentioned
The solution of PVDF mass fractions 17% is made in mixed solution, 12h is stirred under the conditions of 60 DEG C, the mixing for obtaining transparent and homogeneous is molten
Liquid；
(2) in 1.5ml/h injection speed, 18kv spinning voltages, received (roller rotating speed 800r/min) using roller
Under the conditions of carry out electrostatic spinning；
(3) electrostatic spinning film is put into baking oven after spinning terminates, 3-48h is dried under the conditions of 60 DEG C makes solvent complete
Volatilization.Obtained film is standby；
(4) 1g PEO, 0.3g LiClO are taken4It is put into 10-25ml ACN and is sufficiently stirred to form uniform solution, is divided into four parts
Add a certain amount of LLTO nanofibers (LLTO NWs) thereto respectively, the mass fraction that LLTO NWs are made be 5% it is mixed
Solution is closed, is sufficiently stirred at room temperature；
(5) mixed solution in previous step is put into vacuum drying apparatus and vacuumizes 10min, then poured on processing release paper,
30 DEG C of -50 DEG C of heating 1-2h on panel heater are placed in, 30 DEG C of -50 DEG C of heating 48h in vacuum drying chamber is subsequently placed in, is had
Composite solid electrolyte film；
(6) the composite solid electrolyte film both sides being attached to the electrostatic spinning film in step (3) in step (5), and
With 100-500Pa pressure compaction, the composite electrolyte of sandwich structure is obtained；
(7) AC impedance method is used, the electrical conductivity for the solid electrolyte for testing the sandwich structure under the conditions of 25 DEG C is
0.5×10-3s/cm。
Embodiment 2
(1) by DMF and DMK according to mass ratio 1:1 is made into that mixed solution is standby, takes appropriate PVDF powder to be added to above-mentioned
The solution of PVDF mass fractions 17% is made in mixed solution, 12h is stirred under the conditions of 60 DEG C, the mixing for obtaining transparent and homogeneous is molten
Liquid；
(2) in 1.5ml/h injection speed, 18kv spinning voltages, received (roller rotating speed 800r/min) using roller
Under the conditions of carry out electrostatic spinning；
(3) electrostatic spinning film is put into baking oven after spinning terminates, 3-48h is dried under the conditions of 60 DEG C makes solvent complete
Volatilization.Obtained film is standby；
(4) 1g PEO, 0.3g LiClO are taken4It is put into 10-25ml ACN and is sufficiently stirred to form uniform solution, is divided into four parts
Add a certain amount of LLTO nanofibers (LLTO NWs) thereto respectively, the mass fraction that LLTO NWs are made be 10% it is mixed
Solution is closed, is sufficiently stirred at room temperature；
(5) mixed solution in previous step is put into vacuum drying apparatus and vacuumizes 10min, then poured in silicone oil paper,
30 DEG C of -50 DEG C of heating 1-2h on panel heater are placed in, 30 DEG C of -50 DEG C of heating 48h in vacuum drying chamber is subsequently placed in, is answered
Close electrolytic thin-membrane；
(6) the composite solid electrolyte film both sides being attached to the electrostatic spinning film in step (3) in step (5), and
With 100-500Pa pressure compaction, the composite electrolyte of sandwich structure is obtained；
(7) AC impedance method is used, the electrical conductivity for the solid electrolyte for testing the sandwich structure under the conditions of 25 DEG C is
1.9×10-3s/cm。
Embodiment 3
(1) by DMF and DMK according to mass ratio 1:1 is made into that mixed solution is standby, takes appropriate PVDF powder to be added to above-mentioned
The solution of PVDF mass fractions 17% is made in mixed solution, 12h is stirred under the conditions of 60 DEG C, the mixing for obtaining transparent and homogeneous is molten
Liquid；
(2) in 1.5ml/h injection speed, 18kv spinning voltages, received (roller rotating speed 800r/min) using roller
Under the conditions of carry out electrostatic spinning；
(3) electrostatic spinning film is put into baking oven after spinning terminates, 3~48h is dried under the conditions of 60 DEG C makes solvent complete
Full volatilization.Obtained film is standby；
(4) 1g PEO, 0.1-0.3g LiClO are taken4It is put into 10-25ml ACN and is sufficiently stirred to form uniform solution, is divided into
Four parts of difference add a certain amount of LLTO nanofibers (LLTO NWs) thereto, and the mass fraction that LLTO NWs are made is 15%
Mixed solution, be sufficiently stirred at room temperature；
(5) mixed solution in previous step is put into vacuum drying apparatus and vacuumizes 10min, then poured in silicone oil paper,
30 DEG C of -50 DEG C of heating 1-2h on panel heater are placed in, 30 DEG C of -50 DEG C of heating 48h in vacuum drying chamber is subsequently placed in, is answered
Close solid electrolyte film；
(6) the composite solid electrolyte film both sides being attached to the electrostatic spinning film in step (3) in step (5), and
With 100-500Pa pressure compaction, the composite electrolyte of sandwich structure is obtained；
(7) AC impedance method is used, the electrical conductivity that the solid electrolyte of the sandwich structure is tested under the conditions of 25 DEG C is 3
×10-3s/cm。
Embodiment 4
(1) by DMF and DMK according to mass ratio 1:1 is made into that mixed solution is standby, takes appropriate PVDF powder to be added to above-mentioned
The solution of PVDF mass fractions 17% is made in mixed solution, 12h is stirred under the conditions of 60 DEG C, the mixing for obtaining transparent and homogeneous is molten
Liquid；
(2) in 1.5ml/h injection speed, 18kv spinning voltages, received (roller rotating speed 800r/min) using roller
Under the conditions of carry out electrostatic spinning；
(3) electrostatic spinning film is put into baking oven after spinning terminates, 3~48h is dried under the conditions of 60 DEG C makes solvent complete
Full volatilization.Obtained film is standby；
(4) 1g PEO, 0.1-0.3g LiClO are taken4It is put into 10-25ml ACN and is sufficiently stirred to form uniform solution, is divided into
Four parts of difference add a certain amount of LLTO nanofibers (LLTO NWs) thereto, and the mass fraction that LLTO NWs are made is 20%
Mixed solution, be sufficiently stirred at room temperature；
(5) mixed solution in previous step is put into vacuum drying apparatus and vacuumizes 10min, then poured in silicone oil paper,
30 DEG C of -50 DEG C of heating 1-2h on panel heater are placed in, 30 DEG C of -50 DEG C of heating 48h in vacuum drying chamber is subsequently placed in, is answered
Close solid electrolyte film；
(6) the composite solid electrolyte film both sides being attached to the electrostatic spinning film in step (3) in step (5), and
With 100-500Pa pressure compaction, the composite electrolyte of sandwich structure is obtained；
(7) AC impedance method is used, the electrical conductivity for the solid electrolyte for testing the sandwich structure under the conditions of 25 DEG C is
1.7×10-3s/cm。
Claims (10)
1. a kind of composite electrolyte of sandwich structure, it is characterized in that it includes porous membrane and composite solid electrolyte material,
The porous membrane is fitted in the both sides of the composite solid electrolyte material, and the porous membrane is by high molecular polymer group
Into the porous membrane is adsorbed with liquid electrolyte.
2. the composite electrolyte of sandwich structure according to claim 1, it is characterised in that the high molecular polymer is
Polyacrylonitrile, polymethyl methacrylate, Kynoar, polyethylene glycol oxide, the one or more of bacteria cellulose.
3. the composite electrolyte of sandwich structure according to claim 1, it is characterised in that described solid state electrolysis material
Expect for inorganic solid electrolyte, organic solid-state electrolyte, inorganic nano-filler one or more.
4. the composite electrolyte of sandwich structure according to claim 3, it is characterised in that described inorganic solid electrolyte
Matter is the solid electrolyte of oxide system or the solid electrolyte of sulfide systems；The liquid electrolyte is lithium salts and organic
Solvent forms；The lithium salts is the one or more among lithium perchlorate, lithium hexafluoro phosphate, double trifluoromethanesulfonimide lithiums；
The organic solvent is ethylene carbonate, propene carbonate, the one or more of diethyl carbonate.
5. the composite electrolyte of sandwich structure according to claim 4, it is characterised in that described oxide system
Solid electrolyte is LLTO, LATP, LLZO, LATP, LAGP one or more.
6. the composite electrolyte of sandwich structure according to claim 4, it is characterised in that described sulfide systems
Solid electrolyte LGPS, LPS, LS-BS-LI one or more.
7. the composite electrolyte of sandwich structure according to claim 3, it is characterised in that described organic solid-state electrolysis
Matter is polyacrylonitrile, polymethyl methacrylate, Kynoar, the one or more of polyethylene glycol oxide.
8. the composite electrolyte of sandwich structure according to claim 3, it is characterised in that the inorganic nano-filler is
Alundum (Al2O3), silica, the one or more of lithium nitride.
A kind of 9. preparation method of the composite electrolyte of sandwich structure, it is characterized in that comprising the following steps：
(1) polymer is put into container, adds solvent and be made into spinning solution, carry out electrostatic spinning, obtain porous membrane；
(2) organic solid-state electrolyte dissolution is added in acetonitrile and thereto inorganic solid electrolyte, inorganic nano-filler it
One or more, it is sufficiently stirred at room temperature, forms homogeneous mixed solution；
(3) mixed solution in the step (2) is put into the bubble for vacuumizing and being removed in solution in vacuum drying apparatus, then poured
In silicone oil paper, be placed on panel heater 30 DEG C of -50 DEG C of heating 1-2h, be subsequently placed in vacuum drying chamber 30 DEG C -50 DEG C plus
Hot 48h, obtain composite solid electrolyte film；
(4) electrostatic spinning film in the step (1) is attached to the composite solid electrolyte film two in the step (3)
Side, and with 100-500Pa pressure compaction, obtain the composite electrolyte of sandwich structure.
10. the preparation method of the composite electrolyte of sandwich structure according to claim 9, it is characterised in that the step
(2) inorganic solid electrolyte or inorganic nano-filler account for the 5-20% of gross mass in；The gross mass is organic solid-state electrolyte
With the quality sum of inorganic solid electrolyte or inorganic nano-filler.
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| CN115020801A (en) * | 2022-08-08 | 2022-09-06 | 国联汽车动力电池研究院有限责任公司 | Solid electrolyte composite membrane and preparation method and application thereof |
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