CN107492681A - Solid electrolyte film and preparation method thereof - Google Patents
Solid electrolyte film and preparation method thereof Download PDFInfo
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- CN107492681A CN107492681A CN201710676766.5A CN201710676766A CN107492681A CN 107492681 A CN107492681 A CN 107492681A CN 201710676766 A CN201710676766 A CN 201710676766A CN 107492681 A CN107492681 A CN 107492681A
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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
- H01M10/05—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
- H01M10/0565—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
- H01M10/058—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
- H01M2300/0082—Organic polymers
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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
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Abstract
This application discloses a kind of solid electrolyte film and preparation method thereof, the solid electrolyte film includes solid electrolyte layer and is compound in the composite bed on a solid electrolyte layer at least surface, the composite bed selects the high molecular polymer with certain lithium ion conduction ability, and its preparation method includes step：Porosity is prepared up to the polymeric matrix of 60~90% continuous three-dimensional net structure using phase separation method；Polymeric matrix, which is immersed in the slurry containing solid electrolyte powder, pulls out drying, obtains solid electrolyte layer；The upper composite bed of solid electrolyte layer surface coating, obtains solid electrolyte film.Inorganic solid electrolyte particle is embedded into the polymer film of three-dimensional net structure by solid electrolyte film of the present invention, obtain the solid electrolyte layer with high ionic conductivity, good processing characteristics and mechanical performance, while there is in the surface one side coating of solid electrolyte layer or double-coated the polymer of certain lithium ion conduction ability to reduce interface impedance.
Description
Technical field
The application belongs to technical field of lithium ion, more particularly to a kind of solid electrolyte film and preparation method thereof.
Background technology
At present, flammable liquid organic electrolyte is used in commercial li-ion battery, can be discharged in charge and discharge process can
Combustion property gas, in the dead of night, corroding electrode even occur it is on fire, burning etc. security incident.Inorganic solid electrolyte, there is high ion
Electrical conductivity, room temperature is up to 10-3Scm-1, while there is higher heat endurance and electrochemical stability, can be special in high temperature etc.
Worked under environment, can effectively suppress in the dead of night, corroding electrode the problems such as, greatly improve the security performance of lithium ion battery, so
And inorganic solid electrolyte exist it is crisp and hard, without elasticity not easy processing, especially its big with the impedance of electrode contact interface, lithium
Ion seriously inhibits its application in the problems such as transmission of electrode interior.Solid polymer electrolyte, it can overcome inorganic solid
The shortcomings that body electrolyte, there is relatively low electrolyte/electrode interface impedance and excellent machinability and flexility, but its
The electrical conductivity of room temperature lithium ion is too low, and (electrical conductivity only has 10-7Scm-1), some organic small point is often added in actual use
The plasticizer of son improves electrical conductivity, and the security performance of the introducing of organic plasticizers inevitably deterioration battery.
The content of the invention
It is inorganic in the prior art to overcome it is an object of the invention to provide a kind of solid electrolyte film and preparation method thereof
Crisp and hard bad mechanical property existing for solid electrolyte film, without elasticity not easy processing, with the impedance of electrode contact interface is big, lithium from
Son is electrode interior is transmitted the problems such as.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of solid electrolyte film, including solid electrolyte layer and is compound in the solid
The composite bed on a dielectric substrate at least surface, the composite bed select the high molecular polymerization with certain lithium ion conduction ability
Thing.
Preferably, in above-mentioned solid electrolyte film, the high molecular polymer is selected from Kynoar, gathers inclined difluoro
One or more combinations in ethene-hexafluoropropene, polymethyl methacrylate, polyethylene glycol oxide, polyacrylonitrile polymer.
Preferably, in above-mentioned solid electrolyte film, the thickness of described composite bed is in 0.5~5 micron, porosity
0.1~40%.
Preferably, in above-mentioned solid electrolyte film, the solid electrolyte layer includes having continuous three-dimensional grid knot
The polymeric matrix of structure and the inorganic solid electrolyte particle being embedded in the polymer matrix body.
Preferably, in above-mentioned solid electrolyte film, the thickness of the solid electrolyte film at 2.5~100 microns, Gu
Mass fraction of the body dielectric substrate in solid electrolyte film is 70~95%.
Preferably, in above-mentioned solid electrolyte film, the solid electrolyte layer thickness is 2~100 microns, porosity
For 0.1~15%.
Preferably, in above-mentioned solid electrolyte film, the polymeric matrix is poly- at 0.02~5 micron by diameter
The continuous three-dimensional network of compound composition, the polymer be arbitrary chain polymer, or the chain polymer containing side chain, this
The molecular weight of polymer is not less than 100,000.
Preferably, in above-mentioned solid electrolyte film, the particle diameter of the inorganic solid electrolyte particle is micro- for 0.01~5
Rice.
Accordingly, disclosed herein as well is a kind of preparation method of solid electrolyte film, including step：
(1) porosity, is prepared up to the polymeric matrix of 60~90% continuous three-dimensional net structure using phase separation method；
(2), polymeric matrix, which is immersed in the slurry containing solid electrolyte powder, pulls out drying, obtains solid electrolyte
Layer；
(3), the upper composite bed of solid electrolyte layer surface coating, obtains solid electrolyte film.
Preferably, in the preparation method of above-mentioned solid electrolyte film, in the step (3), by shifting coating side
Formula composite bed in the coating of solid electrolyte layer surface.
Compared with prior art, the advantage of the invention is that：Inorganic solid electrolyte particle is embedded into polymerization by the present invention
In the three-dimensional structure of thing perforated membrane, high conductivity can be obtained, there is certain flexible solid electrolyte, in its surface recombination
A thin layer of polyelectrolyte floor, the problem of electrolysis/solid electrolyte interface larger interface impedance can be efficiently solved,
The obtained solid electrolyte film of sandwich construction is prepared, there is high electrical conductivity, good pliability, low interface impedance,
It is a kind of solid electrolyte for holding promise for room temperature all-solid lithium-ion battery.
Brief description of the drawings
, below will be to embodiment or existing in order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in application, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 show the structural representation of solid electrolyte film in first embodiment of the invention；
Fig. 2 show the structural representation of solid electrolyte film in second embodiment of the invention.
Embodiment
Present embodiment discloses a kind of solid electrolyte film, including solid electrolyte layer 1 and it is compound in the solid electricity
The composite bed 2 on a matter layer at least surface is solved, the composite bed 2 is from the high molecular polymerization with certain lithium ion conduction ability
Thing.
With reference to shown in Fig. 1, in the first embodiment, the one side of solid electrolyte layer 1 is formed with composite bed 2.
With reference to shown in Fig. 2, in a second embodiment, the two sides of solid electrolyte layer 1 is each formed with composite bed 2.
In the technical scheme, the high molecular polymer has in lithium battery solvent, sode cell or other battery solvents
Certain swelling character, the high molecular polymer are the polymer with certain lithium ion conduction ability.
In a preferred embodiment, the high molecular polymer is selected from Kynoar (PVDF), polyvinylidene fluoride-six
The polymer such as fluoropropene (PVDF-HFP), polymethyl methacrylate (PMMA), polyethylene glycol oxide (PEO), polyacrylonitrile (PAN)
In one or more.
Further, for the thickness of described composite bed at 0.5~5 micron, porosity is 0.1~40%.
Further, the solid electrolyte layer includes polymeric matrix, Yi Jiqian with continuous three dimensional network structure
Enter the inorganic solid electrolyte particle in the polymer matrix body.
Further, the thickness of the solid electrolyte film is at 2.5~100 microns, and solid electrolyte layer is in solid electrolytic
Mass fraction in plasma membrane is 70~95%.
Further, the solid electrolyte layer thickness is 2~100 microns, and porosity is 0.1~15%.
Further, the continuous three dimensional network that the polymeric matrix is made up of diameter in 0.02~5 micron of polymer
Network, the polymer are arbitrary chain polymer, or the chain polymer containing side chain, the molecular weight of the polymer are not less than
100000.
Further, the particle diameter of the inorganic solid electrolyte particle is 0.01~5 micron.Inorganic solid electrolyte particle
Refer to that there is the solid electrolyte of certain ionic conduction characteristic, be that there is consolidating for certain lithium ion conduction ability further
Body electrolyte, inorganic solid electrolyte particle are thoroughly dispersed in the three-dimensional network being made up of polymer.
In a preferred embodiment, inorganic solid electrolyte particle can with it is following be one or more in electrolyte：Such as
Ca-Ti ore type Li0.5La0.5TiO3, NASICON types LiZr2(PO4)3And LiTi2(PO4)3, LISICON types Li14Zn(GeO4)4, layer
Shape Li3N-type, Garnet types Li5La3M2O12(M=Ta, Nb), amorphous LiPON, new sulfide compounds LiGeP2S12；Either increase
The compound of other inert powders, inert powder can be that such as aluminum oxide, silica have certain electrolyte energy of adsorption
The material of power, to increase the swelling of solid electrolyte film in the electrolytic solution, and then improve the electrical conductivity of solid electrolyte film.
The embodiment of the present application also discloses a kind of preparation method of solid electrolyte film, including step：
(1), use phase separation method prepare thickness for 1~100 micron, diameter 0.02~5 micron, porosity up to 60~
The polymeric matrix of 90% continuous three-dimensional net structure；
(2), polymeric matrix, which is immersed in the slurry containing solid electrolyte powder, pulls out drying, obtain thickness for 2~
100 microns, porosity be 0.1~15% solid electrolyte layer；
(3), the upper composite bed of solid electrolyte layer surface coating, obtains solid electrolyte film.
In the step (1), phase separation method includes thermally induced phase separation and solvent causes phase separation method.
In the step (3), by shifting coating method composite bed in the coating of solid electrolyte layer surface.
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
Embodiment 1-6 prepares the solid electrolyte film of sandwich construction according to following technique, and specific process parameter is shown in Table 1.
Phase separation method prepares polyethene microporous membrane：
(1), molecular weight is 1 × 106The blending of ultra-high molecular weight polyethylene fluoropolymer resin and atoleine, high temperature 150
DEG C it is melt into certain density polyolefin homogeneous phase solution → extruded through double screw extruder through certain thickness die head, casting film-forming
Cool in → 20 DEG C of water-baths, the certain stretching ratio biaxially oriented film in → 120 DEG C of evaporation solvent → 120 DEG C of generation phase separation →
The film that extraction is removed after diluent → stretching extraction under the conditions of offer some tension guarantee film is unshrinkable is further small
Width stretching and thermal finalization, are made certain thickness and the polyethene microporous membrane of porosity.
(2) polymer microporous film of high porosity, is immersed in the Li7La containing 3 μm3Zr2O12(LLZO) solid electrolytic
Drying is pulled out in the slurry of matter powder, obtains certain thickness and the solid electrolyte layer of porosity.
(3) it is compound, by shifting the method applied composite bed on solid electrolyte layer surface one side or dual coating
The thickness control of layer is at 0.5~5 micron, and 0.1~40%, it is consolidating with sandwich construction to finally obtain thickness for porosity control
Body dielectric film.
Technological parameter prepared by the solid electrolyte layer of table 1.
Embodiment 7
(1), phase separation method prepares Kynoar-hexafluoropropene microporous barrier：Molecular weight is 4 × 105Polyphosphazene polymer it is inclined
PVF-hexafluoropropene is dissolved in DMF (DMF) at room temperature, and the concentration for obtaining polyethylene is 10wt%
Solution, be cast into 200 μm of film, film immersed immediately in 20 DEG C of water-baths and cooled down, dry for 80 DEG C and remove solvents, 160 DEG C are two-way
Stretching, stretching ratio 10*5, obtains the poly- inclined fluorine that thickness is 5 microns, linear diameter is 0.02~5 micron, porosity is 90%
Ethene-hexafluoropropene microporous barrier.
(2), the polymer microporous film of high porosity is immersed in containing the Li that size is 1 μm1.5Al0.5Ge1.5(PO4)3
(LAGP) drying is pulled out in the slurry of solid electrolyte powder, obtains the solid electrolytic that thickness is 15 microns, porosity is 20%
Matter layer.
(3) composite bed, the thickness of composite bed, are covered with the painting of solid electrolyte layer surface one side by shifting the method for coating
At 2 microns, porosity control is finally obtained with sandwich construction, tensile strength is more than 10Mpa, electrical conductivity is 40% for control
10-3S/cm solid electrolyte films.
Embodiment 8
(1), phase separation method prepares Polyacrylonitrile membrane：Molecular weight is 3x105Macromolecule polypropylene nitrile at room temperature
It is dissolved in DMF (DMF), the concentration for obtaining polyacrylonitrile is 10wt% solution, 20 DEG C are immersed immediately
Cooled down in water-bath, 80 DEG C dry remove solvents, 180 DEG C of biaxial tensiones, stretching ratio 10*8, obtain thickness for 8 microns, line it is straight
The Polyacrylonitrile membrane that footpath is 0.02~5 micron, porosity is 90%.
(2), the polymer microporous film of high porosity is immersed in containing the Li that size is 1 μm1.5Al0.5Ge1.5(PO4)3
(LAGP) drying is pulled out in the slurry of solid electrolyte powder, obtains the solid electrolytic that thickness is 15 microns, porosity is 20%
Matter layer.
(3) composite bed, the thickness of composite bed, are covered with the painting of solid electrolyte layer surface one side by shifting the method for coating
At 5 microns, porosity control is finally obtained with sandwich construction, tensile strength is more than 10Mpa, electrical conductivity is 10% for control
10-5S/cm solid electrolyte films.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show and according to the solution of the present invention closely related structure and/or processing step, and eliminate little with relation of the present invention
Other details.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (10)
1. a kind of solid electrolyte film, it is characterised in that including solid electrolyte layer and be compound in the solid electrolyte layer
At least composite bed on a surface, the composite bed select the high molecular polymer with certain lithium ion conduction ability.
2. solid electrolyte film according to claim 1, it is characterised in that：The high molecular polymer is selected from polyvinylidene fluoride
Alkene, polyvinylidene fluoride-hexafluoropropene, polymethyl methacrylate, polyethylene glycol oxide, one kind in polyacrylonitrile polymer or
Multiple combinations.
3. solid electrolyte film according to claim 1, it is characterised in that：The thickness of described composite bed is micro- 0.5~5
Rice, porosity are 0.1~40%.
4. solid electrolyte film according to claim 1, it is characterised in that：The solid electrolyte layer includes having continuously
The polymeric matrix of three dimensional network structure and the inorganic solid electrolyte particle being embedded in the polymer matrix body.
5. solid electrolyte film according to claim 4, it is characterised in that：The thickness of the solid electrolyte film is 2.5
~100 microns, mass fraction of the solid electrolyte layer in solid electrolyte film is 70~95%.
6. solid electrolyte film according to claim 4, it is characterised in that：The solid electrolyte layer thickness is 2~100
Micron, porosity are 0.1~15%.
7. solid electrolyte film according to claim 4, it is characterised in that：The polymeric matrix is 0.02 by diameter
The continuous three-dimensional network of~5 microns of polymer composition, the polymer is arbitrary chain polymer, or the chain containing side chain
Shaped polymer, the molecular weight of the polymer are not less than 100,000.
8. solid electrolyte film according to claim 4, it is characterised in that：The particle diameter of the inorganic solid electrolyte particle
For 0.01~5 micron.
9. the preparation method of any described solid electrolyte film of claim 1 to 8, it is characterised in that including step：
(1) porosity, is prepared up to the polymeric matrix of 60~90% continuous three-dimensional net structure using phase separation method；
(2), polymeric matrix, which is immersed in the slurry containing solid electrolyte powder, pulls out drying, obtains solid electrolyte layer；
(3), the upper composite bed of solid electrolyte layer surface coating, obtains solid electrolyte film.
10. the preparation method of solid electrolyte film according to claim 9, it is characterised in that：In the step (3), lead to
Cross transfer coating method composite bed in the coating of solid electrolyte layer surface.
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Cited By (19)
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| CN109004271A (en) * | 2018-08-01 | 2018-12-14 | 惠州亿纬锂能股份有限公司 | A kind of composite solid electrolyte film and its preparation method and application |
| CN109244314A (en) * | 2018-08-16 | 2019-01-18 | 北京中科海钠科技有限责任公司 | A kind of sodium-ion battery ceramic diaphragm and sodium ion secondary battery and application |
| CN109524719A (en) * | 2018-10-16 | 2019-03-26 | 浙江大学 | Two-layer solid-state electrolyte complex film based on polyacrylonitrile and its preparation method and application |
| CN109950618A (en) * | 2019-03-26 | 2019-06-28 | 西安交通大学 | A kind of solvated composite solid electrolyte and its preparation method and application |
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