CN106099260A - Solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system - Google Patents
Solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system Download PDFInfo
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- CN106099260A CN106099260A CN201610665250.6A CN201610665250A CN106099260A CN 106099260 A CN106099260 A CN 106099260A CN 201610665250 A CN201610665250 A CN 201610665250A CN 106099260 A CN106099260 A CN 106099260A
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- solid electrolyte
- composite diaphragm
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- lithium
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1065—Polymeric electrolyte materials characterised by the form, e.g. perforated or wave-shaped
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
- H01M8/1081—Polymeric electrolyte materials characterised by the manufacturing processes starting from solutions, dispersions or slurries exclusively of polymers
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
Solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system, solid electrolyte composite diaphragm includes polymer barrier film and solid electrolyte crystal layer, polymer membrane thicknesses is 10 50 μm, solid electrolyte crystal layer thickness is 1 20 μm, and solid electrolyte crystal layer uniform fold is at described polymer membrane surface.Its preparation method includes: the preparation of (1) solid electrolyte presoma: by material powder mix homogeneously and carry out high temperature sintering；(2) preparation of solid electrolyte coating liquid: solid electrolyte presoma is the most uniformly mixed with binding agent；(3) polymer barrier film base coated film: solid electrolyte coating liquid is coated in the surface of described membrane for polymer, and is dried 48 hours under the conditions of 50 70 DEG C.Solid electrolyte composite diaphragm together constitutes with flow battery electrolyte system with the electrolyte that both positive and negative polarity flows.The present invention solves conventional batteries and shuttles back and forth the problem that effect is too strong, ionic conductivity is low, mechanical strength is low.
Description
Technical field
The invention belongs to new energy field, particularly to a kind of solid electrolyte composite diaphragm and this composite diaphragm of application
Electrolyte system.
Background technology
Battery is widely used in various field, from electric automobile, handheld device to microchip.Along with society and science and technology
Progressive, the life style of people proposes requirements at the higher level to battery performance, and countries in the world researcher is devoted to research and develop more always
Good electrochmical power source.Lithium battery is the green power supply grown up the nineties in 20th century, is referred to as the leading power supply of 21 century.
Lithium-sulfur cell is a kind of novel lithium ion battery, because of its have high reversible capacity, high voltage, high cycle performance and
The excellent properties such as higher energy density and enjoy favor.But polysulfide that lithium-sulfur cell generates in discharge process is soluble
In the electrolytic solution and penetrate barrier film and move at battery two interpolar with electrolyte, cause the irreversible loss of cell active materials, and
Seriously reduce the cycle performance of battery.This effect is referred to as effect of shuttling back and forth.Effect of shuttling back and forth seriously constrains lithium-sulfur cell
Practicality application and further development.
Additionally, lithium-sulfur cell also to have battery actual capacity relatively low, the most high technological deficiency of barrier film mechanical strength.
For solving these problems, patent CN104103873A proposes a kind of solid electrolyte membrane.This solid electrolyte membrane by
Solid-state electrolyte layer and porous ceramic layer are composited, and wherein solid-state electrolyte layer uniform fold is on porous ceramic layer.This is multiple
Close barrier film and reduce the impact of effect of shuttling back and forth to a certain extent, but use porous ceramic film material the electrical conductivity making barrier film to be shown
Write and decline.
Patent CN104577005A proposes a kind of Ceramic Composite barrier film.This composite diaphragm includes polymeric layer and is compounded in institute
State the ceramic layer on polymeric layer.This Ceramic Composite barrier film significantly enhances the mechanical strength of barrier film, but owing to lithium ion is at pottery
The electric conductivity of enamel coating is not strong, and therefore the electrical conductivity of this composite diaphragm need to improve.
Summary of the invention
The embodiment of the present invention provides a kind of solid electrolyte composite diaphragm, and the preparation side of solid electrolyte composite diaphragm
Method, and utilize the flow battery electrolyte system that this solid electrolyte composite diaphragm formed, works as solving conventional batteries technology
The problem that effect of shuttling back and forth is strong, ionic conductivity is low, mechanical strength is low that septation exists.
Solid electrolyte composite diaphragm, including polymer barrier film and solid electrolyte crystal layer.Polymer membrane thicknesses is 10-
50 μm, solid electrolyte crystal layer thickness is 1-20 μm, solid electrolyte crystal layer uniform fold unilateral at described polymer barrier film or
Double-sided surface.
The material of described solid electrolyte crystal layer is selected from zinc germanate lithium fast-ionic conductor, Li3N and derivant, sulfide
Vitreous electrolyte, Li3LnX6 type solid electrolyte, Li4SiO4 type solid electrolyte and NASICON structural type LiM2 (PO4) 3
One or more in type fast-ionic conductor, the M in described LiM2 (PO4) 3 type fast-ionic conductor is Ti, Zr, Ge, Mg, Al.
The material of described polymer barrier film be polyethylene, polypropylene, polyacrylonitrile, Kynoar or poly(ethylene oxide) and
One or more in its derivant.
The preparation method of above-mentioned solid electrolyte composite diaphragm, specifically includes following steps:
The preparation of solid electrolyte presoma.According to former by respective element of the element ratio of target solid electrolyte crystal layer
Material is evenly mixed in organic solvent, is dried and prepares the mixed uniformly powder of described raw material.By described powder at 650-850 DEG C
Sinter 12-48 hour and prepare described solid electrolyte presoma；
The preparation of solid electrolyte coating liquid.The solid electrolyte presoma obtained the most uniformly is mixed with binding agent
Close, stir 1-24 hour and prepare described solid electrolyte coating liquid；
Polymer barrier film base coated film.The solid electrolyte coating liquid obtained is coated in the one side of described membrane for polymer
Or double-sided surface, and be dried 48 hours under the conditions of 50-70 DEG C, prepare described solid electrolyte composite diaphragm.
The raw material of described respective element is at least in the carbonate of respective metal, phosphate, nitride, silicate
Kind.
Described organic solvent is glycol dimethyl ether, diethylene glycol dimethyl ether, TRIGLYME, TEG diformazan
In ether, NHD, N-N dimethylformamide, oxolane, 1-3-dioxolane, thioether, carbonate-based solvent
At least one or multiple mixture.
Described dry method is at least one in vacuum drying, lyophilization, pneumatic conveying drying, microwave drying.
Based on the flow battery electrolyte system constructed by obtained solid electrolyte composite diaphragm, including described solid-state
Electrolyte composite diaphragm, the electrolyte between described solid electrolyte composite diaphragm and anode and lithium salts, described solid-state electricity
Solve the electrolyte between matter composite diaphragm and battery cathode and lithium salts.
Described electrolyte is flowing.
Described electrolyte flow is natural circulation or forces flowing.
The flow velocity of described electrolyte is 0.05mL/min to 5000L/min.
The component of described electrolyte is glycol dimethyl ether, diethylene glycol dimethyl ether, TRIGLYME, TEG
Dimethyl ether, NHD, N-N dimethylformamide, oxolane, 1-3-dioxolane, thioether, carbonate-based solvent
In at least one or multiple mixture.
The material of described lithium salts includes hexafluoroarsenate lithium, LiBF4, lithium hexafluoro phosphate, two (trimethyl fluoride sulfonyl) Asia
At least one in amine lithium, lithium nitrate, many lithium sulfides.
The solid electrolyte composite diaphragm of the present invention, overcomes conventional membrane and shuttles back and forth the strong defect of effect, improve machinery
Intensity.The preparation method of solid electrolyte composite diaphragm, it is ensured that the end product quality of the solid electrolyte composite diaphragm of the present invention.
It is low that the flow battery electrolyte system utilizing this solid electrolyte composite diaphragm to be formed overcomes ionic conductivity on the whole
Technological deficiency so that battery overall structure performance and charge-discharge performance improve further.
Accompanying drawing explanation
Fig. 1 is the structural representation of solid electrolyte composite diaphragm in the embodiment of the present invention.
Fig. 2 is the structural representation of flow battery electrolyte system in the embodiment of the present invention.
Detailed description of the invention
The present invention proposes a kind of solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system.Solid-state
The structure of electrolyte composite diaphragm is: be combined one layer of solid electrolyte crystal layer in membrane for polymer one side or double-sided surface.This
Structure can be effectively improved effect of shuttling back and forth.The flow battery electrolyte system utilizing the solid electrolyte composite diaphragm of the present invention leads to
Cross and use the design of flowing electrolyte to improve the reaction capacity of battery, reduce effect of shuttling back and forth simultaneously.Below in conjunction with the accompanying drawings and tool
The present invention is described in further detail by body embodiment.
In the embodiment of the present invention, the structure of solid electrolyte composite diaphragm is as shown in Figure 1.As a example by One-sided coatings, solid-state electricity
Solve matter crystal layer 2 and be coated in polymer barrier film 1 single side surface.
In the embodiment of the present invention, the structure of flow battery electrolyte system is as shown in Figure 2.Solid electrolyte crystal layer 2 is coated in
Polymer barrier film 1 single side surface, forms solid electrolyte composite diaphragm, is arranged in battery system.Anode electrolyte 3 and negative pole
It is dissolved with lithium salts in electrolyte 4.Both positive and negative polarity electrolyte is flowing, and anode electrolyte enters battery system by inlet 5, logical
Crossing liquid outlet 6 and flow out battery system, electrolyte liquid enters battery system by inlet 7, flows out battery system by liquid outlet 8
System.The electrolyte of both positive and negative polarity flowing is collectively forming an electrolyte system with solid electrolyte composite diaphragm, lithium salts.
The embodiment example 1 of the preparation method of solid electrolyte composite diaphragm
Li2CO3, GeO2, NH4H2PO3 are evenly mixed in glycol dimethyl ether and N-N bis-with the molar ratio of 1:2:3
In the solvent mixture of methylformamide, pneumatic conveying drying prepares the mixed uniformly powder of raw material.Powder is burnt at 650-850 DEG C
Tie 12-48 hour, prepare solid electrolyte presoma.By the solid electrolyte presoma of gained and binding agent according to the ratio of 1:1
Example, the most uniformly mixes, and stirs 1-24 hour system, obtains the coating of NASICON structural type LiGe2 (PO4) 3 type solid electrolyte
Liquid.Solid electrolyte coating liquid is coated in the double-sided surface of poly(ethylene oxide) barrier film, and wherein poly(ethylene oxide) thickness is 35 μm,
NASICON structural type LiGe2 (PO4) 3 type solid electrolyte crystal layer thickness is 6 μm, and it is little to be dried 48 under the conditions of 50-70 DEG C
Time, prepare solid electrolyte composite diaphragm.
Battery pile is assembled fixing according to positive plate, solid electrolyte composite diaphragm, the order of negative plate successively.Wherein
It is positive pole reaction chamber between positive plate and solid electrolyte composite diaphragm, is negative between negative plate and solid electrolyte composite diaphragm
Pole reaction chamber.
Being dissolved in DOX/ethylene glycol dimethyl ether solution by lithium nitrate, make electrolyte, lithium nitrate concentration is
1mol/L.And electrolyte is stored in the outside fluid reservoir of both positive and negative polarity.
In charge and discharge process, both positive and negative polarity electrolyte enters both positive and negative polarity reaction chamber by circulating pump.Regulation circulating pump makes electrolysis
Flow velocity is 50ml/min.Both positive and negative polarity electrolyte and solid electrolyte composite diaphragm form the electrolyte system of battery system.
The embodiment example 2 of the preparation method of solid electrolyte composite diaphragm
Li2CO3, α-Al2O3, GeO2, NH4H2PO3 are evenly mixed in second two with the molar ratio of 1.5:0.5:1.5:3
In the solvent mixture of diethylene glycol dimethyl ether and N-N dimethylformamide, pneumatic conveying drying prepares the mixed uniformly powder of raw material.By powder
13 hours prepared solid electrolyte presomas are sintered at 850 DEG C.By the solid electrolyte presoma of gained and binding agent according to
The ratio of 1:1, the most uniformly mixes, and stirs 24 hours systems, obtains LAGP type solid electrolyte coating liquid.By solid electrolyte
Coating liquid is coated in the double-sided surface of polyacrylonitrile barrier film, and wherein poly(ethylene oxide) thickness is 25 μm, LAGP type solid electrolyte
Crystal layer thickness is 3 μm, and is dried 12 hours under the conditions of 60-90 DEG C, prepares solid electrolyte composite diaphragm.
Battery pile is assembled fixing according to positive plate, solid electrolyte composite diaphragm, the order of negative plate successively.Wherein
It is positive pole reaction chamber between positive plate and solid electrolyte composite diaphragm, is negative between negative plate and solid electrolyte composite diaphragm
Pole reaction chamber.
Two (trimethyl fluoride sulfonyl) imine lithium is dissolved in DOX/ethylene glycol dimethyl ether solution, makes electricity
Solving liquid, two (trimethyl fluoride sulfonyl) imine lithium concentration is 1mol/L, and is stored in by electrolyte in the outside fluid reservoir of both positive and negative polarity.
In charge and discharge process, both positive and negative polarity electrolyte enters both positive and negative polarity reaction chamber by circulating pump.Regulation circulating pump makes electrolysis
Flow velocity is 167ml/min.Both positive and negative polarity electrolyte, lithium salts and solid electrolyte composite diaphragm form the electrolysis plastid of battery system
System.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto.
Any those familiar with the art is within the technical scope that disclosed herein, according to technical scheme
And inventive concept carries out equivalent or change, all should contain within protection scope of the present invention.
Claims (13)
1. solid electrolyte composite diaphragm, it is characterised in that include polymer barrier film and solid electrolyte crystal layer, polymer barrier film
Thickness is 10-50 μm, and solid electrolyte crystal layer thickness is 1-20 μm, solid electrolyte crystal layer uniform fold described polymer every
Film one side or double-sided surface.
Solid electrolyte composite diaphragm the most according to claim 1, it is characterised in that the material of described solid electrolyte crystal layer
Matter selected from zinc germanate lithium fast-ionic conductor, Li3N and derivant thereof, chalcogenide glass electrolyte, Li3LnX6 type solid electrolyte,
One or more in Li4SiO4 type solid electrolyte and NASICON structural type LiM2 (PO4) 3 type fast-ionic conductor, described
M in LiM2 (PO4) 3 type fast-ionic conductor is Ti, Zr, Ge, Mg, Al.
Solid electrolyte composite diaphragm the most according to claim 1, it is characterised in that the material of described polymer barrier film is
One or more in polyethylene, polypropylene, polyacrylonitrile, Kynoar or poly(ethylene oxide) and derivant thereof.
4. according to the preparation method of the solid electrolyte composite diaphragm described in claims 1 to 3 any one, it is characterised in that
Comprise the following steps:
The preparation of solid electrolyte presoma, according to the element ratio of target solid electrolyte crystal layer by equal for the raw material of respective element
Even mixing in organic solvent, is dried and prepares the mixed uniformly powder of described raw material, sintered by described powder at 650-850 DEG C
Within 12-48 hour, prepare described solid electrolyte presoma；
The preparation of solid electrolyte coating liquid, the most uniformly mixes the solid electrolyte presoma obtained with binding agent,
Stir 1-24 hour and prepare described solid electrolyte coating liquid；
Polymer barrier film base coated film, is coated in the one side of described membrane for polymer or double by the solid electrolyte coating liquid obtained
Side surface, and be dried 48 hours under the conditions of 50-70 DEG C, prepare described solid electrolyte composite diaphragm.
The preparation method of solid electrolyte composite diaphragm the most according to claim 4, it is characterised in that described respective element
Raw material be at least one in the carbonate of respective metal, phosphate, nitride, silicate.
The preparation method of solid electrolyte composite diaphragm the most according to claim 4, it is characterised in that described organic solvent
For glycol dimethyl ether, diethylene glycol dimethyl ether, TRIGLYME, tetraethyleneglycol dimethyl ether, NHD, N-
At least one in N-dimethylformamide, oxolane, 1-3-dioxolane, thioether, carbonate-based solvent or multiple mixing
Thing.
The preparation method of solid electrolyte composite diaphragm the most according to claim 4, it is characterised in that described dry side
Method is at least one in vacuum drying, lyophilization, pneumatic conveying drying, microwave drying.
8. according to the flow battery electrolyte constructed by the solid electrolyte composite diaphragm described in claims 1 to 3 any one
System, it is characterised in that include described solid electrolyte composite diaphragm, described solid electrolyte composite diaphragm and anode it
Between electrolyte and be dissolved in lithium salts therein, electrolyte between described solid electrolyte composite diaphragm and battery cathode and molten
Solution lithium salts wherein.
Flow battery electrolyte system the most according to claim 8, it is characterised in that described electrolyte is flowing.
Flow battery electrolyte system the most according to claim 9, it is characterised in that described electrolyte flow is nature
Circulate or force flowing.
11. flow battery electrolyte systems according to claim 8, it is characterised in that the flow velocity of described electrolyte is
0.05mL/min to 5000L/min.
12. flow battery electrolyte systems according to claim 8, it is characterised in that described lithium salts includes hexafluoroarsenate
At least one in lithium, LiBF4, lithium hexafluoro phosphate, two (trimethyl fluoride sulfonyl) imine lithium, lithium nitrate, many lithium sulfides.
13. flow battery electrolyte systems according to claim 8, it is characterised in that the component of described electrolyte is second
Glycol dimethyl ether, diethylene glycol dimethyl ether, TRIGLYME, tetraethyleneglycol dimethyl ether, NHD, N-N bis-
At least one in methylformamide, oxolane, 1-3-dioxolane, thioether, carbonate-based solvent or multiple mixture.
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| CN201610665250.6A CN106099260A (en) | 2016-08-12 | 2016-08-12 | Solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system |
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| CN201610665250.6A CN106099260A (en) | 2016-08-12 | 2016-08-12 | Solid electrolyte composite diaphragm and preparation method and flow battery electrolyte system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108963327A (en) * | 2017-05-18 | 2018-12-07 | 珠海市赛纬电子材料股份有限公司 | A kind of compound PEO solid electrolyte material of inorganic filler and preparation method and all-solid-state battery |
| CN109755441A (en) * | 2018-12-19 | 2019-05-14 | 宁波革鑫新能源科技有限公司 | A kind of PP diaphragm and preparation method thereof of composite solid electrolyte modification |
| CN112838266A (en) * | 2021-03-23 | 2021-05-25 | 上海电气集团股份有限公司 | Composite electrolyte membrane, preparation method and application thereof, and solid-state lithium battery |
| CN114156600A (en) * | 2021-12-13 | 2022-03-08 | 溧阳天目先导电池材料科技有限公司 | Diaphragm containing mixed conductor coating and preparation method and application thereof |
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Application publication date: 20161109 |