CN106654364A - Ion liquid composite full-solid polymer electrolyte and preparation method and application thereof - Google Patents
Ion liquid composite full-solid polymer electrolyte and preparation method and application thereof Download PDFInfo
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- CN106654364A CN106654364A CN201610914961.2A CN201610914961A CN106654364A CN 106654364 A CN106654364 A CN 106654364A CN 201610914961 A CN201610914961 A CN 201610914961A CN 106654364 A CN106654364 A CN 106654364A
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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
- H01M10/058—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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
Abstract
The invention discloses ion liquid composite full-solid polymer electrolyte and a preparation method and application thereof. The ion liquid composite full-solid polymer electrolyte consists of polymer matrix, ion liquid and lithium salt; the addition amount of the ion liquid is 0.1 to 80 percent of the mass of the polymer matrix; and the lithium salt accounts for 5 to 95 percent by mass of the polymer matrix. Different polymer matrixes are used to be composited with different types of ion liquid, different types of lithium salts are added, and the full-solid composite polymer electrolyte is prepared by virtue of a solution pouring film forming method. The preparation method is simple, the molding is simple, the mechanical performance and the heat stability are good, the ion electric conductivity at a room temperature is relatively high and close to 10<-4> S/cm; and a full-solid lithium ion battery formed by assembling the electrolyte, a positive material and a negative material is safe, environment-friendly and good in electrochemical performance. The ion liquid composite full-solid polymer electrolyte can be applied to the full-solid lithium battery, a full-solid lithium-sulfur battery and other high-performance lithium batteries.
Description
Technical field
The invention belongs to full solid state polymer technical field of lithium ion, more particularly to a kind of ionic liquid is compound complete solid
State polymer dielectric and preparation method and application.
Background technology
In recent years, lithium ion battery as contemporary efficient energy storage device because its is light, high-energy-density the features such as,
With widespread commercial use, the requisite new forms of energy in many fields are had become.However, business-like lithium ion battery with
Based on liquid electrolyte lithium ion battery, mainly it is made up of positive pole, negative pole, liquid electrolyte, barrier film.Such battery is in use
Side reaction corroding electrode is frequently accompanied by, the service life of battery is reduced, and electrolyte is easily leaked, and there is very big safety
Hidden danger.Full solid state polymer electrolyte lithium ion battery receives people's extensive concern, mainly due to battery in it is all solid state
Polymer dielectric not only can conduction carrier, and while can play barrier film effect.With conventional liquid electrolyte lithium-ion
Battery is compared, and full solid state polymer electrolyte lithium ion battery has higher energy density, and battery appearance design is more flexible
Various, security and the feature of environmental protection are significantly improved.It can be seen that, full solid state polymer lithium ion battery is that a kind of performance is more excellent
Good lithium ion battery, has become the focus of lithium battery research.Polymer dielectric is mainly by polymeric matrix and lithium salts group
Into.At present, it is the linear polyoxygenated to lithium salts with certain dissolving and conducting power to study more polymer electrolyte matrix
Ethene and its derivative, but easily crystallize under linear polyethylene glycol oxide room temperature, it is unfavorable for the migration of carrier, therefore this is birdsed of the same feather flock together
The room-temperature conductivity of polymer electrolyte is relatively low, and only 10-7 S cm-1And mechanical performance is poor.Compared with linear polyethylene glycol oxide,
Merlon with polar group, polyimides, polyamide, polyester, polyethers, polysulfide, polyphosphazene, polyurethane or polysulfones etc. gather
Compound has excellent film forming, and mechanical performance is higher, but they are combined the full solid state polymer electrolyte of acquisition with lithium salts
Electrical conductivity is relatively low, it is impossible to meet practical requirement.
In sum, there is the migration for being unfavorable for carrier in existing polymer electrolyte matrix, and room-temperature conductivity is relatively low,
Mechanical performance is poor, it is impossible to meet the problem of practical requirement.
The content of the invention
It is an object of the invention to provide a kind of ionic liquid compound all-solid polymer electrolyte and preparation method thereof with
Using, it is intended to solve existing polymer electrolyte matrix and there is the migration for being unfavorable for carrier, room-temperature conductivity is relatively low, machinery
Poor-performing, it is impossible to meet the problem of practical requirement.
The present invention is achieved in that a kind of ionic liquid compound all-solid polymer electrolyte, and the ionic liquid is answered
Close full solid state polymer electrolyte to be made up of polymeric matrix, ionic liquid and lithium salts；
The addition of the ionic liquid is the 0.1 ~ 80% of polymer matrix weight；The lithium salts accounts for the quality of polymeric matrix
Fraction is 5 ~ 95%.
Further, the polymeric matrix includes Merlon, polyimides, polyamide, polyester, polyethers, polyphosphazene, poly-
Urethane, polysulfones, polyformaldehyde, polyacrylonitrile, polyvinyl chloride, polysulfide, Kynoar, polyphosphate, polyacrylate, polyethers
Ester, polydioxolane, PPI, polytetrafluoroethylene (PTFE), polyhexafluoropropylene, containing heteroatomic polyethylene, containing heteroatomic poly-
One or more in propylene, polysiloxanes or their block copolymer or graft polymers or random copolymer, in electrolysis
Play a supportive role in matter, for electrolyte mechanical strength is provided, increase film forming；
Described ionic liquid include cation be imidazole ring, pyridine ring, tri-n-butylamine and pyrroles's ring structure, anion be chlorine from
Son, tetrafluoro boric acid anion, hexafluorophosphoric acid anion, bis trifluoromethyl sulfimide anion, perchloric acid anion, oxalic acid are cloudy
One or more in ion, trifluoromethane sulfonic acid anion, toluene sulfonic acide anion structure, play in the electrolyte dissolved salt work
With, be electrolyte increase ionic conductivity.
The lithium salts is lithium perchlorate, lithium hexafluoro phosphate, hexafluoroarsenate lithium, LiBF4, dioxalic acid lithium borate, difluoro
One kind in Lithium bis (oxalate) borate, trifluoromethyl sulfonic acid lithium, bis trifluoromethyl sulfimide lithium, for electrolyte lithium ion is provided；
Another object of the present invention is to a kind of preparation method of the ionic liquid compound all-solid polymer electrolyte is provided,
The preparation method of the ionic liquid compound all-solid polymer electrolyte is comprised the following steps：
Step one, lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
Step 2, weighs polymeric matrix, ionic liquid and lithium salts and is dissolved in solvent, stirs to formation homogeneous solution；
Step 3, solution is poured in Teflon mould, and room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum drying
24 hours, obtain composite solid polymer dielectric.
Further, the preparation method of the ionic liquid compound all-solid polymer electrolyte is comprised the following steps：
Step one, lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
Step 2, weighs polymeric matrix, lithium salts and is dissolved in solvent, stirs to formation homogeneous solution；
Step 3, above-mentioned solution is poured in Teflon mould, and room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum
It is dried 24 hours, obtains solid polymer electrolyte；
Step 4, above-mentioned solid polymer electrolyte is immersed in ionic liquid, immersion a period of time, 60 DEG C is placed in after taking-up very
Sky is dried 24h, obtains composite solid polymer dielectric.
Further, the solvent is dimethyl sulfoxide (DMSO), tetrahydrofuran, acetone, acetonitrile, DMF, diformazan
One kind in base sulfoxide, dichloromethane, chloroform；The solvent load is 2 ~ 15 times of polymer matrix weight.
Another object of the present invention is to provide a kind of ionic liquid compound all-solid polymer electrolyte manufacture
Lithium ion battery.
Further, the lithium ion battery is by positive electrode, full solid state polymer electrolyte and negative material composition；
The active material of the positive electrode includes LiFePO4, ferric metasilicate lithium, cobalt acid lithium, lithium nickelate, the mangaic acid of inorganic material
Lithium, lithium nickel cobalt dioxide and nickel ion doped binary material, cobalt nickel lithium manganate ternary material, and polymeric material free radical polyalcohol,
Conducting polymer, Organic polysulfur compound, many skeleton carbon-sulfur polymers, conjugation carbonyl polymerization thing；
The bonding agent of described positive electrode includes Kynoar, polytetrafluoroethylene (PTFE), sodium alginate, PEO, poly- second
Glycol, polyvinyl alcohol, carboxylic acid methyl sodium cellulosate coordinate butadiene-styrene rubber, polyacrylate；The binding agent accounts for positive electrode
1% ~ 20%wt；
The conductive additive of described positive electrode includes conductive black, Graphene, conductive acetylene, fullerene, CNT；Institute
The conductive additive stated accounts for 0% ~ 20%wt of positive electrode；
Described negative material includes lithium metal and its alloy, graphite and Graphene, carbon-silicon composite material, tin-based material.
Further, positive electrode, all-solid-state composite polymer electrolyte and negative material are sequentially placed into encapsulation to constitute entirely
Solid lithium ion battery.
Another object of the present invention is to provide a kind of ionic liquid compound all-solid polymer electrolyte manufacture
All-solid lithium-ion battery.
Another object of the present invention is to provide a kind of ionic liquid compound all-solid polymer electrolyte manufacture
Solid lithium battery
Another object of the present invention is to provide a kind of the complete solid of ionic liquid compound all-solid polymer electrolyte manufacture
State lithium-sulfur cell.
Ionic liquid compound all-solid polymer electrolyte that the present invention is provided and preparation method and application, ionic liquid
Due to there is high electrical conductivity, chemical, difficult volatilization good with electrochemical stability, not burning；By ionic liquid and poly- carbonic acid
The polymer such as ester, polyimides, polyamide, polyester, polyvinyl chloride, polysulfide, polyethers, polyphosphazene, polyurethane, polysulfones or its block
Copolymer or graft copolymer or atactic polymer are blended, and the composite polymer electrolyte of preparation can be provided simultaneously with ion
The good characteristic of both liquid and polymer, not only raw material are relatively inexpensive is easy to get, preparation process is simple, good mechanical performance,
Can have higher ionic conductivity and good electrochemical stability simultaneously.So, polymer is combined with ionic liquid,
A kind of new method of economical and efficient can not only be provided to prepare high conductivity polymer dielectric film, and polymerization can be widened
Range of application of the thing in terms of lithium ion battery, with important theoretical significance and practical value.
Full solid state polymer electrolyte in the present invention is using ionic liquid and polymeric matrix, lithium salts combination process system
It is standby.Comparatively speaking, prepared composite polymer electrolyte raw material are relatively inexpensive to be easy to get, preparation process is simple, while having
Excellent mechanical performance and higher electrical conductivity, safety and environmental protection.May be used on all-solid lithium-ion battery, solid lithium battery,
In all solid state lithium-sulfur cell and other high-performance lithium batteries.
Prepared by the all-solid-state composite polymer electrolyte of the present invention easy, and shaping is simple, and mechanical performance and heat endurance are good
Good, conductivity at room temperature is higher, and close 10-4S/cm（The room-temperature conductivity of polymer dielectric is relatively low, and only 10-7 S cm-1
And mechanical performance is poor）.This electrolyte and positive electrode（As cobalt acid lithium, LiMn2O4, LiFePO4, ferric metasilicate lithium,
Li4Ti5O12、Li2V2O5, it is lithium nickel cobalt dioxide, nickle cobalt lithium manganate, free radical polyalcohol, conducting polymer, Organic polysulfur compound, many
Skeleton carbon-sulfur polymer, conjugation carbonyl polymerization thing etc.）, negative material（The carbon-based material such as lithium and its alloy, graphite-like, antimony carbon are answered
Condensation material, silicon-carbon complex class material, tin-based material etc.）The all-solid lithium-ion battery safety and environmental protection of assembling, chemical property is good
It is good, and solid lithium battery, all solid state lithium-sulfur cell are can be applicable to, and in other high-performance lithium batteries.
Description of the drawings
Fig. 1 is ionic liquid compound all-solid polymer electrolyte lithium battery schematic diagram provided in an embodiment of the present invention
Fig. 2 is that the electrical conductivity temperature of the compound Merlon electrolyte of the intermediate ion liquid of embodiment provided in an embodiment of the present invention 1 is closed
System's figure.
Fig. 3 is the compound Merlon electrolyte heat endurance figure of the intermediate ion liquid of embodiment provided in an embodiment of the present invention 1.
Fig. 4 is the compound Merlon electrolyte electrochemical window of the intermediate ion liquid of embodiment provided in an embodiment of the present invention 1
Figure.
Fig. 5 is the electrical conductivity temperature of the intermediate ion liquid compound polyimide electrolyte of embodiment provided in an embodiment of the present invention 4
Degree graph of a relation.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
Ionic liquid compound all-solid polymer electrolyte provided in an embodiment of the present invention is by polymeric matrix, ionic liquid
With lithium salts composition.
The polymeric matrix includes Merlon, polyimides, polyamide, polyester, polyethers, polyphosphazene, polyurethane, poly-
It is sulfone, polyformaldehyde, polyacrylonitrile, polyvinyl chloride, polysulfide, Kynoar, polyphosphate, poly-（Methyl）Acrylate, polyether ester,
Polydioxolane, PPI, polytetrafluoroethylene (PTFE), polyhexafluoropropylene, containing heteroatomic polyethylene, containing heteroatomic poly- third
One or more in alkene, polysiloxanes etc. or their block copolymer or graft polymers or random copolymer.
Described ionic liquid includes that cation is the structures such as imidazole ring, pyridine ring, tri-n-butylamine and pyrrole ring, and anion is
Chlorion, tetrafluoro boric acid anion, hexafluorophosphoric acid anion, bis trifluoromethyl sulfimide anion, perchloric acid anion, grass
One or more in the structures such as acid anion, trifluoromethane sulfonic acid anion, toluene sulfonic acide anion, the ionic liquid
Addition for polymer matrix weight 0.1 ~ 80%.
The optional lithium perchlorate of the lithium salts, lithium hexafluoro phosphate, hexafluoroarsenate lithium, LiBF4, dioxalic acid lithium borate, two
One kind in fluorine Lithium bis (oxalate) borate, trifluoromethyl sulfonic acid lithium and bis trifluoromethyl sulfimide lithium, preferred bis trifluoromethyl sulphonyl
Imine lithium.It is 5 ~ 95% that the lithium salts accounts for the mass fraction of polymeric matrix.
The preparation method of ionic liquid compound all-solid polymer electrolyte provided in an embodiment of the present invention is solution cast
Method.
The preparation method of ionic liquid compound all-solid polymer electrolyte provided in an embodiment of the present invention includes following step
Suddenly：
1）Lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
2）Weigh a certain amount of polymeric matrix, ionic liquid and lithium salts to be dissolved in solvent, strong agitation is uniform molten to being formed
Liquid；
3）Above-mentioned solution is poured in Teflon mould, room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum drying 24
Hour, obtain composite solid polymer dielectric.
The preparation method of ionic liquid compound all-solid polymer electrolyte provided in an embodiment of the present invention also includes following
Step：
1）Lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
2）Weigh a certain amount of polymeric matrix, lithium salts to be dissolved in solvent, strong agitation is to forming homogeneous solution；
3）Above-mentioned solution is poured in Teflon mould, room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum drying 24
Hour, obtain solid polymer electrolyte；
4）Above-mentioned solid polymer electrolyte is immersed in ionic liquid, immersion a period of time, 60 DEG C of vacuum are placed in after taking-up and are done
Dry 24h, obtains composite solid polymer dielectric.
Solvent in the preparation method of the ionic liquid compound all-solid polymer electrolyte is dimethyl sulfoxide (DMSO), tetrahydrochysene
One kind in furans, acetone, acetonitrile, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), dichloromethane, chloroform.The solvent load
For 2 ~ 15 times of polymer matrix weight.It is preferred that tetrahydrofuran.
The application of the ionic liquid compound all-solid polymer electrolyte includes the polymer dielectric all solid state
Application in lithium ion battery, solid lithium battery, all solid state lithium-sulfur cell and other high-performance lithium batteries.
Application of the ionic liquid compound all-solid polymer electrolyte in lithium ion battery, further includes complete
Solid state lithium battery, the application in all solid state lithium-sulfur cell and in other high-performance lithium batteries.
The lithium battery is that, by positive electrode, above-mentioned full solid state polymer electrolyte and negative material are constituted.
The active material of described positive electrode includes LiFePO4, ferric metasilicate lithium, cobalt acid lithium, the nickel acid of inorganic material
Lithium, LiMn2O4, lithium nickel cobalt dioxide and nickel ion doped binary material, cobalt nickel lithium manganate ternary material etc., and polymeric material freedom
Based polyalcohol, conducting polymer, Organic polysulfur compound, many skeleton carbon-sulfur polymers, conjugation carbonyl polymerization thing etc..
The bonding agent of described positive electrode include Kynoar, polytetrafluoroethylene (PTFE), sodium alginate, PEO,
Polyethylene glycol, polyvinyl alcohol, carboxylic acid methyl sodium cellulosate coordinate butadiene-styrene rubber, polyacrylate etc..Described binding agent is accounted for
1% ~ 20%wt of positive electrode.
The conductive additive of described positive electrode includes conductive black, Graphene, conductive acetylene, fullerene, carbon nanometer
Pipe etc..Described conductive additive accounts for 0% ~ 20%wt of positive electrode.
Described negative material include the carbon-based material such as lithium metal and its alloy, graphite and Graphene, carbon-silicon composite material,
Tin-based material etc..
Ionic liquid compound all-solid polymer electrolyte provided in an embodiment of the present invention and preparation method and application, will
Positive electrode, above-mentioned all-solid-state composite polymer electrolyte, negative material is sequentially placed encapsulation and constitutes all solid state lithium ion electricity
Pond.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polytetramethylene carbonate diol 0.1g, LiBF4（LiBF4）
0.03g, tetrafluoro boric acid 1- butyl -3- methylimidazoles（MeImBF4）Ionic liquid 0.03g, adds 5ml tetrahydrofuran solutions, by force
Strong stirring forms homogeneous phase solution, and solution is poured in polytetrafluoroethylene (PTFE) grinding tool, and solvent volatilization 3h, is subsequently placed in 60 under room temperatureoC is true
Sky is dried 12h, obtains polymer dielectric.Heat decomposition temperature is 263.5oC, meets harsh temperature conditions and uses, electrostrictive polymer
The room-temperature conductivity of solution matter is 2.16 × 10-4S/cm.Positive electrode, polymer dielectric, negative material are sequentially overlapped and are placed in
In CR2016 battery cases, all-solid lithium-ion battery is formed.
Embodiment 2
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polytetramethylene carbonate diol 0.1g, bis trifluoromethyl sulphonyl is sub-
Amine lithium（LiTFSI）0.015g, bis trifluoromethyl sulfimide 1- butyl -3- methylimidazoles（MeImTFSI）Ionic liquid
0.03g, adds 5ml tetrahydrofuran solutions strong agitation to homogeneous phase solution, and solution is poured in polytetrafluoroethylene (PTFE) grinding tool, under room temperature
Solvent volatilization 3h, is subsequently placed in 60oC is vacuum dried 12h, obtains polymer dielectric.The room-temperature conductivity of polymer dielectric
For 4.35 × 10-5S/cm.Positive electrode, polymer dielectric, negative material are sequentially overlapped and are placed in CR2016 battery cases,
Form all-solid lithium-ion battery.
Embodiment 3
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polytetramethylene carbonate diol 0.1g, lithium hexafluoro phosphate 0.012g,
Hexafluorophosphoric acid 1- butyl -3- methylimidazoles（MeImPF6）Ionic liquid 0.03g, adds 5ml tetrahydrofuran solutions strong agitation extremely
Homogeneous phase solution, solution is poured in polytetrafluoroethylene (PTFE) grinding tool, and solvent volatilization 3h, is subsequently placed in 60 under room temperatureoC is vacuum dried 12h,
Obtain polymer dielectric.The room-temperature conductivity of polymer dielectric is 3.42 × 10-5S/cm.By positive electrode, electrostrictive polymer
Xie Zhi, negative material is sequentially overlapped and is placed in CR2016 battery cases, forms all-solid lithium-ion battery.
Embodiment 4
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polyimides 0.1g, bis-trifluoromethylsulfoandimide lithium
（LiTFSI）0.011g, bis trifluoromethyl sulfimide 1- butyl -3- methylimidazoles（MeImTFSI）Ionic liquid 0.03g, plus
Enter 5ml tetrahydrofuran solutions strong agitation to homogeneous phase solution, solution is poured in polytetrafluoroethylene (PTFE) grinding tool, solvent volatilization under room temperature
3h, is subsequently placed in 60oC is vacuum dried 12h, obtains polymer dielectric.The room-temperature conductivity of polymer dielectric be 4.53 ×
10-5S/cm.Positive electrode, polymer dielectric, negative material are sequentially overlapped and are placed in CR2016 battery cases, forms complete solid
State lithium ion battery.
Embodiment 5
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polyimides 0.1g, LiBF4（LiBF4）0.03g,
Tetrafluoro boric acid 1- butyl -3- methylimidazoles（MeImBF4）Ionic liquid 0.03g, adds 5ml tetrahydrofuran solutions strong agitation extremely
Homogeneous phase solution, solution is poured in polytetrafluoroethylene (PTFE) grinding tool, and solvent volatilization 3h, is subsequently placed in 60 under room temperatureoC is vacuum dried 12h,
Obtain polymer dielectric.The room-temperature conductivity of polymer dielectric is 1.04 × 10-4S/cm.By positive electrode, electrostrictive polymer
Xie Zhi, negative material is sequentially overlapped and is placed in CR2016 battery cases, forms all-solid lithium-ion battery.
Embodiment 6
By lithium salts in 80oIt is dried 24 hours in C vacuum drying ovens, weighs polyimides 0.1g, lithium hexafluoro phosphate 0.012g, hexafluoro phosphorus
Sour 1- butyl -3- methylimidazoles（MeImPF6）Ionic liquid 0.03g, adds 5ml tetrahydrofuran solutions strong agitation to mixing
Liquid, solution is poured in polytetrafluoroethylene (PTFE) grinding tool, and solvent volatilization 3h, is subsequently placed in 60 under room temperatureoC is vacuum dried 12h, obtains
Polymer dielectric.The room-temperature conductivity of polymer dielectric is 3.27 × 10-5S/cm.By positive electrode, polymer electrolytic
Matter, negative material is sequentially overlapped and is placed in CR2016 battery cases, forms all-solid lithium-ion battery.
The application effect of the present invention is explained in detail with reference to all-solid-state composite polymer electrolyte performance characterization.
Characterized using thermal behaviors of the DSC and TGA to composite polymer electrolyte, using ac impedance technology to compound
The electrical conductivity and interface performance of polymer dielectric is characterized.Using electricity of the linear sweep voltametry to composite polymer electrolyte
Chemical window is characterized.The transference number of ions of composite polymer electrolyte is measured using electric current steady state method.Using indigo plant
Electricity（LAND）Battery test system test full solid state polymer lithium ion battery cycle performance at different temperatures.
All-solid-state composite polymer lithium battery performance test is comprised the following steps：
1. the preparation of positive plate
By positive electrode, binding agent, conductive additive according to 80：10：After 10 mass ratio is well mixed, a certain amount of N is added dropwise,
N-2- methyl pyrrolidones（NMP）After grinding is uniform, by gained, material will be coated on aluminium foil, first 80 oCUnder the conditions of dry, then
In 120 oCDry under vacuum condition, roll-in, punching continues dry for standby after weighing, by size cutting.
2. the preparation of negative plate
By negative material, binding agent, conductive additive according to 80：10：After 10 mass ratio is well mixed, a certain amount of N is added dropwise,
N-2- methyl pyrrolidones（NMP）After grinding is uniform, by gained, material will be coated on Copper Foil, first 80oDry under the conditions of C,
Then at 120 oCDry under vacuum condition, roll-in, punching continues dry for standby after weighing, by size cutting.
3. battery assembling
Positive plate, described all-solid-state composite polymer electrolyte, negative plate are sequentially placed encapsulation and constitute all solid state lithium ion
Battery.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of ionic liquid compound all-solid polymer electrolyte, it is characterised in that the ionic liquid is combined all solid state poly-
Polymer electrolyte is made up of polymeric matrix, ionic liquid and lithium salts；
The addition of the ionic liquid is the 0.1 ~ 80% of polymer matrix weight；The lithium salts accounts for the quality of polymeric matrix
Fraction is 5 ~ 95%.
2. ionic liquid compound all-solid polymer electrolyte as claimed in claim 1, it is characterised in that the polymer matrix
Body include Merlon, polyimides, polyamide, polyester, polyethers, polyphosphazene, polyurethane, polysulfones, polyformaldehyde, polyacrylonitrile,
It is polyvinyl chloride, polysulfide, Kynoar, polyphosphate, polyacrylate, polyether ester, polydioxolane, PPI, poly-
Tetrafluoroethene, polyhexafluoropropylene, containing heteroatomic polyethylene, common containing heteroatomic polypropylene, polysiloxanes or their block
One or more in polymers or graft polymers or random copolymer；
Described ionic liquid include cation be imidazole ring, pyridine ring, tri-n-butylamine and pyrroles's ring structure, anion be chlorine from
Son, tetrafluoro boric acid anion, hexafluorophosphoric acid anion, bis trifluoromethyl sulfimide anion, perchloric acid anion, oxalic acid are cloudy
One or more in ion, trifluoromethane sulfonic acid anion, toluene sulfonic acide anion structure；
The lithium salts is lithium perchlorate, lithium hexafluoro phosphate, hexafluoroarsenate lithium, LiBF4, dioxalic acid lithium borate, difluoro oxalate
One kind in lithium borate, trifluoromethyl sulfonic acid lithium, bis trifluoromethyl sulfimide lithium.
3. a kind of preparation method of ionic liquid compound all-solid polymer electrolyte as claimed in claim 1, it is characterised in that
The preparation method of the ionic liquid compound all-solid polymer electrolyte is comprised the following steps：
Step one, lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
Step 2, weighs polymeric matrix, ionic liquid and lithium salts and is dissolved in solvent, stirs to formation homogeneous solution；
Step 3, solution is poured in Teflon mould, and room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum drying
24 hours, obtain composite solid polymer dielectric.
4. the preparation method of ionic liquid compound all-solid polymer electrolyte as claimed in claim 3, it is characterised in that institute
The preparation method for stating ionic liquid compound all-solid polymer electrolyte is comprised the following steps：
Step one, lithium salts is dried 24 hours in 80 DEG C of vacuum drying ovens；
Step 2, weighs polymeric matrix, lithium salts and is dissolved in solvent, stirs to formation homogeneous solution；
Step 3, above-mentioned solution is poured in Teflon mould, and room temperature volatilization is removed after most of solvent, 60 DEG C of vacuum
It is dried 24 hours, obtains solid polymer electrolyte；
Step 4, above-mentioned solid polymer electrolyte is immersed in ionic liquid, immersion a period of time, 60 DEG C is placed in after taking-up very
Sky is dried 24h, obtains composite solid polymer dielectric.
5. the preparation method of ionic liquid compound all-solid polymer electrolyte as claimed in claim 3, it is characterised in that institute
Solvent is stated for dimethyl sulfoxide (DMSO), tetrahydrofuran, acetone, acetonitrile, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), dichloromethane, chlorine
One kind in imitative；The solvent load is 2 ~ 15 times of polymer matrix weight.
6. a kind of lithium of the ionic liquid compound all-solid polymer electrolyte as described in any one of claim 1 or 2 manufacture from
Sub- battery.
7. lithium ion battery as claimed in claim 6, it is characterised in that the lithium ion battery is by positive electrode, Quan Gu
State polymer dielectric and negative material are constituted；
The active material of the positive electrode includes LiFePO4, ferric metasilicate lithium, cobalt acid lithium, lithium nickelate, the mangaic acid of inorganic material
Lithium, lithium nickel cobalt dioxide and nickel ion doped binary material, cobalt nickel lithium manganate ternary material, and polymeric material free radical polyalcohol,
Conducting polymer, Organic polysulfur compound, many skeleton carbon-sulfur polymers, conjugation carbonyl polymerization thing；
The bonding agent of described positive electrode includes Kynoar, polytetrafluoroethylene (PTFE), sodium alginate, PEO, poly- second
Glycol, polyvinyl alcohol, carboxylic acid methyl sodium cellulosate coordinate butadiene-styrene rubber, polyacrylate；The binding agent accounts for positive electrode
1% ~ 20%wt；
The conductive additive of described positive electrode includes conductive black, Graphene, conductive acetylene, fullerene, CNT；Institute
The conductive additive stated accounts for 0% ~ 20%wt of positive electrode；
Described negative material includes lithium metal and its alloy, graphite and Graphene, carbon-silicon composite material, tin-based material；
Positive electrode, all-solid-state composite polymer electrolyte and negative material are sequentially placed into encapsulation and constitute all solid state lithium ion electricity
Pond.
8. a kind of manufacture of the ionic liquid compound all-solid polymer electrolyte as described in any one of claim 1 or 2 is complete solid
State lithium ion battery.
9. a kind of manufacture of the ionic liquid compound all-solid polymer electrolyte as described in any one of claim 1 or 2 is complete solid
State lithium battery.
10. a kind of manufacture of the ionic liquid compound all-solid polymer electrolyte as described in any one of claim 1 or 2 is complete solid
State lithium-sulfur cell.
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