CN109802173A - A kind of three-phase organic/inorganic plural gel state polymer dielectric and preparation method thereof - Google Patents
A kind of three-phase organic/inorganic plural gel state polymer dielectric and preparation method thereof Download PDFInfo
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- CN109802173A CN109802173A CN201910068961.9A CN201910068961A CN109802173A CN 109802173 A CN109802173 A CN 109802173A CN 201910068961 A CN201910068961 A CN 201910068961A CN 109802173 A CN109802173 A CN 109802173A
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Abstract
The present invention relates to a kind of three-phase organic/inorganic plural gel state polymer dielectrics and preparation method thereof, which solve introduce the technical issues of PEO causes dielectric film mechanical properties decrease, it contains g-C3N4, PVDF-HFP and PEO, the pattern of g-C3N4 is in lamella and microspheroidal, g-C3N4 is distributed in PVDF-HFP and PEO system, and the quality of g-C3N4 accounts for the 0.1%~20% of the electrolyte gross mass.Invention also provides preparation methods.The present invention can be used for the preparation field of quasi- solid lithium ion battery.
Description
Technical field
The present invention relates to a kind of battery materials and preparation method thereof, specifically a kind of to be applied to quasi- solid lithium ion electricity
The three-phase organic/inorganic plural gel state polymer dielectric in pond and preparation method thereof.
Background technique
With popularizing for intelligent electronic device, the requirement for the shape, size of secondary cell is continuously improved；Meanwhile it is right
It is also continuously improved in the requirement of battery energy density and power density, bring safety problem also receives significant attention therewith.It is solidifying
Important component of the colloidal polymer electrolyte as quasi- solid lithium ion battery, for the safe and reliable of lithium ion battery
Decisive role is played in the performances such as property, recycling.
For organic/inorganic composite electrolyte, the addition of inorganic particle can lower the crystallinity of polymeric matrix, promote
Ion is realized along molecule segment and is migrated.But at room temperature, ion still difficulty migrates across electrolyte.If in polymer matrix
Liquid solvent is introduced in body, is formed gel polymer electrolyte, on the one hand can be guaranteed its ionic conductivity and organic electrolysis
Liquid phase is close, on the other hand, the absorption of electrolyte and its certain mechanical strength can be arrived and greatly improve safety.And it is inorganic
The dispersing uniformity of filler in the polymer affects the ionic conductivity and mechanical property of dielectric film.
It is although able to achieve pore-creating using PEO, while promoting ionic conductivity, but mechanical strength can reduce.Chen etc. exists
PEO is added in PVDF-HFP, has probed into PEO different additive amount and effect and subsequent infiltration electrolyte institute is generated for hole
Obtain ionic conductivity [the Liquan Chen et al.Journal of Power Sources 157 of dielectric film
(2006)501-506]。
Summary of the invention
The present invention be exactly in order to solve introduce PEO cause dielectric film mechanical properties decrease the technical issues of, meanwhile, guarantee
Added inorganic filler in a polymer matrix evenly dispersed, the present invention have chosen a kind of preparation method is simple, density is small,
The stable two-dimensional material of physicochemical properties, g-C3N4 are introduced into PVDF-HFP and PEO, obtain a kind of three-phase it is organic/
Inorganic compounding gel state electrolyte.
For this purpose, the present invention provides a kind of three-phase organic/inorganic plural gel state polymer dielectric, containing g-C3N4,
The pattern of PVDF-HFP and PEO, the g-C3N4 are in lamella and microspheroidal, and the g-C3N4 is distributed in PVDF-HFP and PEO body
In system, the quality of the g-C3N4 accounts for the 0.1%~20% of the electrolyte gross mass.
Preferably, the quality of PVDF-HFP accounts for the electrolyte gross mass 10%~95%, and the quality Zhan of the PEO is total
Quality 5%~90%.
Preferably, it is 130000 that PEO relative molecular weight Mn, which is 300000~1000000, PVDF-HFP relative molecular weight Mn,.
Preferably, for lamella g-C3N4 having a size of 600nm*600nm, microballoon g-C3N4 diameter is 1 μm.
Present invention simultaneously provides a kind of three-phase organic/inorganic plural gel state method for preparing polymer electrolytes, packets
It includes following steps: (1) by g-C3N4 ultrasonic disperse in different solvents, the g-C3N4 dispersion of different quality volumetric concentration is made
Liquid；(2) substance obtained in the step (1) is added in the solution of PVDF-HFP and PEO；(3) by institute in the step (2)
It obtains substance and film is made；(4) film will be made in the step (3) and be transferred to glove box infiltration electrolyte to get gel state is arrived
Polymer dielectric.
Preferably, the solvent selection in step (1) is n,N-Dimethylformamide, isopropanol, deionized water, ethyl alcohol one kind
Or multiple combinations；Ultrasonic time 1-12 hours；G-C3N4 dispersion liquid mass-volume concentration 0.5mg/ml~5mg/ml.
Preferably, in step (3), using solution casting method, mixed liquor is cast on polyfluortetraethylene plate, is dried molten
Agent 40-80 DEG C, is heat-treated 4-24 hours in vacuum drying oven, film is made.
Preferably, electrolyte contains electrolyte lithium salts, electrolyte solvent and ethers in step (4)；The electrolyte lithium salts
For lithium perchlorate, lithium hexafluoro phosphate, bis- (flutolanil) imine lithiums, one or more groups of bis- (trifluoromethanesulfonamide) imine lithiums
It closes.
Preferably, electrolyte solvent is one of dimethyl carbonate, methyl ethyl carbonate, vinyl carbonate or a variety of groups
It closes.
Preferably, ethers is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and tetrem two
One of alcohol dimethyl ether is a variety of.
The invention has the advantages that lamella and microspheroidal g-C3N4 are introduced into PVDF-HFP+PEO system by the present invention,
By reducing polymeric matrix crystallinity, improves hole generating state, improve the mechanical property and electrochemistry of dielectric film
Energy.(1) simplest one kind that the preparation method of g-C3N4 is chosen in the present invention, and microspheroidal g-C3N4 disperses and removes to it
Advantageously at more lamella；(2) electrolyte thin membrane preparation method provided by the invention is simple, using solution casting method, utilizes
It is separated into hole, step is simple to operation；(3) addition of g-C3N4 has the mechanical property of gel polymer electrolyte bright
It is aobvious to be promoted, while the crystallinity of polymeric matrix can be reduced to a certain extent；And the generation of hole is for electrolyte
More preferably, ontology impedance substantially reduces adsorption effect, and ionic conductivity improves.
Detailed description of the invention
Fig. 1 is the g-C3N4XRD curve of 2 two kinds of patterns of embodiment 1 and embodiment；
Fig. 2 is that microspheroidal g-C3N4TEM schemes in embodiment 2；
Fig. 3 is obtained dielectric film surface SEM figure in embodiment 3；
Fig. 4 is dielectric film ontology impedance spectra in embodiment 2,4,5.
Specific embodiment
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 real
It applies content described in example and is merely to illustrate the present invention, without this hair described in claims should will not be limited
It is bright.
Embodiment 1
(1) 1g urea powder is taken, grinds in alms bowl and mills 10-15 minutes, until without bulk particle.It pours into crucible, in Muffle furnace
Middle heat treatment.3 DEG C/min of heating rate, until 550 DEG C, keep the temperature 4 hours.Obtain the g-C3N4 of lamella accumulation.
(2) by g-C3N4 obtained by (1), 60mg is taken, 30ml isopropanol is added, ultrasound 8 hours obtains g-C3N4 white suspension
Dispersion liquid.
(3) 0.8g PVDF-HFP, 0.2g PEO are taken, dispersion liquid 2.5ml in (2) is added, adds 8ml DMF, 60 DEG C of water
Bath stirring 24 hours.It is more than half to solvent volatilization by solution-cast on polyfluortetraethylene plate, 80 DEG C of vacuum drying oven are transferred to, is protected
Temperature 12 hours.Obtain film, about 100 μm of film thickness.
(4) film is transferred to glove box, impregnating electrolyte, (electrolyte is that lithium hexafluoro phosphate mixes dimethyl carbonate, carbon
The mixed solution of sour methyl ethyl ester and vinyl carbonate, mass ratio are dimethyl carbonate: methyl ethyl carbonate: vinyl carbonate=1:
1:1, concentration 1M) 10 seconds.Final gained is gel polymer electrolyte.
Embodiment 2
(1) 0.378g melamine powder, 0.387g cyanuric acid powder are taken, heating stirring is dissolved in dimethyl sulfoxide respectively
In, until solution is clarified.Two glasss of solution are mixed, white precipitate is obtained, are filtered, it is small that white precipitate is placed in 80 DEG C of baking ovens 24
When.It pours into crucible, is heat-treated in retort.Argon atmosphere, 3 DEG C/min of heating rate, until 550 DEG C, keep the temperature 4 hours.I.e.
Obtain the g-C3N4 of lamella accumulation.
(2) by g-C3N4 obtained by (1), 60mg is taken, 30ml isopropanol is added, it is faint yellow outstanding to obtain g-C3N4 for ultrasound 8 hours
Floating dispersion liquid.
(3) it takes 0.85g PVDF-HFP, 0.15g PEO, dispersion liquid 2.5ml in (2) is added, add 8ml DMF, 60 DEG C
Stirring in water bath 24 hours.It is more than half to solvent volatilization by solution-cast on polyfluortetraethylene plate, 80 DEG C of vacuum drying oven are transferred to,
Heat preservation 12 hours.Obtain film, about 100 μm of film thickness.
(4) film is transferred to glove box, impregnating electrolyte, (electrolyte is that lithium hexafluoro phosphate mixes dimethyl carbonate, carbon
The mixed solution of sour methyl ethyl ester and vinyl carbonate, mass ratio are dimethyl carbonate: methyl ethyl carbonate: vinyl carbonate=1:
1:1, concentration 1M) 10 seconds.Final gained is gel polymer electrolyte.
Embodiment 3
(1) 0.378g melamine powder, 0.387g cyanuric acid powder are taken, heating stirring is dissolved in dimethyl sulfoxide respectively
In, until solution is clarified.Two glasss of solution are mixed, white precipitate is obtained, are filtered, it is small that white precipitate is placed in 80 DEG C of baking ovens 24
When.It pours into crucible, is heat-treated in retort.Argon atmosphere, 3 DEG C/min of heating rate, until 550 DEG C, keep the temperature 4 hours.I.e.
Obtain the g-C3N4 of lamella accumulation.
(2) by g-C3N4 obtained by (1), 60mg is taken, 30ml DMF is added, ultrasound 8 hours obtains the faint yellow suspension of g-C3N4
Dispersion liquid.
(3) it takes 0.75g PVDF-HFP, 0.25g PEO, dispersion liquid 2.5ml in (2) is added, add 8ml DMF, 60 DEG C
Stirring in water bath 24 hours.It is more than half to solvent volatilization by solution-cast on polyfluortetraethylene plate, 80 DEG C of vacuum drying oven are transferred to,
Heat preservation 12 hours.Obtain film, about 100 μm of film thickness.
(4) film is transferred to glove box, impregnating electrolyte, (electrolyte is that lithium hexafluoro phosphate mixes dimethyl carbonate, carbon
The mixed solution of sour methyl ethyl ester and vinyl carbonate, mass ratio are dimethyl carbonate: methyl ethyl carbonate: vinyl carbonate=1:
1:1, concentration 1M) 10 seconds.Final gained is gel polymer electrolyte.
Embodiment 4
(1) 0.378g melamine powder, 0.387g cyanuric acid powder are taken, heating stirring is dissolved in dimethyl sulfoxide respectively
In, until solution is clarified.Two glasss of solution are mixed, white precipitate is obtained, are filtered, it is small that white precipitate is placed in 80 DEG C of baking ovens 24
When.It pours into crucible, is heat-treated in retort.Argon atmosphere, 3 DEG C/min of heating rate, until 550 DEG C, keep the temperature 4 hours.I.e.
Obtain the g-C3N4 of lamella accumulation.
(2) by g-C3N4 obtained by (1), 60mg is taken, 30ml DMF is added, ultrasound 8 hours obtains the faint yellow suspension of g-C3N4
Dispersion liquid.
(3) 0.7g PVDF-HFP, 0.3g PEO are taken, dispersion liquid 2.5ml in (2) is added, adds 8ml DMF, 60 DEG C of water
Bath stirring 24 hours.It is more than half to solvent volatilization by solution-cast on polyfluortetraethylene plate, 80 DEG C of vacuum drying oven are transferred to, is protected
Temperature 12 hours.Obtain film, about 100 μm of film thickness.
(4) film is transferred to glove box, impregnating electrolyte, (electrolyte is that lithium hexafluoro phosphate mixes dimethyl carbonate, carbon
The mixed solution of sour methyl ethyl ester and vinyl carbonate, mass ratio are dimethyl carbonate: methyl ethyl carbonate: vinyl carbonate=1:
1:1, concentration 1M) 10 seconds.Final gained is gel polymer electrolyte.
Embodiment 5
(1) 0.378g melamine powder, 0.387g cyanuric acid powder are taken, heating stirring is dissolved in dimethyl sulfoxide respectively
In, until solution is clarified.Two glasss of solution are mixed, white precipitate is obtained, are filtered, it is small that white precipitate is placed in 80 DEG C of baking ovens 24
When.It pours into crucible, is heat-treated in retort.Argon atmosphere, 3 DEG C/min of heating rate, until 550 DEG C, keep the temperature 4 hours.I.e.
Obtain the g-C3N4 of lamella accumulation.
(2) by g-C3N4 obtained by (1), 60mg is taken, 30ml DMF is added, ultrasound 8 hours obtains the faint yellow suspension of g-C3N4
Dispersion liquid.
(3) 1g PVDF-HFP, 0g PEO are taken, dispersion liquid 2.5ml in (2) is added, adds 8ml DMF, 60 DEG C of water-baths
Stirring 24 hours.It is more than half to solvent volatilization by solution-cast on polyfluortetraethylene plate, 80 DEG C of vacuum drying oven are transferred to, heat preservation
12 hours.Obtain film, about 100 μm of film thickness.
(4) film is transferred to glove box, impregnating electrolyte, (electrolyte is that lithium hexafluoro phosphate mixes dimethyl carbonate, carbon
The mixed solution of sour methyl ethyl ester and vinyl carbonate, mass ratio are dimethyl carbonate: methyl ethyl carbonate: vinyl carbonate=1:
1:1, concentration 1M) 10 seconds.Final gained is gel polymer electrolyte.
Claims (10)
1. a kind of three-phase organic/inorganic plural gel state polymer dielectric, characterized in that it contains g-C3N4, PVDF-HFP
And the pattern of PEO, the g-C3N4 are in lamella and microspheroidal, the g-C3N4 is distributed in PVDF-HFP and PEO system, described
The quality of g-C3N4 accounts for the 0.1%~20% of the electrolyte gross mass.
2. three-phase organic/inorganic plural gel state polymer dielectric according to claim 1, it is characterised in that described
The quality of PVDF-HFP accounts for the electrolyte gross mass 10%~95%, and the quality of the PEO accounts for the electrolyte gross mass 5%
~90%.
3. three-phase organic/inorganic plural gel state polymer dielectric according to claim 1, it is characterised in that described
PEO relative molecular weight Mn is that 300000~1000000, PVDF-HFP relative molecular weight Mn is 130000.
4. three-phase organic/inorganic plural gel state polymer dielectric according to claim 1, it is characterised in that described
Layer g-C3N4 is lamella accumulation, and having a size of 600nm*600nm, microballoon g-C3N4 diameter is 1 μm.
5. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes as described in claim 1, it is characterized in that
Include the following steps:
(1) by g-C3N4 ultrasonic disperse in different solvents, the g-C3N4 dispersion liquid of different quality volumetric concentration is made；
(2) substance obtained in the step (1) is added in the solution of PVDF-HFP and PEO；
(3) film is made in obtained material in the step (2)；
(4) film will be made in the step (3) and be transferred to glove box infiltration electrolyte to get gel polymer electrolysis is arrived
Matter.
6. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes according to claim 5, feature
It is that solvent selection in the step (1) is n,N-Dimethylformamide, isopropanol, deionized water, ethyl alcohol is a kind of or more
Kind combination；Ultrasonic time 1-12 hours；G-C3N4 dispersion liquid mass-volume concentration 0.5mg/ml~5mg/ml.
7. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes according to claim 5, feature
It is in the step (3), using solution casting method, mixed liquor is cast on polyfluortetraethylene plate, dry out solvent, in vacuum
In baking oven, 40-80 DEG C, it is heat-treated 4-24 hours, film is made.
8. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes according to claim 5, feature
It is in the step (4) that electrolyte contains electrolyte lithium salts, electrolyte solvent and ethers；The electrolyte lithium salts is perchloric acid
One or more combinations of lithium, lithium hexafluoro phosphate, bis- (flutolanil) imine lithiums, bis- (trifluoromethanesulfonamide) imine lithiums.
9. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes according to claim 8, feature
It is that the electrolyte solvent is one of dimethyl carbonate, methyl ethyl carbonate, vinyl carbonate or multiple combinations.
10. three-phase organic/inorganic plural gel state method for preparing polymer electrolytes according to claim 8, special
Sign is that the ethers is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and tetraethylene glycol two
One of methyl ether is a variety of.
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| CN111073184A (en) * | 2019-12-04 | 2020-04-28 | 北京理工大学 | Gel electrolyte film for secondary battery, preparation and application thereof |
| CN111313083A (en) * | 2020-03-13 | 2020-06-19 | 东华大学 | Composite solid electrolyte film and preparation and application thereof |
| CN111354972A (en) * | 2020-02-06 | 2020-06-30 | 华南理工大学 | Composite solid electrolyte material and preparation method and application thereof |
| CN111952673A (en) * | 2020-08-20 | 2020-11-17 | 陕西科技大学 | High-performance all-solid-state lithium battery and preparation method thereof |
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| CN112117487A (en) * | 2019-06-20 | 2020-12-22 | 新奥科技发展有限公司 | Electrolyte material, preparation method thereof, solid electrolyte and battery |
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| CN112117487A (en) * | 2019-06-20 | 2020-12-22 | 新奥科技发展有限公司 | Electrolyte material, preparation method thereof, solid electrolyte and battery |
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| CN112542611A (en) * | 2019-09-20 | 2021-03-23 | 北京石墨烯研究院 | Composition for gel electrolyte, flexible battery and preparation method thereof |
| CN111073184A (en) * | 2019-12-04 | 2020-04-28 | 北京理工大学 | Gel electrolyte film for secondary battery, preparation and application thereof |
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| CN111354972B (en) * | 2020-02-06 | 2021-06-25 | 华南理工大学 | Composite solid electrolyte material and preparation method and application thereof |
| CN111313083A (en) * | 2020-03-13 | 2020-06-19 | 东华大学 | Composite solid electrolyte film and preparation and application thereof |
| CN111313083B (en) * | 2020-03-13 | 2023-02-28 | 东华大学 | Composite solid electrolyte film and preparation and application thereof |
| CN111952673A (en) * | 2020-08-20 | 2020-11-17 | 陕西科技大学 | High-performance all-solid-state lithium battery and preparation method thereof |
| CN111952674A (en) * | 2020-08-20 | 2020-11-17 | 陕西科技大学 | Fluorine-doped carbon nitride-polymer composite solid electrolyte and preparation method and application thereof |
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