CN103903871A - Electrochemical power supply diaphragm, manufacturing method thereof, electrochemical battery or capacitor - Google Patents
Electrochemical power supply diaphragm, manufacturing method thereof, electrochemical battery or capacitor Download PDFInfo
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- CN103903871A CN103903871A CN201210586822.3A CN201210586822A CN103903871A CN 103903871 A CN103903871 A CN 103903871A CN 201210586822 A CN201210586822 A CN 201210586822A CN 103903871 A CN103903871 A CN 103903871A
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides an electrochemical power supply diaphragm and a manufacturing method thereof. The method includes the steps that polyvinylidene fluoride-hexafluoropropylene is dissolved in acetone to prepare a polyvinylidene fluoride-hexafluoropropylene acetone solution with the mass concentration of 5-20%, then deionized water is added into the solution, and the mixture is uniformly stirred to obtain emulsion; the mass content of the deionized water in the emulsion is 1-10%; organic short fibers are added into the emulsion, and the mixture is uniformly mixed to obtain mixed emulsion; the obtained mixed emulsion is coated on a clean glass substrate, the glass substrate is removed after the mixed emulsion is dried, and accordingly the electrochemical power supply diaphragm is obtained. The organic short fibers are one or more of PET fibers, PAN fibers and aramid fibers. The electrochemical power supply diaphragm is proper in aperture and good in heat resistance and safety, and safety of an electrochemical battery or a capacitor can be effectively improved. The invention further provides the electrochemical battery or the capacitor using the diaphragm.
Description
Technical field
The present invention relates to electrochemical field, particularly relate to a kind of electrochemical power source barrier film and preparation method thereof.The invention still further relates to a kind of electrochemical cell or capacitor.
Background technology
Along with the development of human being's production power, increasing running car is in city, streets and lanes, rural.Popularizing to people's life of automobile brings great convenience.But incident problem is also more and more serious.The consumption of the non-renewable energy resources such as oil is constantly accelerated, and the impact that the discharge of vehicle exhaust causes to environment also constantly expands.At present, people are in order to address these problems proposition Development of EV, to replacing orthodox car.And whether key is wherein to have energy density, power density enough large, cycle life long enough, safe and reliable electrokinetic cell replace internal combustion engine.And the key that determines electrokinetic cell fail safe is barrier film wherein, its main function is that isolated both positive and negative polarity is to prevent the problem such as battery self discharging and the two poles of the earth short circuit.
The barrier film that lithium ion battery generally adopts is at present porous polyolefin barrier film.But this barrier film is not only poor to electrolytical wettability, and heat resisting temperature is on the low side.For improving the fail safe of lithium ion battery and ultracapacitor, just must improve the thermal endurance of barrier film.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of electrochemical power source barrier film and preparation method thereof, the method is using Kynoar-hexafluoropropylene as host material, and add organic short fiber, gained electrochemical power source membrane pore size is applicable to, heat resistance is good, safe, thus the fail safe that can effectively improve electrochemical cell or capacitor.The present invention is corresponding a kind of electrochemical cell or the capacitor of providing also.
First aspect, the invention provides a kind of preparation method of electrochemical power source barrier film, comprises the following steps:
Kynoar-hexafluoropropylene is dissolved in in acetone, to be mixed with mass concentration be Kynoar-hexafluoropropylene acetone soln of 5 ~ 20%, then adds deionized water in above-mentioned solution, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 1 ~ 10%;
In above-mentioned emulsion, add organic short fiber, after mixing, obtain mixed emulsion;
Gained mixed emulsion is coated on clean glass substrate, after oven dry, removes described glass substrate, obtain electrochemical power source barrier film;
Wherein, in described Kynoar-hexafluoropropylene, the mass content of described hexafluoropropylene is 1 ~ 10%; Described organic short fiber is one or more in PET fiber, PAN fiber and aramid fiber.
Preferably, the mass concentration of described Kynoar-hexafluoropropylene acetone soln is 8 ~ 12%.
The polymer that the random copolymer (PVDF-HFP) of vinylidene and hexafluoropropylene is partially crystallizable, owing to adding the copolymerization effect of hexafluoropropylene to make its degree of crystallinity lower, the easier swelling electrolytic liquid of its pars amorpha and improve conductance, and crystalline portion makes barrier film have certain mechanical strength, the mass content of hexafluoropropylene need be controlled at OK range.
Preferably, in described Kynoar-hexafluoropropylene, the mass content of described hexafluoropropylene is 4 ~ 8%.
Kynoar-hexafluoropropylene (PVDF-HFP) is dissolved in acetone solvent, then adds non-solvent deionized water, stir and obtain the emulsion of mixed system.In emulsion, the content of deionized water directly affects porosity and the pore size of gained electrochemical power source barrier film, thereby finally affects air penetrability and the conductance of barrier film.
Preferably, in described emulsion, the mass content of deionized water is 1 ~ 6%.
In order to improve the hot strength of electrochemical power source barrier film, in barrier film preparation process, add organic short fiber, organic short fiber can be one or more in PET fiber, PAN fiber and aramid fiber.These organic short fibers have very strong tensile property, good dispersion property, and therefore it adds the mechanical property that can strengthen electrochemical power source barrier film, thereby improves the safety in utilization of barrier film.
Preferably, the diameter of described organic short fiber is 1 ~ 10 micron, and length is 1 ~ 5 centimetre.
The mixed emulsion that has added organic short fiber is coated on clean glass substrate, after oven dry, removes glass substrate, obtain electrochemical power source barrier film.
The mode of described coating is not done particular restriction.Preferably, the mode of described coating comprises blade coating or spraying.
Preferably, described drying operation carries out under air or vacuum condition, and bake out temperature is 40 ~ 100 ℃.More preferably, described bake out temperature is 60 ~ 80 ℃.
Preferably, drying time is 6 ~ 12 hours.
Above-mentioned gained electrochemical power source barrier film, in its host material Kynoar-hexafluoropropylene, Kynoar has high-melting-point, therefore makes barrier film have very high heat resisting temperature; In preparation process, can effectively control pore opening (aperture) and how many (porosity) of barrier film simultaneously by the addition of adjusting deionized water, thereby regulate air penetrability and the conductance of barrier film; In addition, also add organic short fiber in preparation process, thereby improved well the hot strength of electrochemical power source barrier film, improved the safety in utilization of barrier film, this membrane pore size is applicable to, and is applicable to lithium ion battery and ultracapacitor.
Second aspect, the invention provides a kind of electrochemical power source barrier film being prepared by above-mentioned preparation method.The porosity of this electrochemical power source barrier film is 35 ~ 50%, and average pore size is 20 ~ 100nm, and thickness is 20 ~ 30 μ m.
The third aspect, the invention provides a kind of electrochemical cell or capacitor, the described electrochemical power source barrier film that the barrier film of this electrochemical cell or capacitor adopts second aspect present invention to provide.
Electrochemical power source barrier film provided by the invention and preparation method thereof, has following beneficial effect:
(1) electrochemical power source barrier film of the present invention, using dystectic Kynoar-hexafluoropropylene as host material, makes barrier film have very high heat resisting temperature; In preparation process, can effectively control aperture and the porosity of barrier film simultaneously by the addition of adjusting deionized water, thereby regulate air penetrability and the conductance of barrier film; In addition, also add organic short fiber in preparation process, thereby improved well the hot strength of electrochemical power source barrier film, improved the safety in utilization of barrier film, this barrier film is applicable to lithium ion battery and ultracapacitor;
(2) preparation method of electrochemical power source barrier film of the present invention is simply effective, and cost is low, is applicable to large-scale production.
Accompanying drawing explanation
The cycle performance resolution chart of the lithium ion battery that Fig. 1 provides for the embodiment of the present invention 5.
Embodiment
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment 1
A preparation method for electrochemical power source barrier film, comprises the following steps:
(1) PVDF-HFP that is 1% by the mass content of hexafluoropropylene HFP joins in acetone, stirs, and is mixed with PVDF-HFP mass concentration and is 10% PVDF-HFP acetone soln;
(2) in above-mentioned solution, add deionized water, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 4%;
(3) be 2 microns to adding diameter in above-mentioned emulsion, the PET fiber of long 3 centimetres, and after being uniformly mixed, obtain mixed emulsion;
(4) gained mixed emulsion is sprayed on clean glass substrate, the baking oven that is placed in 60 ℃ is dried 8 hours, removes described glass substrate, and obtaining thickness is the electrochemical power source barrier film of 20 μ m.
The electrochemical power source barrier film that the present embodiment is made carries out porosity, aperture and air penetrability and measures.Wherein, porosity and aperture adopt porosity instrument to measure, and air penetrability is measured by air penetrability measuring instrument.After measured, the porosity of the present embodiment gained electrochemical power source barrier film is 40%, and average pore size is 50nm, and air penetrability is 150s/100cc.Separately record the broken film temperature of electrochemical power source barrier film higher than 150 ℃.
Embodiment 2
A preparation method for electrochemical power source barrier film, comprises the following steps:
(1) PVDF-HFP that is 4% by the mass content of hexafluoropropylene HFP joins in acetone, stirs, and is mixed with PVDF-HFP mass concentration and is 20% PVDF-HFP acetone soln;
(2) in above-mentioned solution, add deionized water, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 10%;
(3) be 1 micron to adding diameter in above-mentioned emulsion, the aramid fiber of long 5 centimetres, and after being uniformly mixed, obtain mixed emulsion;
(4) by gained mixed emulsion blade coating on clean glass substrate, be placed in dry 10 hours of the baking oven of 80 ℃, remove described glass substrate, obtaining thickness is the electrochemical power source barrier film of 30 μ m.
The electrochemical power source barrier film that the present embodiment is made carries out porosity, aperture and air penetrability and measures.Wherein, porosity and aperture adopt porosity instrument to measure, and air penetrability is measured by air penetrability measuring instrument.After measured, the porosity of the present embodiment gained electrochemical power source barrier film is 50%, and average pore size is 100nm, and air penetrability is 200s/100cc.Separately record the broken film temperature of electrochemical power source barrier film higher than 150 ℃.
Embodiment 3
A preparation method for electrochemical power source barrier film, comprises the following steps:
(1) PVDF-HFP that is 10% by the mass content of hexafluoropropylene HFP joins in acetone, stirs, and is mixed with PVDF-HFP mass concentration and is 8% PVDF-HFP acetone soln;
(2) in above-mentioned solution, add deionized water, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 1%;
(3) be 10 microns to adding diameter in above-mentioned emulsion, the PAN fiber of long 1 centimetre, and after being uniformly mixed, obtain mixed emulsion;
(4) by gained mixed emulsion blade coating on clean glass substrate, be placed in dry 6 hours of the baking oven of 100 ℃, remove described glass substrate, obtaining thickness is the electrochemical power source barrier film of 30 μ m.
The electrochemical power source barrier film that the present embodiment is made carries out porosity, aperture and air penetrability and measures.Wherein, porosity and aperture adopt porosity instrument to measure, and air penetrability is measured by air penetrability measuring instrument.After measured, the porosity of the present embodiment gained electrochemical power source barrier film is 35%, and average pore size is 20nm, and air penetrability is 800s/100cc.Separately record the broken film temperature of electrochemical power source barrier film higher than 150 ℃.
Embodiment 4
A preparation method for electrochemical power source barrier film, comprises the following steps:
(1) PVDF-HFP that is 8% by the mass content of hexafluoropropylene HFP joins in acetone, stirs, and is mixed with PVDF-HFP mass concentration and is 12% PVDF-HFP acetone soln;
(2) in above-mentioned solution, add deionized water, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 6%;
(3) be 5 microns to adding diameter in above-mentioned emulsion, the PAN fiber of long 3 centimetres, and after being uniformly mixed, obtain mixed emulsion;
(4) by gained mixed emulsion blade coating on clean glass substrate, be placed in dry 12 hours of the baking oven of 40 ℃, remove described glass substrate, obtaining thickness is the electrochemical power source barrier film of 25 μ m.
The electrochemical power source barrier film that the present embodiment is made carries out porosity, aperture and air penetrability and measures.Wherein, porosity and aperture adopt porosity instrument to measure, and air penetrability is measured by air penetrability measuring instrument.After measured, the porosity of the present embodiment gained electrochemical power source barrier film is 45%, and average pore size is 60nm, and air penetrability is 500s/100cc.Separately record the broken film temperature of electrochemical power source barrier film higher than 150 ℃.
Embodiment 5
A kind of electrochemical cell, its barrier film adopts the prepared electrochemical power source barrier film of embodiment 1, and concrete preparation process is:
Take 9.2g LiFePO4,0.5g conductive black Super P and 0.3g PVDF, and add 20g NMP, fully stir and make it to become the slurry mixing.Then by its blade coating in the aluminum foil current collector of cleaning through ethanol, under the vacuum of 0.01MPa, 80 ℃ are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into positive plate.Equally, take 4.6g graphite, 0.25g conductive black Super P and 0.15g PVDF, and add 10g NMP, fully stir and make it to become the slurry mixing, then by its blade coating on the Copper Foil collector cleaning through ethanol, be pressed into negative plate.
By above-mentioned positive plate, the prepared electrochemical power source barrier film of embodiment 1, above-mentioned negative plate in order stack of laminations dress up battery core, use again battery housing seal battery core, toward the ethylene carbonate electrolysis of solutions liquid that injects the lithium hexafluoro phosphate of 1mol/L in battery container, sealing liquid injection port, obtains lithium ion battery.
Meanwhile, adopt conventional pp barrier film (single-layer polypropylene microporous barrier) to obtain control cell according to above-mentioned identical operation assembling.
With CHI660A electrochemical workstation, the lithium ion battery assembling in the present embodiment is put into the high-temperature cabinet constant temperature 2h of 70 ℃ ± 2 ℃, then carry out constant current charge-discharge test with 1C electric current, its result as shown in Figure 1, as can be seen from Figure 1, the initial discharge capacity of this lithium ion battery is 896mAh, after 25 circulations, discharge capacity slightly declines, there is not bubbling in battery, the fail safe that barrier film is described is good, and adopt control cell prepared by conventional pp barrier film after same test process, battery generation bubbling, battery gross distortion.The cycle performance resolution chart of the lithium ion battery that Fig. 1 provides for the present embodiment.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a preparation method for electrochemical power source barrier film, is characterized in that, comprises the following steps:
Kynoar-hexafluoropropylene is dissolved in in acetone, to be mixed with mass concentration be Kynoar-hexafluoropropylene acetone soln of 5 ~ 20%, then adds deionized water in above-mentioned solution, after stirring, obtain emulsion; In described emulsion, the mass content of deionized water is 1 ~ 10%;
In above-mentioned emulsion, add organic short fiber, after mixing, obtain mixed emulsion;
Gained mixed emulsion is coated on clean glass substrate, after oven dry, removes described glass substrate, obtain electrochemical power source barrier film;
Wherein, in described Kynoar-hexafluoropropylene, the mass content of described hexafluoropropylene is 1 ~ 10%; Described organic short fiber is one or more in PET fiber, PAN fiber and aramid fiber.
2. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, the mass concentration of described Kynoar-hexafluoropropylene acetone soln is 8 ~ 12%.
3. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, in described emulsion, the mass content of deionized water is 1 ~ 6%.
4. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, in described Kynoar-hexafluoropropylene, the mass content of described hexafluoropropylene is 4 ~ 8%.
5. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, the diameter of described organic short fiber is 1 ~ 10 micron, and length is 1 ~ 5 centimetre.
6. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, the mode of described coating comprises blade coating or spraying.
7. the preparation method of electrochemical power source barrier film as claimed in claim 1, is characterized in that, described drying operation carries out under air or vacuum condition, and bake out temperature is 40 ~ 100 ℃.
8. the preparation method of electrochemical power source barrier film as claimed in claim 7, is characterized in that, described bake out temperature is 60 ~ 80 ℃.
9. the electrochemical power source barrier film being made by the arbitrary described preparation method of claim 1 to 8, is characterized in that, the porosity of described electrochemical power source barrier film is 35 ~ 50%, and average pore size is 20 ~ 100nm, and thickness is 20 ~ 30 μ m.
10. electrochemical cell or a capacitor, is characterized in that, the barrier film of this electrochemical cell or capacitor adopts electrochemical power source barrier film claimed in claim 9.
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Cited By (7)
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| CN104282869A (en) * | 2014-09-12 | 2015-01-14 | 广东工业大学 | Preparation method of coating type organic/inorganic composite membrane of lithium battery |
| CN109285985A (en) * | 2017-07-20 | 2019-01-29 | 天津凯普瑞特新能源科技有限公司 | A kind of PVDP lithium battery diaphragm |
| CN109378427A (en) * | 2018-09-17 | 2019-02-22 | 名添科技（深圳）有限公司 | A kind of non-woven fabrics basement membrane and preparation method thereof |
| CN109818054A (en) * | 2018-12-11 | 2019-05-28 | 天津工业大学 | A kind of lithium ion battery electrolyte and preparation method thereof having multilevel structure |
| CN110407605A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of preparation process of porous super capacitor material |
| CN110408281A (en) * | 2019-08-20 | 2019-11-05 | 西安鸿钧睿泽新材料科技有限公司 | Heat-insulated, energy-saving coating of one kind and preparation method thereof |
| CN114520396A (en) * | 2022-01-24 | 2022-05-20 | 哈尔滨工业大学 | Piezoelectric composite diaphragm for lithium metal battery and preparation method and application thereof |
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| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104282869A (en) * | 2014-09-12 | 2015-01-14 | 广东工业大学 | Preparation method of coating type organic/inorganic composite membrane of lithium battery |
| CN104282869B (en) * | 2014-09-12 | 2016-06-29 | 广东工业大学 | A kind of preparation method of application type lithium battery organic/inorganic composite diaphragm |
| CN109285985A (en) * | 2017-07-20 | 2019-01-29 | 天津凯普瑞特新能源科技有限公司 | A kind of PVDP lithium battery diaphragm |
| CN109378427A (en) * | 2018-09-17 | 2019-02-22 | 名添科技（深圳）有限公司 | A kind of non-woven fabrics basement membrane and preparation method thereof |
| CN109818054A (en) * | 2018-12-11 | 2019-05-28 | 天津工业大学 | A kind of lithium ion battery electrolyte and preparation method thereof having multilevel structure |
| CN110407605A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of preparation process of porous super capacitor material |
| CN110408281A (en) * | 2019-08-20 | 2019-11-05 | 西安鸿钧睿泽新材料科技有限公司 | Heat-insulated, energy-saving coating of one kind and preparation method thereof |
| CN114520396A (en) * | 2022-01-24 | 2022-05-20 | 哈尔滨工业大学 | Piezoelectric composite diaphragm for lithium metal battery and preparation method and application thereof |
| CN114520396B (en) * | 2022-01-24 | 2024-02-27 | 哈尔滨工业大学 | Piezoelectric composite diaphragm for lithium metal battery and preparation method and application thereof |
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Application publication date: 20140702 |