CN104479166A - Preparation method of PVDF (polyvinylidene fluoride) mixture lithium-ion battery separator - Google Patents
Preparation method of PVDF (polyvinylidene fluoride) mixture lithium-ion battery separator Download PDFInfo
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Abstract
The invention relates to a preparation method of a PVDF (polyvinylidene fluoride) pore membrane material used for a lithium-ion battery separator. With adoption of an NIPS (nonsolvent-induced phase separation) method, PVDF, HDPE (high-density polyethylene), PSF (polysulfone) and PVP (polyvinyl pyrrolidone) are proportionally mixed, heated and dissolved in a solvent, and a casting solution is obtained; the casting solution form a basic membrane through tape casting, the obtained basic membrane is immersed into deionized water or an organic solventnormal hexane, cyclohexane, absolute ethyl alcohol, methyl alcoholtoluene or xylene, the solvent in the separator is removed, vacuum drying is performed, and the separator is formed. The method has a simple process, parameters are easy to control, and compared with an ordinary commercial separator, physical properties of wettability, mechanical property, ionic conductivity and the like as well as electrochemical properties of electrochemical stability, rate capability and the like of the prepared PVDF mixture lithium-ion battery separator are greatly improved.
Description
Technical field
The present invention relates to a kind of technology of preparing of polymers function film, particularly one be used for lithium ion battery every
The preparation method of the polyvinylidene difluoride (PVDF) mixture microporous membrane material of film.
Background technology
Along with as high performance, lightweight and automobile power source with the Enlargement Tendency, require that lithium-ion secondary cell, lighium polymer secondary battery and ultracapacitor (double layer capacitor and similar electrical condenser) such secondary cell have high-energy-density, Large Copacity and good safety performance.Wherein lithium ion battery separator plays extremely crucial and important role.Barrier film, between the anode and negative electrode of battery, plays insulating effect, and provides the path of ionic conduction by maintaining electrolytic solution, if the temperature of battery becomes too high, then in order to cut off electric current, a part of melting of barrier film, provides the closing function blocking pore.If temperature raises and barrier film melting further, then produce macropore, be short-circuited between the anode and cathode, this temperature is called short circuit temperature, usually, barrier film preferably has low closing temperature and higher short circuit temperature.When polyethylene diagrams, when battery abnormal heating, short circuit temperature is about 140 DEG C.Simultaneously along with the continuous growth of power cell demand, barrier film mechanical property also becomes the important factor determining electromobile safety performance day by day.
The barrier film being widely used in lithium ion battery is at present mainly polyalkene diaphragm, and its preparation technology divides dry method and wet method two kinds.The maximum defect of polyalkene diaphragm is that the contact of itself and organic electrolyte is poor, is not easily soaked by electrolytic solution, has a strong impact on the raising of ionic conductivity.Thus, in order to prepare the high-energy-density and jumbo secondary cell with Good Security, prepare a kind of Good Heat-resistance, percent thermal shrinkage is little, physical strength is high and there is because of high ionic conductivity the barrier film of excellent cycle performance and important.
PVDF is widely used in barrier film preparation owing to having good chemical stability and good electrolyte contacts performance, but because it belongs to semicrystalline polymeric, independent film forming difficulty, needs to add some pore-forming materials or form multipolymer to improve its film forming properties with other materials usually.It is polymer blended or simply add SiO that existing document mainly comprises the polar organic such as PVDF and PVA, PEG about the preparation of PVDF barrier film
2, Al
2o
3and TiO
2electrochemistry and the physical property modifications of barrier film are carried out in doping Deng inorganic particle.But often there is various performance deficiency in them, such as one-sided resistance to elevated temperatures is poor, physical strength is not high, the low electrochemistry caused of ionic conductivity is bad or material preparation process complicated difficult with the shortcoming of large-scale promotion application.
US4588633 discloses a kind of lithium ion battery separator preparation method, and the method comprises ultrahigh molecular weight polyethylene(UHMWPE) and mineral oil to add by a certain percentage in stirrer carries out stirring and dissolving, and wherein, mineral oil and poly ratio are 10 ~ 99:1.Above-mentioned formula enhances film strength, and barrier film also meets the requirement of lithium ion battery to barrier film substantially, but there is following defect: the diaphragm micro-hole aperture of formation is uneven, causes ionic conductivity low and then affect its performance in the battery.
No. 2005-209570th, Japanese Laid-Open Patent discloses following content: the two sides heat-resistant resin solution such as aromatic polyamide, polyimide, polyethersulfone, polyetherketone, polyetherimide of the fusing point with more than 200 DEG C being coated on polyalkene diaphragm, and be impregnated in solidification liquid, carry out washing, dry, preparation is coated with the polyalkene diaphragm of heat-resistant resin, but the barrier film that the method prepares often exists the problems such as bad mechanical property, ionic conductivity are low.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polyvinylidene difluoride (PVDF) mixture lithium ion battery separator.
For solving this technical problem, the present invention adopts following scheme:
The composition of polyvinylidene difluoride (PVDF) mixture barrier film of the present invention comprises: polyvinylidene difluoride (PVDF) PVDF, high density polyethylene and polysulfones PSF.Wherein the weight-average molecular weight of HDPE is 2.0 × 10
5-2.5 × 10
6/ mol.
Its preparation method comprises the following steps:
A) the choosing of solvent: DMAc, DMF etc.
B) preparation of original film-casting liquid: added to by PVP in solvent, then directly mixes sealing with PVDF, HDPE and PSF and obtains.
C) preparation of homogeneous phase film-casting liquid: original film-casting liquid is placed in well heater and heats certain hour, then stir, standing and defoaming can obtain.
D) basement membrane curtain coating: by the homogeneous phase film-casting liquid curtain coating on substrate obtained, then adjusts the preparation that scraper parameter carries out different thickness barrier film.
E) be separated: the film obtained after scraping immerses in non-solvent and carries out phase-splitting pore-forming.Then for some time is left standstill.
F) film is dried: standing metacneme is added in vacuum drying oven the solvent that heat abstraction is residual.
Preferably, described step (a) is with in (b), and pore-forming material PVP adds in solvent DMAc or DMF by the mass percent of 1.0-4.0.
Preferably, in described step (b), solvent and pore-forming material PVP mixed solution mass percent are that the addition of 75.5-87.5, HDPE and PSF presses PVDF, and the composition mass percent of HDPE and PSF is (10-20): (1.0-1.5): (1.5-3.0) adds.
Preferably, in described step (c), Heating temperature is 60-80 DEG C, and heat-up time is 5-8h, then stirs, and churning time is 2-3h, and standing and defoaming 24-28h after stirring, finally obtains homogeneous phase film-casting liquid.
Preferably, in described step (d), scraper parameter adjusts according to required different thickness barrier film, does not have preset parameter.
Preferably, in described step (e), non-solvent is in deionized water or immerses the heavy a kind of or wherein several mixing of organic solvent-normal hexane, hexanaphthene, dehydrated alcohol, methyl alcohol, toluene or dimethylbenzene.Time of repose is 12-24h.
Preferably, in described step (f), vacuum drying oven heat drying temperature is 70-90 DEG C, and heat-up time is 5-7h.Finally obtain finished film.
Preferably, in described step (f), the barrier film porosity prepared reaches 60%-80%, and ionic conductivity is 2.0-4.0 × 10
-3s/cm, at temperature is 170-190 DEG C, dimensional stability is good.
A kind of polyvinylidene difluoride (PVDF) mixture lithium ion battery separator, it adopts the preparation method of above-mentioned polyvinylidene difluoride (PVDF) mixture lithium ion battery separator to obtain.
Compared with prior art, the barrier film that this patented technology obtains has excellent physics and chemical property, solve the problem that industrial application septation physics and electrochemistry can not get both, preparation technology is simple, parameter easily controls, and has widened diaphragm application territory, not only can apply at electronic equipment for consumption, also the large-scale application because of its outstanding physicals thus conveniently in power cell field, improves the safety performance of electromobile.
Embodiment
Below by way of specific embodiment, the present invention is described in further detail.
embodiment 1
(1) the choosing of solvent: solvent is DMAc.
(2) preparation of original film-casting liquid: first measure 76.2gDMAc, by pore-forming material PVP by 4.0 mass percent add formation mixed solution, again by PVDF by 15.0 mass percent add, then by HDPE and PSF respectively by 1.4 and 3.4 mass percents add.
(3) preparation of homogeneous phase film-casting liquid: original film-casting liquid is placed in well heater and heats, Heating temperature is 65 DEG C, and heat-up time is 7h, then stirs with magnetic stirring apparatus, carries out the standing and defoaming of 24h after stirring 2h.
(4) basement membrane curtain coating: by curtain coating on clean smooth glass plate after absorbent cotton is dried of the homogeneous phase film-casting liquid that obtains, adjustment scraper parameter carries out knifing.
(5) be separated: the film obtained after scraping immerses in deionized water and carries out phase-splitting pore-forming and leave standstill 24h.
(6) film is dried: standing metacneme is vacuumized heat drying at 70 DEG C in vacuum drying oven, and time of drying, to be 6h vacuum tightness be, and 0.01MPa removes that residual solvent obtains thickness is 30 μm of finished product barrier films.
embodiment 2
(1) the choosing of solvent: solvent is DMAc.
(2) preparation of original film-casting liquid: first measure 86.2gDMAc, by pore-forming material PVP by 1.0 mass percent add formation mixed solution, again by PVDF by 10.0 mass percent add, then by HDPE and PSF respectively by 1.2 and 1.6 mass percents add.
(3) preparation of homogeneous phase film-casting liquid: original film-casting liquid is placed in well heater and heats, Heating temperature is 78 DEG C, and heat-up time is 5h, then stirs with magnetic stirring apparatus, carries out the standing and defoaming of 24h after stirring 2.5h.
(4) basement membrane curtain coating: by curtain coating on clean smooth glass plate after absorbent cotton is dried of the homogeneous phase film-casting liquid that obtains, adjustment scraper parameter carries out knifing.
(5) be separated: the film obtained after scraping immerses in deionized water and carries out phase-splitting pore-forming and leave standstill 24h.
(6) film is dried: standing metacneme is vacuumized heat drying at 80 DEG C in vacuum drying oven, and time of drying, to be 5h vacuum tightness be, and 0.01MPa removes that residual solvent obtains thickness is 30 μm of finished product barrier films.
embodiment 3
(1) the choosing of solvent: solvent is DMF.
(2) preparation of original film-casting liquid: first measure 80.2gDMAc, by pore-forming material PVP by 3.0 mass percent add formation mixed solution, again by PVDF by 12.0 mass percent add, then by HDPE and PSF respectively by 1.4 and 3.4 mass percents add.
(3) preparation of homogeneous phase film-casting liquid: original film-casting liquid is placed in well heater and heats, Heating temperature is 70 DEG C, and heat-up time is 6h, then stirs with magnetic stirring apparatus, carries out the standing and defoaming of 24h after stirring 2.5h.
(4) basement membrane curtain coating: by curtain coating on clean smooth glass plate after absorbent cotton is dried of the homogeneous phase film-casting liquid that obtains, adjustment scraper parameter carries out knifing.
(5) be separated: the film obtained after scraping immerses in deionized water and carries out phase-splitting pore-forming and leave standstill 24h.
(6) film is dried: standing metacneme is vacuumized heat drying at 80 DEG C in vacuum drying oven, and time of drying is 5h, and vacuum tightness is that 0.01MPa removes residual solvent to obtain thickness be 35 μm of finished product barrier films
Assembled by such scheme 1 polyvinylidene difluoride (PVDF) barrier film performance of lithium ion battery test and contrast step as follows:
A) PP/PE/PP barrier film is chosen: employing is comparatively advanced in the market and the PP/PE/PP barrier film that the Celgard company generally applied provides carries out performance comparison test;
B) battery assembling: assembled battery adopts LiCoO
2for positive pole, metallic lithium is negative pole, the 1.0 M LiPF that electrolytic solution provides for Dongguan China fir China fir
6-ethylene carbonate (EC)/dimethyl carbonate (DMC)/ethyl methyl carbonate (EMC) (1:1:1, v/v/v);
C) battery physics and electrochemical property test: the test mainly comprising electrochemical stability, thermal contraction, porosity, withstand voltage, tightness and melting temperature (Tm) etc.
Claims (10)
1. a preparation method for polyvinylidene difluoride (PVDF) mixture lithium ion battery separator, is characterized in that:
The preparation of original film-casting liquid: pore-forming material PVP is added in solvent DMAc or DMF by the mass percent of 1.0-5.0, gained mixed solution and PVDF, be of a size of HDPE and PSF of 1-200nm by (70-88): (10-25): (0.5-1.5): (1.5-3.5) mass percent directly mixes sealing and namely obtains initial film-casting liquid;
The preparation of homogeneous phase film-casting liquid: original film-casting liquid is placed in well heater and heats at 55-80 DEG C, then stir, standing and defoaming can obtain;
Basement membrane curtain coating: by the homogeneous phase film-casting liquid curtain coating on substrate obtained, then utilize scraper to obtain the barrier film of different film thickness;
Be separated: the film obtained after scraping immerses in non-solvent and carries out phase-splitting pore-forming, then leaves standstill;
Film is dried: heated in vacuum drying oven by standing metacneme, heat drying temperature is 70-90 DEG C, and time of drying is 5-8h, removes residual solvent.
2. the preparation method of a lithium ion battery separator as claimed in claim 1, it is characterized in that: described battery diaphragm is by polyvinylidene difluoride (PVDF) PVDF, high density polyethylene and polysulfones PSF form, and solvent and pore-forming material mixed solution mass percent are 75.5-87.5.
3. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: pore-forming material PVP by mass percentage 1.0-4.0 adds.
4. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: described battery diaphragm is made up of polyvinylidene difluoride (PVDF) PVDF, and its composition mass percent is 10-20.
5. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: described battery diaphragm is made up of PSF, and its composition mass percent is 1.5-3.0.
6. the preparation method of a lithium ion battery separator as claimed in claim 1, it is characterized in that: described battery diaphragm is made up of HDPE, its composition mass percent is 1.0-1.5, and the high-density HDPE of interpolation is nanometer HDPE particle, and size range is 80-200nm.
7. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: the Heating temperature described in (b) step is 60-80 DEG C, and heat-up time is 5-8h, and churning time is 2-3h, and the standing and defoaming time is 24-28h.
8. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: the direct curtain coating of gained homogeneous phase film-casting liquid becomes basement membrane, and gained basement membrane at room temperature immerses 12-24h in non-solvent.
9. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: non-solvent is in deionized water or immerses the heavy a kind of or wherein several mixing of organic solvent-normal hexane, hexanaphthene, dehydrated alcohol, methyl alcohol, toluene or dimethylbenzene.
10. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that: in vacuum, heat drying temperature is 70-90 DEG C, and time of drying is 5-7h.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104953072A (en) * | 2015-07-24 | 2015-09-30 | 中南大学 | Preparation method of lithium ion battery diaphragm |
| CN105118946A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105118948A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105514482A (en) * | 2016-01-29 | 2016-04-20 | 中南大学 | Preparation method of functional diaphragm of lithium sulfur battery |
| CN105789524A (en) * | 2016-04-29 | 2016-07-20 | 宁德卓高新材料科技有限公司 | Preparation method of polyvinyl alcohol isolating membrane and isolating membrane prepared |
| CN107221628A (en) * | 2017-06-19 | 2017-09-29 | 武汉艾特米克超能新材料科技有限公司 | A kind of preparation method of lithium battery diaphragm, lithium battery diaphragm and lithium ion battery |
| CN108630862A (en) * | 2017-03-17 | 2018-10-09 | 银隆新能源股份有限公司 | The preparation method of micro-pore septum is blended in a kind of lithium ion battery |
| CN110600657A (en) * | 2019-09-27 | 2019-12-20 | 宁德卓高新材料科技有限公司 | Preparation method of filamentous vinylidene fluoride polymer composite coating diaphragm |
| CN111755647A (en) * | 2019-03-27 | 2020-10-09 | 中南大学 | Preparation method of lithium-air battery composite diaphragm |
| CN112242588A (en) * | 2020-08-14 | 2021-01-19 | 安徽德亚电池有限公司 | Preparation method of lithium battery ceramic composite membrane |
| CN113488738A (en) * | 2021-07-08 | 2021-10-08 | 青岛大学 | Composite separator for secondary battery, method for producing same, secondary battery, and electric device |
| CN113769586A (en) * | 2021-10-26 | 2021-12-10 | 天津工业大学 | Preparation method of double-layer hollow fiber loose nanofiltration membrane for dye desalination |
| CN114891250A (en) * | 2022-05-05 | 2022-08-12 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
| CN115172991A (en) * | 2022-06-20 | 2022-10-11 | 哈尔滨工业大学 | Composite diaphragm material and preparation method and application thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104953072A (en) * | 2015-07-24 | 2015-09-30 | 中南大学 | Preparation method of lithium ion battery diaphragm |
| CN105118946A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105118948A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105514482A (en) * | 2016-01-29 | 2016-04-20 | 中南大学 | Preparation method of functional diaphragm of lithium sulfur battery |
| CN105514482B (en) * | 2016-01-29 | 2018-01-09 | 中南大学 | A kind of preparation method of lithium-sulfur cell function barrier film |
| CN105789524A (en) * | 2016-04-29 | 2016-07-20 | 宁德卓高新材料科技有限公司 | Preparation method of polyvinyl alcohol isolating membrane and isolating membrane prepared |
| CN108630862A (en) * | 2017-03-17 | 2018-10-09 | 银隆新能源股份有限公司 | The preparation method of micro-pore septum is blended in a kind of lithium ion battery |
| CN107221628B (en) * | 2017-06-19 | 2023-10-13 | 宁波柔创纳米科技有限公司 | Preparation method of lithium battery diaphragm, lithium battery diaphragm and lithium ion battery |
| CN107221628A (en) * | 2017-06-19 | 2017-09-29 | 武汉艾特米克超能新材料科技有限公司 | A kind of preparation method of lithium battery diaphragm, lithium battery diaphragm and lithium ion battery |
| CN111755647A (en) * | 2019-03-27 | 2020-10-09 | 中南大学 | Preparation method of lithium-air battery composite diaphragm |
| CN110600657A (en) * | 2019-09-27 | 2019-12-20 | 宁德卓高新材料科技有限公司 | Preparation method of filamentous vinylidene fluoride polymer composite coating diaphragm |
| CN112242588A (en) * | 2020-08-14 | 2021-01-19 | 安徽德亚电池有限公司 | Preparation method of lithium battery ceramic composite membrane |
| CN113488738A (en) * | 2021-07-08 | 2021-10-08 | 青岛大学 | Composite separator for secondary battery, method for producing same, secondary battery, and electric device |
| CN113769586A (en) * | 2021-10-26 | 2021-12-10 | 天津工业大学 | Preparation method of double-layer hollow fiber loose nanofiltration membrane for dye desalination |
| CN114891250A (en) * | 2022-05-05 | 2022-08-12 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
| CN114891250B (en) * | 2022-05-05 | 2023-09-15 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
| CN115172991A (en) * | 2022-06-20 | 2022-10-11 | 哈尔滨工业大学 | Composite diaphragm material and preparation method and application thereof |
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Application publication date: 20150401 |