CN103094517A - Composite battery membrane and preparation method thereof - Google Patents
Composite battery membrane and preparation method thereof Download PDFInfo
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- CN103094517A CN103094517A CN2012105386502A CN201210538650A CN103094517A CN 103094517 A CN103094517 A CN 103094517A CN 2012105386502 A CN2012105386502 A CN 2012105386502A CN 201210538650 A CN201210538650 A CN 201210538650A CN 103094517 A CN103094517 A CN 103094517A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a composite battery membrane and a preparation method thereof. The composite battery membrane comprises a porous base membrane, a porous inorganic layer compounded on at least one surface of the porous base membrane, and a porous closing layer compounded on the surface of the porous inorganic layer, wherein the porous inorganic layer is clamped between the porous closing layer and the porous base membrane. The composite battery membrane provided by the invention has the properties of low-temperature closing and high-temperature resistance; and the 'dusting' problem of the membrane added with inorganic particles can be effectively solved. Compared with the prior art, the composite battery membrane provided by the invention has a simple and convenient production process, is convenient and flexible in thickness control, and good in machining property.
Description
Technical field
The application relates to the battery diaphragm field, particularly relates to a kind of composite battery separator film, the application of this composite battery separator film in high-performance power battery and preparation method of composite battery separator film who is suitable for high-performance power battery.
Background technology
The fail safe of battery is that the safety problem of the significant problem of battery industry circle, particularly electrokinetic cell has greatly limited its commercial applications always.
The polymer micro battery diaphragm that commercialization is used comprises polyethylene (PE), high density polyethylene (HDPE) (HDPE) or polypropylene (PP) barrier film, the dry method barrier film of producing with celgard company, or the wet method barrier film that Japan's east combustion, Asahi Chemical Industry are produced is representative.Industry has realized that namely that very early the security performance that this barrier film uses is low in battery.Therefore, developed again afterwards three layers of composite diaphragm of PP/PE/PP (US Patent No. 5691077), when temperature rose to 130 ℃ of left and right, the middle PE layer melted and closes the hole of PP layer, thereby had the self closing merit, thereby had improved the security performance of battery.But the thermal stability of three layers of barrier film or limited, the SC service ceiling temperature of 160 ℃ of only having an appointment.Under the situation of battery thermal runaway, even realized the closing function of 130 ℃ of left and right, internal temperature of battery also will continue upper punch, and probably surpass 160 ℃, and therefore, still there is very large potential safety hazard in the composite diaphragm of three layers.
In addition, in prior art, the blowout disk that also has coating heatproof inorganic particulate on porous matrix, i.e. applying porous inorganic layer on the porous basement membrane, the more representational heatproof barrier film that comprises that MAT announces in Chinese patent CN101069302, and the high-energy battery barrier film announced in Chinese patent CN1679183 of German Degussa.Above blowout disk or the blowout disk that is similar to it, although improved in fact the heat resistance of barrier film, but in fact do not improve the security performance of barrier film, because this barrier film does not have the self closing mechanism under high temperature, although itself does not fuse barrier film, but battery temperature continues to rise, and finally still security incident can occur.Another problem of this coating barrier film is " dry linting " problem of manufacturing and use procedure, the barrier film of coating heatproof inorganic particulate, in order to guarantee the heat resistance of coating, generally only add a small amount of adhesive, and owing to also must guaranteeing the porousness of inorganic particulate coating, in coating, the bonding force of particle is more weak, thereby causes barrier film " dry linting ", cause diaphragm failures, and hinder battery manufacture.
At present, what can solve preferably the barrier film resistance to elevated temperatures is the blowout disk of Degussa preparation, and this blowout disk is mainly, prepares respectively basement membrane and closes layer film, and then being combined with each other both are stacked.At first, due to the restriction of prior art, the thickness of this blowout disk is larger, greater than 50 μ m, affects the serviceability of barrier film; Secondly, the complicated process of preparation of this blowout disk in stacked compound process, breakage or fold occur unavoidably, affects the quality of blowout disk.
Summary of the invention
The application's purpose is to provide a kind of new composite battery separator film, the preparation method of this composite battery separator film, and the application of this composite battery separator film in high-performance power battery.
To achieve these goals, the application has adopted following technical scheme:
The application's one side discloses a kind of composite battery separator film, comprise the porous basement membrane, be compound at least one surperficial porous inorganic layer of porous basement membrane, and the porous that is compound in the porous inorganic layer surface closes layer, and porous inorganic layer is located in porous and closes between layer and porous basement membrane.
In the application, porous is closed one or more in low density polyethylene (LDPE), LLDPE, Tissuemat E, OPE, Fischer-Tropsch wax, beeswax or the ethylene-vinyl acetate copolymer of layer as primary raw material; Preferred porous is closed layer take Tissuemat E and/or OPE as primary raw material.
Further, in composite battery separator film, the Thickness Ratio of each layer is, porous basement membrane: porous inorganic layer: porous is closed layer=100-150:10-60:10-60; Preferably, porous basement membrane: porous inorganic layer: porous is closed layer=100-150:20-40:20-40.
The thickness of the application's composite battery separator film is 15-40 μ m.
Contain inorganic particulate and adhesive in the application's porous inorganic layer; The average grain diameter of inorganic particulate is 0.1-10 μ m, and the mass ratio of inorganic particulate and adhesive is between 0.1:1.0 to 1.0:0.1; Inorganic particulate is selected from least a in the oxide particle of aluminium, silicon, magnesium and zirconium or hydride particle; Adhesive is selected from least a in Kynoar, Kynoar-hexafluoropropylene copolymer, polyacrylonitrile, polymethyl methacrylate, polyvinylpyrrolidone, poly-ethyl acetate, cellulose-acetate propionate, polyethylene-ethyl acetate copolymer and polyimides.Wherein, Kynoar-hexafluoropropylene copolymer that is Kynoar be hexafluoropropylene altogether, polyethylene-ethyl acetate copolymer that is polyethylene-altogether-ethyl acetate
Further, the porous basement membrane take polyethylene, polypropylene, Kynoar, Kynoar altogether one or more in hexafluoropropylene, PETG or polyimides as primary raw material; The aperture of porous basement membrane is 0.1 μ m-100 μ m, and porosity is 35%-70%, and thickness is 9-30 μ m.
The application's another side also discloses the application's the application of composite battery separator film in high-performance power battery.
The application's one side again discloses the preparation method of a kind of the application's composite battery separator film, comprising: a. mixes acquisition inorganic particulate slurries with inorganic particulate and adhesive in solvent; B. the inorganic particulate slurries are applied over the upper porous inorganic layer that forms at least one surface of porous basement membrane; C. apply the polymer solution of closing layer on porous inorganic layer, form porous after solidifying and close layer; Wherein, the solvent in step a is selected from acetone, N, N '-dimethyl formamide, N, at least a in N '-dimethylacetylamide, N-2-methyl pyrrolidone, dimethyl sulfoxide (DMSO) or oxolane.
Further, in the application's preparation method, applying in step b and step c is specially any one in printing, compacting, roller coat, blade coating, dip-coating, spraying or perfusion, is preferably dip-coating.
Owing to adopting above technical scheme, the application's beneficial effect is:
The application's composite battery separator film has that low temperature is closed and resistance to elevated temperatures, has effectively avoided adding the processing problems such as " dry lintings " of the barrier film of inorganic particulate.Compared with prior art, the production technology of the application's composite battery separator film is easy, and THICKNESS CONTROL is convenient, flexible, and processing characteristics is good.
Description of drawings
Fig. 1 is the structural representation of the composite battery separator film of the embodiment of the present application.
Embodiment
The application is larger for existing blowout disk thickness, and the problem of complicated process of preparation provides a kind of technique simple, the controlled composite battery separator film preparation method of prepared blowout disk thickness out.The method is mainly to apply one deck porous inorganic layer at least at least one surface of porous basement membrane, and then applies at least one deck porous close layer on porous inorganic layer.The application's who obtains thus composite battery separator film, solved simultaneously not only that low temperature is closed, resistance to elevated temperatures and problems such as " dry lintings ", and, the amount that can simple and effective control applies, thus make the thickness of the composite battery separator film of preparation can satisfy the instructions for use of different batteries.
The preferred thickness of the application's composite battery separator film is 15-40 μ m, need to prove, this thickness range be composite battery separator film in the situation that guarantee that low temperature is closed, resistance to elevated temperatures and avoid " dry linting ", the thinner thickness that can reach, be appreciated that if need to strengthen resistance to elevated temperatures or other purpose, can apply porous inorganic layer thicker, perhaps porous is closed layer and apply thicklyer, to prepare the composite battery separator film greater than 40 μ m thickness.Also need to prove, according to prior art, the thickness of porous basement membrane is the thinnest can reach 9 μ m, and the minimum 1.5 μ m that also can reach of the thickness of each layer that applies in the application, therefore, the composite battery separator film for preparing 15 μ m can be accomplished fully, even in the situation that the employing single face applies, can also accomplish thinner.
In the application, porous inorganic layer and porous are closed layer be compound in the epilamellar method of porous and be specially any one in printing, compacting, roller coat, blade coating, dip-coating, spraying or perfusion.The mode that the application preferably adopts dip-coating is closed layer with porous inorganic layer and porous respectively and is applied on the porous basement membrane, preferably, first adhesive is added in solvent, the preparation binder solution, and then add inorganic particulate, be uniformly dispersed, obtain the inorganic particulate slurries, by dip coating, slurries are coated on the porous basement membrane; And then dip-coating close the layer polymer solution or emulsion, wherein the mass fraction of polymer solution or emulsion or solid content are 10wt%-60wt%.The composite battery separator film of preparation as shown in Figure 1, two equal dip-coatings in surface of porous basement membrane 1 have porous inorganic layer 2, then on the surface of porous inorganic layer 2 again dip-coating have porous to close layer 3.Be appreciated that, the application's basic conception mode is, the mode that employing applies applies one deck porous again and closes layer on porous inorganic layer, therefore, also can be only a surface of composite battery separator film be applied, namely prepare the three-decker that porous is closed a porous inorganic layer of sandwiched between layer and porous basement membrane.
In the application, take polyethylene, polypropylene, Kynoar, Kynoar altogether one or more in hexafluoropropylene, PETG or polyimides as primary raw material, adopt conventional dry method or wet method to be prepared into the porous basement membrane; And the aperture of the preferred porous basement membrane of the application is 0.1 μ m-100 μ m, and porosity is 35%-70%, and thickness is 9-30 μ m.Need to prove, except the porous basement membrane of above-mentioned material, be appreciated that other thin polymer film that can buy on market equally also can be used for the application.
Need to prove, in the application, the effect that porous is closed layer is that low temperature closes, and therefore, is appreciated that fusing point in prior art or softening point may be used to the application at the thermoplastic resin of 80-140 ℃; In the application, preferably adopt fusing point or softening point at the thermoplastic resin of 80-120 ℃.Concrete, porous is closed one or more in low density polyethylene (LDPE), LLDPE, Tissuemat E, OPE, Fischer-Tropsch wax, beeswax or the ethylene-vinyl acetate copolymer of layer as primary raw material; Preferred porous is closed layer take Tissuemat E and/or OPE as primary raw material.In the application's execution mode, adopt polythene wax emulsion to be coated with to form the Tissuemat E porous and close layer, adopt oxidized polyethylene wax emulsion to be coated with to form the OPE porous and close layer.
In the application, porous inorganic layer adopts the inorganic particulate slurries to apply and forms, and in the inorganic particulate slurries, the mass ratio of inorganic particulate and adhesive is between 0.1:1.0 to 1.0:0.1; The mass ratio of solvent and solid content is between 1.0:0.2 to 1.0:0.5.Namely form porous inorganic layer after being applied in the epilamellar inorganic particulate slurry dried of porous, in porous inorganic layer, the mass ratio of inorganic particulate and adhesive is between 0.1:1.0 to 1.0:0.1.Need to prove, in dry process, solvent can be removed, and inorganic particulate and adhesive can be retained; Therefore, in porous inorganic layer in the mass ratio of inorganic particulate and adhesive and initial inorganic particulate slurries the mass ratio of inorganic particulate and adhesive suitable.
Also by reference to the accompanying drawings the application is described in further detail below by specific embodiment.Following examples only further illustrate the application, should not be construed as the restriction to the application.
Comparative Examples
The polyvinylidene fluoride that is 5wt% with mass fraction adds in acetone, and in 50 ℃ of lower stirring and dissolving 12 hours, to prepare uniform binder solution, with Al
2O
3Powder is according to polyvinylidene fluoride: Al
2O
3The weight ratio of=10:90 is added in prepared binder solution, and ball milling 12 hours is with Al
2O
3Powder is pulverized and is scattered in binder solution, namely makes the inorganic particulate slurries.By dip coating, made inorganic particulate slurries are coated on microporous polypropylene membrane, the porosity of microporous polypropylene membrane is 50%, controls the amount of dip-coating, and after making drying, the thickness of the porous inorganic layer of each face of microporous polypropylene membrane is about 3 μ m.In the microporous barrier of preparation, the two sides of porous basement membrane is coated with porous inorganic layer, i.e. porous inorganic layer+porous basement membrane+porous inorganic layer, and gross thickness is 24 μ m, porosity is 48%.This microporous barrier is after 130 ℃ of lower heat treatment 10min, and the Gurley value is about 300, do not show heat and close performance, and in the processing use procedure, the inorganic particulate obscission is obvious.
Method according to Comparative Examples prepares microporous barrier, i.e. porous inorganic layer+porous basement membrane+porous inorganic layer.this microporous barrier be impregnated in the 20%wt polythene wax emulsion 5 seconds, then take out dry 20min in 50 ℃ of baking ovens, namely obtain this routine porous and close the composite battery separator film that layer+porous inorganic layer+porous basement membrane+porous inorganic layer+porous is closed layer, porous close the layer with porous inorganic layer be sandwiched in porous close the layer and the porous basement membrane in the middle of, wherein the Tissuemat E coating of each face be porous close the layer thickness be 3 μ m, this routine composite battery separator film gross thickness is 30 μ m, has approximately 400 Gurley value, 100 ℃ of closing temperatures, be warming up to 105 value stabilizations of Gurley when spending more than 2000.
In its processing use procedure as battery diaphragm, without the particle obscission, after being prepared into battery, its broken film temperature is greater than 200 ℃.
Method according to Comparative Examples prepares microporous barrier, i.e. porous inorganic layer+porous basement membrane+porous inorganic layer, and wherein the adhesive of inorganic particulate slurries replaces with polyacrylonitrile, and all the other are identical with Comparative Examples.The microporous barrier of preparation be impregnated in the 20%wt oxidized polyethylene wax emulsion 5 seconds, then take out dry 20min in 50 ℃ of baking ovens, namely obtain this routine porous close layer+porous inorganic layer+porous basement membrane+porous inorganic layer+porous close the layer composite battery separator film, wherein the Tissuemat E coating of each face be porous close the layer thickness be 3 μ m.The gross thickness of the composite battery separator film that this is routine is 30 μ m, Gurley value 380, and after 110 ℃ of lower heat treatment 10min, the Gurley value rises to approximately 2500, and namely closing temperature is 110 ℃.In its processing use procedure as battery diaphragm, without the particle obscission, after being prepared into battery, its broken film temperature is greater than 200 ℃.
Method according to Comparative Examples prepares microporous barrier, it is porous inorganic layer+porous basement membrane+porous inorganic layer, and, adopt polymethyl methacrylate to replace polyvinylidene fluoride as the adhesive of inorganic particulate slurries, simultaneously, adopt the polyethene microporous membrane of porosity 50% to replace microporous polypropylene membrane as basement membrane, all the other are identical with Comparative Examples.The microporous barrier of preparation be impregnated in 30%wt low-melting-point polyethylene wax emulsion 5 seconds, then take out dry 30min in 40 ℃ of baking ovens, namely obtain this routine porous close layer+porous inorganic layer+porous basement membrane+porous inorganic layer+porous close the layer composite battery separator film, wherein the Tissuemat E coating of each face be porous close the layer thickness be 3 μ m.This routine composite battery separator film gross thickness is 30 μ m, and the Gurley value is 380, and after 80 ℃ of lower heat treatment 10min, the Gurley value rises to approximately 2200, and namely closing temperature is 80 ℃.In its processing use procedure as battery diaphragm, without the particle obscission, after being prepared into battery, its broken film temperature is greater than 200 ℃.
In addition, with the microporous polypropylene membrane that uses in the composite battery separator film of the microporous barrier of above-mentioned Comparative Examples, embodiment 1-3 preparation and each embodiment, polyethene microporous membrane in 150 ℃ process 1h carry out vertical percent thermal shrinkage and laterally percent thermal shrinkage measure.Measurement result is as shown in table 1.
Table 1 percent thermal shrinkage is measured
| Sample | Vertical percent thermal shrinkage | Horizontal percent thermal shrinkage |
| The PP basement membrane | 30.0% | 2.0% |
| The PE basement membrane | 85.0% | 80.0% |
| Comparative Examples | 7.0% | 0 |
| |
6.8% | 0 |
| |
6.8% | 0 |
| |
28.0% | 24．0% |
At the same temperature, shrinkage is lower, and its thermal endurance is better; As shown in table 1, the composite battery separator film thermal endurance of the embodiment of the present application 1,2 preparations improves a lot than Comparative Examples.Embodiment 3 is because the porous basement membrane that adopts is PE, and the thermal endurance of the composite battery separator film of its preparation is than embodiment 1,2 poor; But, to compare with original PE film, thermal endurance has large increase equally.The composite battery separator film that the application is prepared when guaranteeing that thermal endurance and low temperature are closed effect, has not only been avoided inorganic particulate " dry linting ", also effectively reduces the thickness of composite battery separator film.
Above content is the further description of the application being done in conjunction with concrete execution mode, can not assert that the application's concrete enforcement is confined to these explanations.For the application person of an ordinary skill in the technical field, under the prerequisite that does not break away from the application's design, can also make some simple deduction or replace, all should be considered as belonging to the application's protection range.
Claims (10)
1. composite battery separator film, at least one the surperficial porous inorganic layer that comprises the porous basement membrane and be compound in the porous basement membrane, it is characterized in that: comprise that also the porous that is compound in the porous inorganic layer surface closes layer, porous inorganic layer is located in porous and closes between layer and porous basement membrane.
2. composite battery separator film according to claim 1 is characterized in that: described porous is closed one or more in low density polyethylene (LDPE), LLDPE, Tissuemat E, OPE, Fischer-Tropsch wax, beeswax or the ethylene-vinyl acetate copolymer of layer as primary raw material; Preferred porous is closed layer take Tissuemat E and/or OPE as primary raw material.
3. composite battery separator film according to claim 1, it is characterized in that: in described composite battery separator film, the Thickness Ratio of each layer is, porous basement membrane: porous inorganic layer: porous is closed layer=100-150:10-60:10-60; Preferably, porous basement membrane: porous inorganic layer: porous is closed layer=100-150:20-40:20-40.
4. according to claim 1-3 described composite battery separator films of any one, it is characterized in that: the thickness of described composite battery separator film is 15-40 μ m.
5. according to claim 1-3 described composite battery separator films of any one, it is characterized in that: contain inorganic particulate and adhesive in described porous inorganic layer, the mass ratio of inorganic particulate and adhesive is between 0.1:1.0 to 1.0:0.1;
The average grain diameter of described inorganic particulate is 0.1-10 μ m, and described inorganic particulate is selected from least a in the oxide particle of aluminium, silicon, magnesium and zirconium or hydride particle;
Described adhesive is selected from least a in Kynoar, Kynoar-hexafluoropropylene copolymer, polyacrylonitrile, polymethyl methacrylate, polyvinylpyrrolidone, poly-ethyl acetate, cellulose-acetate propionate, polyethylene-ethyl acetate copolymer and polyimides.
6. according to claim 1-5 described composite battery separator films of any one is characterized in that: described porous basement membrane take polyethylene, polypropylene, Kynoar, Kynoar altogether one or more in hexafluoropropylene, PETG or polyimides as primary raw material;
The aperture of described porous basement membrane is 0.1 μ m-100 μ m, and porosity is 35%-70%, and thickness is 9-30 μ m.
7. according to claim 1-6 application of the described composite battery separator film of any one in high-performance power battery.
8. the preparation method of according to claim 1-6 described composite battery separator films of any one, comprise,
A. inorganic particulate and adhesive are mixed acquisition inorganic particulate slurries in solvent;
B. the inorganic particulate slurries are applied over the upper porous inorganic layer that forms at least one surface of porous basement membrane;
C. apply the polymer solution of closing layer on porous inorganic layer, form porous after solidifying and close layer;
Solvent in described step a is selected from acetone, N, N '-dimethyl formamide, N, at least a in N '-dimethylacetylamide, N-2-methyl pyrrolidone, dimethyl sulfoxide (DMSO) or oxolane.
9. preparation method according to claim 8 is characterized in that: applying in described step b and step c is specially any one in printing, compacting, roller coat, blade coating, dip-coating, spraying or perfusion.
10. preparation method according to claim 9, it is characterized in that: applying in described step b and step c is specially dip-coating.
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| CN103354279A (en) * | 2013-06-20 | 2013-10-16 | 深圳中兴创新材料技术有限公司 | Three-layer membrane for lithium ion battery |
| CN103904280A (en) * | 2014-03-27 | 2014-07-02 | 达尼特材料科技（芜湖）有限公司 | Isolating film for lithium ion battery and manufacturing method thereof |
| CN104022250A (en) * | 2014-06-26 | 2014-09-03 | 佛山市盈博莱科技有限公司 | Lithium ion battery diaphragm and preparation method |
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Application publication date: 20130508 |