CN102820446A - Novel lithium ion battery composite diaphragm - Google Patents
Novel lithium ion battery composite diaphragm Download PDFInfo
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- CN102820446A CN102820446A CN2012101944533A CN201210194453A CN102820446A CN 102820446 A CN102820446 A CN 102820446A CN 2012101944533 A CN2012101944533 A CN 2012101944533A CN 201210194453 A CN201210194453 A CN 201210194453A CN 102820446 A CN102820446 A CN 102820446A
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Abstract
The invention relates to a novel lithium ion battery composite diaphragm and its production method. With a polyolefin millipore membrane as the matrix of the diaphragm, both sides of the membrane are respectively coated to form an organic polymer layer and an inorganic granular layer. The coating of the composite diaphragm can guarantee ionic conductivity of the diaphragm and simultaneously raise strength and thermal stability of the diaphragm and reduce heat shrinkage rate of the diaphragm, thus decreasing probability of short circuit in batteries, raising safety of batteries and increasing the service life of batteries.
Description
Technical field
The present invention relates to a kind of novel lithium ion battery composite diaphragm and production method thereof.
Background technology
Lithium ion battery has become the battery of new generation of extensive use owing to having voltage height, specific energy height, having extended cycle life and advantage free from environmental pollution.Lithium rechargeable battery generally is made up of both positive and negative polarity, barrier film, electrolyte and shell.Barrier film is a part important in the battery, and it has unique non-conductive and characteristic of allowing ion to pass through.The effect of barrier film in lithium ion battery is that both positive and negative polarity is kept apart, and prevents short circuit, guarantees that simultaneously lithium ion can pass through freely, and a battery produces current thereby make.Lithium ion battery separator is generally the polyolefin film with microcellular structure, and it is to having long-time stability with electrolyte.
Along with the development of new forms of energy industry, the especially fast development of electric automobile, power-type lithium ion battery has also obtained fast-developing and has used.Compare with common lithium ion battery, power-type lithium ion battery has characteristics such as capacity is big, charging and discharging currents big, security performance requirement height.The polyolefin that is mainly that is used for the lithium ion battery separator manufacturing at present; Compare with other materials; Though polyolefin film has mechanical property and chemical stability preferably, himself performance still is not enough to the security requirement, the especially power lithium battery that guarantee that lithium ion battery is higher.Also there is following problem in the lithium ion battery that with the MIcroporous polyolefin film is barrier film in fail safe with on useful life:
Insufficient strength is high.With cobalt acid lithium be positive pole lithium ion battery in use, the overshoot meeting causes lithium to separate out at negative pole with the form of metal, and then grows the Li dendrite of branch shape easily.When Li dendrite grows into to a certain degree will diaphragm, cause the short circuit of battery, this not only can increase the useful life that the overheated risk of battery also can reduce lithium ion battery greatly.With present technology, the growth of control Li dendrite does not still have good solution, so want to increase the fail safe and the life-span of battery, just must improve the intensity of barrier film.Must increase the thickness of barrier film once regularly wanting to improve intensity, reduce porosity at material, can increase the internal resistance of battery like this, influence the normal use of battery.
Thermal stability is limited.Lithium ion battery can be emitted a large amount of heat because short circuit appears in the defective of barrier film on the one hand in the process of using; The lithium metal of separating out on the other hand, can be with the electrolyte reaction because a large amount of warm of generation.Therefore and the occurrence of large-area short circuit polyethylene still is that polypropylene all can the fusion along with the intensification of battery, causes the whole barrier film will be in the fusion temperature fusion and, so that usually destroys battery because of on fire even blast.And power-type lithium ion battery is tantamount to a time bomb owing to have higher capacity.
Thermal contraction takes place.Because polyalkene diaphragm drawing process and high molecular inherent characteristic, the thermal contraction phenomenon can take place in barrier film when high temperature.Contraction causes barrier film wrinkling, and then makes and be difficult between electrode and the barrier film obtain closely and contact uniformly.In the use of battery, be difficult on the whole surface of electrode, carry out the uniform battery performance of the therefore very difficult acquisition of homogeneous phase electrode reaction and cause electrode in the local excessive loss, reduced the life-span of battery.In addition, when this inhomogeneous state of electrode became serious, electrode reaction possibly only take place in the part, and therefore the localized precipitation of lithium metal possibly take place, and caused fail safe to reduce.
Poor with the electrolyte wetting property.Because polyolefin belongs to non-polar material, the polar organic solvent compatibility of it and electrolyte solution is poor, in battery, only plays the buffer action of both positive and negative polarity room machine; And electrolyte is not had affinity interaction, make electrolyte solution be present in the battery, in battery charging and discharging recycles with free state; This free electrolyte inevitably with positive and negative pole material generation redox side reaction; Electrolyte in the consuming cells causes the battery lean solution, thereby makes battery polarization increase; Be prone to make lithium ion to be reduced into lithium metal and produce the lithium depositing crystalline become Li dendrite, cause barrier film puncture phenomenon.
More than these shortcomings restricted applying of power-type lithium ion battery.
Summary of the invention
The lithium ion battery separator that the purpose of this invention is to provide a kind of enhancing; With publication number be that the main difference part of the invention of CN1514501A is that base material of the present invention is the polyolefin film with microcellular structure of biaxial tension, the film two sides is coated with porous inorganic particulate layer and porous polymeric organic matter layer respectively.
Another object of the present invention provides the method for making above-mentioned composite diaphragm, and the method technology is simple, can make the diaphragm material of all thickness.
The invention has the advantages that have higher intensity, heat-resisting quantity and lower heat-shrinkable, can reduce the probability that battery is short-circuited greatly, effectively extend the life of a cell, increase the security performance of battery.
The MIcroporous polyolefin film of basic unit that is characterized as composite diaphragm of the present invention for processing through biaxial tension, on the basis of this microporous barrier, the front surface coated organic polymer layers, reverse side coating inorganic oxide particle, Fig. 1 is the structural representation of composite diaphragm of the present invention.When this composite diaphragm was manufactured into lithium ion battery, the front of barrier film contacted with the positive pole of lithium ion battery, and reverse side contacts with the negative pole of lithium ion battery.Fig. 2 processes the generalized section of battery for composite diaphragm of the present invention.
The front of composite diaphragm of the present invention is resistant to elevated temperatures organic polymer layers; This layer is adopted the higher polymer manufacturing of fusing point; Like copolymer, PETG, polyethylene glycol oxide, polymethyl methacrylate, poly, polyvinyl chloride, the polyacrylonitrile of Kynoar, vinylidene and hexafluoropropylene, but be not limited to above.Preferred PVF base polymer.Because polyolefin is non-polar polymer, at the polymeric layer of its surface-coated one deck polarity, barrier film is better soaked into electrolyte, also tightr with contacting of positive pole, avoided the localised current distribution inequality and the generation of overheated, the short circuit phenomenon that causes.In addition, because heat release basically all is to produce at negative pole, coat polymer good temperature resistance ability and resistance to wear also make the performance of barrier film get a promotion, and then improve the security performance of lithium ion battery.
The manufacturing approach of organic polymer layers is for to be dissolved in fluoropolymer resin in the organic solvent; Add pore former and other additives; The solution that is dissolved as homogeneous transparent is coated on casting solution on the polyalkene diaphragm as casting solution, remove desolvate and pore former after oven dry promptly get coating.The casting solution polymer concentration is 8%～18%; Preferred 9%～12%; Solvent for use is acetone, oxolane (THF), N; N-dimethylacetylamide (DMAC), N, dinethylformamide (DMF), N-methyl pyrrolidone (NMP), dimethyl sulfoxide (DMSO) (DMSO), triethyl phosphate (TEP) or other can dissolve polymer solvent.Pore former is for dissolving each other with the solvent of dissolve polymer, but organic solvent that can not dissolve polymer, like ethanol, ethylene glycol, 1-butanols, methyl alcohol etc.Other additives can comprise plasticizer, levelling agent etc.The reverse side of composite diaphragm of the present invention is an inorganic oxide layer, and its main component is inorganic oxide nanoparticles and binding agent.Inorganic oxide nanoparticles is selected the oxide particle of Si, Al, Ti and/or Zr for use.Binding agent is chemical property, a thermal stability and chemical stability organic polymer preferably; Like poly, Kynoar, polyethylene glycol oxide, polymethyl methacrylate, PETG, polyvinyl chloride, polyacrylonitrile, but be not limited to above.The oxide skin(coating) that the present invention applies formation has higher hardness, contacts with the negative pole of lithium ion battery, can prevent effectively that barrier film from being punctured by Li dendrite and then be short-circuited; Simultaneously, because the existence of oxide skin(coating) makes the thermal contraction of composite diaphragm descend, reduced barrier film because of the wrinkling probability that breaks down.In addition, the existence of coating makes barrier film be improved to imbibition, the liquid-keeping property of electrolyte, and then has improved the even distribution of charging and discharging currents, causes the cycle performance of lithium ion battery to be improved.
In the lithium ion battery use, the negative pole heating, the existence of inorganic coating can improve the thermal endurance of barrier film, improves the fusing-off temperature of barrier film.Rise to the fusing point of barrier film when battery temperature after, though barrier film generation closed pore effect can make battery close, thermal inertia can make the temperature of battery continue to raise, and finally causes barrier film fusing, and battery short circuit is caused danger.The existence of inorganic layer makes a barrier film fusion and does not fuse, and has guaranteed the safe handling of battery.
The inorganic nanometer oxide particle has unique skin effect, bulk effect and chemical property, has higher hardness, is easy to carry out chemical modification, thereby the inorganic layer of formation and polymeric layer are combined closely; Its microcellular structure makes the coating of its formation have permeability preferably.Consider that stable performance, low in raw material cost are easy to get, the modifying and decorating method ripe, the present invention adopts the oxide particle of Si, Al, Ti and/or Zr.
The manufacturing approach of inorganic oxide layer adds inorganic nanoparticles for binding agent is dissolved in the organic solvent, and the back that under the effect of strong shearing force, is uniformly dispersed adds pore former and other additives; The gained dispersion liquid is coated on the barrier film, remove desolvate and pore former after oven dry promptly get inorganic coating.Solvent for use is acetone, oxolane (THF), N, wherein a kind of of N-dimethylacetylamide (DMAC), N, dinethylformamide (DMF), N-methyl pyrrolidone (NMP), dimethyl sulfoxide (DMSO) (DMSO) and triethyl phosphate (TEP).Pore former is for dissolving each other with the solvent of dissolve polymer, but organic solvent that can not dissolve polymer, like ethanol, ethylene glycol, 1-butanols, methyl alcohol etc.Other additives can comprise silane coupler, levelling agent etc.
The thickness of composite diaphragm intermediate layer polyalkene diaphragm is 10～60 μ m, preferred 20～40 μ m; Signal layer coating thickness is 2～10 μ m, preferred 4～6 μ m; Composite diaphragm thickness is 14～80 μ m, preferred 30～50 μ m.
(Gurley appearance numerical value 100ml) is 200～800s to the composite diaphragm gas permeability, preferred 300～500s.
The present invention further specifies through the indefiniteness embodiment of Fig. 3-Fig. 5 and table 1.
Description of drawings
Fig. 1 is the structural representation of composite diaphragm of the present invention.
Fig. 2 processes the generalized section of battery for composite diaphragm of the present invention.
Fig. 3 is for being that the organic layer that raw material is processed gets stereoscan photograph with PVDF.Can find out that by figure this layer is the state of porosity and looseness, pore size distribution is comparatively even, does not expose the polyolefin layer of substrate, local fine and close situation of not passing through also do not occur.
Fig. 4 is the stereoscan photograph of the inorganic layer processed of raw material for adopting silicon dioxide.Can find out that on scheming the inorganic particulate granulosa distributes comparatively even, the binding agent of the visible wire drawing shape in place, slit has guaranteed that inorganic particle does not come off; Particle is arranged comparatively loose, is easy to the infiltration of electrolyte and sees through
The composite diaphragm production line sketch map of Fig. 5 for being the basis with the biaxially oriented film production line.
Composite diaphragm production method of the present invention can adopt the mode of direct transformation manufacture of polyolefins line online production, also can join the system of unreeling in addition and set up production line separately.
Following indefiniteness embodiment explains the present invention.
[embodiment 1]
Kynoar, NMP, ethylene glycol are pressed the mixed of 10:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the polyalkene diaphragm, place after 10 minutes, immersed volume ratio under the room temperature and be in the mixed liquor of ethanol and water of 1:2 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
Kynoar, nano silicon, NMP, ethylene glycol are pressed the mixed of 5:20:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the reverse side of dry good barrier film of a step, place after 10 minutes, the immersion volume ratio is in the mixed liquor of ethanol and water of 1:2 2 minutes under the room temperature; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
[embodiment 2]
Kynoar, NMP, ethylene glycol are pressed the mixed of 10:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the polyalkene diaphragm, place after 10 minutes, immersed volume ratio under the room temperature and be in the mixed liquor of ethanol and water of 1:2 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
Poly, anhydrous calcium chloride, nano silicon, NMP, ethylene glycol are pressed the mixed of 5:1:20:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the reverse side of dry good barrier film of a step, place after 10 minutes, under the room temperature in the immersion ethanol bath 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
[embodiment 3]
Kynoar, DMAC, ethylene glycol are pressed the mixed of 10:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the polyalkene diaphragm, place after 10 minutes, immersed volume ratio under the room temperature and be in the mixed liquor of ethanol and water of 1:2 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining DMAC and ethylene glycol.
Kynoar, nano silicon, NMP, ethylene glycol are pressed the mixed of 5:20:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the reverse side of dry good barrier film of a step, place after 10 minutes, the immersion volume ratio is in the mixed liquor of ethanol and water of 1:2 2 minutes under the room temperature; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
[embodiment 4]
Kynoar, dimethyl sulfoxide (DMSO), ethylene glycol are pressed the mixed of 10:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the polyalkene diaphragm, place after 10 minutes, immersed volume ratio under the room temperature and be in the mixed liquor of ethanol and water of 1:2 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining dimethyl sulfoxide (DMSO) and ethylene glycol.
Poly, anhydrous calcium chloride, nano silicon, NMP, ethylene glycol are pressed the mixed of 5:1:20:100:3 0; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the reverse side of dry good barrier film of a step, place after 10 minutes, under the room temperature in the immersion ethanol bath 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and ethylene glycol.
[embodiment 5]
The mixed that copolymer, DMAC, the 1-butanols of vinylidene and hexafluoropropylene are pressed 10:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the polyalkene diaphragm, place after 10 minutes, immersed volume ratio under the room temperature and be in the mixed liquor of ethanol and water of 1:2 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining DMAC and 1-butanols.
The mixed that copolymer, DMAC, nano silicon, the 1-butanols of vinylidene and hexafluoropropylene are pressed 5:20:100:30; Heating for dissolving is that the solution of transparent and homogeneous is as casting solution; Be coated on the reverse side of dry good barrier film of a step, place after 10 minutes, under the room temperature in the immersion ethanol bath 2 minutes; Put into temperature after the taking-up and be 60 ℃ baking oven 1 hour, remove remaining NMP and 1-butanols.
The contrast of embodiment properties of sample
With certain company's thick polypropylene diaphragm of 40 μ m is basic unit, applies with the foregoing description method respectively, obtains the sample barrier film, and these samples are detected; And process battery with the sample barrier film, and carrying out thermal shock and detect, the result is as shown in table 1.The data purpose is the performance boost of explanation composite diaphragm of the present invention with respect to former basic unit barrier film in this table, and its numerical value depends on the performance of basic unit's barrier film and the technological parameter of coating procedure, does not represent absolute performance of the present invention.
Table 1
Claims (10)
1. composite diaphragm, it comprises:
The polyolefin film with microcellular structure of biaxial tension, film two sides are coated with inorganic particulate granulosa and polymerized organics layer respectively.
2. the composite diaphragm of claim 1, wherein the inorganic particulate granulosa is the porous inorganic particulate layer.
3. the composite diaphragm of claim 1, wherein the inorganic particulate granulosa is the porous inorganic particulate layer.
4. each composite diaphragm of aforementioned claim, wherein said organic polymer layers adopts dystectic polymer manufacturing.
5. each composite diaphragm of aforementioned claim, wherein said organic polymer is selected from copolymer, PETG, polyethylene glycol oxide, polymethyl methacrylate, poly, polyvinyl chloride, polyacrylonitrile or their mixture of Kynoar, vinylidene and hexafluoropropylene.
6. each composite diaphragm of aforementioned claim, wherein said organic polymer is the PVF base polymer.
7. each composite diaphragm of aforementioned claim, the thickness of wherein said polyolefin film is 10～60 μ m, preferred 20～40 μ m.
8. each composite diaphragm of aforementioned claim, wherein said composite diaphragm thickness is 14～80 μ m, preferred 30～50 μ m.
9. each composite diaphragm of aforementioned claim, (Gurley appearance numerical value 100ml) is 200～800s, preferred 300～500s to the gas permeability of wherein said composite diaphragm.
10. each composite diaphragm of aforementioned claim is used for the purposes of lithium ion battery.
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| CN2012101944533A CN102820446A (en) | 2012-06-15 | 2012-06-15 | Novel lithium ion battery composite diaphragm |
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| CN2012101944533A CN102820446A (en) | 2012-06-15 | 2012-06-15 | Novel lithium ion battery composite diaphragm |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104201414A (en) * | 2014-08-29 | 2014-12-10 | 深圳华粤宝电池有限公司 | Lithium ion battery as well as preparation method thereof and charge method of lithium ion battery |
| CN104377331A (en) * | 2014-11-19 | 2015-02-25 | 新乡市中科科技有限公司 | Separator for lithium ion battery and preparation method of separator |
| CN105118948A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105390643A (en) * | 2014-09-05 | 2016-03-09 | 北京师范大学 | Lithium ion battery composite separation membrane and lithium ion battery containing lithium ion battery composite separation membrane |
| CN105958112A (en) * | 2016-06-24 | 2016-09-21 | 合肥国轩高科动力能源有限公司 | Non-diaphragm lithium ion battery coiled core and preparation method therefor |
| CN106207054A (en) * | 2014-11-13 | 2016-12-07 | 现代自动车株式会社 | The composite diaphragm equipped in monocell and manufacture method thereof |
| CN106252571A (en) * | 2016-08-31 | 2016-12-21 | 乐凯胶片股份有限公司 | A kind of multi-layer porous barrier film for lithium ion battery |
| CN106450433A (en) * | 2016-11-10 | 2017-02-22 | 厦门日臻动力电源科技有限公司 | High-rate high-safety soft package lithium-ion battery and preparation method thereof |
| CN107623099A (en) * | 2017-09-19 | 2018-01-23 | 武汉惠强新能源材料科技有限公司 | A kind of compound multi-layer polyolefin lithium electric separator and preparation method thereof |
| CN107658408A (en) * | 2017-09-19 | 2018-02-02 | 武汉惠强新能源材料科技有限公司 | Compound multi-layer polyolefin lithium electric separator and preparation method thereof |
| CN108336279A (en) * | 2017-12-29 | 2018-07-27 | 武汉中兴创新材料技术有限公司 | A kind of lithium ion battery separator and preparation method thereof of nano-particle coating |
| CN109638203A (en) * | 2018-11-26 | 2019-04-16 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium ion battery separator |
| CN109755438A (en) * | 2017-11-01 | 2019-05-14 | 比亚迪股份有限公司 | Battery diaphragm and preparation method thereof and lithium battery |
| CN114188658A (en) * | 2021-11-15 | 2022-03-15 | 深圳中兴新材技术股份有限公司 | Thin film, preparation method thereof and battery |
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| CN104201414B (en) * | 2014-08-29 | 2017-09-29 | 深圳华粤宝电池有限公司 | The charging method of lithium ion battery and preparation method thereof and lithium ion battery |
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| CN105390643A (en) * | 2014-09-05 | 2016-03-09 | 北京师范大学 | Lithium ion battery composite separation membrane and lithium ion battery containing lithium ion battery composite separation membrane |
| CN106207054A (en) * | 2014-11-13 | 2016-12-07 | 现代自动车株式会社 | The composite diaphragm equipped in monocell and manufacture method thereof |
| CN104377331A (en) * | 2014-11-19 | 2015-02-25 | 新乡市中科科技有限公司 | Separator for lithium ion battery and preparation method of separator |
| CN105118948A (en) * | 2015-09-13 | 2015-12-02 | 中南大学 | Method for preparing lithium ion battery diaphragm |
| CN105958112A (en) * | 2016-06-24 | 2016-09-21 | 合肥国轩高科动力能源有限公司 | Non-diaphragm lithium ion battery coiled core and preparation method therefor |
| CN106252571A (en) * | 2016-08-31 | 2016-12-21 | 乐凯胶片股份有限公司 | A kind of multi-layer porous barrier film for lithium ion battery |
| CN106450433A (en) * | 2016-11-10 | 2017-02-22 | 厦门日臻动力电源科技有限公司 | High-rate high-safety soft package lithium-ion battery and preparation method thereof |
| CN107623099A (en) * | 2017-09-19 | 2018-01-23 | 武汉惠强新能源材料科技有限公司 | A kind of compound multi-layer polyolefin lithium electric separator and preparation method thereof |
| CN107658408A (en) * | 2017-09-19 | 2018-02-02 | 武汉惠强新能源材料科技有限公司 | Compound multi-layer polyolefin lithium electric separator and preparation method thereof |
| CN107658408B (en) * | 2017-09-19 | 2020-11-13 | 武汉惠强新能源材料科技有限公司 | Composite multilayer polyolefin lithium battery diaphragm and preparation method thereof |
| CN109755438A (en) * | 2017-11-01 | 2019-05-14 | 比亚迪股份有限公司 | Battery diaphragm and preparation method thereof and lithium battery |
| CN109755438B (en) * | 2017-11-01 | 2020-09-15 | 比亚迪股份有限公司 | Battery diaphragm, preparation method thereof and lithium battery |
| CN108336279A (en) * | 2017-12-29 | 2018-07-27 | 武汉中兴创新材料技术有限公司 | A kind of lithium ion battery separator and preparation method thereof of nano-particle coating |
| CN109638203A (en) * | 2018-11-26 | 2019-04-16 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium ion battery separator |
| CN114188658A (en) * | 2021-11-15 | 2022-03-15 | 深圳中兴新材技术股份有限公司 | Thin film, preparation method thereof and battery |
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