CN103531734B - A kind of lithium ion battery separator and preparation method - Google Patents
A kind of lithium ion battery separator and preparation method Download PDFInfo
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- CN103531734B CN103531734B CN201310432961.5A CN201310432961A CN103531734B CN 103531734 B CN103531734 B CN 103531734B CN 201310432961 A CN201310432961 A CN 201310432961A CN 103531734 B CN103531734 B CN 103531734B
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- polyethylene layer
- density polyethylene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
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Abstract
The present invention relates to a kind of lithium ion battery separator, be made up of High molecular weight polyethylene layer, high-density polyethylene layer, High molecular weight polyethylene layer, described High molecular weight polyethylene layer is 15 ~ 80 by the degree of branching, molecular weight is the High molecular weight polyethylene composition of 50 ~ 3,000,000, described high-density polyethylene layer is 2 ~ 20 by the degree of branching, and molecular weight is the high density polyethylene (HDPE) composition of 20 ~ 500,000.It prepares the first polyethylene layer material by double screw extruder, prepare the second polyethylene layer material, co-extrusion, masking, extraction, sizing obtain.The outer field aperture of the present invention is comparatively large, contributes to the lyophily performance improving barrier film and electrolyte, and inner-layer thin aperture contributes to electrolyte in barrier film, forms capillarity attraction, and electrolyte fast parent moistens barrier film.Because outer aperture is comparatively large, fiber is also comparatively thick, and percent thermal shrinkage is less, and internal layer aperture is little, and in battery thermal shock process, easy aperture closes, and prevents the short circuit of battery from exploding, and improves security performance.
Description
Technical field
The present invention relates to a kind of lithium ion battery separator and preparation method, be specifically related to a kind of solution barrier film absorbent, solve lithium ion battery separator and the preparation method of barrier film security performance simultaneously.
Background technology
Lithium ion battery separator is that the isolation both positive and negative polarity that plays be applied in lithium ion battery prevents battery short circuit to have one of certain pore structure significant components can guaranteeing the lithium ion battery that lithium ion passes through smoothly simultaneously.
Usual lithium ion battery separator selected materials all has good electrical insulation capability, and the principal element affecting its performance is pore structure.Along with the high performance development trend of lithium ion battery, the performance performance requirement of lithium ion battery separator improves constantly, high-end lithium ion battery particularly power lithium-ion battery requires that barrier film has specific pore structure, this is not only related to that the ion of barrier film is by performance, also affects the safe application performance of battery.
Propose a kind of three layers of barrier film containing coating in patent CN103081171A, its overall aperture requires to be 0.01 ~ 1 μm, and mainly solve the laminated plug-hole problem of three layers of barrier film, its pore diameter range is too wide in range, also has no the aperture design to each Rotating fields.
Up to the present, the aperture structure of barrier film is also in fairly simple characteristic manner, and leading indicator is air permeability and porosity, and does not carry out special requirement to the degree of branching of diaphragm material.Generally for and ensure that barrier film has good absorbent, usually require that the air permeability of barrier film is little, porosity wants high, but the too small membrane pore size that often causes of air permeability is excessive, when battery safety is tested, aperture is not easy to shrink the problem causing closed pore slow, causes the security performance such as acupuncture, thermal shock to test percent of pass low.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of solution barrier film absorbent, solving the lithium ion battery separator of diaphragm closed pore security performance simultaneously.
Another object of the present invention is to the preparation method that a kind of lithium ion battery separator is provided.
For solving the problem, the technical solution adopted in the present invention is as follows:
A kind of lithium ion battery separator, it comprises sandwich diaphragm, be made up of High molecular weight polyethylene layer/high-density polyethylene layer/High molecular weight polyethylene layer, described High molecular weight polyethylene layer is 15 ~ 80 by the degree of branching, molecular weight is the High molecular weight polyethylene composition of 50 ~ 3,000,000, described high-density polyethylene layer is 2 ~ 20 by the degree of branching, and molecular weight is the high density polyethylene (HDPE) composition of 20 ~ 500,000.
The degree of branching is the branched carbon atoms number that 1000 carbon atoms contain.The upper and lower two-layer employing High molecular weight polyethylene of this lithium ion battery separator, the degree of branching is 15 ~ 80, and molecular weight is 50 ~ 3,000,000, provides good intensity and heat-shrinkable, improves lyophily performance.Preferably, the degree of branching of described High molecular weight polyethylene layer is 40 ~ 60.Intermediate layer adopts high density polyethylene (HDPE), and the degree of branching is 2 ~ 20, and molecular weight is 20 ~ 500,000, can provide less aperture, and improve ion by performance, closed pore temperature is low, and closed pore speed is fast.
The High molecular weight polyethylene of layer structure must have the degree of branching of >15, and the high density polyethylene (HDPE) in intermediate layer must have the degree of branching of <20.Battery diaphragm of the present invention requires that polyolefine material has the specific degree of branching, and hinder large between the polyethylene molecule that the degree of branching is large, in Thermal inactive process, major part maintains original frame structure, and make the membrane pore size of preparation comparatively large, thermal contraction is less; And hinder less between the little polyethylene molecule of the degree of branching, when Thermal inactive occurs in extrudate cooling, polyethylene molecule spacing reduces, and aperture structure originally shrinks so form fine pore structure.
As further technical scheme of the present invention, the porosity of described High molecular weight polyethylene layer is greater than 45%, and the porosity of described high-density polyethylene layer is 30 ~ 45%.
As further technical scheme of the present invention, the average pore diameter of described High molecular weight polyethylene layer is 0.15 ~ 0.3 μm, and the average pore diameter of described high-density polyethylene layer is 0.02 ~ 0.15 μm.
Preferably, the average pore diameter of described High molecular weight polyethylene layer is 0.2 ~ 0.25 μm, and the average pore diameter of described high-density polyethylene layer is 0.04 ~ 0.08 μm.
Battery diaphragm intermediate layer of the present invention has less aperture, can close aperture in time, close current when high-temperature test, improves the security performance of battery.In addition, because aperture is less, there is good capillary imbibition ability, the wetting velocity of barrier film can be improved.Battery diaphragm skin of the present invention has larger aperture and less thermal contraction, be conducive to the contact angle reducing electrolyte, improve the wetting property of barrier film, there is less thermal contraction simultaneously, prevent barrier film thermal histories septation from shrinking and cause battery pole piece directly to contact.
If the aperture of battery diaphragm is more than 0.3 μm, easily makes the metal particle of positive and negative pole material through barrier film, do not have the buffer action of barrier film.If aperture is less than 0.02 μm, easily make the wetting property of barrier film be deteriorated, the larger ion transmission performance affecting battery, macro manifestations is that the power-performance of battery is poor.The present invention finds through research, if aperture is more than 0.3 μm, battery is very easy to smolder on fire when high temperature 130 DEG C of thermal shocks, thus affects the security performance of battery diaphragm.The thermal shock safety feature test of 130 DEG C is the hard requirement of battery industry, and this phenomenon occurs mainly because aperture is excessive, polyethylene micropore closes performance failure, and battery continues intensification to be caused molten the breaking of barrier film and is short-circuited.
As further technical scheme of the present invention, the gross thickness of described battery diaphragm is 12 ~ 40 μm, and in order to keep good closed pore performance, the thickness of described high-density polyethylene layer is more than or equal to 3 μm and is less than or equal to 2/3 of gross thickness.The thickness of battery diaphragm is excessive, and the battery plus-negative plate material of unit volume will be caused to reduce, and reduces the capacity of battery.
A preparation method for lithium ion battery separator, comprises the following steps:
(1) High molecular weight polyethylene layer is prepared: the melting mixing in double screw extruder by High molecular weight polyethylene and paraffin oil, obtains polymer solution A;
(2) high-density polyethylene layer is prepared: the melting mixing in double screw extruder by high density polyethylene (HDPE) and paraffin oil, obtains polymer solution B;
(3) co-extrusion: polymer solution A and polymer solution B is input in the T-shaped die head in three chambeies by the mode of ABA continuously, extrudes from same die orifice after merging together, obtain the melt of ABA three-decker;
(4) masking: by obtained three-decker melt feeding biaxial orientation stretching machine, under 100 ~ 140 DEG C of conditions, carries out bi-directional synchronization stretching or step drawing becomes film;
(5) extract: use extractant extraction to remove the paraffin oil of film surface;
(6) shape: under 100 ~ 140 DEG C of conditions, carry out thermal finalization, obtain lithium ion battery separator.
As further technical scheme of the present invention, the degree of branching of described High molecular weight polyethylene is 15 ~ 80, and molecular weight is 50 ~ 3,000,000; The degree of branching of described high density polyethylene (HDPE) is 2 ~ 20, and molecular weight is 20 ~ 500,000.
As further technical scheme of the present invention, the porosity of described High molecular weight polyethylene layer is greater than 45%, and the porosity of described high-density polyethylene layer is 30 ~ 45%; The average pore diameter of described High molecular weight polyethylene layer is 0.15 ~ 0.3 μm, and the average pore diameter of described high-density polyethylene layer is 0.02 ~ 0.15 μm.
As further technical scheme of the present invention, described in step (1), the mass ratio of High molecular weight polyethylene and paraffin oil is 1:2 ~ 1:6, and the mass ratio of described high density polyethylene (HDPE) and paraffin oil is 1:1 ~ 1:5.
As further technical scheme of the present invention, the extractant described in step (3) is the one of carrene, heptane, n-hexane.
Compared to existing technology, beneficial effect of the present invention is:
1) the outer field aperture of the present invention is larger, contribute to the lyophily performance improving barrier film and electrolyte when material is constant like this, and the fine pore of internal layer can help electrolyte to form capillarity attraction in barrier film, aperture is less, capillarity attraction is larger, contributes to electrolyte parent's profit barrier film fast like this.
2) because outer field aperture is comparatively large, fiber is also comparatively thick, and percent thermal shrinkage is less, and the aperture of internal layer is little, and in battery thermal shock process, easy aperture closes, and close current prevents the short circuit of battery from exploding, and improves security performance.
3) barrier film of the present invention can solve barrier film absorbent, can solve cell safety unfailing performance again, and present invention process is simple, is easy to industrialization.
4) the present invention is compared with existing barrier film production technology, and process conditions are similar, but the physicochemical properties such as the percent thermal shrinkage of product, closed pore temperature are better.
Embodiment
Embodiment 1:
By the high density polyethylene (HDPE) (HDPE of 20% percentage by weight, the degree of branching 10, molecular weight 300,000) add a wherein double screw extruder (diameter 58mm, L/D=48), again the paraffin oil of 80% percentage by weight being joined double screw extruder by side direction feeding, by making HDPE melt extrude under 210 DEG C and 150rpm condition in double screw extruder, forming high density polyethylene (HDPE) solution, the solution obtained is extruded by the sandwich layer of measuring pump from three layers of die head, thickness 500 μm.
Simultaneously by the High molecular weight polyethylene (MDPE of 20% percentage by weight, the degree of branching 40, molecular weight 800,000) add another double screw extruder (diameter 58mm, L/D=48), again the paraffin oil of 80% percentage by weight being joined double screw extruder by side direction feeding, by making MDPE melt extrude under 210 DEG C and 150rpm condition in double screw extruder, forming homogeneous solution, the solution obtained is extruded by two top layers of measuring pump from three layers of die head, the thickness of every layer 500 μm.
Room temperature is cooled to the cooldown rate being greater than 40 DEG C/min by cold water roller by the diaphragm of die head co-extrusion, obtained thickness is about the gel threeply sheet film of 1500 μm, diaphragm then biaxial tension 5 × 5 times at 120 DEG C, film after stretching by washing (hexanes wash), dry and at 120 DEG C thermal finalization 60 second, obtain threeply degree than being the porous multilayer composite diaphragm of 25um for 1:1:1 gross thickness.
Embodiment 2:
Be that the degree of branching of interior hdpe layer is 8 with the difference of embodiment 1, the degree of branching of outer High molecular weight polyethylene is 65.
Embodiment 3:
Be that the Thickness Ratio of trilaminate material is 1:5:1 with the difference of embodiment 1.
Comparative example 1:
Be that three-decker is High molecular weight polyethylene layer with the difference of embodiment 1.
Comparative example 2:
Be that three-decker is high-density polyethylene layer with the difference of embodiment 1.
Method of testing:
1) opening size test method: adopt capillary flow assay method, surface tension is selected to be the infiltration liquid of 15.9mN/m, being entirely the saturated sample of infiltrate by one is placed in sample room, sample room is flowed to by above gaseous sample, liquid in hole is discharged by gas under certain pressure completely, record gas pressure and flow rate, then according to formulae discovery pore size and distribution.
2) battery thermal shock percent of pass: be prepare battery under same process condition, 1h test battery short circuit case of fire at 130 DEG C.
3) wetting velocity: at 25 DEG C, get 20mm wide, the strip barrier film that 30cm is long, immerses electrolyte degree of depth 2cm, the climbing speed of test electrolyte in barrier film.
The performance test results of embodiment and the barrier film shown in comparative example:
Table 1 barrier film test result
As known from Table 1, the present invention is compared with comparative example, and electrolyte contacts angle of the present invention is less, and the lyophily of barrier film and electrolyte is functional, and electrolyte is parent's profit barrier film fast; Percent thermal shrinkage excellent performance, closed pore speed is fast, and battery thermal shock percent of pass is high, and easy aperture closes, and prevents the short circuit of battery from exploding, and improves security performance.The thickness of the battery diaphragm of embodiment 3 is excessive, and cause its thermal shock percent of pass lower, not easily aperture closes, and reduces the security performance of battery, and the short circuit blast of battery easily occurs.
Above-mentioned execution mode is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, change and the replacement of any unsubstantiality that those skilled in the art does on basis of the present invention all belong to the present invention's scope required for protection.
Claims (8)
1. a lithium ion battery separator, is characterized in that: be made up of High molecular weight polyethylene layer, high-density polyethylene layer, High molecular weight polyethylene layer, and wherein high-density polyethylene layer is intermediate layer; Described High molecular weight polyethylene layer is 15 ~ 80 by the degree of branching, and molecular weight is the High molecular weight polyethylene composition of 50 ~ 3,000,000, and described high-density polyethylene layer is 2 ~ 20 by the degree of branching, and molecular weight is the high density polyethylene (HDPE) composition of 20 ~ 500,000;
The average pore diameter of described High molecular weight polyethylene layer is 0.15 ~ 0.3 μm, and the average pore diameter of described high-density polyethylene layer is 0.02 ~ 0.15 μm.
2. lithium ion battery separator according to claim 1, is characterized in that: the porosity of described High molecular weight polyethylene layer is greater than 45%, and the porosity of described high-density polyethylene layer is 30 ~ 45%.
3. lithium ion battery separator according to claim 1, is characterized in that: the average pore diameter of described High molecular weight polyethylene layer is 0.2 ~ 0.25 μm, and the average pore diameter of described high-density polyethylene layer is 0.04 ~ 0.08 μm.
4. lithium ion battery separator according to claim 1, is characterized in that: the gross thickness of described battery diaphragm is 12 ~ 40 μm, and the thickness of described high-density polyethylene layer is more than or equal to 3 μm and is less than or equal to 2/3 of gross thickness.
5. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that comprising the following steps:
(1) High molecular weight polyethylene layer is prepared: the melting mixing in double screw extruder by High molecular weight polyethylene and paraffin oil, obtains polymer solution A;
(2) high-density polyethylene layer is prepared: the melting mixing in double screw extruder by high density polyethylene (HDPE) and paraffin oil, obtains polymer solution B;
(3) co-extrusion: polymer solution A and polymer solution B is input in the T-shaped die head in three chambeies by the mode of ABA continuously, extrudes from same die orifice after merging together, obtain the melt of ABA three-decker;
(4) masking: by obtained three-decker melt feeding biaxial orientation stretching machine, under 100 ~ 140 DEG C of conditions, carries out bi-directional synchronization stretching or step drawing becomes film;
(5) extract: use extractant extraction to remove the paraffin oil of film surface;
(6) shape: under 100 ~ 140 DEG C of conditions, carry out thermal finalization, obtain lithium ion battery separator.
6. a preparation method for lithium ion battery separator as claimed in claim 5, is characterized in that: the porosity of described High molecular weight polyethylene layer is greater than 45%, and the porosity of described high-density polyethylene layer is 30 ~ 45%.
7. the preparation method of a lithium ion battery separator as claimed in claim 5, it is characterized in that: described in step (1), the mass ratio of High molecular weight polyethylene and paraffin oil is 1:2 ~ 1:6, the mass ratio of described high density polyethylene (HDPE) and paraffin oil is 1:1 ~ 1:5.
8. a preparation method for lithium ion battery separator as claimed in claim 5, is characterized in that: the extractant described in step (5) is the one of carrene, heptane, n-hexane.
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| CN201310432961.5A CN103531734B (en) | 2013-09-22 | 2013-09-22 | A kind of lithium ion battery separator and preparation method |
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| CN103531734B true CN103531734B (en) | 2016-04-13 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4148892A1 (en) * | 2015-07-31 | 2023-03-15 | Celgard, LLC | Laminated multilayer membranes, separators, batteries, and methods |
| EP3553849A4 (en) * | 2017-11-08 | 2019-12-04 | LG Chem, Ltd. | Separator and electrochemical device comprising same |
| CN110054855B (en) * | 2019-02-18 | 2021-10-15 | 浙江格尔泰斯环保特材科技股份有限公司 | Polytetrafluoroethylene bubble point membrane and preparation method thereof |
| DE102019112089A1 (en) * | 2019-05-09 | 2020-11-12 | Brückner Maschinenbau GmbH & Co. KG | Film with at least two layers and method for their manufacture |
| CN113745756A (en) * | 2021-08-24 | 2021-12-03 | 中材锂膜有限公司 | Low-closed-pore high-film-breaking polyethylene lithium battery diaphragm and preparation method thereof |
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| DE10038789A1 (en) * | 2000-08-09 | 2002-02-21 | Nbt Gmbh | Nickel/metal hydride secondary element used for a battery comprises a positive nickel hydroxide electrode provided with a three-dimensional metallic conducting structure containing a nickel hydroxide coated with discrete particles of copper |
| JP5450929B2 (en) * | 2007-04-09 | 2014-03-26 | 東レバッテリーセパレータフィルム株式会社 | Polyolefin multilayer microporous membrane, method for producing the same, battery separator and battery |
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| CN100522602C (en) * | 2003-04-04 | 2009-08-05 | 旭化成电子材料株式会社 | Polyolefin microporous membrane |
| CN101208198A (en) * | 2005-06-24 | 2008-06-25 | 东燃化学株式会社 | Polyethylene multilayer microporous membrane, battery separator using same, and battery |
| CN102131571A (en) * | 2008-09-02 | 2011-07-20 | 东丽东燃机能膜合同会社 | Microporous polymeric membranes, methods for making such membranes, and the use of such membranes as battery separator film |
| CN102064300A (en) * | 2010-12-25 | 2011-05-18 | 佛山塑料集团股份有限公司 | Porous composite diaphragm for lithium ion secondary battery and preparation method thereof |
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