CN103531734A - Lithium-ion battery diaphragm and preparation method thereof - Google Patents
Lithium-ion battery diaphragm and preparation method thereof Download PDFInfo
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- CN103531734A CN103531734A CN201310432961.5A CN201310432961A CN103531734A CN 103531734 A CN103531734 A CN 103531734A CN 201310432961 A CN201310432961 A CN 201310432961A CN 103531734 A CN103531734 A CN 103531734A
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- molecular weight
- polyethylene layer
- ion battery
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The invention relates to a lithium-ion battery diaphragm which comprises a high molecular weight polyethylene layer, a high density polyethylene layer and a high molecular weight polyethylene layer, wherein the high molecular weight polyethylene layer comprises high molecular weight polyethylene with a branching coefficient of 15-80 and a molecular weight of 50-3,000,000, and the high density polyethylene layer comprises high density polyethylene with a branching coefficient of 2-20 and a molecular weight of 20-5,00,000. The first polyethylene layer and the second polyethylene layer are prepared by a dual-extruder extruder through steps of co-extruding, film-preparing, extracting and sizing. The lithium-ion battery diaphragm is larger in pole diameter of an outer layer so that the lyophilic performance of the diaphragm and the electrolyte is favorably improved; and the electrolyte forms a capillary suction force in the diaphragm due to the adoption of the hole diameter of an inner layer, and the electrolyte rapidly moisturizes the diaphragm. Due to larger hole diameter of the outer layer, fibers are thicker, and the heat shrinkage is small; and the hole diameter of the inner layer is small, the hole diameter is easily closed in a battery heat impact process, and thus the short circuit explosion of the battery is prevented, and the safety performance is improved.
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 being applied in lithium ion battery prevents that battery short circuit has certain pore structure simultaneously and can guarantee one of significant components of the lithium ion battery that lithium ion passes through smoothly.
Conventionally lithium ion battery separator selected materials all has good electrical insulation capability, and the principal element that affects 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 barrier film to have specific pore structure, this ion that is not only being related to barrier film, by performance, also affects the safe application performance of battery.
In patent CN103081171A, proposed a kind of three layers of barrier film containing coating, it is 0.01～1 μ m that its whole aperture requires, and has mainly solved the laminated plug-hole problem of three layers of barrier film, and its pore diameter range is too wide in range, also has no the aperture design to each layer of structure.
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 the degree of branching of diaphragm material is not carried out to special requirement.Conventionally in order to guarantee that barrier film has good absorbent, conventionally require the air permeability of barrier film little, it is high that porosity is wanted, 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 and causes the slow problem of closed pore, causes the security performance test percent of pass such as acupuncture, thermal shock 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, solve the lithium ion battery separator of diaphragm closed pore security performance simultaneously.
Another object of the present invention is to provide a kind of preparation method of lithium ion battery separator.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
A kind of lithium ion battery separator, it comprises sandwich diaphragm, by High molecular weight polyethylene layer/high-density polyethylene layer/High molecular weight polyethylene layer, formed, described High molecular weight polyethylene layer is 15～80 by the degree of branching, molecular weight is 50～3,000,000 High molecular weight polyethylene composition, described high-density polyethylene layer is 2～20 by the degree of branching, and molecular weight is 20～500,000 high density polyethylene (HDPE) composition.
The degree of branching is the branched carbon atomicity 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, molecular weight is 50～3,000,000, and good intensity and heat-shrinkable are provided, and has improved 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, and less aperture can be provided, and improves ion by performance, and closed pore temperature is low, and closed pore speed is fast.
The High molecular weight polyethylene of layer structure must have>15 the degree of branching, the high density polyethylene (HDPE) in intermediate layer must have<20 the degree of branching.Battery diaphragm of the present invention requires polyolefine material to have the specific degree of branching, hinders greatly between the large polyethylene molecule of the degree of branching, and in thermic phase separation, major part has kept original frame structure, makes the membrane pore size of preparation larger, and thermal contraction is less; And between the little polyethylene molecule of the degree of branching, hinder littlely, when the cooling generation thermic of extrudate is separated, polyethylene molecule spacing is dwindled, so aperture structure originally shrinks, forms 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 μ m, and the average pore diameter of described high-density polyethylene layer is 0.02～0.15 μ m.
Preferably, the average pore diameter of described High molecular weight polyethylene layer is 0.2～0.25 μ m, and the average pore diameter of described high-density polyethylene layer is 0.04～0.08 μ m.
Battery diaphragm of the present invention intermediate layer has less aperture, closed aperture in time when high-temperature test, and close current, improves the security performance of battery.In addition, because aperture is less, there is good capillary imbibition ability, can improve the wetting velocity of barrier film.Battery diaphragm skin of the present invention has larger aperture and less thermal contraction, be conducive to reduce the contact angle of electrolyte, the wetting property that improves barrier film has less thermal contraction simultaneously, prevents that barrier film is shunk by thermal process septation and causes battery pole piece directly to contact.
If the aperture of battery diaphragm surpasses 0.3 μ m, easily make 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 μ m, easily make the wetting property variation of barrier film, the larger ion transmission performance that affects battery, the power-performance that macro manifestations is battery is poor.The present invention is through research discovery, if aperture surpasses 0.3 μ m, battery is very easy to smolder on fire when 130 ℃ of thermal shocks of high temperature, thereby affects the security performance of battery diaphragm.The thermal shock safety feature test of 130 ℃ is the rigid requirement of battery industry, and it is mainly because aperture is excessive that this phenomenon occurs, the closed performance failure of polyethylene micropore, and battery continues to heat up and causes barrier film to melt broken and be short-circuited.
As further technical scheme of the present invention, the gross thickness of described battery diaphragm is 12～40 μ m, and in order to keep good closed pore performance, the thickness of described high-density polyethylene layer is more than or equal to 3 μ m and is less than or equal to 2/3 of gross thickness.The thickness of battery diaphragm is excessive, will cause the battery plus-negative plate material of unit volume to reduce, and reduces the capacity of battery.
A preparation method for lithium ion battery separator, comprises the following steps:
(1) prepare High molecular weight polyethylene layer: the melting mixing in double screw extruder by High molecular weight polyethylene and paraffin oil, obtains polymer solution A;
(2) prepare high-density polyethylene layer: 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 are input in the T-shaped die head in three chambeies continuously by the mode of ABA, extrude from same die orifice after merging together, obtain the melt of ABA three-decker;
(4) masking: resulting three-decker melt is sent into biaxial orientation stretching machine, under 100～140 ℃ of conditions, carry out bi-directional synchronization stretching or step drawing and become film;
(5) extraction: use extractant extraction to remove the paraffin oil of film surface;
(6) sizing: under 100～140 ℃ 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 μ m, and the average pore diameter of described high-density polyethylene layer is 0.02～0.15 μ m.
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 a kind of 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 like this to improve the lyophily performance of barrier film and electrolyte in the situation that material is constant, 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 like this electrolyte parent's profit barrier film fast.
2) because outer field aperture is larger, fiber is also thicker, and percent thermal shrinkage is just less, and the aperture of internal layer is little, and in battery thermal shock process, easily aperture is closed, and close current prevents the short circuit blast of battery, improves security performance.
3) barrier film of the present invention can solve barrier film absorbent, can solve cell safety unfailing performance again, and technique of the present invention is simple, is easy to industrialization.
4) the present invention compares 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 is joined to double screw extruder by side direction feeding, by making HDPE melt extrude, form high density polyethylene (HDPE) solution in double screw extruder under 210 ℃ and 150rpm condition, the solution obtaining is extruded from the sandwich layer of three layers of die head by measuring pump, thickness 500 μ m.
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 is joined to double screw extruder by side direction feeding, by making MDPE melt extrude, form homogeneous solution in double screw extruder under 210 ℃ and 150rpm condition, the solution obtaining is extruded from two top layers of three layers of die head by measuring pump, the thickness 500 μ m of every layer.
Diaphragm by die head co-extrusion is cooled to room temperature to be greater than the cooldown rate of 40 ℃/min by cold water roller, make the gel threeply sheet film that thickness is about 1500 μ m, then 5 * 5 times of biaxial tensiones at 120 ℃ of diaphragm, film after stretching by washing (hexane washing), dry and at 120 ℃ 60 seconds of thermal finalization, obtain the threeply degree porous multilayer composite diaphragm that to compare for 1:1:1 gross thickness be 25um.
Embodiment 2:
Be that with the difference of embodiment 1 degree of branching of interior hdpe layer is 8, the degree of branching of outer High molecular weight polyethylene is 65.
Embodiment 3:
Be that with the difference of embodiment 1 Thickness Ratio of trilaminate material is 1:5:1.
Comparative example 1:
Be that with the difference of embodiment 1 three-decker is High molecular weight polyethylene layer.
Comparative example 2:
Be that with the difference of embodiment 1 three-decker is high-density polyethylene layer.
Method of testing:
1) aperture method of testing: adopt Capillary Flow analytic approach, selecting surface tension is the infiltration liquid of 15.9mN/m, by one, being entirely the sample that infiltrate is saturated is placed in sample room, sample room will be flowed to above gaseous sample, gas under certain pressure is discharged liquid in hole completely, record gas pressure and flow rate, then according to formula calculated hole diameters size and distribution.
2) battery thermal shock percent of pass: be to prepare battery under same process condition, 1h test battery short circuit case of fire at 130 ℃.
3) wetting velocity: at 25 ℃, 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 the barrier film shown in embodiment and comparative example:
Table 1 barrier film test result
As known from Table 1, the present invention compares with comparative example, and electrolyte contact 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 performance is good, and closed pore speed is fast, and battery thermal shock percent of pass is high, and easily aperture is closed, prevents the short circuit blast of battery, improves security performance.The thickness of the battery diaphragm of embodiment 3 is excessive, causes its thermal shock percent of pass lower, is difficult for aperture closure, 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, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (10)
1. a lithium ion battery separator, it is characterized in that: by High molecular weight polyethylene layer, high-density polyethylene layer, High molecular weight polyethylene layer, formed, described High molecular weight polyethylene layer is 15～80 by the degree of branching, molecular weight is 50～3,000,000 High molecular weight polyethylene composition, described high-density polyethylene layer is 2～20 by the degree of branching, and molecular weight is 20～500,000 high density polyethylene (HDPE) composition.
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 2, is characterized in that: the average pore diameter of described High molecular weight polyethylene layer is 0.15～0.3 μ m, and the average pore diameter of described high-density polyethylene layer is 0.02～0.15 μ m.
4. lithium ion battery separator according to claim 3, is characterized in that: the average pore diameter of described High molecular weight polyethylene layer is 0.2～0.25 μ m, and the average pore diameter of described high-density polyethylene layer is 0.04～0.08 μ m.
5. lithium ion battery separator according to claim 1, is characterized in that: the gross thickness of described battery diaphragm is 12～40 μ m, and the thickness of described high-density polyethylene layer is more than or equal to 3 μ m and is less than or equal to 2/3 of gross thickness.
6. a preparation method for lithium ion battery separator as claimed in claim 1, is characterized in that comprising the following steps:
(1) prepare High molecular weight polyethylene layer: the melting mixing in double screw extruder by High molecular weight polyethylene and paraffin oil, obtains polymer solution A;
(2) prepare high-density polyethylene layer: 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 are input in the T-shaped die head in three chambeies continuously by the mode of ABA, extrude from same die orifice after merging together, obtain the melt of ABA three-decker;
(4) masking: resulting three-decker melt is sent into biaxial orientation stretching machine, under 100～140 ℃ of conditions, carry out bi-directional synchronization stretching or step drawing and become film;
(5) extraction: use extractant extraction to remove the paraffin oil of film surface;
(6) sizing: under 100～140 ℃ of conditions, carry out thermal finalization, obtain lithium ion battery separator.
7. a preparation method for lithium ion battery separator as claimed in claim 6, is characterized in that: 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.
8. a preparation method for lithium ion battery separator as claimed in claim 6, 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%; The average pore diameter of described High molecular weight polyethylene layer is 0.15～0.3 μ m, and the average pore diameter of described high-density polyethylene layer is 0.02～0.15 μ m.
9. the preparation method of a lithium ion battery separator as claimed in claim 6, 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.
10. a preparation method for lithium ion battery separator as claimed in claim 6, is characterized in that: the extractant described in step (3) is a kind of of carrene, heptane, n-hexane.
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| CN108352480A (en) * | 2015-07-31 | 2018-07-31 | 赛尔格有限责任公司 | Improved laminated multilayer film, partition board, battery and method |
| CN110054855A (en) * | 2019-02-18 | 2019-07-26 | 浙江格尔泰斯环保特材科技股份有限公司 | A kind of polytetrafluoroethylene (PTFE) bubble point film and preparation method thereof |
| CN110249450A (en) * | 2017-11-08 | 2019-09-17 | 株式会社Lg化学 | Partition and electrochemical appliance including the partition |
| 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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| 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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|---|---|
| CN103531734B (en) | 2016-04-13 |
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