CN108389999A - Organic and inorganic composite coated porous separation film, preparation method and its lithium ion battery - Google Patents
Organic and inorganic composite coated porous separation film, preparation method and its lithium ion battery Download PDFInfo
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- CN108389999A CN108389999A CN201810063661.7A CN201810063661A CN108389999A CN 108389999 A CN108389999 A CN 108389999A CN 201810063661 A CN201810063661 A CN 201810063661A CN 108389999 A CN108389999 A CN 108389999A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic 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
- H01M50/409—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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Abstract
It is a kind of organic,Inorganic compounding coats porous separation film,Preparation method and its lithium ion battery,Wherein,This is organic,Inorganic compounding coating porous separation film includes porous substrate and is attached to organic on two surfaces of porous substrate,Inorganic compounding functional coating,This is organic,Inorganic compounding functional coating includes Kynoar,Inorganic ceramic particle,Aqueous high molecular thickener and waterborne polymeric binder,The value range of the grain size D50 of Kynoar is 2~4um,The copolymerization degree of Kynoar is between 3%~10% and melting temperature is between 115 DEG C~150 DEG C,The weight of Kynoar accounts for described organic,The value range of the weight percent of inorganic compounding functional coating total weight is 20~50%,The value range of the grain size D50 of inorganic ceramic particle is 0.4~0.8um,The weight of inorganic ceramic particle accounts for described organic,The value range of the weight percent of inorganic compounding functional coating total weight is 40~70%.The present invention has the advantages that performance is excellent, manufacturing cost is lower, the security performance of battery and the stability that recycles for a long time are also improved.
Description
Technical field
The present invention relates to field of lithium ion battery, prepared by especially a kind of organic and inorganic composite coated porous separation film
Method and its lithium ion battery.
Background technology
Lithium ion battery with its high-energy density, high working voltage, has had extended cycle life, without note since being commercialized popularization
Recall effect, safety and environmental protection and can be widely used as according to many advantages, such as actual demand flexible design size various portable
The power supply of electronic apparatus, various application field and a variety of different actual demands greatly pushed lithium ion battery material with
And the development of lithium-ion electric pool process.
Currently, the isolation film used in lithium ion battery is largely polyolefin film, such as polyethylene film（PE）, polypropylene screen
（PP）Or polypropylene, polyethylene/polypropylene composite film（PP/PE/PP）, the fusing point of this polyolefin-based isolation film 130 DEG C~
Within the scope of 170 DEG C, it is widely used in lithium ion battery.But in actual use, on the one hand, when encountering as short
Road overcharges, when thermal shock or puncture, and the internal temperature of lithium ion battery can reach 100 DEG C or more, at this point, this poly-
Alkene film is heated just to have larger contraction or melting, and the volume of diaphragm is caused to change, so cause anode and cathode it
Between be in direct contact, there is the phenomenon that internal short-circuit and thermal runaway, make lithium ion battery be easy to catch fire even explode.In addition, by
It is very low in the surface tension of polyolefin film, the wetting capacity for the carbonic ester electrolyte that lithium rechargeable battery is used and imbibition
Ability is all poor, can not meet the requirement of lithium rechargeable battery long circulation life.On the other hand, with lithium ion battery
The exploitation of high volume energy density, high gram volume（360mAh/g）Graphite material, high electrode compacted density, thin collector
Etc. battery designs scheme application so that bulking effect of the negative material in charge and discharge process is more and more apparent, so as to cause
Expansion, deformation and the precipitation of Li dendrite of the battery core in cyclic process, so greatly reduce battery cycle life and
Security reliability.
For the above both of these case, existing way is that first the one or both sides coating inorganic in polyolefine isolating film is made pottery
Porcelain particle, the functional polymer for then coating water-based system or organic solvent system on the two sides of ceramic coating membrane again are poly- inclined
Vinyl fluoride finally obtains the inorganic of level coated structure, organic functional coating improved polyalkene isolation film.Due to inorganic coating
With higher thermal stability, therefore the thermal contraction of entire composite diaphragm is inhibited significantly, while inorganic coating is also with higher
Mechanical strength, this can also reduce Li dendrite or particle and collector burr etc. in battery and puncture isolation film and cause short circuit
Probability, and then improve the reliability and security performance of battery.In addition, inorganic coating also has good electrolyte wellability, change
It has been apt to the chemical property and cycle life of battery.Meanwhile secondary coating is formed by functionalized coating, realizes diaphragm
Effective bonding on surface and battery positive and negative electrode interface improves the interface stickiness of inside battery multilayered structure with this, inhibits Soft Roll
Warpage, deformation and the precipitation of Li dendrite of polymer Li-ion battery, to realize stability and peace that battery recycles for a long time
The improvement of full property.This traditional way undoubtedly solve encountered when polyalkene diaphragm uses in lithium ion battery it is a series of
Problem.
But it is above-mentioned in polyolefine isolating film coating inorganic, organic functional coating, not only operation is not easy to carry out, together
When also result in high material cost and manufacturing cost so that the manufacturing cost of lithium ion battery greatly increases.
Based on the above issues, it is necessory to provide it is a kind of can effectively solve these problems, while reaching safe and environment-friendly, high
Effect and effectively reduce manufacturing cost functional coating scheme, the security performance so as to improve battery and the stabilization that recycles for a long time
Property.
Invention content
In order to overcome the above problem, the present invention provides that a kind of performance is excellent, manufacturing cost is lower, battery to society
The organic and inorganic composite coated porous separation film that security performance and the stability recycled for a long time are also improved.
That the present invention also provides a kind of performances is excellent, manufacturing cost is lower, the security performance of battery and recycles for a long time
The preparation method for the organic and inorganic composite coated porous separation film that stability is also improved.
That the present invention also provides a kind of performances is excellent, manufacturing cost is lower, the security performance of battery and recycles for a long time
The lithium ion battery that stability is also improved.
That the present invention also provides a kind of performances is excellent, manufacturing cost is lower, the security performance of battery and recycles for a long time
The preparation method for the organic and inorganic composite coated porous separation film that stability is also improved.
That the present invention also provides a kind of performances is excellent, manufacturing cost is lower, the security performance of battery and recycles for a long time
The lithium ion battery that stability is also improved.
The technical scheme is that：A kind of organic and inorganic composite coated porous separation film, including porosity base are provided
Material and the organic and inorganic Complex Function coating being attached on two surfaces of the porous substrate, this is organic and inorganic compound
Functional coating includes Kynoar, inorganic ceramic particle, aqueous high molecular thickener and waterborne polymeric binder, spy
Sign is：The value range of the grain size D50 of the Kynoar is 2~4um, and Kynoar is by hexafluoropropene, inclined fluorine
The copolymerization degree of copoly type high molecular polymer made of ethylene copolymer, Kynoar is between 3%~10% and melting temperature
Between 115 DEG C~150 DEG C, the weight of Kynoar accounts for the weight of the organic and inorganic Complex Function total coating weight
The value range of percentage is 20~50%, and the value range of the grain size D50 of inorganic ceramic particle is 0.4~0.8um, weight
The value range for accounting for the weight percent of the organic and inorganic Complex Function total coating weight is 40~70%.
As improvement of the present invention, the inorganic ceramic particle is the electrical insulating material that dielectric constant is more than or equal to 4.
As improvement of the present invention, the inorganic ceramic particle be SiO2, Al2O3, γ-AlOOH, BaSO4, CaO,
One or more of TiO2, ZnO2, MgO, ZrO2 and SnO2.
As improvement of the present invention, the waterborne polymeric binder is phenylethylene ethylene/propenoic acid ester copolymer emulsion, acetic acid
Ethene/acrylic ester copolymer emulsion, vinyl acetate/fatty acid vinyl ester copolymer emulsion, organosilicon acrylic ester copolymerization emulsion,
And at least one of acrylate copolymer emulsion.
As improvement of the present invention, the weight of the waterborne polymeric binder accounts for the organic and inorganic complex function
The value range for changing the weight percent of total coating weight is 2~9%.
As improvement of the present invention, the aqueous high molecular thickener be sodium carboxymethylcellulose, hydroxymethyl cellulose,
At least one of hydroxyethyl cellulose, polyacrylamide, sodium alginate and polyvinyl alcohol.
As improvement of the present invention, the weight of the aqueous high molecular thickener accounts for the organic and inorganic complex function
The value range for changing the weight percent of total coating weight is 1~2%.
As improvement of the present invention, aqueous slurry used by the coating of the organic and inorganic Complex Function coating
Amount of solid content between 30%~50%.
As improvement of the present invention, the value range of the thickness of the organic and inorganic Complex Function coating is 2~6 μ
m。
As improvement of the present invention, the porous substrate is polyethylene film, polypropylene screen, polypropylene, polyethylene/poly-
Propylene composite membrane, cellulose membrane or be polyimide film.
As improvement of the present invention, the value range of the thickness of the porous substrate is 5 μm~25 μm.
As improvement of the present invention, the value range of the porosity of the porous substrate is 20%~70%.
The present invention also provides a kind of preparation methods of above-mentioned organic and inorganic composite coated porous separation film, including with
Lower step：
（S1）, by waterborne polymeric binder dispersion in deionized water formed waterborne polymeric binder solution；
（S2）, inorganic ceramic particle, organic functions polyphosphazene polymer vinylidene be dispersed in deionized water and has dissolved in advance
In water soluble polymer thickener, and it is mixed and is formed uniformly mixed dispersion liquid.
（S3）, to step（S2）Step is added in the mixed dispersion liquid of middle formation（S1）Obtained waterborne polymeric bonds
It in agent solution, is uniformly dispersed, the weight for being adjusted to solid part accounts for the 30%~50% of slurry total amount, obtains coating slurry；
（S4）, by step（S3）Obtained slurry is coated in porous substrate by way of dimple version or by extrusion coated
On two surfaces, organic and inorganic composite coated porous separation film is obtained after drying.
The present invention also provides a kind of lithium ion battery, including anode, cathode, be interval in it is more between the positive electrode and negative electrode
Permeability isolation film and electrolyte, the porous separation film are organic, the nothing described in any one of claim 1 to 13
Machine composite coated porous separation film.
Why the present invention selects function modified coating of the copoly type polyvinylidene fluoride material as diaphragm, be because with
The increase of hexafluoropropene copolymerization content, the crystallinity of polymer reduce in polyvinylidene fluoride polymer main chain, and fusing point reduces, and
Swellbility in electrolyte increases.Since Kynoar belongs to crystalline polymer, and there was only wherein unformed amorphous portion
Point macromolecular chain comes with higher mobility and material to be bonded generates intermolecular interaction, the high score of crystalline portion
Subchain because of the interaction between its regular arrangement architecture and molecule segment, interaction and molecule segment with material to be bonded
Mobility is significantly reduced.In addition, the presence of crystalline structure also can further limit the activity of amorphism polymer segment
Ability.The presence of hexafluoropropene comonomer can break the regularity of polyvinylidene fluoride polymer strand, reduce and gather inclined fluorine
Polyvinyl crystallinity improves the mobility of molecule segment, improves the bonding characteristic of polymer.But with copolymerization degree
It improves, crystallinity reduces, and melting point polymer also declines therewith, and swellbility in the electrolytic solution can also increase therewith.For diaphragm
For the polymer coating on surface, higher polymer swellbility and coating thickness influence whether lithium ion pole piece interface biography
Efficiency is led, to increase battery core internal resistance and activation polarization, causes the embedding lithium of anode insufficient or the excessive embedding lithium of part, it is adjoint
The progress for cyclic process, cause high rate performance decaying and capacity can not reverse recovery and security performance reduction.So
In the present solution, the characteristics of we combine organic, inorganic mixing coating layer, the characteristic of material and lithium ion battery electrochemical system pair
The requirement of coating limits organic Kynoar particle and inorganic ceramic particle first on physical size.It is larger
Kynoar particle and smaller ceramic particle be combined, it can be ensured that larger Kynoar particle appears in coating
Surface, to realize the interface adhesion with lithium battery pole slice, and smaller ceramic particle can be filled in larger polyvinylidene fluoride
Around alkene particle and coating bottom strata, the caking property of diaphragm and battery pole piece not only ensure that in this way, but also realize inorganic ceramic
The filling of grain, solves the problems, such as diaphragm high heat resistance.Secondly, according to the high temperature resistance of diaphragm, diaphragm and battery pole piece
Between cohesive force and circulating battery situation, adjust the copolymerization degree of Kynoar and the weight ratio of itself and inorganic ceramic particle
Example；Therefore, the present invention has that performance is excellent, manufacturing cost is lower, the security performance of battery and the stability recycled for a long time
Also the advantages of obtaining improving.
Specific implementation mode
The present invention provides a kind of organic and inorganic composite coated porous separation film, including porous substrate and is attached to institute
The organic and inorganic Complex Function coating on two surfaces of porous substrate is stated, the organic and inorganic Complex Function coating packet
Containing Kynoar, inorganic ceramic particle, aqueous high molecular thickener and waterborne polymeric binder, the Kynoar
The value range of grain size D50 is 2~4um, and Kynoar is the copoly type high score made of hexafluoropropene, vinylidene copolymerization
The copolymerization degree of sub- polymer, Kynoar is between 3%~10% and melting temperature is between 115 DEG C~150 DEG C, gathers inclined fluorine
The value range that the weight of ethylene accounts for the weight percent of the organic and inorganic Complex Function total coating weight is 20~50%,
The value range of the grain size D50 of inorganic ceramic particle is 0.4~0.8um, and weight accounts for the organic and inorganic Complex Function and applies
The value range of the weight percent of layer total weight is 40~70%.In the present invention, it is preferred that the inorganic ceramic particle is to be situated between
Electric constant is more than or equal to 4 electrical insulating material.
In the present invention, it is preferred that the inorganic ceramic particle is SiO2、Al2O3、γ-AlOOH、BaSO4、CaO、TiO2、
ZnO2、MgO、ZrO2And SnO2One or more of.
In the present invention, it is preferred that the waterborne polymeric binder is phenylethylene ethylene/propenoic acid ester copolymer emulsion, acetic acid second
Alkene/acrylate copolymer emulsion, vinyl acetate/fatty acid vinyl ester copolymer emulsion, organosilicon acrylic ester copolymerization emulsion, with
And at least one of acrylate copolymer emulsion.
In the present invention, it is preferred that the weight of the waterborne polymeric binder accounts for the organic and inorganic Complex Function and applies
The value range of the weight percent of layer total weight is 2~9%.
In the present invention, it is preferred that the aqueous high molecular thickener is sodium carboxymethylcellulose, hydroxymethyl cellulose, hydroxyl
At least one of ethyl cellulose, polyacrylamide, sodium alginate and polyvinyl alcohol.
In the present invention, it is preferred that the weight of the aqueous high molecular thickener accounts for the organic and inorganic Complex Function and applies
The value range of the weight percent of layer total weight is 1~2%.
In the present invention, it is preferred that aqueous slurry consolidates used by the coating of the organic and inorganic Complex Function coating
Body part content is between 30%~50%.
In the present invention, it is preferred that the value range of the thickness of the organic and inorganic Complex Function coating is 2~6 μm.
In the present invention, it is preferred that the porous substrate is polyethylene film, polypropylene screen, polypropylene, polyethylene/poly- third
Alkene composite membrane, cellulose membrane or be polyimide film.
In the present invention, it is preferred that the value range of the thickness of the porous substrate is 5 μm~25 μm.
In the present invention, it is preferred that the value range of the porosity of the porous substrate is 20%~70%.
The present invention also provides a kind of preparation methods of above-mentioned organic and inorganic composite coated porous separation film, including with
Lower step：
（S1）, by waterborne polymeric binder dispersion in deionized water formed waterborne polymeric binder solution；
（S2）, inorganic ceramic particle, organic functions polyphosphazene polymer vinylidene be dispersed in deionized water and has dissolved in advance
In water soluble polymer thickener, and it is mixed and is formed uniformly mixed dispersion liquid.
（S3）, to step（S2）Step is added in the mixed dispersion liquid of middle formation（S1）Obtained waterborne polymeric bonds
It in agent solution, is uniformly dispersed, the weight for being adjusted to solid part accounts for the 30%~50% of slurry total amount, obtains coating slurry；
（S4）, by step（S3）Obtained slurry is coated in porous substrate by way of dimple version or by extrusion coated
On two surfaces, organic and inorganic composite coated porous separation film is obtained after drying.
The present invention also provides a kind of lithium ion battery, including anode, cathode, be interval in it is more between the positive electrode and negative electrode
Permeability isolation film and electrolyte, the porous separation film are the above-mentioned porous sexual isolation of organic and inorganic composite coated
Film.
Embodiment 1
Coating slurry formula is based on siccative weight percent, and coating slurry is by 9wt% waterborne polymerics binder, 1wt% carboxymethyls
Sodium cellulosate, 40wt% Kynoar, four part of 50wt% inorganic ceramics particle composition.Wherein, it is 3% to select copolymerization degree, grain size
Dimension D 50 is 2um, the Kynoar that fusing point is 150 DEG C.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size
For 0.5um.With Al in the present invention2O3To represent, other inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、
MgO、ZrO2, SnO2It is equally applicable to the present invention, the ratio and Al of size dimension particle2O3Equally.Waterborne polymeric binder
Select phenylethylene ethylene/propenoic acid ester copolymer emulsion.In slurry configuration process, solvent is deionized water.Wherein, the weight of solid part accounts for
The slurry total weight about 40wt%.
The preparation process of coating slurry is as follows：
（1）First, waterborne polymeric binder phenylethylene ethylene/propenoic acid ester copolymer emulsion is dispersed in deionized water by the above formula
The middle solution for forming a concentration of 15wt%；
（2）Secondly, by Kynoar, Al2O3The sodium carboxymethylcellulose that particle is dispersed in deionized water and has dissolved in advance
In, and be mixed and be formed uniformly mixed dispersion liquid；
（3）Finally, scattered phenylethylene ethylene/propenoic acid ester copolymer emulsion in advance, dispersion are added into above mixed dispersion liquid
Uniformly, with 150 mesh, slurries filtration is using screen filtration to get to required coating slurry.
It is 12 μm poly- that the coating slurry as made from the above method, which is coated in thickness, using the micro- gravure coater of reverse roll
Ethylene microporous membrane（Porosity is 40%）Two surfaces on, each face coat thickness is about 2 μm, obtains overall thickness and is about
16 μm of organic and inorganic composite coated porous separation film.The porosity that composite porous film is measured with mercury injection apparatus is 41%, with
The basic indifference of porosity of polyethylene micropore film.
The preparation of cathode：
Using graphite as negative electrode active material, weight content is 95 wt%, and using butadiene-styrene rubber as polymeric binder, weight contains
Amount is 3 wt%；Using carbon black as conductive agent.
It is negative electrode active material that cathode, which selects graphite, feeds intake according to formula and prepares negative electrode slurry.It designs, starches by cathode formula
Material solid constituent includes the negative electrode active material of 94 wt%, the butadiene-styrene rubber of 3 wt%（SBR）Polymeric binder, the carboxylic of 1 wt%
The conductive black of sodium carboxymethylcellulose pyce polymer viscosifier and 2 wt%.Negative electrode slurry uses deionized water molten as disperseing
The solid content of agent, slurry is 42 wt%.
Deionized water and sodium carboxymethylcellulose are added in blender by the above proportioning, is sufficiently stirred and dissolves
To aqueous polymer solution.Conductive black is added in the aqueous polymer solution dissolved by formula again, is quickly stirred
Fineness is ground to as 5 μm hereinafter, graphite then is added by formula, dispersion stirs evenly, and finally vacuumizes removing bubble.With 150
Mesh screen filtering obtains required negative electrode slurry.
The manufactured slurry is equably coated in the copper foil two sides that thickness is 10 μm, then pole piece is compacted to one with roll squeezer
Determine thickness, cut-parts, soldering polar ear obtains cathode pole piece.
The preparation of anode：
Anode selects cobalt acid lithium（LiCoO2）For active material, feeds intake according to formula and prepare anode sizing agent.It is designed by anode formula,
Slurry solids ingredient includes the positive active material of 92 wt%, the Kynoar binder of 5 wt% and the conduction of 3 wt%
Carbon black.Anode sizing agent uses N-Methyl pyrrolidone as dispersion solvent, and the solid content of slurry is 45 wt%.
N-Methyl pyrrolidone and Kynoar are added in mixer grinder by the above proportioning, are sufficiently stirred
Dissolving obtains the polymer solution of Kynoar.The Kynoar dissolved is added in conductive black by formula again to gather
In polymer solution, quick agitation grinding to fineness is 5 μm hereinafter, then pressing formula is added cobalt acid lithium, and dispersion stirs evenly, finally
Vacuumize removing bubble.Required anode sizing agent is obtained with the filtering of 150 mesh stainless steel mesh.
It is 12 μm of aluminium foil two sides that above-mentioned manufactured slurry, which is equably coated in thickness, drying, then with roll squeezer by pole piece
It is compacted to certain thickness, cut-parts, soldering polar ear obtains anode pole piece.
The preparation of electrolyte：
By ethylene carbonate EC, propene carbonate PC and dimethyl carbonate DMC according to volume ratio 3：3：4 are configured to mixed solvent,
Then lithium salts lithium hexafluoro phosphate is added（LiPF6）, prepare LiPF6A concentration of 1M, obtain electrolyte after stirring evenly.
The assembling of battery：
By above-mentioned anode pole piece, organic and inorganic composite coated porous separation film and cathode pole piece are wound into battery core, plastic-aluminum combined
Film encapsulates, and vacuum state baking injects quantitative electrolyte after removing moisture, and chemical conversion and volume test are carried out to battery, obtains thick width
Long is respectively the square flexible package lithium ion of 3.6mm, 28mm, 96mm.
Embodiment 2
Embodiment 2 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 8wt% waterborne polymerics binder, 2wt% sodium carboxymethylcelluloses, 40wt% Kynoar, the inorganic potteries of 50wt%
Four part of porcelain particle forms.Wherein, it is 5% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 140 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 30wt%.
Embodiment 3
Embodiment 3 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 9wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 40wt% Kynoar, the inorganic potteries of 50wt%
Four part of porcelain particle forms.Wherein, it is 7% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 130 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 30wt%.
Embodiment 4
Embodiment 4 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 9wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 40wt% Kynoar, the inorganic potteries of 50wt%
Four part of porcelain particle forms.Wherein, it is 9% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 120 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 30wt%.
Embodiment 5
Embodiment 5 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 9wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 30wt% Kynoar, the inorganic potteries of 60wt%
Four part of porcelain particle forms.Wherein, it is 7% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 130 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 50wt%.
Embodiment 6
Embodiment 6 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 9wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 50wt% Kynoar, the inorganic potteries of 40wt%
Four part of porcelain particle forms.Wherein, it is 7% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 130 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 50wt%.
Embodiment 7
Embodiment 7 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 2wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 27wt% Kynoar, the inorganic potteries of 70wt%
Four part of porcelain particle forms.Wherein, it is 7% to select copolymerization degree, and grain size D50 is 2um, the polyvinylidene fluoride that fusing point is 130 DEG C
Alkene.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3It is other to represent
Inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2It is equally applicable to the present invention, it is big
The ratio and Al of small sized particles2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry is matched
During setting, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 50wt%.
Embodiment 8
Embodiment 8 and embodiment 1 are substantially the same, the difference is that, coating slurry formula based on siccative weight percent,
Coating slurry is by 9wt% waterborne polymerics binder, 1wt% sodium carboxymethylcelluloses, 20wt% Kynoar（PVDF）、70wt%
Four part of inorganic ceramic particle forms.Wherein, it is 7% to select copolymerization degree, and grain size D50 is 2um, and fusing point is 130 DEG C poly- inclined
Vinyl fluoride.Inorganic ceramic particle selects Al2O3, the D50 of grain diameter size is 0.5um.With Al in the present invention2O3To represent,
Other inorganic material, such as SiO2、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2, SnO2The present invention is equally applicable to,
The ratio and Al of its size dimension particle2O3Equally.Waterborne polymeric binder selects phenylethylene ethylene/propenoic acid ester copolymer emulsion.Slurry
Expect in configuration process, solvent is deionized water.Wherein, the weight of solid part accounts for the slurry total weight about 50wt%.
The performance of embodiment 1 to 8 and comparative example 1, comparative example 2 and comparative example 3 is more as shown in table 1 below：
By above-mentioned table 1 it is found that（1）In terms of thermal contraction, the thermal contraction of embodiment 1 to embodiment 8 is both less than comparative example 1 and comparison
Example 2, and it is less than comparative example 3, it can be seen that, ceramic particle Al2O3The thermal contraction performance of lithium ion battery separator is affected, and
With Al2O3Content it is more, the thermal contraction performance of lithium ion battery separator is better.
（2）By embodiment 1 to embodiment 4 it is found that in Kynoar（PVDF）Mass percent is identical, polyvinylidene fluoride
Alkene（PVDF）Grain size is identical, ceramic particle Al2O3Mass percent, ceramic particle Al2O3Grain size, coating thickness all same
In the case of, Kynoar（PVDF）Copolymerization degree it is bigger, the fusing point of lithium ion battery separator is lower, lithium ion battery separator
Heat Shrinkage value it is bigger, thermal contraction performance is poorer, while high rate performance value is smaller, and it is also smaller to follow bad pad value.
（3）By embodiment 5 to embodiment 8 it is found that in Kynoar（PVDF）Copolymerization degree is identical, Kynoar
（PVDF）Grain size is identical, ceramic particle Al2O3Grain size, in the case of coating thickness all same, Kynoar（PVDF）Matter
It is bigger to measure percentage, ceramic particle Al2O3Mass percent it is smaller, the Heat Shrinkage value of lithium ion battery separator is bigger, be heat-shrinked
Performance is poorer, while high rate performance value is smaller, and it is also smaller to follow bad pad value.
In the present invention, comparative example 1 is the blank control group of uncoated coating, the polyvinylidene fluoride that has been dual coating of comparative example 2
The control group of alkene, and the mass percent of Kynoar is 90%, comparative example 3 is that single side is coated with ceramic particle Al2O3Pair
According to group.
Claims (14)
1. a kind of organic and inorganic composite coated porous separation film, including porous substrate and it is attached to the porous substrate
Two surfaces on organic and inorganic Complex Function coating, the organic and inorganic Complex Function coating include polyvinylidene fluoride
Alkene, inorganic ceramic particle, aqueous high molecular thickener and waterborne polymeric binder, it is characterised in that：The Kynoar
Grain size D50 value range be 2~4um, Kynoar be by hexafluoropropene and vinylidene copolymerization made of copoly type
The copolymerization degree of high molecular polymer, Kynoar is between 3%~10% and melting temperature is between 115 DEG C~150 DEG C, is gathered
The weight of vinylidene account for the weight percent of the organic and inorganic Complex Function total coating weight value range be 20~
The value range of 50%, the grain size D50 of inorganic ceramic particle are 0.4~0.8um, the weight of inorganic ceramic particle account for it is described it is organic,
The value range of the weight percent of inorganic compounding functional coating total weight is 40~70%.
2. organic and inorganic composite coated porous separation film according to claim 1, it is characterised in that：The inorganic pottery
Porcelain particle is the electrical insulating material that dielectric constant is more than or equal to 4.
3. organic and inorganic composite coated porous separation film according to claim 1, it is characterised in that：The inorganic pottery
Porcelain particle is SiO2、Al2O3、γ-AlOOH、BaSO4、CaO、TiO2、ZnO2、MgO、ZrO2And SnO2One or more of.
4. organic and inorganic composite coated porous separation film according to claim 1, it is characterised in that：It is described aqueous poly-
It is phenylethylene ethylene/propenoic acid ester copolymer emulsion, vinyl acetate/acrylate copolymer emulsion, vinyl acetate/aliphatic acid to close object binder
At least one of vinyl acetate copolymer emulsion, organosilicon acrylic ester copolymerization emulsion and acrylate copolymer emulsion.
5. the porous sexual isolation of organic and inorganic composite coated according to any one claim in Claims 1-4
Film, it is characterised in that：The weight of the waterborne polymeric binder accounts for the organic and inorganic Complex Function total coating weight
The value range of weight percent is 2~9%.
6. organic and inorganic composite coated porous separation film according to claim 1, it is characterised in that：The aqueous height
Molecule thickener be sodium carboxymethylcellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, polyacrylamide, sodium alginate and
At least one of polyvinyl alcohol.
7. the porous sexual isolation of organic and inorganic composite coated according to any one claim in Claims 1-4
Film, it is characterised in that：The weight of the aqueous high molecular thickener accounts for the organic and inorganic Complex Function total coating weight
The value range of weight percent is 1~2%.
8. the porous sexual isolation of organic and inorganic composite coated according to any one claim in Claims 1-4
Film, it is characterised in that：The amount of solid content of aqueous slurry used by the coating of the organic and inorganic Complex Function coating exists
Between 30%~50%.
9. the porous sexual isolation of organic and inorganic composite coated according to any one claim in Claims 1-4
Film, it is characterised in that：The value range of the thickness of the organic and inorganic Complex Function coating is 2~6 μm.
10. the porous sexual isolation of organic and inorganic composite coated according to any one claim in Claims 1-4
Film, it is characterised in that：The porous substrate is polyethylene film, polypropylene screen, polypropylene, polyethylene/polypropylene composite film, fibre
The plain film of dimension or be polyimide film.
11. organic and inorganic composite coated porous separation film according to claim 10, it is characterised in that：It is described porous
Property base material thickness value range be 5 μm~25 μm.
12. organic and inorganic composite coated porous separation film according to claim 10, it is characterised in that：It is described porous
Property base material porosity value range be 20%~70%.
13. a kind of preparation method of the organic and inorganic composite coated porous separation film described in claim 1 to 12, feature
It is：Include the following steps：
（S1）, by waterborne polymeric binder dispersion in deionized water formed waterborne polymeric binder solution；
（S2）, inorganic ceramic particle, organic functions polyphosphazene polymer vinylidene be dispersed in deionized water and has dissolved in advance
In water soluble polymer thickener, and it is mixed and is formed uniformly mixed dispersion liquid；
（S3）, to step（S2）Step is added in the mixed dispersion liquid of middle formation（S1）Obtained waterborne polymeric binder is molten
It in liquid, is uniformly dispersed, the weight for being adjusted to solid part accounts for the 30%~50% of slurry total amount, obtains coating slurry；
（S4）, by step（S3）Obtained slurry is coated in porous substrate by way of dimple version or by extrusion coated
On two surfaces, organic and inorganic composite coated porous separation film is obtained after drying.
14. a kind of lithium ion battery, including anode, cathode, the porous separation film being interval between the positive electrode and negative electrode, with
And electrolyte, it is characterised in that：The porous separation film is organic and inorganic described in any one of claim 1 to 13
Composite coated porous separation film.
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