CN108565381A - Cell coating film slurry, battery diaphragm, secondary cell and preparation method thereof - Google Patents
Cell coating film slurry, battery diaphragm, secondary cell and preparation method thereof Download PDFInfo
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- CN108565381A CN108565381A CN201810289099.XA CN201810289099A CN108565381A CN 108565381 A CN108565381 A CN 108565381A CN 201810289099 A CN201810289099 A CN 201810289099A CN 108565381 A CN108565381 A CN 108565381A
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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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
- C08G65/4056—(I) or (II) containing sulfur
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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
- H01M10/058—Construction or manufacture
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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
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
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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
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/426—Fluorocarbon polymers
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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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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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
- H01M50/451—Separators, membranes or diaphragms characterised by the material having a layered structure comprising layers of only organic material and layers containing 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
- H01M50/457—Separators, membranes or diaphragms characterised by the material having a layered structure comprising three or more layers
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
A kind of cell coating film slurry of present invention offer, battery diaphragm and secondary cell and respective preparation method, the preparation of cell coating film slurry include：The first copolymer is provided, the first copolymer includes tetrafluoroethene；Second copolymer is provided；First copolymer and second copolymer are copolymerized, to obtain slurry copolymer；And the cell coating film slurry is prepared based on the slurry copolymer.Through the above technical solutions, the present invention is designed cell coating film slurry, and use nonaqueous systems, diaphragm and pole piece can be not only bonded together, improve the hardness of battery, and the crystallinity higher of polymer obtained, swelling ratio smaller, adhesive property are more superior；The internal resistance smaller for the battery made, cycle performance are more superior.
Description
Technical field
The invention belongs to technical field of lithium batteries, more particularly to a kind of cell coating film slurry, battery diaphragm, secondary electricity
Pond and preparation method thereof.
Background technology
Lithium ion battery is usually mainly by anode, cathode, diaphragm, electrolyte, battery case composition.Lithium ion battery structure
In, diaphragm is one of the interior layer assembly of key.The main function of diaphragm is to separate the positive and negative electrode of battery, is prevented positive and negative
Pole is in direct contact and short-circuit, while electrolyte ion also to be enable to be passed through in battery charge and discharge process, forms electric current,
When battery operating temperature is abnormal raising, the migrating channels of electrolyte ion are closed, cut-out electric current ensures cell safety.By
This directly affects capacity, cycle and the safety of battery as it can be seen that the performance of diaphragm determines the interfacial structure of battery, internal resistance etc.
The characteristics such as performance, the diaphragm haveing excellent performance play an important role the comprehensive performance for improving battery.
With the development of electric vehicle cause, promotion battery performance is more and more important, existing coating PVDF (polyvinylidene fluorides
Alkene) copolymer diaphragm due to itself it is cementitious can, diaphragm and pole piece can be bonded together, improve the hardness of battery, institute
It is critically important with PVDF copolymers, currently, being applied to the PVDF crystallinity (generally 20%~30% of diaphragm coating in the market
Between), swelling ratio (30%~150%) and adhesive property can not fit entirely into current battery system, so seeking
The stronger PVDF of performance is looked for seem increasingly important.In addition, there are mainly two types of the synthesis modes of existing PVDF, one is homopolymerizations
Object is generally used on positive and negative anodes, and another kind is exactly copolymer, is generally used on lithium ion battery separator, is mainly here
That says applies the PVDF being covered with for lithium ion battery separator, and the daily middle PVDF used is usually by vinylidene (VDF) and six
Made from fluoropropene (HFP) is copolymerized, however, the crystallinity for the PVDF that this copolymerization is got is smaller, and in the electrolytic solution
Swelling coefficient it is bigger, the diaphragm adhesive property being prepared is smaller, larger so as to cause the internal resistance of battery, cycle performance compared with
The problem of difference, influences the performance of battery.
Therefore, how a kind of cell coating film slurry, battery diaphragm and secondary cell and respective preparation method are provided,
It is low to solve above-mentioned existing Kynoar (PVDF) copolymer crystallinity, swelling it is bigger, obtained diaphragm adhesive property compared with
Small, larger so as to cause the internal resistance of battery, the poor problem of cycle performance is necessary.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of cell coating film slurry, electricity
Pond diaphragm and secondary cell and respective preparation, for solving Kynoar (PVDF) copolymer crystallinity in the prior art
Low, swelling is bigger, and obtained diaphragm adhesive property is smaller, larger so as to cause the internal resistance of battery, and cycle performance is poor etc. asks
Topic.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation method of cell coating film slurry,
Include the following steps：
1) the first copolymer is provided, first copolymer includes tetrafluoroethene；
2) the second copolymer is provided；
3) first copolymer and second copolymer are copolymerized, to obtain slurry copolymer；And
4) the cell coating film slurry is prepared based on the slurry copolymer.
As a preferred embodiment of the present invention, second copolymer includes vinylidene, acrylic acid, metering system
At least one of acid, methyl acrylate and ethyl acrylate.
As a preferred embodiment of the present invention, second copolymer is vinylidene.
As a preferred embodiment of the present invention, in the slurry copolymer, the weight percent of the tetrafluoroethene is situated between
Between 0.1%~20%.
As a preferred embodiment of the present invention, the specific steps that step 4) obtains the cell coating film slurry include：
The slurry copolymer is dissolved in the first solvent, the first mixed liquor is obtained, first mixed liquor constitutes the cell coating
Film slurry.
As a preferred embodiment of the present invention, the specific steps that step 4) obtains the cell coating film slurry include：
4-1) the slurry copolymer is dissolved in the first solvent, obtains the first mixed liquor；
Filler 4-2) is provided, the filler is dissolved in the second solvent, the second mixed liquor is obtained；And
Second mixed liquor is mixed with first mixed liquor 4-3), is starched with obtaining the cell coating film
Material.
As a preferred embodiment of the present invention, first solvent include in DMAC, DMF, NMP and acetone at least
It is a kind of.
As a preferred embodiment of the present invention, step 4-2) in, the filler include alchlor, silica,
Titanium dioxide, ceria, calcium carbonate, calcium oxide, zinc oxide, magnesia, Cerium titanate, calcium titanate, barium titanate, lithium phosphate, phosphorus
At least one of sour titanium lithium, titanium phosphate aluminium lithium, lithium nitride and lanthanium titanate lithium.
As a preferred embodiment of the present invention, step 4-2) in, second solvent include DMAC, DMF, NMP and
At least one of acetone.
As a preferred embodiment of the present invention, second solvent is identical as first solvent.
As a preferred embodiment of the present invention, step 4-2) in, it counts in parts by weight, in second mixed liquor, institute
It states filler and is less than 4 parts, second solvent is between 8~50 parts.
As a preferred embodiment of the present invention, step 4-3) in, in the cell coating film slurry, first mixing
The weight percent of liquid is between 50%~90%.
The present invention also provides a kind of preparation methods of battery diaphragm, including：One basement membrane is provided；According to such as above-mentioned any one
Preparation method described in scheme prepares cell coating film slurry；The cell coating film slurry is coated on the basement membrane at least
One surface, to obtain the battery diaphragm.
The present invention also provides a kind of preparation method of secondary cell, the preparation method of the secondary cell includes using as above
State the step of preparation method of the battery diaphragm described in any one scheme prepares battery diaphragm.
The present invention also provides a kind of cell coating film slurry, the raw material for preparing of the cell coating film slurry includes that slurry is total
Polymers, wherein the slurry copolymer is copolymerized to obtain by the first copolymer and the second copolymer, and first copolymer
Including tetrafluoroethene.
As a preferred embodiment of the present invention, second copolymer includes vinylidene, acrylic acid, metering system
At least one of acid, methyl acrylate and ethyl acrylate.
As a preferred embodiment of the present invention, in the slurry copolymer, the weight percent of the tetrafluoroethene is situated between
Between 0.1%~20%.
As a preferred embodiment of the present invention, second copolymer is vinylidene.
As a preferred embodiment of the present invention, the raw material for preparing of the cell coating film slurry further includes the first solvent,
Wherein, the slurry copolymer is dissolved in the first mixed liquor of the first solvent composition, and first mixed liquor constitutes the battery
Coating sizing-agent.
As a preferred embodiment of the present invention, first solvent include in DMAC, DMF, NMP and acetone at least
It is a kind of.
As a preferred embodiment of the present invention, the cell coating film slurry prepare raw material further include the first solvent,
Filler and the second solvent, wherein the slurry copolymer is dissolved in first solvent and constitutes the first mixed liquor, the filler
It is dissolved in second solvent and constitutes the second mixed liquor, first mixed liquor is mixed with second mixed liquor to constitute
Cell coating slurry is stated, and is counted in parts by weight, filler described in second mixed liquor is less than 4 parts, second solvent
Between 8~50 parts, in the obtained cell coating film slurry, the weight percent of first mixed liquor between 50%~
Between 90%.
As a preferred embodiment of the present invention, first solvent include in DMAC, DMF, NMP and acetone at least
It is a kind of；Second solvent includes at least one of DMAC, DMF, NMP and acetone.
As a preferred embodiment of the present invention, second solvent is identical as first solvent.
The present invention also provides a kind of battery diaphragms, including basement membrane；And at least one surface of the basement membrane
Coat, and the coat is the coat prepared using the cell coating film slurry as described in any of the above-described scheme.
The present invention also provides a kind of secondary cell, the secondary cell includes the battery as described in above-mentioned any one scheme
Diaphragm.
As described above, cell coating film slurry, battery diaphragm and secondary cell and the respective preparation method of the present invention,
It has the advantages that：
The present invention is designed cell coating film slurry, and uses nonaqueous systems, not only can be by diaphragm and pole piece
It is bonded together, improves the hardness of battery, and the crystallinity higher of polymer obtained, swelling ratio smaller, adhesive property is more
It is superior；The internal resistance smaller for the battery made, cycle performance are more superior.
Description of the drawings
Fig. 1 is shown as the flow chart of the preparation method of cell coating film slurry provided by the invention.
Fig. 2 is shown as the structural schematic diagram of battery diaphragm provided by the invention.
Fig. 3 is shown as the electromicroscopic photograph of the battery diaphragm coat of the present invention.
Component label instructions
11 basement membranes
21,22 coats
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It please refers to Fig.1 to Fig.3.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, though package count when only display is with related component in the present invention rather than according to actual implementation in diagram
Mesh, shape and size are drawn, when actual implementation form, quantity and the ratio of each component can be a kind of random change, and its
Assembly layout form may also be increasingly complex.
As shown in Figure 1, the present invention provides a kind of preparation method of cell coating film slurry, include the following steps：
1) the first copolymer is provided, first copolymer includes tetrafluoroethene；
2) the second copolymer is provided；
3) first copolymer and second copolymer are copolymerized, to obtain slurry copolymer；And
4) the cell coating film slurry is prepared based on the slurry copolymer.
As an example, second copolymer include vinylidene, acrylic acid, methacrylic acid, methyl acrylate and
At least one of ethyl acrylate.
Specifically, the present invention provides a kind of preparation method of nonaqueous systems cell coating film slurry, it can be used for preparation two
The battery diaphragm of primary cell, in this method, first copolymer and second copolymer refer to being total in subsequent step
Poly- substance, in addition, second copolymer can be one kind in above-mentioned substance, can also be arbitrary two kinds in above-mentioned substance
And two or more combinations, the first copolymer and the second copolymer are copolymerized, cell coating film can be subsequently prepared
The slurry copolymer (PVDF copolymers) of slurry, it is preferable that second copolymer includes vinylidene, acrylic acid, methyl-prop
At least two in olefin(e) acid, methyl acrylate and ethyl acrylate, and one of which is vinylidene, it is further preferred that
Second copolymer is vinylidene, to further simplify technique, cost-effective while reaching superperformance, relatively
In the coated film slurry of the prior art, the slurry copolymer crystallinity is high, and crystallinity is generally between 30%~70%, is swollen
Than small, for swelling ratio between 5~30, adhesive property is more superior, is conducive to the secondary cell subsequently being had excellent performance.
As an example, the specific steps that step 4) obtains the cell coating film slurry include：By the slurry copolymer
It is dissolved in the first solvent, obtains the first mixed liquor, first mixed liquor constitutes the cell coating film slurry.
As an example, in the slurry copolymer, the weight percent of the tetrafluoroethene between 0.1%~20% it
Between.
As an example, first solvent includes at least one of DMAC, DMF, NMP and acetone.
It should be noted that this example provides a kind of institute that obtaining the mode of the cell coating film slurry, will be prepared
It states slurry copolymer to be dissolved in first solvent, first mixed liquor being configured so that can be directly as the electricity
The slurry of pond coated film, further, in the slurry copolymer, the weight percent of the tetrafluoroethene is preferably between 3%~
Between 15%, so as to the coated film slurry being had excellent performance, in addition, selection first solvent, first solvent
Can be any one in NMP (N-Methyl pyrrolidone), DMAC (dimethylacetylamide), acetone, DMF (dimethylformamide)
Kind, it can also be arbitrary two kinds or two or more combinations in above-mentioned solvent, be not specifically limited herein.
As an example, the specific steps that step 4) obtains the cell coating film slurry include：
4-1) the slurry copolymer is dissolved in the first solvent, obtains the first mixed liquor；
Filler 4-2) is provided, the filler is dissolved in the second solvent, the second mixed liquor is obtained；And
Second mixed liquor is mixed with first mixed liquor 4-3), is starched with obtaining the cell coating film
Material.
It should be noted that this example provides another mode for obtaining the cell coating film slurry, institute is obtained first
First mixed liquor of slurry copolymer is stated, secondly, the filler is dissolved in other second solvent, obtains the
Two mixed liquors, then the first mixed liquor configured is mixed with the second mixed liquor configured, it is preferable that described second is mixed
It closes liquid to be added in first mixed liquor, to obtain the cell coating film slurry, wherein the filler can be further
Reduce the gas permeability of the battery diaphragm subsequently prepared.
As an example, first solvent includes at least one of DMAC, DMF, NMP and acetone.
As an example, step 4-2) in, the filler includes alchlor, silica, titanium dioxide, titanium dioxide
Cerium, calcium carbonate, calcium oxide, zinc oxide, magnesia, Cerium titanate, calcium titanate, barium titanate, lithium phosphate, titanium phosphate lithium, titanium phosphate aluminium
At least one of lithium, lithium nitride and lanthanium titanate lithium.
As an example, step 4-2) in, second solvent includes at least one of DMAC, DMF, NMP and acetone.
As an example, second solvent is identical as first solvent.
Specifically, in this example, first solvent can be NMP (N-Methyl pyrrolidone), DMAC (dimethylacetamides
Amine), acetone, any one in DMF (dimethylformamide), can also be arbitrary two kinds or two or more in above-mentioned solvent
Combination；Second solvent can be NMP (N-Methyl pyrrolidone), DMAC (dimethylacetylamide), acetone, DMF (diformazans
Base formamide) in any one, can also be arbitrary two kinds or two or more combinations in above-mentioned solvent.Preferably, institute
It is identical as the type of the second solvent to state the first solvent, thereby may be ensured that and battery diaphragm slurry equality subsequently is prepared
And stability.In addition, the filler can be any one in above-mentioned material, can also be arbitrary two in above-mentioned material
Kind or two or more combinations, are not specifically limited herein.
As an example, in the slurry copolymer, the weight percent of the tetrafluoroethene between 0.1%~20% it
Between.
As an example, step 4-2) in, it counts in parts by weight, in second mixed liquor, the filler is less than 4 parts,
Second solvent is between 8 parts~50 parts.
As an example, step 4-3) in, in the cell coating film slurry, the weight percent of first mixed liquor is situated between
Between 50%~90%.
Specifically, cell coating film of good performance in order to obtain, in this example, in the slurry copolymer, described four
The weight percent of vinyl fluoride is preferably between 0.1%~20% between 3%~15%, in addition, in parts by weight
It counts, in second mixed liquor, the filler is preferably between 2~3 parts, and second solvent is preferably between 20 parts~30 parts,
After second mixed liquor is uniformly dispersed, it is added in 50 parts~90 parts of first mixed liquor, further, described
One mixed liquor is preferably between 60~80 parts, to obtain cell coating film of good performance.
As an example, the particle size of the obtained slurry copolymer is between 0.1 μm~20 μm.
Specifically, the slurry copolymer that the method for the present invention is prepared can be preferably between with size between 2 μm~10 μm,
To which suitable grain size can ensure good performance of copolymer, with the diaphragm and battery being had excellent performance.
In addition, the present invention also provides a kind of cell coating film slurries, wherein the cell coating film slurry preferably uses this
The invention cell coating film slurry preparation method is prepared, and the raw material for preparing of the cell coating film slurry includes slurry
Copolymer, wherein the slurry copolymer is copolymerized to obtain by the first copolymer and the second copolymer, and first copolymerization
Object includes tetrafluoroethene.
As an example, second copolymer include vinylidene, acrylic acid, methacrylic acid, methyl acrylate and
At least one of ethyl acrylate.
Specifically, the present invention provides a kind of preparation method of nonaqueous systems cell coating film slurry, it can be used for preparation two
The battery diaphragm of primary cell, in this method, first copolymer and second copolymer refer to being total in subsequent step
Poly- substance, in addition, second copolymer can be one kind in above-mentioned substance, can also be arbitrary two kinds in above-mentioned substance
And two or more combinations, the first copolymer and the second copolymer are copolymerized, cell coating film can be subsequently prepared
The slurry copolymer of slurry, it is preferable that second copolymer includes vinylidene, acrylic acid, methacrylic acid, acrylic acid first
At least two in ester and ethyl acrylate, and one of which is vinylidene, it is further preferred that second copolymer
For vinylidene, to further simplify technique, cost-effective, painting compared with the existing technology while reaching superperformance
Cloth film slurry, the slurry copolymer crystallinity is high, and crystallinity is generally between 30%~70%, and swelling ratio is small, and swelling ratio is 5
Between~30, adhesive property is more superior, is conducive to the secondary cell subsequently being had excellent performance.
As an example, in the slurry copolymer, the weight percent of the tetrafluoroethene between 0.1%~20% it
Between.
As an example, the raw material for preparing of the cell coating film slurry further includes the first solvent, wherein the slurry copolymerization
Object is dissolved in first solvent and constitutes the first mixed liquor, and first mixed liquor constitutes the cell coating slurry.
Specifically, this example provides a kind of cell coating film slurry being prepared based on the slurry copolymer, will make
The standby obtained slurry copolymer is dissolved in first solvent, and first mixed liquor being configured so that can be direct
As the slurry of the cell coating film, further, in the slurry copolymer, the weight percent of the tetrafluoroethene is preferred
Between 3%~15%, so as to the coated film slurry being had excellent performance, in addition, selection first solvent, described
First solvent can be in NMP (N-Methyl pyrrolidone), DMAC (dimethylacetylamide), acetone, DMF (dimethylformamide)
Any one, can also be arbitrary two kinds or two or more combinations in above-mentioned solvent, be not specifically limited herein.
As an example, the raw material for preparing of the cell coating film slurry further includes the first solvent, filler and the second solvent,
Wherein, the slurry copolymer is dissolved in the first mixed liquor of the first solvent composition, and the filler is dissolved in second solvent
The second mixed liquor is constituted, first mixed liquor is mixed with second mixed liquor to constitute the cell coating slurry,
And count in parts by weight, filler described in second mixed liquor is less than 4 parts, and second solvent is obtained between 8 parts~50 parts
To the cell coating film slurry in, the weight percent of first mixed liquor is between 50%~90%.
As an example, first solvent includes at least one of DMAC, DMF, NMP and acetone；Described second is molten
Agent includes at least one of DMAC, DMF, NMP and acetone.
As an example, second solvent is identical as first solvent.
Specifically, this example provides another cell coating film slurry being prepared based on the slurry copolymer,
First mixed liquor of the slurry copolymer is obtained first, secondly, it is molten that the filler is dissolved in other described second
In agent, the second mixed liquor is obtained, then the first mixed liquor configured is mixed with the second mixed liquor configured, it is preferable that
Second mixed liquor is added in first mixed liquor, to obtain the cell coating film slurry, wherein the filling
Object can further decrease the gas permeability of the battery diaphragm subsequently prepared.
Wherein, cell coating film of good performance in order to obtain, in first mixed liquor, in the slurry copolymer,
The weight percent of the tetrafluoroethene is preferably between 0.1%~20% between 3%~15%, in addition, by weight
Number meter, in second mixed liquor, the filler is preferably between 2~3 parts, and second solvent is preferably between 20 parts~30
Part, after second mixed liquor is uniformly dispersed, it is added in 50 parts~90 parts of first mixed liquor, further, institute
It states the first mixed liquor and is preferably between 60~80 parts, to obtain cell coating film of good performance.
As shown in Fig. 2, the present invention also provides a kind of preparation methods of battery diaphragm, including：One basement membrane 11 is provided；According to such as
Preparation method described in above-mentioned any one scheme prepares the cell coating film slurry；The cell coating film slurry is coated
In at least one surface of the basement membrane, to obtain the battery diaphragm.
The present invention also provides a kind of battery diaphragms, wherein the battery diaphragm preferably use battery provided by the invention every
Membrane preparation method is prepared, and the battery diaphragm includes basement membrane 11, and at least one surface of the basement membrane
Coat 21,22, and the coat is the coating prepared using the cell coating film slurry as described in any of the above-described scheme
Layer.
It should be noted that the cell coating film slurry can also be coated in One-sided coatings in the surface of basement membrane
Two opposite surfaces of basement membrane, wherein the basement membrane 11 can be PE materials or PP materials, but be not limited thereto, preferably
Ground, is coated using intaglio plate roller mode, and specific method is：Slurry is got to by pump in gravure roll, then gravure roll carries out
Rotation is contacted by material strip to gravure roll, then with basement membrane, you can slurry is coated onto on basement membrane, in addition, after slurries coating also
It include the steps that rear water drying.The battery diaphragm adhesive property obtained using cell coating film slurry provided by the invention is more preferable.
The present invention also provides a kind of preparation method of secondary cell, the preparation method of the secondary cell includes using as above
State the step of preparation method of the battery diaphragm described in any one scheme prepares battery diaphragm.
The present invention also provides a kind of secondary cells, wherein the secondary cell preferably uses secondary electricity provided by the invention
Pool preparation method is prepared, and the secondary cell includes the battery diaphragm as described in above-mentioned any one scheme.
The internal resistance of rechargeable battery smaller obtained using cell coating film slurry provided by the invention, cycle performance are more preferable.
With reference to specific embodiment, to battery diaphragm slurry, battery diaphragm and lithium ion battery of the present invention and respectively
Preparation method be further described.
Embodiment 1：
First, it is copolymerized using 5% tetrafluoroethene and 95% vinylidene, vinylidene and tetrafluoroethene is made
Copolymer takes the copolymer of 1.44Kg to be dissolved in the DMAC of 16.56Kg, solid content 8%, first by the aluminium oxide of 0.16Kg
Powder is scattered in inside the DMAC of 1.84Kg, is uniformly dispersed and then the polymer solution 18Kg prepared is added scattered
In alumina fluid dispersion, you can experimental slurries are made.
The PE basement membranes for taking 12 μ m thicks, using gravure roll coating method (the specific side being coated using intaglio plate roller mode
Method is：Slurry is got to by pump in gravure roll, then gravure roll is rotated, by material strip to gravure roll, then with basement membrane into
Row contact, you can slurry is coated onto on basement membrane), by polymer paste be coated in basement membrane unilateral side, coating speed 15m/min,
It crosses water to be dried using three-level baking oven later, oven temperatures at different levels are respectively 50 DEG C, 60 DEG C, 55 DEG C, can be obtained after dry
The thickness of the lithium ion battery separator coated to oil-based polymer, the lithium ion battery separator of the coating is 14 μm, applies thickness
Degree is 2 μm.
Embodiment 2：
First, it is copolymerized using 8% tetrafluoroethene and 92% vinylidene, copolymer is made, take gathering for 1.2Kg
It closes object to be dissolved in the DMAC of 13.8Kg, the alumina powder of 0.4Kg is first scattered in the DMAC of 4.6Kg by solid content 8%
The inside is uniformly dispersed and then the PVDF solution 15Kg prepared is added in scattered alumina fluid dispersion, you can is made real
Test slurry.
The PE basement membranes for taking 12 μ m thicks, using gravure roll coating method (the specific side being coated using intaglio plate roller mode
Method is：Slurry is got to by pump in gravure roll, then gravure roll is rotated, by material strip to gravure roll, then with basement membrane into
Row contact, you can slurry is coated onto on basement membrane), by polymer paste be coated in basement membrane unilateral side, coating speed 15m/min,
It crosses water to be dried using three-level baking oven later, oven temperatures at different levels are respectively 50 DEG C, 60 DEG C, 55 DEG C, can be obtained after dry
The thickness of the lithium ion battery separator coated to oil-based polymer, the lithium ion battery separator of the coating is 14 μm, applies thickness
Degree is 2 μm.
Embodiment 3：
First, it is copolymerized using 15% tetrafluoroethene and 85% vinylidene, copolymer is made, takes 0.8Kg's
Polymer is dissolved in the DMAC of 9.2Kg, and the alumina powder of 0.8Kg is first scattered in 9.2Kg's by solid content 10%
Inside DMAC, it is uniformly dispersed and then the polymer solution 10Kg prepared is added in scattered alumina fluid dispersion, you can
Experimental slurries are made.
The PE basement membranes for taking 12 μ m thicks, using gravure roll coating method (the specific side being coated using intaglio plate roller mode
Method is：Slurry is got to by pump in gravure roll, then gravure roll is rotated, by material strip to gravure roll, then with basement membrane into
Row contact, you can slurry is coated onto on basement membrane), by polymer paste be coated in basement membrane unilateral side, coating speed 15m/min,
It crosses water to be dried using three-level baking oven later, oven temperatures at different levels are respectively 50 DEG C, 60 DEG C, 55 DEG C, can be obtained after dry
The thickness of the lithium ion battery separator coated to oil-based polymer, the lithium ion battery separator of the coating is 14 μm, applies thickness
Degree is 2 μm.
Embodiment 4：
First, it is copolymerized using 8% tetrafluoroethene and 92% acrylic acid, polymer is made, takes the polymerization of 1.6Kg
Object is dissolved in the DMAC of 18.4Kg, and solid content 8% does not add inorganic matter, you can experimental slurries are made.
The PE basement membranes for taking 12 μ m thicks, using gravure roll coating method (the specific side being coated using intaglio plate roller mode
Method is：Slurry is got to by pump in gravure roll, then gravure roll is rotated, by material strip to gravure roll, then with basement membrane into
Row contact, you can slurry is coated onto on basement membrane), by polymer paste be coated in basement membrane unilateral side, coating speed 15m/min,
It crosses water to be dried using three-level baking oven later, oven temperatures at different levels are respectively 50 DEG C, 60 DEG C, 55 DEG C, can be obtained after dry
The thickness of the lithium ion battery separator coated to oil-based polymer, the lithium ion battery separator of the coating is 14 μm, applies thickness
Degree is 2 μm.
Comparative example：
It is copolymerized using 8% hexafluoropropene and 92% vinylidene, Kynoar is made and hexafluoropropene is poly-
Object is closed, takes the polymer of 1.12Kg to be dissolved in the DMAC of 12.88Kg, solid content 8%, first by the alumina powder of 0.48Kg
End is scattered in inside the DMAC of 5.52Kg, is uniformly dispersed and then scattered oxidation is added in the PVDF solution 14Kg prepared
In aluminium dispersion liquid, you can experimental slurries are made.
The PE basement membranes for taking 12 μ m thicks, using gravure roll coating method (the specific side being coated using intaglio plate roller mode
Method is：Slurry is got to by pump in gravure roll, then gravure roll is rotated, by material strip to gravure roll, then with basement membrane into
Row contact, you can slurry is coated onto on basement membrane), by polymer paste be coated in basement membrane unilateral side, coating speed 15m/min,
It crosses water to be dried using three-level baking oven later, oven temperatures at different levels are respectively 50 DEG C, 60 DEG C, 55 DEG C, can be obtained after dry
The thickness of the lithium ion battery separator coated to oil-based polymer, the lithium ion battery separator of the coating is 14 μm, applies thickness
Degree is 2 μm.
The lithium ion battery isolation film properties of above the embodiment of the present invention and comparative example are tested, data see the table below
1：
Table 1
Wherein, polymer crystallinity is tested：It is tested with DSC；Polymer swelling ratio is tested：Dissolve the polymer in DMAC
In, solvent therein is then crossed into water and is extracted, polymer is left behind, a small block film is then cut into, is placed on electrolyte
It is middle to impregnate seven days, it tests it and impregnates front and back weight, weight before swelling ratio=(weight before weight-immersion after immersion)/immersion；Every
Membrane interface bonding test：The diaphragm for taking film surface integral outer appearance without exception, it is 25mm to be punched into width, and length is the sample of 100mm,
Take two diaphragm samples being punched stacked together, with 1MPa pressure on hot press, 100 degree of temperature, 10 meters/min's of speed
Condition hot pressing is used in combination puller system to test two pulling force (unit N) for being bonded together diaphragm, cohesive force=pulling force/0.025
(unit is N/m)；The cycle performance of lithium ion battery is tested：By lithium rechargeable battery, 0.5C multiplying powers charge at room temperature,
0.5C multiplying power dischargings carry out 500 cycles, its capacity retention ratio are calculated using formula successively；Capacity retention ratio=(500 are followed
After ring before capacity/cycle of battery battery room temperature capacity) × 100%；The inner walkway of lithium ion battery：Exchange pressure drop internal resistance
Mensuration because battery is actually equivalent to an active pull-up, therefore applies a fixed frequency and fixed current to battery
(generally using 1KHZ frequencies, 50mA low currents at present), then samples its voltage, a series of through over commutation, filtering etc.
The internal resistance value of the battery is calculated after processing by operational amplifier circuit.
Can be seen that slurry copolymer that the application obtains from the data of table 1 has that crystallinity is high, small bright of swelling coefficient
Aobvious advantage is applied to the adhesive property of the more original polymer of adhesive property of coated film made from coating lithium ion battery separator
Higher, internal resistance of cell smaller obtained in this way, cycle performance are more preferable.
In conclusion a kind of cell coating film slurry of present invention offer, battery diaphragm and secondary cell and respective system
Preparation Method, the preparation of cell coating film slurry include：The first copolymer is provided, first copolymer includes tetrafluoroethene；It provides
Second copolymer；First copolymer and second copolymer are copolymerized, to obtain slurry copolymer；And it is based on
The cell coating film slurry is prepared in the slurry copolymer.Through the above technical solutions, the present invention is to cell coating film
Slurry is designed, and uses nonaqueous systems, can be not only bonded together diaphragm and pole piece, be improved the hardness of battery,
And the crystallinity higher of polymer obtained, swelling ratio smaller, adhesive property are more superior；The internal resistance for the battery made is more
Small, cycle performance is more superior.So the present invention effectively overcomes various shortcoming in the prior art and has high industrial exploitation value
Value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (19)
1. a kind of preparation method of cell coating film slurry, which is characterized in that include the following steps：
1) the first copolymer is provided, first copolymer includes tetrafluoroethene；
2) the second copolymer is provided；
3) first copolymer and second copolymer are copolymerized, to obtain slurry copolymer；And
4) the cell coating film slurry is prepared based on the slurry copolymer.
2. the preparation method of cell coating film slurry according to claim 1, which is characterized in that in step 2), described
Two copolymers include at least one of vinylidene, acrylic acid, methacrylic acid, methyl acrylate and ethyl acrylate.
3. the preparation method of cell coating film slurry according to claim 1, which is characterized in that in step 3), the slurry
Expect in copolymer, the weight percent of the tetrafluoroethene is between 0.1%~20%.
4. the preparation method of cell coating film slurry according to claim 1, which is characterized in that step 4) obtains the electricity
The specific steps of pond coated film slurry include：The slurry copolymer is dissolved in the first solvent, the first mixed liquor is obtained, it is described
First mixed liquor constitutes the cell coating film slurry.
5. the preparation method of cell coating film slurry according to claim 1, which is characterized in that step 4) obtains the electricity
The specific steps of pond coated film slurry include：
4-1) the slurry copolymer is dissolved in the first solvent, obtains the first mixed liquor；
Filler 4-2) is provided, the filler is dissolved in the second solvent, the second mixed liquor is obtained；And
4-3) second mixed liquor is mixed with first mixed liquor, to obtain the cell coating film slurry.
6. the preparation method of cell coating film slurry according to claim 4 or 5, which is characterized in that first solvent
Including at least one of DMAC, DMF, NMP and acetone.
7. the preparation method of cell coating film slurry according to claim 5, which is characterized in that step 4-2) in, it is described
Filler includes alchlor, silica, titanium dioxide, ceria, calcium carbonate, calcium oxide, zinc oxide, magnesia, titanium
At least one of sour cerium, calcium titanate, barium titanate, lithium phosphate, titanium phosphate lithium, titanium phosphate aluminium lithium, lithium nitride and lanthanium titanate lithium.
8. the preparation method of cell coating film slurry according to claim 5, which is characterized in that step 4-2) in, it is described
Second solvent includes at least one of DMAC, DMF, NMP and acetone.
9. the preparation method of cell coating film slurry according to claim 5, which is characterized in that step 4-2) in, by weight
Number meter is measured, in second mixed liquor, the filler is less than 4 parts, and second solvent is between 8~50 parts.
10. the preparation method of cell coating film slurry according to claim 9, which is characterized in that step 4-3) in, it is described
In cell coating film slurry, the weight percent of first mixed liquor is between 50%~90%.
11. a kind of preparation method of battery diaphragm, which is characterized in that including：One basement membrane is provided；According to such as claim 1~10
Any one of described in preparation method prepare cell coating film slurry；The cell coating film slurry is coated on the basement membrane
At least one surface, to obtain the battery diaphragm.
12. a kind of preparation method of secondary cell, which is characterized in that the preparation method of the secondary cell includes using such as right
It is required that the step of preparation method of the battery diaphragm described in 11 prepares battery diaphragm.
13. a kind of cell coating film slurry, which is characterized in that the raw material for preparing of the cell coating film slurry includes slurry copolymerization
Object, wherein the slurry copolymer is copolymerized to obtain by the first copolymer and the second copolymer, and the first copolymer packet
Include tetrafluoroethene.
14. cell coating film slurry according to claim 13, which is characterized in that second copolymer includes inclined fluorine second
At least one of alkene, acrylic acid, methacrylic acid, methyl acrylate and ethyl acrylate；In the slurry copolymer, institute
The weight percent of tetrafluoroethene is stated between 0.1%~20%.
15. cell coating film slurry according to claim 13, which is characterized in that the preparation of the cell coating film slurry
Raw material further includes the first solvent, and first solvent includes at least one of DMAC, DMF, NMP and acetone, wherein described
Slurry copolymer is dissolved in first solvent and constitutes the first mixed liquor, and first mixed liquor constitutes the cell coating slurry.
16. cell coating film slurry according to claim 13, which is characterized in that the preparation of the cell coating film slurry
Raw material further includes the first solvent, filler and the second solvent, wherein the slurry copolymer is dissolved in first solvent and constitutes the
One mixed liquor, the filler are dissolved in second solvent and constitute the second mixed liquor, and first mixed liquor is mixed with described second
It closes liquid and carries out the mixing composition cell coating slurry, and count in parts by weight, filler is small described in second mixed liquor
In 4 parts, second solvent is between 8~50 parts, in the obtained cell coating film slurry, the weight of first mixed liquor
Percentage is between 50%~90%.
17. cell coating film slurry according to claim 16, which is characterized in that first solvent include DMAC,
At least one of DMF, NMP and acetone；Second solvent includes at least one of DMAC, DMF, NMP and acetone.
18. a kind of battery diaphragm, which is characterized in that including basement membrane；And the coating at least one surface of the basement membrane
Layer, the coat are the coat prepared using the cell coating film slurry as described in any one of claim 13~17.
19. a kind of secondary cell, which is characterized in that the secondary cell includes battery diaphragm as claimed in claim 18.
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| PCT/CN2019/081007 WO2019192475A1 (en) | 2018-04-03 | 2019-04-02 | Coating slurries for preparing separators, separators for electrochemical devices and preparation methods therefor |
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| WO2019192475A1 (en) * | 2018-04-03 | 2019-10-10 | Shanghai Energy New Materials Technology Co., Ltd. | Coating slurries for preparing separators, separators for electrochemical devices and preparation methods therefor |
| CN111435761A (en) * | 2019-01-11 | 2020-07-21 | 中信国安盟固利动力科技有限公司 | All-solid-state lithium ion battery and hot-pressing preparation method of multilayer electrolyte membrane thereof |
| WO2021184318A1 (en) * | 2020-03-19 | 2021-09-23 | 宁德新能源科技有限公司 | Method for improving cycle performance of battery, and electronic apparatus |
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| TWI803648B (en) * | 2018-06-12 | 2023-06-01 | 南韓商Ｌｇ化學股份有限公司 | Separator for electrochemical device including inorganic coating layer and method for manufacturing the same |
| CN115104219B (en) * | 2020-11-30 | 2024-03-22 | 宁德时代新能源科技股份有限公司 | Separator, preparation method thereof, and secondary battery, battery module, battery pack and device related to separator |
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| CN111435761A (en) * | 2019-01-11 | 2020-07-21 | 中信国安盟固利动力科技有限公司 | All-solid-state lithium ion battery and hot-pressing preparation method of multilayer electrolyte membrane thereof |
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