CN106928777A - The preparation method of adjustment hole structure coating material, coating coating method and coating - Google Patents
The preparation method of adjustment hole structure coating material, coating coating method and coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/08—Cellulose derivatives
- C09D101/10—Esters of organic acids
- C09D101/14—Mixed esters, e.g. cellulose acetate-butyrate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/365—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/08—Cellulose derivatives
- C09D101/26—Cellulose ethers
- C09D101/28—Alkyl ethers
- C09D101/288—Alkyl ethers substituted with nitrogen containing radicals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/14—Mixed esters
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
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Abstract
The invention discloses a kind of preparation method of adjustment hole structure coating material, coating coating method and coating, method is comprised the following steps:Step S1. weighs cellulose derivative and is dissolved in organic solvent, is evenly stirred until to form solution a;Step S2. weighs inorganic component presoma, the inorganic component presoma is slowly added dropwise into the solution a and is stirred, and the condensation reaction that is hydrolyzed forms solution b;Step S3. forms coating material to catalyst is added in the solution b.The present invention realizes the hydrolysis-condensation reaction by inorganic component presoma and then the polymer orifices structure to regulate and control coating, and the pore structure of formation has homogeneity, and can realize qualitatively controlling varying aperture by the mass fraction of inorganic component presoma;The homogeneous aperture structure that this organic-inorganic coating material hydrolysis-condensation reaction is formed, is conducive to electric current distribution uniform.
Description
Technical field
The present invention relates to a kind of coating material preparation method and coating, more particularly to a kind of adjustment hole structure coating material
Preparation method, coating coating method and coating, it is adaptable to the regulation of polyalkene diaphragm pore structure.
Background technology
Lithium ion battery is because having the advantages that energy density high, memory-less effect, pollution-free self discharge is small, have extended cycle life
And receive more and more attention.Barrier film is lithium ion battery important component, plays isolation positive and negative electrode, it is allowed to lithium ion
The effect for passing through.However, whether safely membrane properties quality directly affects lithium ion battery.
At present, the diaphragm material for being applied to lithium ion battery is mostly TPO, and such as polyethylene, polypropylene or both is multiple
Condensation material etc., polyolefine material has the valency of excellent mechanical property, chemical stability, uniform pore structure and relative moderate
The features such as lattice, but the wetability of the heat endurance of polyalkene diaphragm and electrolyte is poor.In addition, can using Coating
To be effectively improved the heat endurance of polyalkene diaphragm and the poor problem of wetability of electrolyte, but often block barrier film
Hole, be coated with modified membrane surface aperture uneven.
Therefore, need badly and seek a kind of technical scheme solution above technical barrier.
The content of the invention
The technical problem to be solved in the present invention polyalkene diaphragm is made in coating technique of the prior art to be overcome
Into the uneven defect of plug-hole and the modified membrane surface aperture of coating, a kind of making of adjustment hole structure coating material is now provided
Method, coating coating method and coating, the polymerization by the hydrolysis-condensation reaction of inorganic component presoma and then to regulate and control coating
Thing pore structure, the pore structure of formation has homogeneity, and can realize determining by the mass fraction of inorganic component presoma
Property ground control varying aperture.
The present invention is to solve above-mentioned technical problem by following technical proposals:
A kind of preparation method of adjustment hole structure coating material of the present invention, its feature is, the adjustment hole structure coating
The preparation method of material is comprised the following steps:
Step S1. weighs cellulose derivative and is dissolved in organic solvent, is evenly stirred until to form solution a;
Step S2. weighs inorganic component presoma, the inorganic component presoma is slowly added dropwise into the solution a and is stirred
Mix uniform, the condensation reaction that is hydrolyzed forms solution b;
Step S3. forms coating material to catalyst is added in the solution b;In the coating material, the cellulose
The weight percentage of derivative is 15~30%, and the weight percentage of the inorganic component presoma is 4.5~15%, institute
It is 0.5~5% to state the weight percentage of catalyst, and the weight percentage of the organic solvent is 50~80%.
Preferably, the time of the hydrolysis-condensation reaction is 5~12 hours.
Preferably, the cellulose derivative is in cyanethyl cellulose, cellulose acetate propionate or d ritalinic acid cellulose
At least one.
Preferably, the organic solvent is at least one in acetone, butanone or isopropanol.
Preferably, the inorganic component presoma is butyl titanate, zirconium-n-propylate, aluminium isopropoxide or the isopropyl ester of silicic acid four
In at least one.
Preferably, the catalyst be the ammoniacal liquor of 2mol/L, in 1mol/L NaOH or 1mol/L lithium hydroxides one
Kind.
A kind of coating coating method, its feature is that the coating coating method is using the above-mentioned use of the claims
In the coating material of polyalkene diaphragm, the one or both sides of polyalkene diaphragm are coated, dry and obtain polyalkene diaphragm coating.
Preferably, the coating method is dip coating, rolling method, spraying process or cast coat.
Preferably, the drying temperature is 50~70 DEG C, and drying time is 1~10 minute.
A kind of coating, is obtained using above-mentioned coating coating method, and the coating layer thickness is 1~4 μm, and the coating aperture is
80nm~1 μm.
Positive effect of the invention is:
The present invention is prepared and realizes the hydrolysis-condensation reaction by inorganic component presoma and then the polymerization to regulate and control coating
Thing pore structure, the pore structure of formation has homogeneity, and can realize determining by the mass fraction of inorganic component presoma
Property ground control varying aperture;The homogeneous aperture structure that this organic-inorganic coating material hydrolysis-condensation reaction is formed is conducive to electric current
Density Distribution is uniform;The introducing of other inorganic component, improves the stability of diaphragm material and battery, improves the safety of battery
Performance and service life;Polyalkene diaphragm is improve to the wetability of electrolyte, heat endurance and mechanical strength.
Brief description of the drawings
Fig. 1 is polyalkene diaphragm through the scanning electron microscope (SEM) photograph before present invention coating.
Fig. 2 is polyalkene diaphragm through the scanning electron microscope (SEM) photograph after present invention coating.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to described reality
Apply among a scope.
The present invention makes the method and coating coating method and coating of regulation polyalkene diaphragm pore structure coating material, its
In, polyolefin porous membrane be polyethylene porous film, polypropylene porous membrane or polypropylene, polyethylene composite multilayer membrane in extremely
Few one kind, polyalkene diaphragm coating material is the organic inorganic hybridization coating material for polyalkene diaphragm, and its preparation method is
A kind of presoma of inorganic component is hydrolyzed into contracting in organic polymer and reaction forms a kind of organic inorganic hybridization system, passed through
Control the mass fraction of presoma hydrolytic condensation degree and inorganic component presoma to regulate and control the pore structure of coating, can also lead to
The quality hydrolyzable condensation for crossing regulation and control inorganic component presoma reacts the inorganic particulate to form different content, different-grain diameter.Relatively
For other diagram modification methods, this method can not only make coating form uniform pore structure, and with qualitative contrlol
The advantage (polymer coating aperture controllable size is 80nm~1 μm) of pore size.By organic inorganic hybridization coating material
After modification, the heat endurance of barrier film can be improved, fluidity and chemical property etc. is held.
Embodiment one
The cellulose acetate propionate for weighing 1.0g is dissolved in acetone, and stirring forms uniform solution in 30 minutes, weighs 3ml
The isopropyl ester of silicic acid four be slowly added dropwise into the acetone soln for having dissolved cellulose acetate propionate, after stirring 30min, add certain
The ammoniacal liquor of amount, hydrolysis-condensation reaction forms required coating material, the wherein each component and its weight of the coating material after 10 hours
Measuring percentage composition is:
Cellulose acetate propionate:25%;
The isopropyl ester of silicic acid four:5%;
Ammoniacal liquor:1.2%;
Acetone:68.8%;
Magnetic agitation is selected in preparation process, coating method uses dip coating, and drying temperature is 60 DEG C, and drying time is 8
Minute, the polymer coating thickness for being coated with modified membrane surface is 3um, and aperture is 300nm.
Embodiment two
The cyanethyl cellulose for weighing 1.2g is dissolved in butanone, and stirring forms uniform solution in 30 minutes, weighs 5ml's
Zirconium-n-propylate is slowly added dropwise into the butanone solution for having dissolved cyanethyl cellulose, after stirring 30 minutes, adds a certain amount of hydrogen
Sodium oxide molybdena, hydrolysis-condensation reaction forms required coating material, the wherein each component of the coating material and its weight hundred after 8 hours
Point content is:
Cyanethyl cellulose:21%;
Zirconium-n-propylate:7%;
NaOH:0.8%;
Butanone:71.2%;
Magnetic agitation is selected in preparation process, coating method uses dip coating, and drying temperature is 70 DEG C, and drying time is 10
Minute, the polymer coating thickness for being coated with modified membrane surface is 2um, and aperture is 100nm.
Embodiment three
The cellulose acetate propionate for weighing 1.5g is dissolved in isopropanol, and stirring forms uniform solution in 30 minutes, weighs
2.5ml, aluminium isopropoxide be slowly added dropwise into the aqueous isopropanol for having dissolved cellulose acetate propionate, stirring 30 minutes after, plus
Enter a certain amount of ammoniacal liquor, hydrolysis-condensation reaction forms required coating material, the wherein each component of the coating material after 12 hours
And its weight percentage is:
Cellulose acetate propionate:18%;
Aluminium isopropoxide:8%;
Ammoniacal liquor:1.3%;
Isopropanol:72.7%;
Shear agitation is selected in preparation process, coating method uses dip coating, and drying temperature is 60 DEG C, and drying time is 10
Minute, the polymer coating thickness for being coated with modified membrane surface is 4um, and aperture is 600nm.
Example IV
The d ritalinic acid cellulose dissolution of 2.0g is weighed in butanone, stirring forms uniform solution in 30 minutes, weighs 9ml's
Butyl titanate is slowly added dropwise into the butanone solution for having dissolved d ritalinic acid cellulose, after stirring 30 minutes, is added a certain amount of
Lithium hydroxide, hydrolysis-condensation reaction forms required coating material, the wherein each component and its weight of the coating material after 7 hours
Percentage composition is:
D ritalinic acid cellulose:22%;
Butyl titanate:9%;
Lithium hydroxide:0.9%;
Acetone:68.1%;
Magnetic agitation is selected in preparation process, coating method uses dip coating, and drying temperature is 65 DEG C, and drying time is 8
Minute, the polymer coating thickness for being coated with modified membrane surface is 1.5um, and aperture is in 200nm, and it is right that Fig. 1 and Fig. 2 is carried out
According to, hence it is evident that as can be seen that the pore structure of polyalkene diaphragm substantially becomes big.
The present invention prepares a kind of organic inorganic hybridization coating material with Uniform pore structure, the painting of organo-mineral complexing
After layer material modified micropore film, the uniform aperture for being formed can not only improve the energy that polyalkene diaphragm adsorbs electrolyte
Power, therefore ensure that electrode/electrolyte interfacial property is consistent and current density is homogeneous in battery, micropore should be in whole polyolefin
It is evenly distributed in barrier film;And the interface of present invention stabilization is favorably improved battery.
Prepared by the present invention is by inorganic component presoma for the organic-inorganic coating material in lithium ion battery
Hydrolysis-condensation reaction and then the polymer orifices structure to regulate and control coating, the pore structure of formation have homogeneity, and can pass through preceding
The mass fraction of body is driven qualitatively to control varying aperture;Secondly, this organic-inorganic coating material has hydrophilic radical, favorably
In improving barrier film to guarantor's liquid effect of electrolyte;In addition, the introducing of inorganic component, can greatly improve the thermally-stabilised of diaphragm material
Property;The present invention has weight to improving the aspects such as lithium ion battery separator battery safety, chemical property and service life
Want meaning.
The present invention is described in detail above in association with accompanying drawing embodiment, those skilled in the art can be according to upper
State it is bright the present invention is made many variations example.All any modifications within the spirit and principles in the present invention, made, equally replace
Change, improve, should be included within the scope of the present invention.Thus, some of embodiment details should not be constituted to this
The restriction of invention, the scope that will be defined using appended claims of the present invention is used as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of adjustment hole structure coating material, it is characterised in that the system of the adjustment hole structure coating material
Comprised the following steps as method:
Step S1. weighs cellulose derivative and is dissolved in organic solvent, is evenly stirred until to form solution a;
Step S2. weighs inorganic component presoma, and it is equal that the inorganic component presoma is slowly added dropwise into the solution a into stirring
Even, the condensation reaction that is hydrolyzed forms solution b;
Step S3. forms coating material to catalyst is added in the solution b;In the coating material, the cellulose derives
The weight percentage of thing is 15~30%, and the weight percentage of the inorganic component presoma is 4.5~15%, described to urge
The weight percentage of agent is 0.5~5%, and the weight percentage of the organic solvent is 50~80%.
2. the preparation method of adjustment hole structure coating material according to claim 1, it is characterised in that the hydrolytic condensation
The time of reaction is 5~12 hours.
3. the preparation method of adjustment hole structure coating material according to claim 1, it is characterised in that the cellulose spreads out
Biology is at least one in cyanethyl cellulose, cellulose acetate propionate or d ritalinic acid cellulose.
4. the preparation method of adjustment hole structure coating material according to claim 1, it is characterised in that the organic solvent
It is at least one in acetone, butanone or isopropanol.
5. the preparation method of adjustment hole structure coating material according to claim 1, it is characterised in that the inorganic component
Presoma is at least one in butyl titanate, zirconium-n-propylate, aluminium isopropoxide or the isopropyl ester of silicic acid four.
6. the preparation method of adjustment hole structure coating material according to claim 1, it is characterised in that the catalyst is
One kind in the ammoniacal liquor of 2mol/L, 1mol/L NaOH or 1mol/L lithium hydroxides.
7. a kind of coating coating method, it is characterised in that the coating coating method is using described in the claims 1~6
The coating material that the preparation method of any adjustment hole structure coating material is obtained, coats the side or two of polyalkene diaphragm
Side, dries and obtains polyalkene diaphragm coating.
8. coating coating method according to claim 7, it is characterised in that the coating method be dip coating, rolling method,
Spraying process or cast coat.
9. coating coating method according to claim 7, it is characterised in that the drying temperature is 50~70 DEG C, described
Drying time is 1~10 minute.
10. a kind of coating, it is characterised in that the coating is obtained using the coating coating method of the claims 7, the painting
The thickness of layer is 1~4 μm, and the aperture of the coating is 80nm~1 μm.
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CN103408975A (en) * | 2013-08-16 | 2013-11-27 | 上海大学 | Coating material for lithium ion battery diaphragm |
CN105206777A (en) * | 2015-10-26 | 2015-12-30 | 武汉惠强新能源材料科技有限公司 | Lithium battery diaphragm containing porous inorganic oxide capable of conducting lithium ions, and preparation method thereof |
CN106221480A (en) * | 2016-07-26 | 2016-12-14 | 广东工业大学 | A kind of lithium ion battery separator coating and its preparation method and application |
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2017
- 2017-02-23 CN CN201710099849.2A patent/CN106928777A/en active Pending
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CN102181204A (en) * | 2011-03-01 | 2011-09-14 | 佛山市顺德区精进能源有限公司 | Coating for high-temperature-resistant membrane for lithium ion battery and preparation method of high-temperature-resistant membrane |
CN103408975A (en) * | 2013-08-16 | 2013-11-27 | 上海大学 | Coating material for lithium ion battery diaphragm |
CN105206777A (en) * | 2015-10-26 | 2015-12-30 | 武汉惠强新能源材料科技有限公司 | Lithium battery diaphragm containing porous inorganic oxide capable of conducting lithium ions, and preparation method thereof |
CN106221480A (en) * | 2016-07-26 | 2016-12-14 | 广东工业大学 | A kind of lithium ion battery separator coating and its preparation method and application |
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