CN116247374B - High-temperature-resistant ceramic composite lithium battery diaphragm and preparation method thereof - Google Patents
High-temperature-resistant ceramic composite lithium battery diaphragm and preparation method thereof Download PDFInfo
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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
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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
- H01M50/431—Inorganic material
- H01M50/434—Ceramics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a high-temperature-resistant ceramic composite lithium battery diaphragm and a preparation method thereof, and relates to the field of lithium ion batteries; adding a dispersing agent, modified ceramic particles, a thickening agent, a high glass transition temperature binder and a wetting agent into deionized water, and stirring to obtain coating slurry; and coating the coating slurry on one or two sides of the base film, controlling the thickness of the coating, and drying to obtain the high-temperature-resistant ceramic composite lithium battery diaphragm. The invention uses the bonding agents with different properties to enhance the bonding effect among the silane coupling agent, the ceramic particles and the base film, and improves the compactness and the heat resistance.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a high-temperature-resistant ceramic composite lithium battery diaphragm and a preparation method thereof.
Background
With the high-speed development of new energy industry, indexes such as energy density, power density, safety and the like of the lithium ion battery are continuously improved. The separator is one of important components of the lithium ion battery and plays a vital role in the performance of the lithium ion battery. The quality and thickness of the diaphragm affect the energy density of the battery, the connectivity of the holes and the structure of the holes affect the power density, and the high temperature resistance affects the safety. Therefore, development of ultra-thin, highly interconnected pore, high heat resistant separators is currently the focus of research in the lithium ion battery field. Among them, safety is a precondition of wide application of technology, and development of high heat-resistant diaphragm is a serious issue in lithium battery industry at present.
Patent CN113594629a discloses a high temperature resistant coating film, a preparation method and an electrochemical device thereof, wherein slurry containing ultraviolet initiator, ultraviolet crosslinking agent, high molecular emulsion, binder, dispersant and solvent is coated on a polyolefin-based film, and the high temperature resistant composite diaphragm is obtained through ultraviolet irradiation. Patent CN114335892a discloses a high temperature resistant diaphragm and a preparation method thereof, wherein an inorganic binder containing silicon and aluminum is used for replacing an organic binder and ceramic particles to prepare slurry, and the slurry is coated on a polyethylene diaphragm to obtain the high temperature resistant diaphragm. Patent CN115207572a discloses a high-temperature resistant composite membrane and a preparation method thereof, wherein boehmite coated alumina ceramic particles and a high-melting point modified polyacrylic acid aqueous solution binder are adopted to prepare slurry, and the slurry is coated on a polyethylene-based membrane to obtain the high-temperature resistant composite membrane. Patent CN113161684a discloses a high-temperature-resistant and high-strength diaphragm and a preparation method thereof, wherein a water-based ceramic slurry is coated on a base film, the base film is dried, then an aramid slurry is coated, and the high-temperature-resistant diaphragm is obtained through extraction.
The method of in-situ polymerization or organic solvent coating can obviously improve the heat resistance of the diaphragm, however, the method is complex and has higher cost. The use of an inorganic binder instead of a polymeric binder further increases separator quality, which is detrimental to battery energy density improvement. The diaphragm coated on one side with conventional ceramic and adhesive slurry is obviously shrunk at 150 ℃. The heat resistance of the diaphragm can be improved by adopting the high-temperature-resistant adhesive and ceramic blending coating, however, the high-temperature-resistant adhesive has poor adhesion, and the problem of non-compact coating layer and coating leakage exists. Patent CN10981779a discloses a battery separator, a preparation method thereof and a battery, and uses a silane coupling agent to modify the surface of ceramic particles and then mix with a high temperature resistant adhesive for coating, although the silane coupling agent can crosslink with the adhesive, the problem of non-compact coating layer and coating missing can not be avoided because the high temperature resistant adhesive has weak self-adhesion.
Therefore, there is a need to develop a dense, non-slip coated, high temperature resistant ceramic coated separator.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant ceramic composite lithium battery diaphragm and a preparation method thereof, which utilize binders with different properties to enhance the bonding effect among a silane coupling agent, ceramic particles and a base film and improve the compactness and heat resistance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A preparation method of a high-temperature-resistant ceramic composite lithium battery diaphragm comprises the following steps:
(1) Immersing ceramic particles in a silane coupling agent solution, stirring, cleaning and drying for the first time, and then placing the ceramic particles in a low-glass-transition-temperature binder aqueous solution, wherein the glass transition temperature of the low-glass-transition-temperature binder is less than or equal to 50 ℃, and stirring, cleaning and drying for the second time to obtain modified ceramic particles;
(2) Adding a dispersing agent, modified ceramic particles, a thickening agent, a high glass transition temperature binder and a wetting agent into deionized water, and stirring to obtain coating slurry, wherein the glass transition temperature of the high glass transition temperature binder is more than or equal to 150 ℃;
(3) And coating the coating slurry on one or two sides of the base film, controlling the thickness of the coating, and drying to obtain the high-temperature-resistant ceramic composite lithium battery diaphragm.
Preferably, the mass ratio of the ceramic particles to the silane coupling agent solution is (1-5): 10.
Preferably, the silane coupling agent is one of 3-aminopropyl-trimethoxysilane, 3-aminopropyl-triethoxysilane, and N- (2-aminoethyl) -3-aminopropyl trimethoxysilane.
Preferably, the solute concentration of the silane coupling agent solution is 0.01-1mol/L, the solvent is a mixed solution of ethanol and water, and the ethanol accounts for 50-95wt% of the mixed solution.
Preferably, the ceramic particles are one of alumina and boehmite, D (90) is less than or equal to 2um, and D (50) is less than or equal to 0.5um and less than or equal to 0.8um.
Preferably, the temperature of each mechanical stirring in the step (1) is 15-40 ℃, and the stirring time is 0.5-2h; washing with deionized water each time; the first drying temperature is 100-200deg.C, and the drying time is 0.5-1h; the second drying temperature is 40-80deg.C, and the drying time is 3-6h.
Preferably, the low glass transition temperature binder is an acrylic copolymer or a homopolymer with a glass transition temperature less than or equal to 50 ℃, and comprises one of polyethyl acrylate, n-propyl acrylate, n-butyl acrylate, isobutyl acrylate, n-pentyl acrylate, n-hexyl acrylate, 2-ethylhexyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate and polydimethyl amino ethyl methacrylate.
Preferably, the concentration of the low glass transition temperature binder aqueous solution is 1 to 10wt%.
Preferably, in the step (2), the dispersant is 0.05 to 0.5wt%, the modified ceramic particles are 30 to 50wt%, the thickener is 0.05 to 0.5wt%, the high glass transition temperature binder is 3 to 8wt%, and the wetting agent is 0.05 to 0.5 wt%.
Preferably, the dispersing agent is one of fluoroalkyl ethoxyl alcohol ether, fatty alcohol polyoxyethylene ether, ding Bennai sodium sulfonate, hydroxyethyl sodium sulfate and dodecyl sodium sulfate.
Preferably, the thickener is one of carboxymethyl cellulose and sodium carboxymethyl cellulose.
Preferably, the high glass transition temperature binder is an acrylic copolymer or a homopolymer with a glass transition temperature of more than or equal to 150 ℃, and comprises one of polymethacrylic acid, polymethacrylamide and polyacrylamide.
Preferably, the wetting agent is one of fluoroalkyl methoxy ether alcohol, polyacrylic acid, sodium polyacrylate, alkyne glycol vinyl ether, fatty acid polyoxyethylene ether, ammonium polyacrylate, siloxane, polysiloxane and fatty acid salt.
Preferably, in the step (2), the stirring temperature is 15-60 ℃ and the stirring time is 0.5-6h.
Preferably, in the step (3), the coating is performed by adopting a conventional diaphragm coating mode such as a micro concave roller, a wire rod and the like.
Preferably, the base film is a commercial polyethylene separator.
Preferably, the thickness of the coating in the step (3) is 1.5-3um, the drying temperature is 40-80 ℃ and the drying time is 0.5-5min.
The high-temperature-resistant ceramic composite lithium battery diaphragm is prepared by the method.
The beneficial effects of the invention are as follows:
the invention firstly uses the high adhesive property of the adhesive with low glass transition temperature as the adhesive with high adhesive property, loads the adhesive on the surface of ceramic particles through the non-covalent interaction between the adhesive and the silane coupling agent, and increases the adhesive property of the particles; then, the ceramic particles are anchored on the surface of the base film by utilizing the low viscosity and high thermal stability of the high glass transition temperature binder, so that the ceramic particles can maintain the stable size of the diaphragm at high temperature, and the coating is compact and has no leakage coating; solves the problem of heat shrinkage caused by poor heat resistance of the adhesive in the high-temperature environment of the ceramic coating film in the prior art.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a coated surface of a sample prepared in example 2 of the present invention.
FIG. 2 is an SEM photograph of the coated surface of a sample prepared according to comparative example 1 of the present invention.
FIG. 3 is an SEM photograph of the coated surface of a sample prepared according to comparative example 2 of the present invention.
Detailed Description
In order that the above features and advantages of the invention will be readily understood, a more particular description thereof will be rendered by reference to the appended drawings.
Example 1
(1) Preparing a 95wt% ethanol aqueous solution of 1 mol/L3-aminopropyl-trimethoxysilane, and mixing alumina particles with D90 of 2um and D50 of 0.8um according to a mass ratio of 1:10 is immersed in the solution, stirred for 0.5h at 40 ℃, then washed by deionized water, and put into a 100 ℃ oven for drying for 1h. And adding 10wt% of an aqueous solution of polyethyl acrylate into the dried alumina, stirring at 40 ℃ for 0.5h, cleaning with deionized water, and drying at 40 ℃ for 6h to obtain the modified ceramic particles.
(2) Adding 0.5wt% of fluoroalkyl ethoxy alcohol ether into deionized water, wherein the modified ceramic particles in the step (1) are 30wt%, carboxymethyl cellulose is 0.5wt%, polymethacrylic acid is 8wt%, fluoroalkyl methoxy ether alcohol is 0.5wt%, and stirring is carried out at 60 ℃ for 0.5h, so as to obtain coating slurry.
(3) And (3) coating the coating slurry in the step (2) on one side of a commercial polyethylene diaphragm through a micro-concave roller, wherein the thickness of the coating is 3um, and drying at 40 ℃ for 5min to obtain the high-temperature-resistant ceramic-coated composite lithium battery diaphragm.
Example 2
(1) Preparing a 75wt% ethanol aqueous solution of 0.1 mol/L3-aminopropyl-trimethoxysilane, and mixing alumina particles with D90 of 2um and D50 of 0.8um according to a mass ratio of 3:10 is immersed in the solution, stirred for 1h at 35 ℃, then washed by deionized water, and dried for 0.5h in a 200 ℃ oven. And adding 8wt% of an aqueous solution of polyethyl acrylate into the dried alumina, stirring at 35 ℃ for 1h, cleaning with deionized water, and drying at 60 ℃ for 5h to obtain the modified ceramic particles.
(2) Adding 0.25wt% of fluoroalkyl ethoxy alcohol ether into deionized water, 40wt% of modified ceramic particles, 0.1% of carboxymethyl cellulose, 5wt% of polymethacrylic acid, 0.2% of fluoroalkyl methoxy ether alcohol and stirring at 40 ℃ for 3 hours to obtain coating slurry.
(3) And (3) coating the coating slurry in the step (2) on one side of a commercial polyethylene diaphragm through a micro-concave roller, wherein the thickness of the coating is 2um, and drying at 60 ℃ for 2min to obtain the high-temperature-resistant ceramic-coated composite lithium battery diaphragm.
Example 3
(1) Preparing a 50wt% ethanol aqueous solution of 0.01 mol/L3-aminopropyl-triethoxysilane, and mixing alumina particles with D90 of 1.5um and D50 of 0.5um according to a mass ratio of 5:10 is immersed in the water, stirred for 2 hours at 15 ℃, washed by deionized water, and put into a baking oven at 150 ℃ for drying for 1 hour. And adding the dried alumina into a 1wt% hydroxyethyl polyacrylate aqueous solution, stirring at 15 ℃ for 2 hours, cleaning with deionized water, and drying at 80 ℃ for 3 hours to obtain the modified ceramic particles.
(2) Adding 0.05wt% of sodium hydroxyethyl sulfate into deionized water, 50wt% of modified ceramic particles, 0.05wt% of carboxymethyl cellulose, 3wt% of polymethacrylic acid, 0.05% of fluoroalkyl methoxy ether alcohol and stirring at 15 ℃ for 6 hours to obtain coating slurry.
(3) And (3) coating the coating slurry in the step (2) on two sides of a commercial polyethylene diaphragm through a micro-concave roller, wherein the thickness of the coating is 1.5um, and drying for 1min at 80 ℃ to obtain the high-temperature-resistant ceramic coating composite lithium battery diaphragm.
Comparative example 1
In this comparative example, the ceramic particles of example 2 were directly coated as a film from step (2) without modification.
Comparative example 2
In this comparative example, the ceramic particles of example 2 were modified only with a silane coupling agent, were not modified with a binder, and were coated to form a film by step (2).
The properties of the separators prepared in the above examples and comparative examples are shown in table 1.
Table 1 separator properties prepared in examples and comparative examples
From table 1, it can be seen that the separator coated with the coupling agent/high-adhesion binder modified ceramic particles (example 2) has higher separator peel strength and lower heat shrinkage than the separator unmodified (comparative example 1) and modified by the coupling agent alone (comparative example 2). The scanning electron microscope of the attached drawing shows that the surface of the embodiment 2 is compact and has no defect, and the comparative examples 1 and 2 have missing coating defects, which again show that the coupling agent/high-adhesion modified ceramic particles provided by the invention can effectively improve the coating compactness and the heat resistance of the polyethylene film.
The testing method comprises the following steps: the separator was tested for thickness, air permeability, 180℃C/1 h heat shrinkage according to GB/T36363-2018. The peeling strength is tested by adopting a double-sided adhesive tape pasting method, the stretching speed is 250mm/min, and the effective test interval is 50mm. The morphology of the coated surface of the samples was characterized using a JSM-7500F scanning electron microscope.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The preparation method of the high-temperature-resistant ceramic composite lithium battery diaphragm is characterized by comprising the following steps of:
(1) Immersing ceramic particles in a silane coupling agent solution, stirring, cleaning and drying for the first time, and then placing the ceramic particles in a low glass transition temperature binder aqueous solution, wherein the low glass transition temperature binder is an acrylic copolymer or homopolymer with the glass transition temperature less than or equal to 50 ℃, and stirring, cleaning and drying for the second time to obtain modified ceramic particles;
(2) Adding a dispersing agent, modified ceramic particles, a thickening agent, a high glass transition temperature binder and a wetting agent into deionized water, wherein the high glass transition temperature binder is an acrylic copolymer or a homopolymer with the glass transition temperature of more than or equal to 150 ℃, and stirring to obtain coating slurry;
(3) And coating the coating slurry on one or two sides of the base film, controlling the thickness of the coating, and drying to obtain the high-temperature-resistant ceramic composite lithium battery diaphragm.
2. The method of claim 1, wherein the mass ratio of ceramic particles to silane coupling agent solution is (1-5): 10.
3. The method of claim 1 or 2, wherein,
The silane coupling agent is one of 3-aminopropyl-trimethoxy silane, 3-aminopropyl-triethoxy silane and N- (2-aminoethyl) -3-aminopropyl trimethoxy silane; and/or
The solute concentration of the silane coupling agent solution is 0.01-1mol/L, the solvent is a mixed solution of ethanol and water, and the mass fraction of the ethanol in the mixed solution is 50-95wt%; and/or
The ceramic particles are one of alumina and boehmite, D (90) is less than or equal to 2um, D (50) is less than or equal to 0.5um and less than or equal to 0.8um.
4. The method of claim 1, wherein in step (1),
The temperature of each stirring is 15-40 ℃, and the stirring time is 0.5-2h; and/or
Washing with deionized water each time; and/or
The first drying temperature is 100-200deg.C, and the drying time is 0.5-1h; and/or
The second drying temperature is 40-80deg.C, and the drying time is 3-6h.
5. The method of claim 1, wherein,
The low glass transition temperature binder comprises one of polyethyl acrylate, n-propyl polyacrylate, n-butyl polyacrylate, isobutyl polyacrylate, n-pentyl polyacrylate, n-hexyl polyacrylate, 2-ethylhexyl polyacrylate, hydroxyethyl polyacrylate, hydroxypropyl polyacrylate and dimethylaminoethyl polymethacrylate; and/or
The concentration of the aqueous binder solution with low glass transition temperature is 1-10wt%.
6. The method of claim 1, wherein the dispersant in step (2) is 0.05 to 0.5wt%, the modified ceramic particles are 30 to 50wt%, the thickener is 0.05 to 0.5wt%, the high glass transition temperature binder is 3 to 8wt%, and the wetting agent is 0.05 to 0.5 wt%.
7. The method of claim 1 or 6, wherein,
The dispersing agent is one of fluoroalkyl ethoxyl alcohol ether, fatty alcohol polyoxyethylene ether, ding Bennai sodium sulfonate, hydroxyethyl sodium sulfate and dodecyl sodium sulfate; and/or
The thickener is one of carboxymethyl cellulose and sodium carboxymethyl cellulose; and/or
The high glass transition temperature binder comprises one of polymethacrylic acid, polymethacrylamide and polyacrylamide; and/or
The wetting agent is one of fluoroalkyl methoxy ether alcohol, polyacrylic acid, sodium polyacrylate, alkyne glycol vinyl ether, fatty acid polyoxyethylene ether, ammonium polyacrylate, siloxane, polysiloxane and fatty acid salt.
8. The method according to claim 1, wherein the stirring temperature in the step (2) is 15 to 60 ℃ and the stirring time is 0.5 to 6 hours.
9. The method of claim 1, wherein in step (3),
The thickness of the coating is 1.5-3um; and/or
The drying temperature is 40-80deg.C, and the drying time is 0.5-5min.
10. A high temperature resistant ceramic composite lithium battery separator prepared by the method of any one of claims 1-9.
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| CN117878529A (en) * | 2024-03-13 | 2024-04-12 | 宁波长阳科技股份有限公司 | Low-moisture high-heat-resistance ceramic coating diaphragm and preparation method thereof |
| CN118738765B (en) * | 2024-08-28 | 2025-01-17 | 深圳好电科技有限公司 | Diaphragm slurry composition, composite ceramic diaphragm and secondary battery |
| CN119231087A (en) * | 2024-09-26 | 2024-12-31 | 江苏北星新材料科技有限公司 | A ceramic coated lithium ion battery separator and preparation method thereof |
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| JP2014149935A (en) * | 2013-01-31 | 2014-08-21 | Nippon Zeon Co Ltd | Secondary battery separator, method for manufacturing secondary battery separator, and secondary battery |
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