CN113131090A - Diaphragm coating material, diaphragm, preparation method of diaphragm and battery cell - Google Patents

Diaphragm coating material, diaphragm, preparation method of diaphragm and battery cell Download PDF

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Publication number
CN113131090A
CN113131090A CN202110408446.8A CN202110408446A CN113131090A CN 113131090 A CN113131090 A CN 113131090A CN 202110408446 A CN202110408446 A CN 202110408446A CN 113131090 A CN113131090 A CN 113131090A
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diaphragm
weight
coating material
mixed solution
parts
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刘振国
孙祥军
杜立成
闫龙
王辉
梁世硕
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Kunshan Bao Innovative Energy Technology Co Ltd
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Kunshan Bao Innovative Energy Technology Co Ltd
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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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • 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
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C09D127/16—Homopolymers or copolymers of vinylidene fluoride
    • 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
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
    • 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
    • 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
    • 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
    • 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
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • 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
    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
    • 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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Abstract

The application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery core, and belongs to the technical field of batteries. The diaphragm coating material comprises 20-50 parts by weight of inorganic material particles, 1-10 parts by weight of binder and 80-120 parts by weight of solvent. The inorganic material particles comprise bimetallic composite oxide particles, and the bimetallic composite oxide is obtained by sintering layered double-hydroxyl composite metal oxide. The diaphragm coating layer is made of the bimetal composite oxide and can absorb and adsorb hydrofluoric acid, water and carbon dioxide in an electric core system, so that gas expansion of the electric core is effectively reduced, dissolution of positive metal is reduced, and the cycle life of the electric core is prolonged. The bimetal composite oxide absorbing the moisture and the carbon dioxide can be changed into the layered double-hydroxide-radical composite metal oxide again, and the layered double-hydroxide-radical composite metal oxide can release the water and the carbon dioxide at a high temperature state, so that the flame retardant effects of reducing the concentration of combustion gas and blocking oxygen are achieved, and the safety of the battery core is improved.

Description

Diaphragm coating material, diaphragm, preparation method of diaphragm and battery cell
Technical Field
The application relates to the technical field of batteries, in particular to a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery core.
Background
The lithium ion battery has the advantages of high energy density, long cycle life, no memory effect, environmental protection and the like, thereby being widely applied to the fields of digital electronics, power and energy storage.
The lithium ion battery mainly comprises a positive electrode, a negative electrode, a diaphragm and electrolyte. The diaphragm is one of the most critical inner layer assemblies in the structure of the lithium battery, and the diaphragm mainly has the functions of separating the positive and negative pole pieces to prevent the short circuit of the battery and simultaneously ensuring the normal passing of ions during charging and discharging to ensure the normal work of the battery. Therefore, the performance of the separator directly affects the capacity, rate, life, safety, and other properties of the battery.
The main components of the diaphragm are Polyethylene (PE) and polypropylene (PP) organic films, and the traditional PE and PP organic diaphragms have the problems of low melting point, insufficient mechanical strength and the like in the actual use process, and are easy to cause battery short circuit under extreme conditions. Inorganic ceramic materials (such as alumina and boehmite) have attracted attention due to the advantages of high melting point, good chemical stability, good affinity with electrolyte and the like, so that the composite diaphragm (organic materials are used as a bottom film, and ceramic particles are used as coating materials) improved by ceramic coating is concerned.
Disclosure of Invention
The application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell, which can effectively reduce moisture, carbon dioxide and hydrofluoric acid in a battery cell system, thereby effectively reducing gas expansion of the battery cell, reducing dissolution of positive metal, and improving cycle life and safety of the battery cell.
The embodiment of the application is realized as follows:
in a first aspect, the present disclosure provides a separator coating material including 20 to 50 parts by weight of inorganic material particles, 1 to 10 parts by weight of a binder, and 80 to 120 parts by weight of a solvent.
The inorganic material particles comprise bimetallic composite oxide particles, and the bimetallic composite oxide is obtained by sintering layered double-hydroxyl composite metal oxide.
In the technical scheme, the layered double-hydroxyl composite metal oxide has an inorganic supermolecular intercalation structure which is assembled by a main body laminate with positive charges and interlayer anions through the interaction of non-covalent bonds. The layered double-hydroxy composite metal oxide is sintered to obtain the double-metal composite oxide, and in the sintering process, the layered double-hydroxy composite metal oxide dehydrates and anions.
The diaphragm coating layer is made of the bimetal composite oxide and can absorb and adsorb water and carbon dioxide in the electric core system, so that the gas expansion of the electric core is effectively reduced. The bimetal composite oxide absorbing moisture and carbon dioxide can be changed into a layered double-hydroxyl composite metal oxide containing carbonate and hydroxyl again, and under the high-temperature thermal runaway state of the battery cell, the layered double-hydroxyl composite metal oxide can absorb heat and release water and carbon dioxide, so that the flame-retardant effect of reducing the temperature of the battery cell, the concentration of combustion gas and blocking oxygen is achieved, and the safety of the battery cell is improved.
Meanwhile, the diaphragm coating layer made of the bimetal composite oxide can adsorb and neutralize hydrofluoric acid in an electric core system, so that the dissolution of positive metal is reduced, the stability of the electric core is improved, and the service life of the electric core is prolonged.
In combination with the first aspect, in a first possible example of the first aspect of the present application, the bimetal composite oxide is obtained by sintering the layered double hydroxide composite metal oxide at 400 to 550 ℃ for 2 to 6 hours.
In a second possible example of the first aspect of the present application in combination with the first aspect, the inorganic material particles further include layered double-hydroxy composite metal oxide particles.
In the above examples, the inorganic material particles in the separator coating material of the present application may further include layered double hydroxy composite metal oxide particles, which are also capable of adsorbing and neutralizing hydrofluoric acid in the electrical core system.
In a third possible example of the first aspect of the present application in combination with the first aspect, the layered double hydroxy composite metal oxide has a chemical formula of M2+ 1-xM3+ x(OH)2]An- x/n·mH2O, wherein A is a cation and A comprises CO3 2-，M2+Is a divalent metal cation, M3+Is a trivalent metal cation.
In the above example, when the layered double-hydroxy composite metal oxide containing carbonate is in a high-temperature thermal runaway state of the battery cell, the layered double-hydroxy composite metal oxide can absorb heat and release water and carbon dioxide, so that the flame retardant effects of reducing the temperature of the battery cell, the concentration of combustion gas and blocking oxygen are achieved, and the safety of the battery cell is improved.
In a fourth possible example of the first aspect of the present application in combination with the first aspect, the content of the bimetal composite oxide particles in the inorganic material particles is equal to or greater than 20 wt%.
With reference to the first aspect, in a fifth possible example of the first aspect of the present application, the particle size of the inorganic material particles is 100 to 1000 nm.
In a sixth possible example of the first aspect of the present application in combination with the first aspect, the binder includes any one or more of polyvinyl alcohol, polyacrylic acid, polyvinylidene fluoride, polyimide, and polyacrylonitrile.
In a second aspect, the present application provides a method for preparing a separator, which comprises coating the above-mentioned separator coating material on the surface of a substrate.
Optionally, the coating amount of the diaphragm coating material is 1-10 g/m2。
In the technical scheme, the preparation method of the diaphragm is simple and convenient, and the prepared diaphragm is stable in performance.
In a third aspect, the present application provides a separator, which is produced according to the above-described method for producing a separator.
In above-mentioned technical scheme, the coating of the diaphragm of this application has the fire resistance, improves the security of electric core, and the coating of diaphragm can also adsorb and neutralize hydrofluoric acid in the electric core system, improves the stability and the life-span of electric core.
In a fourth aspect, the present examples provide a battery cell comprising the separator described above.
In above-mentioned technical scheme, the coating layer of the diaphragm of this application can absorb water and carbon dioxide in the electric core system to make the electric core gas inflation including the diaphragm lower. The battery core has the characteristics of high safety, good stability and long service life.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a picture of a cell of example 3 after heating to 130 ℃ and holding for 30 min;
FIG. 2 is a picture of the cell of example 4 after heating to 130 ℃ and holding for 30 min;
fig. 3 is a picture of the cell of comparative example 1 after heating to 130 ℃ and holding for 30 min.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following specifically describes a separator coating material, a separator, a preparation method thereof, and a battery cell in the embodiments of the present application:
the application provides a diaphragm coating material, which comprises 20-50 parts by weight of inorganic material particles, 1-10 parts by weight of binder and 80-120 parts by weight of solvent.
The inorganic material particles comprise bimetal composite oxide particles, and the bimetal composite oxide (LDO) is obtained by sintering layered double-hydroxyl composite metal oxide.
Layered double hydroxide metal oxides (LDHs), also known as Hydrotalcite-Like Compounds, are the generic names of Hydrotalcite (HT) and Hydrotalcite-Like Compounds (HTs). The layered double-hydroxy composite metal oxide belongs to an anion intercalation layered compound, and interlayer anions of the layered double-hydroxy composite metal oxide have interchangeability.
The chemical general formula of the layered double-hydroxyl composite metal oxide is M2+ 1-xM3+ x(OH)2]An- x/n·mH2O, wherein M2+、M3+Is a metal cation constituting the main body plate layer, An-Is an interlayer anion, and x is more than or equal to 0.2 and less than or equal to 0.33.
M2+Comprising Mg2+、Ni2+、Co2+、Zn2+Or Cu2+；
M3+Including Al3+、Cr3+、Fe3+、Sc3+、Ce3+Or Ti3+；
An-Comprising NO3 -、CO3 2-、Cl-、OH-、SO4 2-、PO4 3-Or C6H4(COO)2 2-。
The layered double-hydroxy composite metal oxide can be written as MM-A-LDH, and the double-metal composite oxide can be written as MM-LDO.
The application introduces a method for preparing a layered double-hydroxyl composite metal oxide by adopting a coprecipitation method, which comprises the following steps:
s1, dissolving divalent metal salt AY2And soluble trivalent metal salt BY3Dissolving in AY at a molar ratio of n:12And BY3Preparing a first mixed solution in the good solvent;
s2, mixing the molar ratio OH-/(A2++B3+) NaOH and molar ratio (M) of 1: Mn-/Al3+Na of s:1n(M)n-Dissolving in a good solvent to prepare a second mixed solution;
s3, dropwise adding the second mixed solution into the first mixed solution, adjusting the pH to 9-12, keeping the temperature at 60-80 ℃, heating and stirring for 12-72 hours, aging to obtain slurry, filtering and drying the slurry to obtain a crude product, and cleaning the crude product to obtain the layered double-hydroxy composite metal oxide powder.
Wherein n is more than or equal to 1 and less than or equal to 4, m is more than or equal to 1 and less than or equal to 3, and s is more than or equal to 1 and less than or equal to 4. Alternatively, the soluble divalent metal salt AY2Including Mg (NO)3)2、Co(NO3)2、Ni(NO3)2、Zn(NO3)2、MgCl2、CoCl2、NiCl2And ZnCl2Any one or more of them.
Alternatively, a soluble trivalent metal salt BY3Is Al (NO)3)3、Fe(NO3)3、Cr(NO3)3、Ce(NO3)3、Ti(NO3)3、AlCl3、FeCl3、CrCl3、CeCl3And TiCl3Any one or more of them.
Optionally, the good solvent comprises deionized water.
Alternatively, the anionic sodium salt Nan(M)n-Including Na2CO3、Na2SO4、Na2MoO4And Na2WO4And the like.
The method for producing the layered double-hydroxy composite metal oxide may be an ion exchange method or a thermal decomposition self-repair method, as well as the methods described in the present application.
The bimetal composite oxide has self-repairing and memory effects. The layered double-hydroxide composite metal oxide is thermally decomposed in a specific high-temperature sintering process, so that interlayer bound water, interlayer anions and laminate hydroxide are removed, and an ordered layered structure of the layered double-hydroxide composite metal oxide is destroyed, so that the double-metal composite oxide is obtained. The bimetal composite oxide is added into an anion solution or is partially or completely restored into the layered double-hydroxide composite metal oxide in the atmosphere of water vapor, carbon dioxide and the like.
The bimetal composite oxide is obtained by sintering a layered double-hydroxyl composite metal oxide at 400-550 ℃ for 2-6 h.
In one embodiment of the present application, the sintering temperature may be 500 ℃. In other embodiments of the present application, the sintering temperature may be 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃ or 550 ℃.
In one embodiment of the present application, the sintering time may be 4 hours. In other embodiments of the present disclosure, the sintering time may be 2h, 2.5h, 3h, 3.5h, 4.5h, 5h, 5.5h, or 6 h.
It should be noted that, when the sintering temperature of the layered double hydroxide composite metal oxide is low, the layered double hydroxide composite metal oxide cannot complete dehydration and anion; when the sintering temperature of the layered double-hydroxy composite metal oxide is higher, the obtained double-metal composite oxide loses self-repairing and memory effects and cannot be recovered into the layered double-hydroxy composite metal oxide.
The bimetal composite oxide is adopted as a raw material to prepare a diaphragm coating material, the diaphragm coating material is coated on the surface of a diaphragm substrate to form a composite diaphragm, and the composite diaphragm is made into a battery core. The bimetal composite oxide in the composite diaphragm can absorb and adsorb water and carbon dioxide in the electric core system, so that the water and the carbon dioxide in the electric core system are reduced, and the gas expansion of the electric core is effectively reduced. The bimetal composite oxide absorbing water and carbon dioxide is changed into a layered double hydroxide composite metal oxide containing carbonate and hydroxide. Under the high-temperature thermal runaway state of the battery cell, interlayer bound water, interlayer carbonate ions and laminate hydroxyl water of the layered double-hydroxyl composite metal oxide are released in the forms of water and carbon dioxide, and the water and the carbon dioxide can play the flame-retardant roles of reducing the concentration of combustion gas and blocking oxygen. In addition, the process of dehydration and carbon dioxide of the layered double-hydroxyl composite metal oxide is an endothermic reaction, so that heat can be absorbed, the temperature of the battery cell can be reduced, the safety of the battery cell is further improved, and the battery cell is prevented from burning and exploding.
Hydrofluoric acid also exists in the electric core system, and the hydrofluoric acid can corrode the positive electrode active material, so that positive electrode metal cations are dissolved out, the positive electrode structure is unstable, the active material is lost, and the capacity loss of the electric core is caused. In addition, the dissolved positive metal cations can be deposited on the surface of the negative electrode to damage a negative electrode SEI film, and further increase the ohmic resistance of the battery cell, so that the service life of the battery cell is shortened.
The bimetal composite oxide of the present application can reduce hydrofluoric acid in an electric core system from two aspects: on one hand, the bimetal composite oxide can adsorb and absorb water in the electric core system, hydrofluoric acid in the electric core system is generated by water reaction, and the hydrofluoric acid generated in the electric core system is reduced after the water in the electric core system is reduced; on the other hand, the bimetal composite oxide can adsorb and neutralize hydrofluoric acid in the electric core system, so that the hydrofluoric acid in the electric core system is reduced, and the stability and the service life of the electric core are improved.
The bimetal composite oxide particles of the present application may be made of one or more bimetal composite oxides. That is, the bimetallic composite oxide particles may include one or more different bimetallic composite oxide particles.
For example, the bimetallic composite oxide particles of the present application may be based solely on ZnAl-CO3-LDH A layered double hydroxide composite metal oxide sintered product, also based on ZnAl-CO3The layered double-hydroxyl composite metal oxides of-LDH and MgAl-OH-LDH are sintered to obtain products.
The inorganic material particles may be entirely of the bimetal composite oxide, or partially of the bimetal composite oxide.
Optionally, the content of the bimetallic composite oxide particles in the inorganic material particles is more than or equal to 20 wt%.
Optionally, the content of the bimetallic composite oxide particles in the inorganic material particles is more than or equal to 30 wt%.
Optionally, the content of the bimetallic composite oxide particles in the inorganic material particles is more than or equal to 50 wt%.
Optionally, the content of the bimetallic composite oxide particles in the inorganic material particles is more than or equal to 80 wt%.
The inorganic material particles also include layered double-hydroxy composite metal oxide particles.
The layered double-hydroxyl composite metal oxide can also adsorb and neutralize hydrofluoric acid in an electric core system, reduce the hydrofluoric acid in the electric core system, and improve the stability and the service life of the electric core.
Alternatively, the layered double hydroxide composite metal oxide made into the layered double hydroxide composite metal oxide particle includes carbonate.
Under the high-temperature thermal runaway state of the battery cell, interlayer bound water of carbonate-containing layered double-hydroxyl composite metal oxide particles, interlayer carbonate ions and laminate hydroxyl water are released in the form of water and carbon dioxide, and the water and the carbon dioxide can play a flame-retardant role in reducing the concentration of combustion gas and blocking oxygen. The battery can absorb heat, is favorable for reducing the temperature of the battery cell, further improves the safety of the battery cell, and prevents the battery cell from burning and exploding.
The inorganic material particles may also include alumina and/or boehmite.
Optionally, the particle size of the inorganic material particles is 100-1000 nm.
The binder comprises any one or more of polyvinyl alcohol, polyacrylic acid, polyvinylidene fluoride, polyimide and polyacrylonitrile.
The solvent includes water or N-methylpyrrolidone (NMP).
The diaphragm coating material also comprises 0-5 parts by weight of a dispersing agent and 0-1 part by weight of an auxiliary agent.
Wherein the dispersant comprises sodium carboxymethylcellulose (CMC-Na) and/or sodium acrylate.
The auxiliary agent comprises any one or more of a defoaming agent, a leveling agent and a wetting agent.
Optionally, the diaphragm coating material comprises 30-40 parts by weight of inorganic material particles, 2-8 parts by weight of binder, 80-100 parts by weight of solvent, 0-3 parts by weight of dispersant and 0-1 part by weight of auxiliary agent.
When the diaphragm coating material comprises the dispersing agent and the impregnating compound, the preparation method comprises the following steps:
s11, mixing the first dispersing agent and the solvent, and uniformly stirring at a high speed to prepare a third mixed solution;
s12, mixing the inorganic material particles with the third mixed solution, uniformly stirring at a high speed, and performing ball milling to obtain a fourth mixed solution;
s13, mixing the second dispersing agent and the fourth mixed solution, and uniformly stirring at a high speed to prepare a fifth mixed solution;
and S14, mixing the binder and the fifth mixed solution, and uniformly stirring at a high speed to obtain a sixth mixed solution.
And S15, mixing the impregnating compound and the sixth mixed solution, uniformly stirring at a high speed, and filtering to obtain the membrane coating material.
When the diaphragm coating material does not contain a dispersing agent and a wetting agent, the preparation method comprises the following steps:
s21, mixing the binder and the solvent, and uniformly stirring at a high speed to prepare a seventh mixed solution;
and S22, mixing the inorganic material particles with the seventh mixed solution, uniformly stirring at a high speed, ball-milling, and filtering to obtain the membrane coating material.
The application also provides a preparation method of the diaphragm, which comprises the step of coating the diaphragm coating material on the surface of a substrate.
Optionally, the coating amount of the diaphragm coating material is 1-10 g/m2。
Optionally, the matrix comprises polypropylene or polyethylene.
The bimetallic composite oxide particles and the layered double-hydroxyl composite metal oxide particles are nanosheets with regular shapes, the nanosheets are coated on the surface of the diaphragm substrate through the adhesive to form a diaphragm coating layer, and the nanosheets are in a porous structure on the surface of the substrate, so that the infiltration of electrolyte can be increased, and the conduction of lithium ions can be guaranteed.
The application also provides a diaphragm prepared according to the preparation method of the diaphragm.
The diaphragm of this application has the fire resistance, improves the security of electric core, and the diaphragm can also adsorb and neutralize hydrofluoric acid in the electric core system, improves the stability and the life-span of electric core.
The application also provides a battery cell, which comprises the diaphragm.
The battery core has the characteristics of high safety, good stability and long service life.
The following describes a separator coating material, a separator, a preparation method thereof, and a battery cell in further detail with reference to examples.
Example 1
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 40 parts by weight of MgAl-LDO powder into the third mixed solution, stirring for 2 hours at 1000rpm, and carrying out ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 2
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 4 parts by weight of polyvinylidene fluoride binder in 80 parts by weight of N-methyl pyrrolidone, and stirring for 2 hours at 500rpm to prepare a seventh mixed solution;
and S2, adding 40 parts by weight of MgAl-LDO powder into the seventh mixed solution, stirring for 2 hours at 1000rpm, ball-milling the uniformly dispersed solution, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 3
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1.5 parts by weight of sodium acrylate dispersing agent in 90 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 50 parts by weight of MgAl-LDO powder into the third mixed solution, stirring for 2 hours at 1000rpm, and carrying out ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 8 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3.5 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 4
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 20 parts by weight of MgAl-LDO powder and 20 parts by weight of alumina ceramic powder into the third mixed solution, stirring for 2 hours at 1000rpm, and performing ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 5
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, mixing 20 parts by weight of MgAl-LDO powder and 20 parts by weight of MgAl-CO3LDH powder is added into the third mixed solution, the third mixed solution is stirred for 2 hours at the speed of 1000rpm, and the evenly dispersed solution is ball-milled to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 6
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 40 parts by weight of ZnAl-LDO powder into the third mixed solution, stirring for 2 hours at 1000rpm, and carrying out ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 7
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, mixing 20 weight parts of MgAl-LDO powder and 10 weight parts of MgAl-CO3Adding LDH powder and 10 parts by weight of boehmite powder into the third mixed solution, stirring for 2 hours at 1000rpm, and performing ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 8
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 5 parts by weight of polyvinylidene fluoride binder in 80 parts by weight of N-methyl pyrrolidone, and stirring for 1h at 500rpm to prepare a seventh mixed solution;
and S2, adding 40 parts by weight of ZnAl-LDO powder into the seventh mixed solution, stirring for 2 hours at 1000rpm, ball-milling the uniformly dispersed solution, and filtering to obtain the diaphragm coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Example 9
The embodiment of the application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 8 parts by weight of MgAl-LDO powder and 32 parts by weight of boehmite powder into the third mixed solution, stirring for 2 hours at 1000rpm, and performing ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution 3008, and stirring for 0.5h at 800rpm to obtain a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Comparative example 1
The application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 40 parts by weight of alumina ceramic powder into the third mixed solution, stirring for 2 hours at 1000rpm, and carrying out ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Comparative example 2
The application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, adding 40 parts by weight of boehmite powder into the third mixed solution, stirring for 2 hours at 1000rpm, and performing ball milling on the uniformly dispersed solution to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Comparative example 3
The application provides a diaphragm coating material, a diaphragm, a preparation method of the diaphragm and a battery cell.
1. Separator and method for producing same
S1, dissolving 1 part by weight of sodium acrylate dispersing agent in 80 parts by weight of water, and stirring for 1h under the condition of 500rpm to obtain a third mixed solution;
s2, mixing 40 weight parts of MgAl-CO3LDH powder is added into the third mixed solution, the third mixed solution is stirred for 2 hours at the speed of 1000rpm, and the evenly dispersed solution is ball-milled to obtain a fourth mixed solution;
s3, adding 10 parts by weight of sodium carboxymethyl cellulose solution dispersant with solid content of 4% into the fourth mixed solution, and stirring for 0.5h under the condition of 800rpm to obtain a fifth mixed solution;
s4, adding 3 parts by weight of polyacrylic acid binder into the fifth mixed solution, and stirring for 0.5h at 800rpm to prepare a sixth mixed solution;
s5, adding 0.5 part by weight of siloxane impregnating compound into the sixth mixed solution, stirring for 0.5h at 500rpm, and filtering to obtain the membrane coating material.
2. Separator and method for producing same
The surface of a polyethylene base material having a thickness of 9 μm was coated with a coating amount of 4.5g/m2And preparing the diaphragm.
3. Battery cell
The prepared diaphragm is used for preparing a lithium ion battery, wherein the anode active material of the lithium ion battery is a ternary material NCM811, and the cathode active material is artificial graphite.
Test example 1
The battery cells prepared in examples 1 to 9 and comparative examples 1 to 3 were taken, and the volume expansion rate of the battery cells and the content of metal elements in the negative electrode plate after 100 cycles of the battery cells were tested, as shown in table 1:
TABLE 1
Figure BDA0003022987940000181
Figure BDA0003022987940000191
It can be seen from comparison of examples 1 to 9 and comparative examples 1 to 3 that the separator prepared by using the bimetal composite oxide particles as the raw material of the separator coating material can effectively reduce the gas expansion of the battery cell and reduce the dissolution of the positive electrode metal.
Test example 2
The cells prepared in example 3, example 4 and comparative example 1 were taken and fully charged, and then the fully charged cells were placed in an incubator, which was heated to 130 ℃ at a heating rate of 5 ℃/min and kept at 130 ℃ for 30min, and the cells were observed.
As shown in fig. 1-2, cells of examples 3 and 4 did not spontaneously ignite, while cells of comparative example 1 did spontaneously ignite, as shown in fig. 3.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A membrane coating material, characterized in that the membrane coating material comprises: 20-50 parts by weight of inorganic material particles, 1-10 parts by weight of a binder and 80-120 parts by weight of a solvent;
the inorganic material particles comprise bimetal composite oxide particles, and the bimetal composite oxide is obtained by sintering layered double-hydroxyl composite metal oxide.
2. The membrane coating material as claimed in claim 1, wherein the bimetal composite oxide is obtained by sintering a layered double-hydroxy composite metal oxide at 400-550 ℃ for 2-6 h.
3. The membrane coating composition of claim 1, wherein the inorganic material particles further comprise layered double hydroxy composite metal oxide particles.
4. The membrane coating material of claim 3, wherein the layered double hydroxide composite metal oxide has a chemical formula of M2+ 1-xM3+ x(OH)2]An- x/n·mH2O, wherein A is an anion and A comprises CO3 2-，M2+Is a divalent metal cation, M3 +Is a trivalent metal cation.
5. The membrane coating material as claimed in any one of claims 1 to 4, wherein the content of the bimetal composite oxide particles in the inorganic material particles is not less than 20 wt%.
6. The separator coating material according to any one of claims 1 to 4, wherein the particle size of the inorganic material particles is 100 to 1000 nm.
7. The membrane coating material as claimed in any one of claims 1 to 4, wherein the binder comprises any one or more of polyvinyl alcohol, polyacrylic acid, polyvinylidene fluoride, polyimide and polyacrylonitrile.
8. A method for producing a separator, characterized by comprising applying the separator coating material according to any one of claims 1 to 7 on a surface of a substrate;
optionally, the coating amount of the diaphragm coating material is 1-10 g/m2。
9. A separator produced by the method for producing a separator according to claim 8.
10. A cell comprising the separator of claim 9.
CN202110408446.8A 2021-04-15 2021-04-15 Diaphragm coating material, diaphragm, preparation method of diaphragm and battery cell Withdrawn CN113131090A (en)

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