WO2015154320A1 - 一种新型改性无纺布锂离子电池隔膜及其制备方法 - Google Patents
一种新型改性无纺布锂离子电池隔膜及其制备方法 Download PDFInfo
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- H—ELECTRICITY
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- 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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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
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- 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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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/426—Fluorocarbon polymers
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/429—Natural polymers
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/429—Natural polymers
- H01M50/4295—Natural cotton, cellulose or wood
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- 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
- H01M50/437—Glass
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- 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
- H01M50/443—Particulate material
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- H—ELECTRICITY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the invention relates to a novel modified non-woven lithium ion battery separator, and to a preparation method of the battery separator.
- Polyethylene and polypropylene separators currently in commercial use are more suitable for digital batteries such as mobile phones and cameras.
- this type of diaphragm there are some shortcomings in this type of diaphragm: On the one hand, when the melting temperature of the polyolefin is lower than 165 °C, the battery may be melted when the external temperature is too high or accidentally hit, causing the battery to be short-circuited, resulting in battery burning. Explosion; On the other hand, the polyolefin electrolyte has poor ability to maintain electrolyte capacity, resulting in poor battery cycle life, high current charge and discharge performance. The lack of safety and electrical performance of such diaphragms limits their use in power storage batteries.
- the patent CN102629679A provides a three-layer nanofiber lithium ion composite membrane, which has good thermal stability, high porosity, good liquid absorption capacity, and is improved by hot pressing composite. Mechanical strength.
- the three-layer composite structure is formed by electrospinning, the peel strength of the separator is low, resulting in a large interfacial impedance, and the internal resistance of the battery is still large, which is not conducive to large current charging and discharging of the power storage battery, and The aperture is too large, the high-voltage insulation is poor during battery manufacturing, and the short-circuit rate in the battery is as high as 10%.
- Patent CN1679185 provides a ceramic diaphragm suitable for high power lithium ion batteries.
- the separator is coated with a ceramic coating on a substrate of the nonwoven fabric, and has oxide particles of elements of Al, Zr, Si and an inorganic material having an ion conductive function.
- the biggest advantage of the separator is high ion conductivity, high melting point above 250 °C, good thermal stability and good electrochemical stability.
- the prepared battery is excellent in high current charge and discharge performance.
- the inorganic material of the diaphragm coating layer is exposed on the outer surface, and is easy to absorb water, thereby producing a suction of the diaphragm. The water is extremely high. It is difficult to remove the moisture by the ordinary baking process in the battery manufacturing process.
- the water will react with the electrolyte, causing the battery to swell and the internal resistance is increased.
- the battery electrochemical performance is deteriorated, such as large capacity loss of the battery, poor cycle life, and the like.
- the brittle inorganic coating has poor adhesion to the flexible substrate, resulting in poor mechanical handling during processing of the battery, and the separator is prone to problems such as bending voids, cracks, and damage, resulting in short circuit of the battery. If the problem of battery bubbling is to be solved, a longer baking time or a higher temperature to remove water in the process of preparing the battery increases the possibility of damage and shedding of the brittle inorganic coating.
- the strength of the diaphragm is poor, and the processing requirement of high-speed automatic winding cannot be satisfied, the puncture resistance of the pole piece is poor, and the short circuit rate is high.
- the above diaphragms are optimized for different performances, but we can see from the above analysis that there is still much room for improvement. Because the power storage battery is required to be a high-capacity and high-power charge and discharge battery, it has high requirements on the diaphragm in terms of safety performance and electrical performance, so the diaphragm should have good thermal stability and electrochemical stability at the same time. High performance, high lithium ion conductivity, excellent liquid retention, low moisture content, and easy battery processing. Summary of the invention
- the present invention provides a novel modified non-woven lithium ion battery separator, and the present invention.
- the invention also provides a method of preparing the battery separator.
- a novel modified non-woven lithium ion battery separator comprising a modified non-woven substrate and a composite filler thereof:
- the filler is filled in the pores of the modified nonwoven fabric substrate, and at this time, the pores of the nonwoven fabric substrate are filled with a filler; preferably, the filler is from the pore of the modified nonwoven fabric substrate.
- the thickness of the separator Extending the inside and outside to coat the entire modified non-woven fabric substrate, the thickness of the separator being 1-10 times the thickness of the modified non-woven fabric substrate, more preferably The thickness of the separator is 1-2 times the thickness of the modified nonwoven fabric substrate.
- the structure of the modified non-woven lithium ion battery separator is a layer of non-woven fiber layer in the middle, and the nonwoven fabric is non-woven.
- the pores of the cloth substrate are filled with a filler, and the surface of the nonwoven fabric substrate is also coated with a filler;
- the modified non-woven substrate the pores having a pore size of 1-50000 nm are distributed on the substrate to ensure the thickness of the non-woven modified composite film and the uniformity of the pore structure; And the liquid surface tension and other factors, the substrate porosity is 30-95%, the porosity is more than 30%, the prepared membrane has better liquid absorption and liquid retention ability, ensuring the conduction of lithium ions in the diaphragm, making the system
- the obtained battery has a small internal resistance, which is favorable for high-power charging and discharging of the battery, but the porosity is greater than 95%, which may result in insufficient strength of the non-woven substrate, and the obtained separator battery has poor processability and low yield.
- the modified non-woven substrate comprises a low melting point material and a high melting point material, the low melting point material is subjected to melt crystallization treatment, and the high melting point material is 85-99.9% of the total weight of the modified non-woven substrate, and the rest is a low melting point material.
- the high melting point material is a mixture of one or more of polyester, polyolefin, nitrile polymer, aromatic polyimide, and polyether having a melting point of 200 ° C, wherein the polyester includes but is not limited to Polyethylene terephthalate (PET), poly(p-phenylene terephthalate) (PPT), polybutylene terephthalate (PBT), poly(phthalic acid)
- PET Polyethylene terephthalate
- PPT poly(p-phenylene terephthalate)
- PBT polybutylene terephthalate
- Polyolefin fibers include, but are not limited to, poly(4-decylpentene) materials
- celluloses include, but are not limited to, polyvinyl acetal-nanocrystalline cellulose, tencel materials
- polynitrites include, but are not limited to, Polyacrylonitrile (PAN) materials
- Polyimides include, but are not limited to, aromatic polyimide materials
- the low melting point material is one or more of a polyolefin having a melting point of 50 to 199 ° C, a polyvinyl alcohol, a polystyrene, a thermally bonded polyester, and a fluorine-based polymer.
- a substrate made of a low melting point material and a high melting point material is used, so that the substrate has a bimodal melting point.
- the low melting point material having a small part by weight starts to soften and melt, and changes the original fiber shape. Appearance, reforming the surface to form a uniform structure, and the high-melting body material with a large weight The material did not change due to its high temperature stability.
- the heat pressure is released, the previously melted low-melting melt gradually solidifies or recrystallizes, and the high-melting-point materials are tightly compounded together, thereby improving the strength and surface flatness of the entire substrate, and the tensile strength can reach 60 MPa.
- the puncture strength can reach 3N.
- the low melting point material comprises from 0.1 to 15% by weight of the substrate, and the high melting point material comprises from 85 to 99.9% by weight of the substrate.
- the content of the low melting point material exceeds 15%, the poorer the high temperature heat shrinkage property of the obtained substrate, the more easily the separator shrinks at high temperature, resulting in short-circuit explosion of the positive and negative electrodes of the battery; the content of the low melting point material is less than 0.1%, and the prepared membrane surface The greater the roughness, the worse the thickness of the hook, and the worse the mechanical strength, the lower the pass resistance of the insulation breakdown short circuit test.
- the preferred melt crystallization treatment refers to a process in which a low melting point material is heated to be melted at a temperature of 0 to 10 ° C above its melting point, and then cooled to cool it.
- the melting temperature is 0-10 ° C above the melting point of the low melting point material, so that the low melting point material having a small weight fraction is softened and melted, and the original fiber morphology is changed, and the surface is evenly formed and the weight is re-formed.
- the high-melting-point host material does not change due to its high-temperature stability.
- the cooled crystallization of the melted low-melting melt closely bonds the high-melting substance together, thereby increasing the strength of the entire substrate.
- the filler on the modified nonwoven fabric substrate comprises an organic polymer, a first filler material and/or a second filler material, wherein:
- the organic polymer is one or a combination of two or more of a fluorine-based polymer, a rubber, an ester polymer, a cellulose, a starch, etc.
- the fluorine-based polymer includes, but not limited to, polyvinylidene fluoride, poly Vinylidene fluoride-hexafluoropropylene, polytetrafluoroethylene, polyvinylidene fluoride-trichloroethylene
- the rubber includes but not limited to styrene butadiene rubber, carboxylated styrene butadiene rubber, nitrile rubber, silicone rubber
- Polymers include, but are not limited to, polydecyl methacrylate, polyethyl methacrylate, polybutyl methacrylate, poly glyceryl acrylate, polyethylene glycol acrylate, polyethylene vinyl acetate, polyvinyl acetate
- the cellulose includes, but is not limited to, cellulose acetate,
- the selected organic polymer has an electrolyte-clearing ability to ensure the liquid absorption and liquid retention of the separator, thereby ensuring the ionic conductivity of the separator and the cycle performance of the battery.
- the organic polymer chosen should have suitable creep properties and wettability with the filler material to better agglomerate and encase the filler material.
- the first filler material is an inorganic particle having a particle diameter of from 1 to 2000 nm, preferably from 10 to 1000 nm, further preferably from 50 to 500 nm.
- the first filler material is an inorganic nanoparticle, which mainly functions to fill the pores of the non-woven fabric and improve the high temperature stability of the separator, including but not limited to one of inorganic oxide nanoparticles, inorganic nitride nanoparticles, ore nanoparticles. kind or several.
- the inorganic oxide nanoparticles are at least one of silica, alumina, titania, zirconia, magnesia, magnesium hydroxide, cerium oxide, oxidized iron, iron oxide and cerium oxide;
- the nitride nanoparticles are at least one of silicon nitride, titanium nitride and boron nitride;
- the ore nanoparticles are calcium carbonate, calcium sulfate, aluminum hydroxide, potassium titanate, barium titanate, talc, kaolin At least one of clay, high cold stone, pyrophyllite, montmorillonite, mica, bentonite, calcium silicate, magnesium silicate, diatomaceous earth and silica sand.
- the shape of the first filling material may be spherical, nearly spherical, dumbbell-shaped, rod-shaped, or the like.
- the second filler is a fiber particle having a particle diameter of from 1 to 10000 nm, preferably having a particle diameter of from 100 to 5,000 nm, more preferably from 300 to 3,000 nm.
- the second filler material is fiber particles, the fiber particles are wollastonite fiber, glass fiber, lignin, cellulose nanofiber, acrylic fiber, nylon fiber, polyester fiber, aramid One or a mixture of two or more of fibers, polyimide fibers, and the like.
- the modified nonwoven fabric substrate material is one or a mixture of a polyester, a polyolefin, a cyanopolymer, and a polyimide.
- the first filler material is an inorganic oxide particle.
- the second filling material is one or a mixture of wollastonite fibers, lignin, cellulose.
- a preparation method of a novel modified non-woven lithium ion battery separator comprising the following steps: a.
- Making a non-woven fiber layer processing a high-melting material and a low-melting material into a non-woven fiber layer, and the processing may be melt-blown, spunbonding, paper making, hydroentanglement, needle punching, hot rolling One of them, wherein the weight of the high melting point material accounts for 85-99.9% of the total weight of the nonwoven fabric fiber layer, and the balance is a low melting point material; the above process can adjust the pore size and pores of the nonwoven fiber layer by adjusting parameters Rate is controlled.
- the high melting point material is one or more of a polyester having a melting point of >200° (polyester, polyolefin, nitrile polymer, aromatic polyimide, polyether);
- the low melting point material is a polyolefin having a melting point of 50-199 ° C, a polyvinyl alcohol, a polystyrene, a heat-bonding polyester, a fluorine-based polymer;
- melt crystallization treatment means that the low melting point material is above the melting point of the low melting point material used in the step a- It is heated by heating at a temperature of 10 ° C, and then cooled to cool the crystallization process.
- the melting temperature is 0-10 ° C above the melting point of the low melting point material used in the step a, so that the low melting point material having a small part by weight is softened and melted, and the original fiber morphology is changed, and the surface is uniformly formed into a uniform structure.
- the high-melting-point host material having a large weight does not change due to its high-temperature stability.
- the cooling crystallization of the melted low-melting melt closely bonds the high-melting substance together, thereby raising the entire base.
- the strength of the material is further dried to ensure that the moisture content of the nonwoven fabric is as low as possible.
- Preparation of filler slurry The first filler material and the second filler material are dried. Mixing the organic polymer, the first solvent and the second solvent in a weight ratio of 1: (5 ⁇ 50): (0.1 ⁇ 10), stirring and heating to dissolve, adding the dried first filling material and/or the first Two filling materials, evenly mixed;
- the organic polymer is a fluorine-based polymer, a rubber, an ester polymer, cellulose, starch, or the like.
- the fluorine-based polymer includes, but not limited to, polyvinylidene fluoride, polyvinylidene fluoride-hexafluoropropylene, polytetrafluoroethylene, polyvinylidene fluoride-trichloroethylene
- the rubber includes but is not limited to styrene-butadiene rubber, carboxylated styrene butadiene rubber, nitrile rubber, silicone rubber
- the ester polymer includes, but is not limited to, polydecyl methacrylate, polyethyl methacrylate, polydecyl acrylate Ester, polyglyceryl acrylate, polyethylene glycol acrylate, polyethylene-vinyl acetate, polyvinyl acetate
- the cellulose includes, but is not limited to, cellulose a
- the first solvent is one or a mixture of two or more of a ketone solvent, an amide solvent, and an ester solvent; wherein the ketone solvent includes, but is not limited to, acetone, butanone, and N-mercaptopyrrolidone; the amide solvent includes Not limited to NN dimercaptoacetamide, NN dimercaptoamide; ester solvents include, but are not limited to, triethyl phosphate, tridecyl phosphate, and ethyl acetate.
- the second solvent is one or a mixture of two or more of water, an alcohol solvent, and a surface hydrocarbon solvent; the second solvent is water, an alcohol solvent, one or a mixture of two or more hydrocarbon solvents;
- the alcohol solvent includes, but is not limited to, decyl alcohol, ethanol, propanol, isopropanol, isobutanol, ethylene glycol, n-butanol, glycerin;
- the surface hydrocarbon solvent includes, but is not limited to, trichloromethane, Dichlorodecane.
- the second solvent selected has a boiling point higher than the boiling point of the first solvent by more than 10 °C.
- the agitation heating temperature should be below the boiling point of the first solvent, preferably below the boiling point of the first solvent by 10 °C or less. If the heating temperature is too high, the solvent volatilizes too quickly, causing the slurry to easily cause agglomeration due to excessive local temperature.
- step d filling the non-woven fabric: the filler slurry prepared in step c is filled on the modified non-woven fabric substrate obtained in step b;
- Removing the solvent removing the solvent from the non-woven fabric layer subjected to the d-step processing by extraction, drying, etc., to obtain a preliminary non-woven lithium ion battery separator;
- step f. post-treatment heating the preliminary non-woven lithium ion battery separator prepared in step e to the The melting point of organic polymer is above 5-30 °C;
- a third solvent which is one or a mixture of two or more of water, a ketone solvent, an amide solvent, an ester solvent, an alcohol solvent, and a hydrocarbon solvent.
- the organic polymer will further tightly enclose the filler material and make the membrane moisture less and stronger. Although the organic polymer may creep during this process and the coating pore structure changes, the pore structure of the coating void does not change, so that the separator does not undergo large heat shrinkage. Moreover, the inorganic particles are surrounded by the organic polymer, and most of the inorganic particles are isolated from the air, which greatly reduces the water absorption of the inorganic particles. After the treated membrane was placed in air at normal temperature and humidity for several months, it still maintained a low water content.
- the third solvent may be the same as or different from the first solvent, and is preferably acetone, water or N-N decyl sulfoxide.
- the organic polymer may be dissolved to change the pore structure of the coating, but it should not affect the excellent properties of the separator.
- a corresponding auxiliary agent may contribute to the film formation, but may not cause any adverse effects on the battery system.
- the adjuvant may include, but is not limited to, one or more of a dispersing agent, an antifoaming agent, a surfactant, and the like.
- the dispersing agent may be a commercially available dispersing agent such as one or more of polyvinylpyrrolidone (PVP), sodium carboxymethylcellulose, sodium polyacrylate, and the like.
- PVP polyvinylpyrrolidone
- the dispersing agent may be a commercially available dispersing agent such as one or more of polyvinylpyrrolidone (PVP), sodium carboxymethylcellulose, sodium polyacrylate, and the like.
- the surfactant is commercially available, for example, one or more of a fluorosurfactant, a silicon-containing surfactant, a polyether surfactant, and the like.
- the antifoaming agent is commercially available, for example, one or more of natural fats, silicone antifoaming agents, high carbon alcohols, polyether antifoaming agents, and the like.
- the weight ratio of the total weight of the first filler material and the second filler material to the organic polymer is (1:5) - (5:1); the second filler material accounts for a filling material and a second The ratio of the total weight of the filler material is 0-50%.
- the prepared lithium electronic battery separator may be added or compounded with additional mechanical treatment, such as hot calendering, centrifugation, stretching treatment, etc., as needed. . If you want to increase the porosity, you can consider increasing the stretching process. If you want to reduce the porosity, you can consider increasing the rolling or centrifuging.
- the invention provides a novel lithium ion battery separator, which can achieve the following technical effects:
- the unique non-woven substrate can greatly improve the strength of the diaphragm, ensure the battery winding processability, and improve the battery yield.
- the special organic polymer coated inorganic particle structure can greatly reduce the water absorption of the battery separator, reduce the possibility of moisture entering the battery system, and avoid the battery blow and internal resistance caused by excessive moisture and electrolyte reaction. It becomes larger, thereby improving the rate discharge performance and service life of the battery.
- the invention also provides a preparation method of a novel lithium ion battery separator, which has the advantages of simple operation, low cost, low moisture content, good chemical stability and high mechanical strength, and improves the yield and service life of the battery. And security.
- Fig. 1 is a schematic view showing the structure of a modified non-woven lithium ion battery separator of Example 1.
- Modified non-woven substrate 2. Filler.
- Example 1 95 g of high melting point PET fiber having a melting point of 250 ° C, 5 g of a low melting point PET fiber having a melting point of 150 ° C were copied into a nonwoven fabric web layer by a wet paper making method, and the nonwoven fabric web layer was melted. Crystallization treatment, the temperature was 155 ° C, and then cooled to obtain a modified non-woven fabric having a porosity of 58%, an average pore diameter of llum, a puncture strength of 3.0 N, a heat shrinkage of 150 ° C lh of 1%, and a thickness of 16 ⁇ m.
- Substrate 1 Taking filler 2, the filler includes aluminum oxide, PVDF;
- the melt-crystallized nonwoven fabric was dried, and the drying temperature was 90 ° C for 1 min.
- 40 g of aluminum oxide having a particle diameter of 250 nm was placed in an oven at a temperature of 100 ° C. The time is 4h.
- the modified non-woven fabric lithium ion battery separator comprises a modified non-woven fabric substrate 1 and a filler 2, wherein the filler 2 is filled in the pores of the modified non-woven fabric substrate 1 and extends outward. The entire modified nonwoven fabric substrate 1 is coated.
- a modified non-woven lithium ion battery separator was prepared according to the method of Example 1, except that 0.5 g of low melting point PET fiber having a melting point of 150 ° C was added to obtain a puncture strength of 2.2 N, 150 ° C lh heat shrinkage. It is a 0.5% nonwoven substrate.
- a modified non-woven lithium ion battery separator was prepared according to the method of Example 1, except that 16.8 g of a low melting point PET fiber having a melting point of 150 ° C was added to obtain a puncture strength of 3.2 N, and a heat shrinkage of 150 ° C lh was obtained. 5% non-woven substrate.
- a modified non-woven lithium ion battery separator was prepared according to the method of Example 1, except that the filling was performed.
- the thickness of the back diaphragm is the same as that of the non-woven substrate before filling, which is 16um.
- a modified non-woven lithium ion battery separator was prepared in accordance with the method of Example 1, except that a modified nonwoven fabric substrate was produced by a meltblown process.
- a modified non-woven lithium ion battery separator was prepared in the same manner as in Example 1 except that 40 g of aluminum oxide having a particle diameter of 250 nm was placed in an oven at a temperature of 80 ° C for a period of 1 min.
- a modified non-woven lithium ion battery separator was prepared in the same manner as in Example 1 except that 20 g of wollastonite fiber particles having a particle diameter of 1200 nm were added.
- a modified non-woven lithium ion battery separator was prepared in the same manner as in Example 1, except that the organic polymer was selected from PVDF-HFP having a melting point of 145 ° C, and the first solvent was selected from methyl ethyl ketone.
- a modified non-woven lithium ion battery separator was prepared in the same manner as in Example 1 except that the first filler was made of magnesium hydroxide having a particle diameter of 800 nm.
- a modified non-woven lithium ion battery separator was prepared according to the method of Example 1, except that the preliminary non-woven composite membrane was immersed in water (1 - 5 ) min, and then dried to obtain the present invention. Modified non-woven lithium ion battery separator.
- a modified non-woven lithium ion battery separator was prepared according to the method of Example 1, except that the initial The step non-woven composite membrane was hot pressed at a temperature of 180 °C.
- a lithium ion battery separator was prepared in accordance with the method of Example 1, except that a modified nonwoven fabric substrate was prepared without adding a 150 ° C low melting point PET material.
- a lithium ion battery separator was prepared in accordance with the method of Example 1, except that 24 g of a low melting point PET material having a melting point of 150 ° C was added to prepare a modified nonwoven fabric substrate.
- a lithium ion battery separator was prepared in the same manner as in Example 1 except that the nonwoven fabric substrate and the aluminum oxide were not dried.
- a lithium ion battery separator was prepared in the same manner as in Example 1 except that it did not undergo any post-treatment process.
- a lithium ion battery composite separator was prepared in accordance with the method of Example 1, except that the substrate was coated with a single layer PE film.
- the positive electrode is made of lithium cobalt oxide LiCo02
- the negative electrode is made of graphite
- the electrolyte of the battery is made of ethylene carbonate.
- Ester (EC): Diethyl carbonate (DEC): Dimethyl carbonate (DMC) volume ratio 1:1:1 solution, electrolyte added solute is 1 mol/L lithium hexafluoroacetate LiPF6, respectively
- the separators of Examples 1-6 and Comparative Examples 1-5 were used for battery performance evaluation.
- Example 1 2.0 1.0 3.1 58 Example 2 1.0 0.5 2.3 40 Example 3 6.0 5.0 3.3 70 Example 4 1.5 0.8 3.0 65 Example 5 2.8 1.0 2.8 65 Example 6 2.2 1.2 3.1 57 Example 7 2.0 1.0 3.4 57 Implementation Example 8 3.0 2.0 2.9 56 Example 9 2.2 1.2 3.2 58 Example 10 2.0 1.0 3.2 60 Example 11 2.2 1.1 3.5 70 Comparative Example 1 1.8 0.8 1.0 30 Comparative Example 2 10.0 8.2 3.4 68 Comparative Example 3 2.0 1.2 3.0 57 Comparative Example 4 2.2 1.2 2.2 38 Comparative Example 5 8.0 4.2 3.5 90 Comparative Example 6 9.5 5.4 3.2 88 Comparative Example 7 3.0 2.0 0.8 28 The test results from Table 1 show that the separator of the present invention has a lower ratio than the ordinary ceramic separator.
- the separator prepared by the specific high and low melting point characteristics of the non-woven fabric substrate of the present invention has sufficient puncture tensile strength while ensuring low heat shrinkage performance. , to ensure the processing rate and safety of the diaphragm battery. Water content test results after different baking times
- Comparative example 1 485 315 198 160 Comparative Example 2 498 332 210 169 Comparative Example 3 1592 1125 802 565
- Comparative Example 7 642 428 306 255 The test results from Table 2 show that the separator of the present invention has a lower water content than a conventional ceramic separator. Compared with Comparative Examples 3, 4, and 6, the separator composed of the substrate and the filling structure of the present invention has a low water content and requires less processing due to the particularity of processing and the structure of the organic polymer-coated inorganic particles. Baking time.
- each of the examples prepared 100 batteries. During the preparation of the battery, the cells were baked in a vacuum oven at 85 ° C for 24 hours, and then the battery was subjected to an insulation breakdown short circuit test, and batteries tested for different voltages. Statistics are performed by the number. The test results are shown in Table 3.
- Comparative Example 5 100 100 Comparative Example 6 100 100 Comparative Example 7 50 5
- the test results from Table 3 show that the separator of the present invention has better insulation resistance than the conventional non-woven membrane separator, and the pass rate of the 250V breakdown short test is up to 100%, while the ordinary nonwoven membrane pass rate is 5%.
- the separator composed of the substrate and the filler structure of the present invention has a large insulation resistance and a high battery yield due to the specificity of the substrate and the coating structure of the coating. .
- Acupuncture At room temperature, when charging at a constant current of 0.5C to a charge limit voltage of 4.2V, turn off the constant voltage charging 3.5 ⁇ or the current is reduced to 0.02C, the charging is cut off, and the battery after charging is 3.0 ⁇ 8.0mm in diameter. of Iron nails, piercing the battery vertically at a speed of 21-40mm/sec, the standard is no fire, no explosion.
- Short circuit Tested according to the national standard GB/T18287-2013 method, the standard is judged to be non-flammable, non-explosive, and the outer surface temperature is lower than 150 °C.
- Overcharge According to the national standard GB/T18287-2013 method to test, the standard is no fire, no explosion. The test results are shown in Table 4.
- the test results show that the battery prepared by the separator of the present invention is superior in safety performance test,
- Rate discharge Test according to the national standard GB/T18287-2013 method.
- Cyclic performance using the equipment BS-9300 performance tester, 1C rate charge and discharge cycle test, using constant current constant voltage charging system (CC-CV) and constant current discharge system, charging and discharging voltage range 3.0 ⁇ 4.2 V, First, it is charged to 4.2 V with a constant current of 1 C, and then charged to a current of less than 20 mA at a constant voltage of 4.2 V, and then discharged at a constant current of 1 C to a final voltage of 3.0 V, and thus cycled 500 times to collect the cycle data.
- CC-CV constant current constant voltage charging system
- Example 1 99.5 95.0 90.0 83.0 75.0 98.5 99.5 4 87.0 17.0
- Example 2 99.6 96.5 90.8 83.2 76.2 98.8 99.6 4 87.5 16.8
- Example 3 99.0 94.5 89.0 81.5 74.0 98.0 99.0 4 86.0 17.5
- Example 4 99.5 95.5 91.0 85.0 77.5 97.0 98.5 5 86.5 16.5
- Example 5 99.2 95.8 90.5 84.0 76.0 97.5 98.8 4 86.8 16.8
- Example 6 99.0 94.2 88.5 81.0 73.0 96.0 97.5 6 85.0 18.0
- Example 8 99.0 96.0 92.5 85.0 78.0 97.0 98.5 4 86.0 16.8
- Example 98.0 93.0 87.5 80.2 72.0 96.5 98.0 5 84.5 18.0
- Example 10 98.5 94.5 88.5 81.0 74.5 97.0 98.0 5 85.5 17.5
- the substrate and the filler of the invention impart the thickness and pore size of the separator, good electrochemical stability, excellent liquid retention and liquid absorption, and extremely low water absorption, so that the battery prepared by the separator of the invention has excellent performance. Rate of discharge performance and cycle life.
- the above embodiments are merely preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention belong to the present invention. The scope of the claim.
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Abstract
Description
Claims
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JP2016561758A JP6133520B2 (ja) | 2014-04-10 | 2014-04-30 | 新型改質不織布リチウムイオン電池用セパレータ及びその製作方法 |
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CN114300741A (zh) * | 2021-12-27 | 2022-04-08 | 合肥国轩高科动力能源有限公司 | 用于制备热固型pan基复合固态电解质膜的原料组合物、固态电解质膜及制备与应用 |
CN114649636A (zh) * | 2022-01-06 | 2022-06-21 | 李鑫 | 具有液固两相热压粘结性能的干法极片及含油隔膜 |
CN114649636B (zh) * | 2022-01-06 | 2023-08-18 | 北京沐昱新能源科技有限公司 | 具有液固两相热压粘结性能的干法极片及含油隔膜 |
CN118073778A (zh) * | 2024-04-19 | 2024-05-24 | 蜂巢能源科技股份有限公司 | 一种复合隔膜及其制备方法、电池 |
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JP6133520B2 (ja) | 2017-05-24 |
CN103928649B (zh) | 2016-08-24 |
KR20160129868A (ko) | 2016-11-09 |
JP2017510960A (ja) | 2017-04-13 |
CN103928649A (zh) | 2014-07-16 |
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