WO2007125827A1 - 非水電解質二次電池用セパレータおよび非水電解質二次電池 - Google Patents
非水電解質二次電池用セパレータおよび非水電解質二次電池 Download PDFInfo
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- WO2007125827A1 WO2007125827A1 PCT/JP2007/058613 JP2007058613W WO2007125827A1 WO 2007125827 A1 WO2007125827 A1 WO 2007125827A1 JP 2007058613 W JP2007058613 W JP 2007058613W WO 2007125827 A1 WO2007125827 A1 WO 2007125827A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/02—Details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/04—Construction or manufacture in general
- H01M10/0431—Cells with wound or folded electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/04—Construction or manufacture in general
- H01M10/0436—Small-sized flat cells or batteries for portable equipment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/423—Polyamide resins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
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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
Definitions
- Nonaqueous electrolyte secondary battery separator and nonaqueous electrolyte secondary battery are nonaqueous electrolyte secondary battery separator and nonaqueous electrolyte secondary battery
- the present invention relates to a separator for a non-aqueous electrolyte secondary battery and a non-aqueous electrolyte secondary battery.
- the present invention relates to a separator that provides a nonaqueous electrolyte secondary battery excellent in safety and output characteristics, and a nonaqueous electrolyte secondary battery including the separator.
- Non-aqueous electrolyte secondary batteries are actively used in small electronic devices such as mobile phones and laptop computers because they have a higher capacity and higher energy density than conventional secondary batteries. .
- a non-aqueous electrolyte secondary battery includes a non-aqueous electrolyte, a positive electrode, and a negative electrode.
- the nonaqueous electrolyte is generally composed of a nonaqueous solvent and a lithium salt dissolved in the nonaqueous solvent.
- the positive electrode includes a positive electrode active material and a positive electrode current collector carrying the positive electrode active material.
- As the positive electrode active material a material capable of reversibly occluding and releasing lithium ions and exhibiting a stable potential is preferably used.
- the negative electrode includes a negative electrode active material and a negative electrode current collector that carries the negative electrode active material.
- As the negative electrode active material a material capable of reversibly occluding and releasing lithium ions and exhibiting a stable potential is preferably used.
- the positive electrode and the negative electrode are, for example, a sheet shape or a strip shape.
- a separator made of an insulating porous material is interposed between the positive electrode and the negative electrode.
- the electrode group is produced by winding the positive electrode and the negative electrode together with a separator interposed therebetween, or laminating the positive electrode and the negative electrode via the separator.
- a non-aqueous electrolyte secondary battery is produced by housing the electrode group together with a non-aqueous electrolyte in a battery case of various shapes (square, cylindrical, etc.).
- the heat resistance of the separator strongly depends on the material. Therefore, a separator in which a layer made of a heat-resistant aramid resin and a porous layer having a shutdown function are laminated has been studied.
- the shutdown function is a function that melts when the battery generates heat and closes the hole to prevent the movement of lithium ions.
- a porous layer having a shutdown function becomes a substantially nonporous layer at a high temperature.
- the separator for a non-aqueous electrolyte secondary battery is required to satisfy the functions of reducing the thickness, ensuring lithium ion permeability, ensuring safety at high temperatures, and the like.
- a separator having a heat-resistant layer containing a nitrogen-containing aromatic polymer that is a heat-resistant resin and ceramic powder has been proposed.
- the heat-resistant layer is provided on the surface of a substrate made of fiber, nonwoven fabric, paper or porous film.
- the weight per unit area of the proposed substrate is 40 g / m 2 or less, and the thickness of the substrate is 70 ⁇ or less (see Patent Document 1).
- Patent Document 1 discloses an example of a polyethylene porous film force base material.
- Patent Document 2 discloses a separator comprising a polyethylene porous film (thickness 16 / Im) and a aramide resin film (thickness 5 ⁇ m).
- Patent Document 1 Japanese Patent No. 3175730
- Patent Document 2 JP 2004-349146 A
- Patent Documents 1 and 2 are beneficial in that excellent safety can be ensured by adding a shutdown function and heat resistance to the separator. Meanwhile, the separator There is no specific description regarding the correlation between thinning, lithium ion permeability, and safety.
- an object of the present invention is to provide a separator that is thin without compromising safety, has excellent durability, and does not deteriorate the output characteristics of a nonaqueous electrolyte secondary battery.
- Another object of the present invention is to provide a non-aqueous electrolyte secondary battery that can be reduced in size by optimizing the configuration of the separator, has excellent output characteristics, and is excellent in safety. Means to solve
- the present invention provides a first porous layer (A layer) having a shutdown characteristic that becomes a substantially non-porous layer at a high temperature, and a second porous layer (B) containing a amide resin and an inorganic material.
- Layer is a separator for a non-aqueous electrolyte secondary battery, wherein the thickness of the A layer relative to the thickness (T) of the B layer
- (T) ratio (T / T) is 2.5 or more and 13 or less.
- the present invention also provides a positive electrode that reversibly absorbs and releases lithium ions, a negative electrode that reversibly absorbs and releases lithium ions, a separator interposed between the positive electrode and the negative electrode, and a non-aqueous solution.
- the present invention relates to a non-aqueous electrolyte secondary battery in which the separator is a separator for a non-aqueous electrolyte secondary battery.
- the present invention it is possible to provide a separator that is excellent in durability even when it is thin, does not deteriorate the output characteristics of the battery, and can ensure the safety of the battery. According to the present invention, it is possible to provide a non-aqueous electrolyte secondary battery that can be miniaturized, has excellent output characteristics, and is excellent in safety.
- FIG. 1 is a perspective view in which a part of an example of a nonaqueous electrolyte secondary battery of the present invention is cut away.
- FIG. 2 is a partial cross-sectional view of a separator for a nonaqueous electrolyte secondary battery of the present invention.
- the separator for a non-aqueous electrolyte secondary battery of the present invention comprises a substantially non-porous layer at a high temperature.
- a separator is obtained.
- the ratio (T / T) of the thickness (T) of the A layer to the thickness (T) of the B layer is 2.5 or more and 13 or less.
- the thickness of the insulator can be reduced, lithium ion permeability is ensured, and high output characteristics can be maintained.
- an electrode group consisting of a positive electrode, a negative electrode, and a separator can be efficiently stored in a small battery case. Therefore, a high capacity non-aqueous electrolyte secondary battery can be obtained.
- the A layer is preferably a porous layer made of a thermoplastic resin.
- the A layer is preferably a substantially non-porous layer at a temperature of 80 ° C. or higher and 180 ° C. or lower, preferably 110 to 140 ° C.
- Such an A layer has excellent shutdown characteristics.
- the substantially non-porous layer has a Gurley value (air permeability) of 5000 seconds / lOOmL or more.
- the porous layer made of a thermoplastic resin is preferably a porous layer made of a polyethylene resin having a melting point of 110 to 140 ° C., for example. By using polyethylene as the thermoplastic resin, a separator having excellent reliability and stability can be obtained.
- the sum of the thickness of the A layer and the thickness of the B layer (T + T) is not less than 11 ⁇ and not more than 22 ⁇ .
- the electrode group of the nonaqueous electrolyte secondary battery is generally configured by winding a positive electrode and a negative electrode together with a separator interposed therebetween. Therefore, if the thickness of the separator is too large, the volume of the electrode group increases and the storage efficiency in the battery case decreases. In addition, if the thickness of layer B is too large, the cycle characteristics may deteriorate. T + T is set to 11 to 22 111, and the storage efficiency of the electrode group is increased.
- the charge / discharge cycle and output characteristics can be improved.
- the content of the aramid resin contained in the B layer is preferably 20 to 45% by weight, more preferably 25 to 40% by weight. Increasing the aramid resin content improves the heat resistance of the separator. However, the content of aramid resin is too high As a result, the lithium ion permeability in layer B decreases, the resistance to lithium ion migration increases, and the output characteristics deteriorate. On the other hand, if the content of the aramid resin is reduced, the output characteristics are improved. However, if the content of the aramid resin is too small, the heat resistance and mechanical strength of the separator are lowered. By setting the content of the aramid resin contained in the B layer to 20 to 45% by weight, a separator having excellent heat resistance without decreasing the lithium ion permeability in the B layer can be obtained.
- the porosity of layer A is preferably 37% or more and 48% or less, more preferably 39 to 47%.
- the porosity is 37. If it is less than 0 , the lithium ion permeability in the A layer may decrease, and the output characteristics may deteriorate. On the other hand, if the porosity exceeds 48%, the mechanical strength of the separator decreases, and the holes in the A layer easily deform. Therefore, the lithium ion permeability becomes non-uniform, and the cycle characteristics may deteriorate. In addition, if the porosity force exceeds S48%, the shutdown characteristics may be degraded, and the reliability of the nonaqueous electrolyte secondary battery may be degraded. By setting the porosity of the A layer to 37 to 48%, it is possible to obtain a highly reliable non-aqueous electrolyte secondary battery excellent in safety while maintaining output characteristics.
- the separator for a non-aqueous electrolyte secondary battery of the present invention has an air permeability of 150 seconds / lOOmL or more and 400 ⁇ / lOOmL or less S, preferably 160 to 350 ⁇ / lOOmL Force S More preferred.
- the separator has such an air permeability, it is easy to maintain the permeability of lithium ions in the separator and to immediately ensure reliability such as heat resistance.
- the separator for a nonaqueous electrolyte secondary battery of the present invention preferably has a piercing strength of 250 gf or more, more preferably 300 gf or more.
- a separator having a piercing strength of 250 gf or more has a particularly high mechanical strength and excellent reliability.
- the present invention includes a non-aqueous electrolyte secondary battery including the separator.
- a non-aqueous electrolyte secondary battery including the above separator is excellent in output characteristics, excellent in reliability such as safety, and suitable for downsizing.
- a non-aqueous electrolyte secondary battery of the present invention includes a non-aqueous electrolyte, a positive electrode, a negative electrode, and the above-described separator.
- the positive electrode and the negative electrode are, for example, a sheet shape or a strip shape.
- a wound electrode group is produced by winding a sheet-like positive electrode and negative electrode together with a separator interposed therebetween.
- strip-shaped positive and negative electrodes By laminating, a stacked electrode group can be obtained.
- a non-aqueous electrolyte secondary battery is manufactured by housing the electrode group together with a non-aqueous electrolyte in a battery case of various shapes (square, cylindrical, etc.).
- FIG. 1 is a perspective view in which a part of a rectangular nonaqueous electrolyte secondary battery according to an embodiment of the present invention is cut away.
- a nonaqueous electrolyte secondary battery has an electrode group 1 formed by winding a positive electrode and a negative electrode together with a separator interposed therebetween.
- Electrode group; L is a non-aqueous electrolyte (not shown)
- a resin frame (not shown) that separates the electrode group 1 from the sealing plate 5 and prevents the positive electrode lead 2 or the negative electrode lead 3 from contacting the battery case 4 is provided above the electrode group 1.
- the sealing plate 5 is provided with an external negative electrode terminal 6 and a nonaqueous electrolyte injection hole, and the injection hole is closed with a plug 8.
- the positive electrode lead 2 is connected to the lower surface of the sealing plate 5, and the negative electrode lead 3 is connected to the external negative electrode terminal 6.
- the external negative electrode terminal 6 is insulated from the sealing plate 5 by the gasket 7.
- FIG. 2 is a partial cross-sectional view of a separator for a nonaqueous electrolyte secondary battery.
- the separator 9 includes a first porous layer 10 (A layer) having a shutdown characteristic that becomes a substantially non-porous layer at a high temperature, and a amide resin and an inorganic material provided on the surface of the A layer 10. It is composed of the second porous layer 1 1 (B layer).
- a layer first porous layer 10
- B layer the second porous layer 1 1
- Ratio (T / T) is set to 2.5 or more and 13 or less.
- the A layer is preferably a substantially non-porous layer at a temperature of 80 ° C or higher and 180 ° C or lower.
- the layer A is preferably made of a thermoplastic resin, for example, a polyolefin resin.
- Examples of olefins constituting the polyolefin resin include ethylene, propylene, butene, hexene and the like.
- Specific examples of the polyolefin resin include polyethylene resins such as low density polyethylene, linear polyethylene (ethylene mono-olefin copolymer), high density polyethylene, polypropylene, ethylene monopropylene copolymer, and the like.
- Examples include propylene-based resins, poly (4-methylpentene 1), poly (butene 1), and ethylene acetate butyl copolymer.
- the content of the polyethylene resin in the thermoplastic resin is preferably 60% by weight or more and 100% by weight or less.
- the layer A can contain an additive as required, as long as the shutdown characteristics are not impaired.
- the additive include inorganic or organic fillers used for the purpose of reinforcement, nonionic surfactants, and the like.
- the amount of the filler contained in the A layer is preferably 15 to 85 parts by volume per 100 parts by volume of the thermoplastic resin (for example, 40 to 230 parts by weight per 100 parts by weight of the thermoplastic resin).
- layer A made of polyolefin in order to improve its thermal stability and processability, stretching aids, stabilizers, antioxidants, ultraviolet absorbers, flame retardants, nonionic surfactants are used. Etc. can be added.
- fatty acid esters or low molecular weight polyolefin resins are used as additives.
- the amount of additive contained in layer A is preferably 1% by weight or less.
- an inorganic material having electrical insulation can be widely used.
- an inorganic material having electrical insulation can be widely used.
- Magnesium fluoride, titanium oxide, alumina, zinc oxide, zeolite, glass powder, etc. are preferred.
- calcium carbonate, hydrated talcite, barium sulfate, magnesium hydroxide, alumina and the like are preferable in terms of fineness of particle size, yield of potatoes, and immediate moisture reduction. These may be used alone or in combination of two or more.
- Examples of the organic filler contained in the layer A include particles or fibers of a homopolymer or copolymer of a butyl monomer; particles or fibers of a polycondensation resin such as a melamine resin or a urea resin. These can be used alone or in combination of two or more.
- Examples of the butyl monomer include styrene, butyl ketone, acrylonitrile, methyl methacrylate, ethyl methacrylate, glycidyl methacrylate, glycidyl acrylate, Examples include methyl acrylate.
- the B layer contains a aramide resin and an inorganic material.
- aramid resin examples include para-oriented aromatic polyamide (hereinafter referred to as “para-amide”), meta-oriented aromatic polyamide (hereinafter referred to as “meta-aramide”), and the like.
- para-amide para-oriented aromatic polyamide
- metal-aramide meta-oriented aromatic polyamide
- pararamid is preferred because it has a high mechanical strength and is easily porous.
- Pararamide can be obtained, for example, by condensation polymerization of an aromatic diamine having an amino group at the para position and an aromatic dicarboxylic acid halide having an asinole group at the para position. Therefore, in pararamid, an amide bond exists at the para position of the aromatic ring or a position corresponding thereto.
- Pararamide has, for example, repeating units such as 4,4′-biphenylene group, 1,5 naphthalene group, and 2,6 naphthalene group.
- paraamide examples include poly (paraphenylene terephthalamide), poly (parabenzamide), poly (4,4'-benzanilide terephthalamide), poly (paraphenylene terephthalamide 4, 4 ' -Biphenylenedicarboxylic acid amide), poly (paraphenylene 2,6 naphthalenedicarbonic acid amide), poly (2-capped paraphenylene terephthalamide), paraphenylene terephthalanolamide / 2,6 dichloroparaphenylene Examples include terephthalamide copolymers. These may be used alone or in combination of two or more.
- the inorganic material alumina, silica, titanium dioxide, dinoleconium oxide and the like are preferable. These may be used alone or in combination of two or more.
- the average particle size of the inorganic material is preferably, for example, 0.01 to l / im.
- the amount of the inorganic material contained in the layer B is preferably 120 to 400 parts by weight, particularly preferably 150 to 300 parts by weight, per 100 parts by weight of the aramide resin.
- a pore-forming agent can be used to obtain a porous structure.
- the pore-forming agent is preferably one that can be removed by washing with water after stretching the raw material sheet of layer A or layer B.
- the pore-forming agent is preferably water-soluble so that it can be removed with a neutral, acidic or alkaline aqueous solution.
- Polyethylene, fillers, necessary additives (eg nonionic surfactants), etc. 2 Mix using existing mixing equipment such as a shaft kneader, twin rolls, Banbury mixer, Henschel mixer, and single screw extruder.
- the resulting mixture is formed into a sheet with a desired thickness by existing film forming methods such as inflation, calendering, and T-die extrusion.
- the obtained sheet is preferably stretched by uniaxial or biaxial stretching.
- Paralamid resin is soluble in polar organic solvents. Therefore, the paraamide resin is dissolved in a solvent to prepare a low-viscosity paraamide solution suitable for coating. Next, the obtained resin solution is mixed with an inorganic material to prepare a raw material slurry for layer B.
- the raw material slurry for layer B is preferably controlled to a viscosity suitable for application to the surface of layer A.
- the intrinsic viscosity of the B-layer paraamide resin is preferably from 1.0 dL / g to 2.8 dL / g, more preferably from 1.7 dL / g to 2.5 dLZg. If the intrinsic viscosity is less than 1. OdLZg, a B layer with sufficient strength may not be obtained. On the other hand, if the intrinsic viscosity exceeds 2.8 dL / g, the pararamide solution may become unstable and film formation may be difficult.
- the intrinsic viscosity of pararamide is measured by the following method. First, dissolve 0.5 g of pararamide resin in lOOmL of concentrated sulfuric acid with a concentration of 96-98% by weight to prepare a mixed solution of pararamide resin and concentrated sulfuric acid. Using the Ubbelohde capillary viscometer, measure the flow time at 30 ° C for the obtained mixed solution and concentrated sulfuric acid with a concentration of 96 to 98% by weight. From the obtained flow time ratio, the intrinsic viscosity is obtained by the following equation.
- Intrinsic viscosity ln (T / T) / C [Unit: dL / g]
- T is the flow time of the mixed solution of paralamid resin and concentrated sulfuric acid
- T is the concentration 96
- Examples of the polar organic solvent in which the para-amide resin is dissolved include a polar amide solvent or a polar urea solvent. Specific examples include N, N-dimethylformaldehyde, N, N-dimethylacetamide, N-methyl_2-pyrrolidone, tetramethylurea, and the like. These may be used alone or in combination of two or more.
- the raw material slurry of layer B is applied to the surface of layer A with a desired thickness.
- inorganic material Force Tangled with S-Aramid resin the inorganic material is uniformly dispersed in the Aramid resin.
- the content of aramid resin in the total of the aramid resin and inorganic material contained in the raw material slurry is
- the content of the aramid resin exceeds 45% by weight, the lithium ion permeability in the B layer may decrease. As a result, the required battery output characteristics may not be obtained. If the content of the aramid resin is less than 20% by weight, the strength of the B layer may decrease.
- the positive electrode includes a positive electrode active material and a positive electrode current collector carrying the positive electrode active material.
- the sheet-like positive electrode is composed of a belt-like positive electrode current collector and a positive electrode mixture layer carried on both surfaces thereof.
- As the positive electrode active material a material capable of reversibly occluding and releasing lithium ions and exhibiting a stable potential is preferably used.
- the positive electrode current collector a metal foil made of aluminum (A1) or the like, a carbon thin film, a thin film of a conductive resin, or the like can be used.
- the positive electrode current collector may be surface-treated with carbon or the like.
- the positive electrode mixture layer contains a positive electrode active material as an essential component.
- a positive electrode active material for example, a lithium-containing composite oxide such as LiCoO, LiNiO, LiMnO, LiMnO is used. This
- the positive electrode active material may be surface-treated with a metal oxide, lithium oxide, a conductive agent, or the like, or the surface may be hydrophobized.
- a positive electrode active material may be used individually by 1 type, and may be used in combination of 2 or more type.
- the positive electrode mixture layer may contain various optional components.
- the positive electrode mixture layer includes, for example, a conductive agent and a positive electrode binder.
- Conductive agents include various natural graphites and various artificial graphites; carbon blacks such as acetylene black, ketchen black, channel black, furnace black, lamp black, and thermal black; conductive fibers such as carbon fiber and metal fiber Carbon fluoride; Metal powders such as aluminum; Conductive whiskers such as zinc oxide and potassium titanate; Conductive metal oxides such as titanium oxide; Organic conductivity such as vinylene derivatives A material etc. can be used. These may be used alone or in combination of two or more.
- PVDF polyvinylidene fluoride
- modified PVDF polytetrafluoroethylene
- polyethylene polypropylene
- aramid resin polyamide, polyimide, polyamidoimide
- polyacrylonitrile polyacrylic acid
- polyacrylic Acid methyl ester polyacrylic acid ethyl ester, polyacrylic acid hexyl ester, polymethacrylic acid, polymethacrylic acid methyl ester, polymethacrylic acid ethyl ester, polymethacrylic acid hexyl ester, poly (acetate) butyrate, polybutyropyrrolidone
- polyether poly Ether sulfone, hexafluoropolypropylene, styrene butadiene rubber (SBR), modified SBR, carboxymethylcellulose (CMC), and the like
- SBR styrene butadiene rubber
- CMC carboxymethylcellulose
- tetrafluoroethylene hexafluoroethylene propylene, perfluororenoanolenovininoreatenore, futu ⁇ vinylidene, chlorotriphenoloethylene, ethylene, propylene, pentafluoropropylene, fluoromethylvinyl ether, acrylic acid,
- copolymers selected for strength, such as xagene may be used.
- the positive electrode binder one kind may be used alone, or two or more kinds may be used in combination.
- the negative electrode includes a negative electrode active material and a negative electrode current collector carrying the same.
- a sheet-like negative electrode comprises a strip-like negative electrode current collector and a negative electrode mixture layer carried on both sides thereof.
- the negative electrode active material a material capable of reversibly occluding and releasing lithium ions and exhibiting a stable potential is preferably used.
- the negative electrode current collector a metal foil made of stainless steel, nickel, copper, titanium, or the like, a carbon thin film, a thin film of a conductive resin, or the like can be used.
- the negative electrode current collector should be surface-treated with carbon, nickel, titanium, etc.
- the negative electrode mixture layer contains a negative electrode active material as an essential component.
- a negative electrode active material as an essential component.
- Various types of natural black lead and various artificial graphites; silicon-based composite materials (silicides, etc.); lithium alloys containing at least one selected from tin, aluminum, zinc, magnesium, etc .; various alloys that react with lithium Materials can be used.
- the negative electrode mixture layer may contain various optional components.
- the negative electrode binder those exemplified as the positive electrode binder can be arbitrarily selected and used.
- SBR and modified SBR are carboxymethylcellulose (CM
- C) is preferably used in combination with cellulosic resins.
- the non-aqueous electrolyte preferably comprises a non-aqueous solvent and a lithium salt dissolved in the non-aqueous solvent.
- the nonaqueous electrolyte material is selected in consideration of the redox potential of the active material.
- Preferred lithium salts include LiPF, LiBF, LiCIO, LiAlCl, LiSbF, LiSCN,
- LiCF SO LiN (CF CO), LiN (CF SO), LiAsF, LiB CI, lower aliphatic cal
- Lithium borate LiF, LiCl, LiBr, Lil, LiBCl, bis (1,2_benzenediolate (2
- Lithium borate bis (2, 3 _Naphthalenedioleate (2_) _ ⁇ , 0,) Lithium borate, bis (2, 2, 1 biphenyldiolate (2_) _ ⁇ , ⁇ ') Lithium borate, bis (5-Fluoro-2-olate 1-Benzenesulfonic acid, 10,000, O') Lithium borate, (CF
- Non-aqueous solvents for dissolving lithium salts include ethylene carbonate (EC), propylene power-bonate (PC), butylene carbonate (BC), dimethyl carbonate (DMC), germanol carbonate (DEC), ethylmethyl.
- Methyl Formate Methyl Acetate, Methyl Propionate, Ethyl Propionate, Dimethoxymethane, ⁇ -Butyrolataton, ⁇ -Valerolataton, 1,2-Diethoxyethane, 1,2- Tetrahydrofuran derivatives such as dimethoxyethane, ethoxymethoxyethane, trimethoxymethane, tetrahydrofuran, 2-methyltetrahydrofuran, dioxolane derivatives such as dimethyl sulfoxide, 1,3-dioxolane, 4_methyl_1,3-dioxolane, formamide , Acetamide, dimethylform Muamide, acetonitrile, propylnitrile, nitromethane, ethyl monoglyme, triesterol phosphate, acetate ester, propionate ester, sulfolane, 3-methyls
- the non-aqueous electrolyte further includes vinylene carbonate (VC), cyclohexyl benzene, biphenyl, diphenyl ether, vinyl ethylene carbonate (VEC), divinyl ethylene carbonate, phenyl ethylene carbonate, diallyl carbonate, May contain additives such as fluoroethylene carbonate, catechol carbonate, butyl acetate, ethylene sulfite, propan sultone, trifluoropropylene carbonate, dibenzofuran, 2,4-difluoroainol, 0_terphenyl, m-terphenyl, etc. Les. These may be used alone or in combination of two or more.
- a polymer electrolyte that has been made non-fluidized by holding the non-aqueous electrolyte in a polymer is also applicable.
- the polymer that holds the non-aqueous electrolyte for example, polyethylene oxide, polypropylene oxide, polyphosphazene, polyaziridine, polyethylenesulfide, polybutal alcohol, polyvinylidene fluoride, polyhexafluoropropylene, etc. are used. Can. These can be used alone or in combination of two or more.
- An inorganic material may be used as the solid electrolyte.
- the hydroxide was sufficiently washed with water and dried to obtain a positive electrode active material precursor.
- the obtained precursor and lithium carbonate were mixed so that the molar ratio of lithium, nickel, and cobalt was 1.02: 0.80: 0.20.
- the mixture was calcined at 600 ° C. for 10 hours and pulverized.
- the pulverized fired product was fired again at 900 ° C. for 10 hours, and then pulverized and classified to obtain a lithium-containing composite oxide represented by the formula: Li Ni Co O.
- 1 kg of the positive electrode active material (average particle size 12 / m) made of the obtained lithium-containing composite oxide was manufactured by Kureha Chemical Co., Ltd.
- a positive electrode mixture paste was prepared by stirring for 30 minutes at 30 ° C. using a double-arm kneader together with 0.5 kg, acetylene black 40 g, and an appropriate amount of NMP.
- the obtained positive electrode mixture paste was applied to both surfaces of a 20 ⁇ m-thick aluminum foil serving as a positive electrode current collector, and dried at 120 ° C. for 15 minutes. Thereafter, the positive electrode current collector carrying the positive electrode mixture was rolled so that the total thickness was 160 zm.
- the obtained electrode plate was cut into a width that could be inserted into a rectangular battery case having a height of 50 mm, a width of 34 mm, and a thickness of 5 mm to obtain a positive electrode.
- a predetermined positive electrode lead was connected to the positive electrode.
- BM-400B an aqueous dispersion containing 40% by weight of modified styrene-butadiene rubber
- CMC carboxymethylcellulose
- the obtained negative electrode mixture paste was applied to both sides of a 12 / m-thick copper foil serving as a negative electrode current collector and dried. Thereafter, the negative electrode current collector carrying the negative electrode mixture was rolled so that the total thickness was 160 ⁇ .
- the obtained electrode plate was cut into a width that could be inserted into a rectangular battery case having a height of 50 mm, a width of 34 mm, and a thickness of 5 mm to obtain a negative electrode.
- a predetermined negative electrode lead was connected to the negative electrode.
- the obtained polyolefin resin composition was rolled with a roll and formed into a sheet.
- the obtained polyethylene sheet (PE sheet) was immersed in a bath containing a hydrochloric acid aqueous solution to dissolve and remove calcium carbonate. Thereafter, the PE sheet was washed with water and dried. The dried PE sheet was stretched with a tenter stretching machine to obtain a porous polyethylene film (A layer).
- the roll temperature of the polyolefin resin composition during roll rolling is set to 149 ° C to 152 ° C
- the thickness after rolling is set to a range of 70 ⁇ m to 80 ⁇ m
- the temperature during tenter stretching is further set.
- 100 ° C ⁇ Set in the range of 110 ° C and obtained various A layers with thickness, porosity, air permeability and piercing strength as shown in Table 1A, 2A, 3A, 4A and 5A .
- TPC terephthalic acid dichloride
- Alumina powder (average particle size 0.16 / m) was added to and dispersed in the obtained pararamid solution to prepare a raw material slurry for layer B having various contents of aramid resin.
- the content of the aramid resin in the total of the aramid resin and the alumina powder was changed to 16% by weight, 20% by weight, 33% by weight, 45% by weight or 50% by weight.
- a layer B raw material slurry having a different aramid resin content is used and applied to the layer A.
- various B layers having aramid content and thickness as shown in Tables 1A, 2A, 3A, 4A and 5A were formed, and various separators were obtained.
- the negative electrode and the positive electrode were wound with a separator 9 interposed therebetween to form an electrode group 1 having a substantially elliptical cross section.
- 30 identical electrode groups 1 were prepared.
- the sealing plate 5 and the positive electrode lead 2 were electrically connected, and the external negative electrode terminal 6 provided on the sealing plate 5 and the negative electrode lead 3 were electrically connected in a state surrounded by the gasket 7.
- the sealing plate 5 and the open end of the battery case 4 were welded.
- LiPF was dissolved in lmol / L in a mixed solvent of ethylene carbonate and propylene carbonate in a volume ratio of 1: 1.
- the thickness was measured according to a method according to JIS standard K7130-1992.
- the A layer was cut into a square having a side length of 10 cm, and the weight W (g) and the thickness T (cm) were measured. Next, using the value of the true specific gravity D (g / cm 3 ) of the A layer, the porosity (%) was obtained from the following formula.
- the Gurley value (second ZlOOmL) of the separator was measured using a B-type densometer (Toyo Seiki Seisakusho Co., Ltd.) according to the method according to JIS standard P8117. [0075] (4) Puncture strength
- the separator was fixed with a ⁇ 12 mm washer, and the pin was pierced at a speed of 200 mm / min into the fixed separator, and the maximum stress (gf) at that time was determined as the piercing strength.
- the pin shape was a pin diameter of ⁇ lmm and a tip of 0.5R.
- the low temperature rate characteristics, cycle characteristics, heating test, and leakage failure were evaluated in the following manner.
- the battery was placed in a 20 ° C environment, charged with a constant current of 0.1C until it reached 4.2V, and charged with a constant voltage of 4.2V for 5 hours. Next, the charged battery was left in a 10 ° C environment for 60 minutes, and then discharged at a current of 1C (1000mA). The ratio of the obtained discharge capacity to the initial capacity (C) was determined as the capacity maintenance ratio (%).
- the battery was repeatedly charged and discharged under the following conditions at an ambient temperature of 20 ° C.
- the battery was charged at a constant current of 1 ⁇ OA until the battery voltage reached 4.2V, and then charged at a constant voltage of 4.2V until the current value dropped to 50mA.
- the battery after charging was paused for 30 minutes.
- the battery was discharged at a constant current at a current value of 0.2 A until the battery voltage dropped to 3.0 V.
- the discharged battery was paused for 30 minutes. This charge / discharge cycle was taken as one cycle, and the charge / discharge cycle was repeated until the discharge capacity reached 50% of the initial capacity (C). Cycle at that time
- the battery was placed in a heating tank, and the heating tank was raised to 140 ° C at a temperature rising rate of 5 ° C / min and left in that state for 10 minutes. After that, the battery temperature is monitored and the battery temperature reaches the maximum. High temperature was measured.
- Table IB shows the evaluation results when the thickness of the separator is fixed at 16 zm and the ratio of the thickness of the A layer to the thickness of the B layer is changed as shown in Table 1A.
- Samples 1 to 3 are examples, and samples C1 and C2 are comparative examples.
- the ratio of the thickness of the A layer to the thickness of the B layer is in the range of 2.5 or more and 13 or less. Good results were obtained in the properties, the number of 50% maintenance cycles and the heating test. Also, no leak failure was observed.
- sample CI the ratio of the thickness of the A layer to the thickness of the B layer was 2.0
- the low-temperature rate characteristics were low and the number of 50% maintenance cycles was small. This is thought to be due to the fact that the permeability of lithium ions decreased and resistance increased because layer B was relatively thick.
- sample C2 (the ratio of the thickness of the A layer to the thickness of the B layer was 13.5), the low temperature rate characteristics and the number of 50% maintenance cycles were similar to those of the sample 4. However, the maximum temperature in the heating test of sample C4 was about 20 ° C higher than that of samples:! It is thought that the heat resistance was reduced because the B layer was thin.
- the ratio of the thickness of the A layer to the thickness of the B layer is fixed at 4.3, and the evaluation result when the total of the thickness of the A layer and the thickness of the B layer is changed is shown in Table 2B. .
- the ratio of the thickness of the A layer to the thickness of the B layer is 4.3.
- the ratio of the thickness of the A layer to the thickness of the B layer is 4.3, the thickness of the separator is 16 / im, and the content of the aramid resin is 20 to 45 in Sanpunore 2, 7 and 8 by weight 0/0, the low-temperature rate characteristics, with 50% maintaining cycle rate and heating test, good results were obtained. Also, no leak failure was observed.
- Samples 2, 7, and 8 were compared, there was a tendency that the content of the aramide resin increased, the low-temperature rate characteristics slightly decreased, and the number of 50% maintenance cycles decreased. This is because the permeation of lithium ions in the B layer decreased and the resistance increased as the content of the aramid resin increased.
- Table 4A the thickness of the A layer and the thickness of the B layer are fixed, and the aramid resin contained in the B layer Table 4B shows the evaluation results when the content ratio of A is fixed and the porosity of layer A and the air permeability of the separator are changed.
- the ratio of the thickness of the A layer to the thickness of the B layer is 4.3, the thickness of the separator is 16 zm, and the content of the aramid resin contained in the B layer is 33% by weight.
- Table 5A the evaluation results when the thickness of layer A and the thickness of layer B are fixed, the content of aramid resin contained in layer B is fixed, and the piercing strength of the separator is changed are shown in Table 5B. Shown in. The piercing strength was changed by controlling the roll temperature during the production of the A layer and the temperature during stretching.
- the ratio of the thickness of the A layer to the thickness of the B layer is 4.3
- the separator thickness is 16 ⁇ m
- the content of the aramid resin contained in the B layer Samples 2 11 12 and 13 with a rate of 33% by weight and a separator piercing strength of 250 gf or more gave good results in the low-temperature rate characteristics, the number of 50% maintenance cycles and the heating test. Also, no leak failure was observed.
- a rectangular nonaqueous electrolyte secondary battery having an electrode group in which electrodes are wound has been described.
- the shape of a battery to which the present invention can be applied is not limited to a rectangular shape.
- the present invention can be applied to a cylindrical battery, a flat battery, a coin battery, and a laminate battery.
- the battery for small equipment was examined, but the present invention is also effective for a large-sized large-capacity battery such as a power source for electric vehicles and power storage.
- the present invention can be used for various non-aqueous electrolyte secondary batteries, and is particularly useful for non-aqueous electrolyte secondary batteries for small devices that require excellent output characteristics and safety.
- the present invention can be applied to a prismatic battery, a cylindrical battery, a flat battery, a coin battery, a laminate battery, and the like.
- the present invention is also useful for power sources for electric vehicles, large power storage devices, and the like.
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Abstract
Description
Claims
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CN200780001406XA CN101356665B (zh) | 2006-04-28 | 2007-04-20 | 非水电解质二次电池用隔膜及非水电解质二次电池 |
US12/091,666 US8404377B2 (en) | 2006-04-28 | 2007-04-20 | Separator for use in non-aqueous electrolyte secondary battery and non-aqueous electrolyte secondary battery |
KR1020087012257A KR101094603B1 (ko) | 2006-04-28 | 2007-04-20 | 비수 전해질 이차전지용 세퍼레이터 및 비수 전해질 이차전지 |
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JP2006126211A JP5095121B2 (ja) | 2006-04-28 | 2006-04-28 | 非水電解質二次電池用セパレータおよび非水電解質二次電池 |
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US20090148762A1 (en) | 2009-06-11 |
JP5095121B2 (ja) | 2012-12-12 |
CN101356665A (zh) | 2009-01-28 |
US8404377B2 (en) | 2013-03-26 |
KR20080086437A (ko) | 2008-09-25 |
JP2007299612A (ja) | 2007-11-15 |
CN101356665B (zh) | 2011-07-13 |
KR101094603B1 (ko) | 2011-12-15 |
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