CN102498591B - Base material for lithium ion secondary battery, and separator for lithium ion secondary battery - Google Patents

Base material for lithium ion secondary battery, and separator for lithium ion secondary battery Download PDF

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Publication number
CN102498591B
CN102498591B CN201080040812.9A CN201080040812A CN102498591B CN 102498591 B CN102498591 B CN 102498591B CN 201080040812 A CN201080040812 A CN 201080040812A CN 102498591 B CN102498591 B CN 102498591B
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base material
short fiber
fiber
rechargeable battery
lithium rechargeable
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CN102498591A (en
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江角真一
大山圭介
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Mitsubishi Paper Mills Ltd
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Mitsubishi Paper Mills Ltd
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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
    • H01M50/44—Fibrous material
    • 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
    • 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
    • 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
    • H01M50/443—Particulate material
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Cell Separators (AREA)
  • Nonwoven Fabrics (AREA)
  • Paper (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

Disclosed is a base material for a lithium ion secondary battery, which is characterized by comprising a non-woven fabric of polyester short fibers and containing polyester ultra-short fibers having an average fiber diameter of 5.0 [mu]m or less and a fiber length of 2 mm or less as an essential component. The base material is highly safe when over-charged and can be formed into a complex suitably. Also disclosed is a separator for a lithium ion secondary battery, which is produced using the base material.

Description

Lithium rechargeable battery base material and separator for lithium ion secondary battery
Technical field
The present invention relates to the lithium rechargeable battery base material that can be suitable for the lithium rechargeable battery such as lithium rechargeable battery, lithium ion polymer secondary cell, and use the separator for lithium ion secondary battery of this base material.
Background technology
In recent years, along with the universal of portable electronic device and high performance thereof, the secondary cell with high-energy-density is expected.As this battery, the lithium rechargeable battery of organic electrolyte (nonaqueous electrolytic solution) is used to receive publicity.The average voltage of this lithium rechargeable battery can reach about 3 times of secondary cell in the past and alkaline secondary cell, for about 3.7V, therefore there is high-energy-density, but, because it can not use the electrolyte of water system as alkaline secondary cell, thus use the nonaqueous electrolytic solution with sufficient oxidation-reduction resistance.Because nonaqueous electrolytic solution is flammable, thus there is danger on fire etc., in it uses, need careful attention in fail safe.Consider that some causes the situation waiting danger on fire, the especially danger that overcharges.
In order to prevent overcharging, about existing non-aqueous secondary battery, charging with constant voltage, constant current, being assembled with accurate IC (protective loop) in the battery.The cost that this protective loop relates to is large, also becomes the main cause that non-aqueous secondary battery cost is uprised.
When preventing from overcharging with protective loop, certainly also can be contemplated to protective loop can not the situation of works fine, and being difficult to be referred to as is safe in itself.In existing non-aqueous secondary battery, for when overcharging protective loop damaged, overcharged time destroy the object of battery safely, mounting safety valve, PTC element, manage to make dividing plate have hot fuse function.But, even if install above-mentioned device, according to the condition causing overcharging, really can't ensure fail safe when overcharging, in fact still have now the fire accident of non-aqueous secondary battery to occur.
As dividing plate, the membrane-like porous plasma membrane that most use is made up of polyolefin such as polyethylene, it has when internal temperature of battery is blocking microporous close to melting when 130 DEG C, thus prevent the hot fuse function (cut-out function) of the movement of lithium ion, cut-out electric current, no matter but implied because which kind of situation is when temperature rises further have the possibility of polyolefin self melting and short circuit, thermal runaway.Therefore, even if having now been developed the thermal endurance dividing plate of also not melting and contraction at close to the temperature of 200 DEG C.
The non-weaving cloth be made up of polyester fiber, the non-weaving cloth being mixed with the aramid fiber as heat resistant fibre in polyester fiber is had as thermal endurance dividing plate, but because aperture greatly internal short-circuit occurs, thus impracticable (for example, referring to patent documentation 1 ~ 3).On the other hand, report the example that the non-weaving cloth making to be made up of polyester fiber and the membrane-like porous film stack be made up of polyolefin carry out Composite, and be coated with by the surface containing filler particles or resin in non-weaving cloth or woven cloths the example (for example, referring to patent documentation 4 ~ 6) that the Composite carried out makes it to have thermal endurance.But about the non-weaving cloth used as base material, because hole is large, surface smoothness is low, the deviation that thus there is surface when carrying out Composite by surface coating is large, and the quality problems easily causing that the compound such as filler particles or resin compound comes off etc.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2003-123728 publication (without foreign counterpart)
Patent documentation 2: Japanese Unexamined Patent Publication 2007-317675 publication (No. 2001/67536th, International Publication
Pamphlet, U.S. Patent Application Publication No. 2003/0003363 specification)
Patent documentation 3: Japanese Unexamined Patent Publication 2006-19191 publication (without foreign counterpart)
Patent documentation 4: Japanese Unexamined Patent Publication 2005-293891 publication (without foreign counterpart)
Patent documentation 5: Japanese Unexamined Patent Application Publication 2005-536857 publication (International Publication No. 2004/021476 pamphlet, U.S. Patent Application Publication No. 2006/0024569 specification)
Patent documentation 6: Japanese Unexamined Patent Publication 2007-157723 publication (International Publication No. 2006/062153 pamphlet, U.S. Patent Application Publication No. 2007/0264577 specification)
Summary of the invention
Invent problem to be solved
Problem of the present invention is to provide fail safe when overcharging high and the lithium rechargeable battery base material being suitable for Composite, and uses the separator for lithium ion secondary battery of this base material.
Solve the means of problem
The present inventor, in order to solve above-mentioned problem lucubrate, found that:
(1) lithium rechargeable battery base material, it is characterized in that, in the lithium rechargeable battery base material be made up of the non-weaving cloth of Polyester short fiber, be less than 5.0 μm containing fiber diameter and fibre length is that the Polyester extremely short fiber of below 2mm is as essential component;
(2) the lithium rechargeable battery base material described in above-mentioned (1), wherein, the length-width ratio (fibre length/fibre diameter) of Polyester extremely short fiber is 20 ~ 800;
(3) above-mentioned (1) or the lithium rechargeable battery base material described in (2), wherein, relative to non-weaving cloth, the content of Polyester extremely short fiber is 1 ~ 30 quality %;
(4) separator for lithium ion secondary battery, it is characterized in that, to the lithium rechargeable battery base material according to any one of claims 1 to 3, implement to be selected from following at least one process: the process of the process of dipping or the slurry of coating containing inorganic or organic filler particles, dipping or the slurry of coating containing resin, by the process of the process of multiple aperture plasma membrane laminated integratedization, dipping or applying solid electrolyte or gel-like electrolyte.
Invention effect
The feature of lithium rechargeable battery base material (1) of the present invention is, be made up of the non-weaving cloth of Polyester short fiber, and be less than 5.0 μm and fibre length is that the Polyester extremely short fiber of below 2mm is as essential component containing fiber diameter, compared with lithium rechargeable battery base material in the past, compactness and uniformity are all excellent.Thus, when carrying out Composite by surface coating, the deviation on surface is little, and is difficult to coming off of compound compound occurs, and can realize good quality.In addition, because it is made up of Polyester short fiber, thus high, when overcharging the fail safe of thermal endurance is high.
The length-width ratio (fibre length/fibre diameter) of Polyester extremely short fiber is the lithium rechargeable battery base material (2) of 20 ~ 800 and the lithium rechargeable battery base material (3) that is made up of the non-weaving cloth of the Polyester extremely short fiber containing 1 ~ 30 quality %, and the compactness necessary as base material and uniformity are more excellent.
The lithium rechargeable battery base material (1) of the application of the invention, (2) and (3), can provide separator for lithium ion secondary battery of the present invention.
Embodiment
Below, lithium rechargeable battery base material of the present invention is described in detail.Lithium rechargeable battery base material of the present invention is the non-weaving cloth of Polyester short fiber, it is characterized by, and is less than 5.0 μm and fibre length is that the Polyester extremely short fiber of below 2mm is as essential component containing fiber diameter.Still need explanation, fiber diameter refers to the arithmetic average of the fibre diameter of 10 fibers measured with microscope photographing 3000 times of enlarged photographs.
In lithium rechargeable battery base material of the present invention, when the fiber diameter of Polyester extremely short fiber is more than 5.0 μm, because the number of fiber in thickness direction tails off, thus cannot guarantee necessary compactness.In addition, when fibre length is more than 2mm, because fiber overlap to each other becomes many, and the number of fiber in entirety tails off, and thus cannot guarantee necessary uniformity.The preferred fiber diameter of Polyester extremely short fiber is 0.5 ~ 5.0 μm, and preferred fibre length is 0.05 ~ 2mm.
And then in order to obtain the balance of compactness and uniformity, more preferably the length-width ratio (fibre length/fibre diameter) of Polyester extremely short fiber is 20 ~ 800, more preferably 80 ~ 700.
In secondary lithium batteries base material of the present invention, the preferred content of Polyester extremely short fiber is 1 ~ 30 quality %, is more preferably 5 ~ 20 quality %.During less than 1 quality %, then can not improve compactness and uniformity, during more than 30 quality %, then cannot show as the necessary intensity of base material.
The fiber diameter of the short fiber beyond the Polyester extremely short fiber contained in lithium rechargeable battery base material of the present invention is preferably 0.1 ~ 10.0 μm.During more than 10.0 μm, because the number of fiber of thickness direction tails off, thus possibly cannot guarantee necessary compactness, during less than 0.1 μm, be difficult to stably manufacture fiber.Preferred fiber diameter is 0.5 ~ 5.0 μm.
The mass area ratio of lithium rechargeable battery base material of the present invention is preferably 6.0 ~ 30.0g/m 2.This is because, more than 30.0g/m 2time, only base material just occupies the more than half of dividing plate, becomes the effect being difficult to obtain Composite generation, less than 6.0g/m 2time, become and be difficult to obtain uniformity, there is the tendency surface easily after Composite producing large deviation.Be more preferably 8.0 ~ 20.0g/m 2.Still need explanation, mass area ratio refers to quantitative (level ground is measured, the grams of every square of rice paper) of the method specified based on JSI P 8124 (paper and paperboard-quantitative determination process).
Polyester (pole) short fiber can be heat fused (pole) short fiber (adhesive (pole) short fiber), also can be non-heat fused (pole) short fiber.When using as heat fused (pole) short fiber, the composite fibre or single component type etc. of core-sheath-type, core shift type, parallel type, fabric of island-in-sea type, tangerine lobe type, multiple bimetal type can be enumerated, for the viewpoint obtaining uniformity, be preferably the fiber of single component type.
In the present invention, Polyester can enumerate such as polyethylene terephthalate system, polybutylene terephthalate system, polytrimethylene terephthalate system, Polyethylene Naphthalate system, poly-naphthalenedicarboxylic acid fourth diester-based, polyethylene terephthalate system etc.These can be used alone or are combined two or more.In these, when for lithium rechargeable battery base material, the polyethylene terephthalate system of preferred excellent heat resistance.
The Composite of lithium rechargeable battery base material of the present invention is had no particular limits, can obtain separator for lithium ion secondary battery of the present invention by implementing the following processing lithium rechargeable battery base material of the present invention, these process can be enumerated: the process of the process of dipping or the slurry of coating containing inorganic or organic filler particles, dipping or the slurry of coating containing resin, by the process etc. of the process of multiple aperture plasma membrane laminated integratedization, dipping or applying solid electrolyte or gel-like electrolyte.
In lithium rechargeable battery base material of the present invention, the manufacture method as non-weaving cloth can use formation fleece, and makes the method for fibres bond in fleece, fusion, entanglement.Gained non-weaving cloth can be used as it is, and also can use the laminated body be made up of multi-disc.As fibroreticulate manufacture method, such as, there are the damp process of the dry process of combing method, air laid etc., copy paper method etc., spun-bond process, fusion method etc.Wherein, the net obtained by damp process is even and fine and close, can be suitable as lithium rechargeable battery base material.Damp process is following method: fiber dispersion is formed in water uniform copy paper slurry, this copy paper slurry is used the paper machine with silk screens such as at least one cylinder, fourdrinier wire, tiltings and obtains fleece.
As the method by web manufacture non-weaving cloth, current entangling process, needle point method, adhesives method etc. can be used.When particularly using above-mentioned damp process when paying attention to uniformity, preferably implementing adhesives method and to bond heat fused (pole) short fiber.By adhesives method, by uniform net form uniformly non-weaving cloth.For the wet type non-weaving cloth manufactured like this, adjust thickness preferably by calender etc. applies pressure or make thickness uniformizing.But, preferably pressurize at the temperature (temperature than low more than 20 DEG C of the fusing point of heat fused (pole) short fiber) that can not make heat fused (pole) staple sheath membranization.
In lithium rechargeable battery base material of the present invention, when manufacturing non-weaving cloth with damp process, as the fibre length of the fiber beyond Polyester extremely short fiber, preferably greater than 2mm and at below 7mm, more preferably 3 ~ 5mm.When fibre length is more than 7mm, owing to taking into account fiber diameter, be therefore likely difficult to loosen collagen fibre by damp process, generation texture is bad, likely occurs to form good fibroreticulate problem.On the other hand, fiber beyond Polyester extremely short fiber and Polyester extremely short fiber are wound around mutually, the intensity of base material can be made to improve, when the fibre length of the fiber therefore beyond Polyester extremely short fiber is below 2mm, likely cannot show as the necessary intensity of base material.
Here, the necessary intensity of base material has been can tolerate the intensity of rollback to short circuit during battery after dividing plate, and puncture strength can as an index.Preferred puncture strength is more than 30g.Be more preferably more than 50g.
Embodiment
The present invention is described in more detail by the following examples, but the present invention is not by the restriction of the present embodiment.Still need explanation, " part " and " percentage " in embodiment, when illustrating in advance, is all in mass.
Embodiment 1
By fineness 0.06dtex (fiber diameter 2.4 μm), the polyethylene terephthalate (PET) of the oriented crystalline of fibre length 3mm is 40 parts, short fiber, fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 1mm, the PET system extremely short fiber 10 parts of the oriented crystalline of length-width ratio 329, with fineness 0.2dtex (fiber diameter 4.3 μm), 50 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.2g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.2g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 2
By 49 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 1 part of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 1mm, length-width ratio 329, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.6g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.6g/m 2, thickness 18 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 3
By 49.3 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 0.7 part of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 1mm, length-width ratio 329, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.5g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.5g/m 2, thickness 18 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 4
By 20 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 30 parts of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 1mm, length-width ratio 329, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.8g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.8g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 5
By 17 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 33 parts of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 1mm, length-width ratio 329, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.6g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.6g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 6
By 40 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 10 parts of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 2mm, length-width ratio 658, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.0g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.0g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 7
By 40 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 10 parts of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 0.6mm, length-width ratio 197, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.9g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.9g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 8
By fineness 0.06dtex (fiber diameter 2.4 μm), 40 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.1dtex (fiber diameter 3.0 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 1mm, the adhesive PET system extremely short fiber 20 parts of length-width ratio 232, with fineness 0.2dtex (fiber diameter 4.3 μm), 30 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's extremely short fiber and adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.1g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.1g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 9
By fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 1mm, the PET system extremely short fiber 10 parts of the oriented crystalline of length-width ratio 424, fineness 0.06dtex (fiber diameter 2.4 μm), 30 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.1dtex (fiber diameter 3.0 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 1mm, the adhesive PET system extremely short fiber 20 parts of length-width ratio 232, with fineness 0.2dtex (fiber diameter 4.3 μm), 30 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's extremely short fiber and adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.3g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.3g/m 2, thickness 18 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 10
By fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 1mm, the PET system extremely short fiber 10 parts of the oriented crystalline of length-width ratio 424, fineness 0.06dtex (fiber diameter 2.4 μm), 30 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.1dtex (fiber diameter 3.0 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 0.1mm, the adhesive PET system extremely short fiber 20 parts of length-width ratio 23, with fineness 0.2dtex (fiber diameter 4.3 μm), 30 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's extremely short fiber and adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.8g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.8g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 11
By fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 1mm, the PET system extremely short fiber 10 parts of the oriented crystalline of length-width ratio 424, fineness 0.06dtex (fiber diameter 2.4 μm), 30 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.1dtex (fiber diameter 3.0 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 0.05mm, the adhesive PET system extremely short fiber 20 parts of length-width ratio 11, with fineness 0.2dtex (fiber diameter 4.3 μm), 30 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's extremely short fiber and adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.3g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.3g/m 2, thickness 16 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 12
By the PET system extremely short fiber 20 parts of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 0.6mm, length-width ratio 254,20 parts, the PET system short fiber of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 3mm, be mixed together with 60 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.1g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.1g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 13
By the PET system extremely short fiber 20 parts of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 2mm, length-width ratio 849,20 parts, the PET system short fiber of the oriented crystalline of fineness 0.1dtex (fiber diameter 3.0 μm), fibre length 3mm, be mixed together with 60 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.4g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.4g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 14
By fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 1mm, the PET system extremely short fiber 20 parts of the oriented crystalline of length-width ratio 424, fineness 0.06dtex (fiber diameter 2.4 μm), 20 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.3dtex (fiber diameter 5.3 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, with fineness 0.2dtex (fiber diameter 4.3 μm), 50 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.9g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.9g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 15
By fineness 0.004dtex (fiber diameter 0.70 μm), fibre length 0.5mm, the PET system extremely short fiber 10 parts of the oriented crystalline of length-width ratio 714, fineness 0.06dtex (fiber diameter 2.4 μm), 20 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.1dtex (fiber diameter 3.0 μm), 20 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, with fineness 0.2dtex (fiber diameter 4.3 μm), 50 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.7g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.7g/m 2, thickness 16 μm non-weaving cloth, as lithium rechargeable battery base material.
Embodiment 16
By fineness 0.004dtex (fiber diameter 0.70 μm), 10 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 1mm, the PET system extremely short fiber 20 parts of the oriented crystalline of length-width ratio 424, fineness 0.1dtex (fiber diameter 3.0 μm), 20 parts, the PET system short fiber of the oriented crystalline of fibre length 3mm, with fineness 0.2dtex (fiber diameter 4.3 μm), 50 parts, the adhesive PET system short fiber of fibre length 3mm is mixed together, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 9.8g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 9.8g/m 2, thickness 16 μm non-weaving cloth, as lithium rechargeable battery base material.
Comparative example 1
By 50 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.2g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.2g/m 2, thickness 17 μm non-weaving cloth, as lithium rechargeable battery base material.
Comparative example 2
By 40 parts, the PET system short fiber of the oriented crystalline of fineness 0.06dtex (fiber diameter 2.4 μm), fibre length 3mm, the PET system extremely short fiber 10 parts of the oriented crystalline of fineness 0.3dtex (fiber diameter 5.3 μm), fibre length 2mm, be mixed together with 50 parts, the adhesive PET system short fiber of fineness 0.2dtex (fiber diameter 4.3 μm), fibre length 3mm, at the dissociation in water of pulper, under blender stirs, be prepared as and manufacture paper with pulp uniformly with slurry (1% concentration).Use damp process, this being manufactured paper with pulp by cylinder paper machine is ferreted out with slurry, makes adhesive PET system's bonding short fibers and shows non-weaving cloth intensity, produce quantitative 10.5g/m by the revolving driers of 120 DEG C 2, wide 50cm non-weaving cloth.Then, carry out calendering process with roll temperature 180 DEG C, produce quantitative 10.5g/m 2, thickness 19 μm non-weaving cloth, as lithium rechargeable battery base material.
Evaluate
Following evaluation is carried out to the lithium rechargeable battery base material that embodiment and comparative example obtain, shows the result in table 1.
The heat characteristic of base material
Polyethylene (PE) microporous film (it is existing known dividing plate) of embodiment 1 ~ 16 and the base material of comparative example 1 ~ 2 and the thickness 20 μm as comparative example 3 is placed 30 minutes in the thermostat of 150 DEG C, measure the shrinkage of each base material, thus evaluate heat characteristic.Being determined as follows of shrinkage is carried out.Cut out the substrate sheets of 5cm × 5cm, be clipped in between fixing 2 glass sheets of clip, place in the thermostat of 150 DEG C after 30 minutes and take out, measure the length of each substrate sheets, the minimizing ratio of length is shrinkage compared with the length before test.
The manufacture of dividing plate
By tabular boehmite (average grain diameter: 1 μm, length-width ratio: 10) 1000g, water 800g, isopropyl alcohol 200g, polyvinyl butyral resin 375g put into container, utilize mixer (trade name: ス リ mono-ヮ Application モ mono-タ mono-, the chemical society in new east manufactures) stir and make it disperse in 1 hour, form uniform sizing material.Respectively by the non-weaving cloth of embodiment 1 ~ 16 and comparative example 1 ~ 2 in this slurry, after carrying out coating sizing-agent by lift coating (drawing げ Tu cloth Shang I), by between the gap with predetermined distance, dry afterwards, obtain the dividing plate that each one side has thickness 3 μm of perforated membranes.
The coating evaluation of base material
Thickness for any 10 positions of the dividing plate manufactured is implemented to measure, if its difference is below 1 μm, represents with zero, if, represented with △ below 2 μm more than 1 μm, if more than 2 μm, with × represent.Still need explanation, thickness refers to the value that the method specified by JIS B 7502 is measured, that is, the value measured by outside micrometer when representing 5N load.
The intensity of base material
Embodiment 1 ~ 16 and the base material of comparative example 1 ~ 2 are trimmed into the wide strip of 50mm.Test film is installed on desktop Material Testing Machine (trade name: STA-1150, (strain) ォ リ ェ Application テ ッ Network manufactures) to go up on the 40mm φ fixed frame of configuration, the relative sample face of metal needle (manufacture of (strain) ォ リ ェ Application テ ッ Network) certain speed with 50mm/ minute at a right angle making tip be set to the diameter 1.0mm of circle (curvature 1.6) is fallen until run through.Measurement maximum load (g) now, it can be used as puncture strength.To puncture strength more than 1 Specimen Determination, 5 positions, if to puncture strength minimum in all measured values at more than 50g, represented with zero, if at more than 30g and less than 50g, represented with △, if less than 30g, with × represent.
Table 1
The lithium rechargeable battery base material that embodiment obtains is made up of the non-weaving cloth of PET system short fiber, it is characterized by, be less than 5 μm containing fiber diameter and fibre length is that the PET system extremely short fiber of below 2mm is as essential component, compared with lithium rechargeable battery base material in the past, compactness and uniformity are all excellent.Thus, the good result that surface deviation is little when being carried out Composite by surface coating can be obtained.In addition, owing to being made up of PET, thus at 150 DEG C, almost can not see thermal contraction, do not produce distortion in fact at visual derection level.Therefore, thermal endurance is high, and fail safe when overcharging is high.
The length-width ratio (fibre length/fibre diameter) of Polyester extremely short fiber is 20 ~ 800, and the content of Polyester extremely short fiber is the embodiment 1,2,4,6 ~ 10,12,15 and 16 of 1 ~ 30 quality %, coating and intensity two aspect all excellent.The content of embodiment 13 more than 800 of length-width ratio (fibre length/fibre diameter) embodiment 11 less than 20 of Polyester extremely short fiber, the length-width ratio (fibre length/fibre diameter) of Polyester extremely short fiber and Polyester extremely short fiber is less than the embodiment 3 of 1 quality %, when carrying out Composite by surface coating, the deviation on surface increases slightly.The content of Polyester extremely short fiber is more than the embodiment 5 of 30 quality %, and intensity has some to reduce.
In addition, as the fiber beyond Polyester extremely short fiber, containing fiber diameter more than in the embodiment 14 of the fiber of 5 μm, also showing the surface deviation when being carried out Composite by surface coating has the tendency that change is large.
On the other hand, the lithium rechargeable battery base material that comparative example 1 obtains, the fiber diameter of wherein used PET system short fiber is 2.4 μm, fibre length is 3mm, owing to being not less than 5.0 μm containing fiber diameter and fibre length is the PET system extremely short fiber of below 2mm, thus sufficient requirement cannot be met in the necessary uniformity of lithium rechargeable battery base material.Therefore, result produces the deviation on surface when carrying out Composite by surface coating.
The lithium rechargeable battery base material that comparative example 2 obtains, the fiber diameter being the PET system extremely short fiber of below 2mm due to wherein fibre length is 5.3 μm, has exceeded 5.0 μm, thus can not meet sufficient requirement in compactness.Therefore, result produces the deviation on surface when carrying out Composite by surface coating.
About the comparative example 3 being equivalent to dividing plate in the past, percent thermal shrinkage is large, when using it for battery, produces the contraction of dividing plate when internal temperature reaches the abnormal excessive charging of 150 DEG C, likely cause short circuit due to positive pole and cathode contact, have problems in fail safe.
Industrial applicibility
Lithium rechargeable battery base material of the present invention, can be suitable for the separator for lithium ion secondary battery such as lithium rechargeable battery, lithium ion polymer secondary cell etc.

Claims (2)

1. lithium rechargeable battery base material, it is characterized in that, being made up of the non-weaving cloth of polyethylene terephthalate system short fiber and by the process of the process of implementing to be selected from dipping or the slurry of coating containing inorganic or organic filler particles, dipping or the slurry of coating containing resin, at least one process of the process of the process of multiple aperture plasma membrane laminated integratedization, dipping or applying solid electrolyte or gel-like electrolyte is become in the lithium rechargeable battery base material of separator for lithium ion secondary battery, be 5.0 containing fiber diameter μbelow m and fibre length is that the polyethylene terephthalate system extremely short fiber of below 2mm is as essential component, wherein this fiber diameter refers to the arithmetic average of the fibre diameter of 10 fibers measured with microscope photographing 3000 times of enlarged photographs, is 1 ~ 30 quality % relative to the content of non-weaving cloth polyethylene terephthalate system extremely short fiber.
2. lithium rechargeable battery base material according to claim 1, wherein, the length-width ratio of polyethylene terephthalate system extremely short fiber and fibre length are 20 ~ 800 with the ratio of fibre diameter.
3. lithium rechargeable battery base material according to claim 1, wherein, the length-width ratio of polyethylene terephthalate system extremely short fiber and fibre length are 80 ~ 700 with the ratio of fibre diameter.
4. lithium rechargeable battery base material according to claim 1, wherein, the fiber diameter of polyethylene terephthalate system extremely short fiber is 0.5 ~ 5.0 μm, fibre length is 0.05 ~ 2mm.
5. the lithium rechargeable battery base material according to any one of Claims 1 to 4 wherein, is 5 ~ 20 quality % relative to the content of non-weaving cloth polyethylene terephthalate system extremely short fiber.
6. separator for lithium ion secondary battery, is characterized in that, uses the lithium rechargeable battery base material according to any one of claim 1 ~ 5.
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