WO2015065122A1 - 전기화학소자용 분리막의 제조방법 및 그로부터 제조된 전기화학소자용 분리막 - Google Patents
전기화학소자용 분리막의 제조방법 및 그로부터 제조된 전기화학소자용 분리막 Download PDFInfo
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- WO2015065122A1 WO2015065122A1 PCT/KR2014/010393 KR2014010393W WO2015065122A1 WO 2015065122 A1 WO2015065122 A1 WO 2015065122A1 KR 2014010393 W KR2014010393 W KR 2014010393W WO 2015065122 A1 WO2015065122 A1 WO 2015065122A1
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- WO
- WIPO (PCT)
- Prior art keywords
- separator
- electrochemical device
- porous
- slurry
- polyolefin film
- Prior art date
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- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 125000005313 fatty acid group Chemical group 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- CASZBAVUIZZLOB-UHFFFAOYSA-N lithium iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Li+] CASZBAVUIZZLOB-UHFFFAOYSA-N 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D67/0002—Organic membrane manufacture
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/0025—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching
- B01D67/0027—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching by stretching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/0002—Organic membrane manufacture
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/003—Organic membrane manufacture by inducing porosity into non porous precursor membranes by selective elimination of components, e.g. by leaching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D71/262—Polypropylene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/91—Heating, e.g. for cross linking
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
- H01M50/406—Moulding; Embossing; Cutting
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- H—ELECTRICITY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- H01M50/451—Separators, membranes or diaphragms characterised by the material having a layered structure comprising layers of only organic material and layers containing inorganic material
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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
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/494—Tensile strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the present invention relates to a method for manufacturing a separator for an electrochemical device, and to a separator for an electrochemical device manufactured therefrom, and more particularly, to a method for manufacturing a separator for an electrochemical device having an improved mechanical / thermal performance and an electric produced therefrom. It relates to a separator for chemical devices.
- the electrochemical device is the most attracting field in this respect, and the development of a secondary battery capable of charging and discharging has been the focus of attention, and in recent years in the development of such a battery in order to improve the capacity density and specific energy
- the research and development of the design of the battery is progressing.
- a composite separator including a porous coating layer on which at least one surface of a polyolefin porous substrate having a plurality of pores is coated with a slurry including inorganic particles or organic particles and a binder polymer has been proposed.
- the inorganic / organic particles in the coating layer coated on the polyolefin porous substrate serve as a support for maintaining the physical form of the coating layer, thereby suppressing thermal contraction of the polyolefin porous substrate when the lithium ion battery is overheated.
- the conventional process for preparing such a separator includes extruding a polyolefin resin composition, stretching the extruded resin composition to obtain a film on a sheet, and extracting a plasticizer from the obtained separator to obtain a porous film.
- the heat setting process is subject to the limitation that the polyolefin film must be made at a temperature such that the polyolefin film is not melted.
- the heat setting process is subject to the limitation that the polyolefin film must be made at a temperature such that the polyolefin film is not melted.
- Japanese Patent No.5543715 discloses (i) a step of melt-kneading a polyolefin resin and a plasticizer, or a polyolefin resin, a plasticizer and an inorganic agent, and (ii) a step of stretching the obtained extrudate, (iii) a plasticizer or a plasticizer;
- the manufacturing method of the separator for nonaqueous electrolyte batteries containing the process of extracting an inorganic agent is disclosed. However, since this is not a method of coating a slurry such as inorganic particles after the porous substrate is formed, the order of slurry coating and heat setting steps and specific conditions thereof are not mentioned.
- Korean Patent No. 10-0406690 is a multi-component film used as a separator for an electrochemical device i) providing a polymer support layer film; ii) dissolving the gelling polymer in a solvent to prepare a gelling polymer solution; iii) preparing a multilayer film by forming a gelling polymer layer on one or both sides of the support layer film of step i) from the gelling polymer solution of step ii); And iv) stretching the multilayer film of step iii) and then thermally fixing the multilayer film.
- this document merely coats the gelling polymer solution on the porous substrate to form a gelling polymer layer, and does not disclose a step of forming the porous coating layer by coating a slurry including organic particles or inorganic particles.
- the gelled polymer layer is first coated on the polymer support layer film, and then the obtained multilayer film is stretched and heat-set, and in the case of the composite film having a porous coating layer containing organic particles and / or inorganic particles, after coating
- stretching there is a problem such as cracks in the coating layer in the TD direction, there is a limit to the application.
- the present invention has been made in consideration of the above-described problems, the problem to be solved by the present invention, the composite membrane formed with a porous coating layer is more structurally stabilized, the process cost is reduced, the electrochemical that can improve the production yield It is to provide a method for manufacturing a separator for the device.
- Extruding the resin composition containing the polyolefin and the plasticizer Stretching the extruded resin composition to obtain a polyolefin film; Extracting the plasticizer from the obtained polyolefin film to obtain a porous polyolefin film; Coating a slurry for forming a porous coating layer on at least one surface of the porous polyolefin film; And heat-setting the slurry-coated porous polyolefin film to obtain a composite separator in which a porous coating layer is formed.
- the stretching of the extruded resin composition may be performed at least one uniaxial stretching in the MD direction or the TD direction, or at least one biaxial stretching in the MD direction and the TD direction.
- the temperature of the heat setting is Tm-1 °C or less, where Tm may be the melting point of the polyolefin.
- the temperature of the heat setting may be 131 °C to 134 °C.
- the heat setting may be performed using a heat source directed in a direction perpendicular to the surface of the slurry coated on the porous polyolefin film.
- the polyolefin is polyethylene; Polypropylene; Polybutylene; Polypentene: polyhexene: polyoctene: one or more copolymers of ethylene, propylene, butene, pentene, 4-methylpentene, hexene, octene, or mixtures thereof.
- the plasticizer may include paraffin oil, mineral oil, wax, soybean oil, phthalic acid esters, aromatic ethers, fatty acids having 10 to 20 carbon atoms; Fatty acid alcohols having 10 to 20 carbon atoms; And it may include one or more selected from the group consisting of fatty acid esters.
- the porous polyolefin film may have a thickness of 5 to 50 ⁇ m, and a pore size and porosity may be 0.01 to 50 ⁇ m and 10 to 95%, respectively.
- the slurry for forming the porous coating layer may include one or more kinds of particles of an inorganic particle and an organic particle, a binder polymer, and a solvent.
- the binder polymer may be polyvinylidene fluoride-co-hexafluoropropylene, polyvinylidene fluoride-co-trichloroethylene, polymethylmethacrylate, Polybutylacrylate, polyacrylonitrile, polyvinylpyrrolidone, polyvinylacetate, ethylene vinyl acetate copolymer (polyethylene-co-vinyl acetate), polyethylene oxide (polyethylene oxide, cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate, cyanoethylpullulan, cyanoethylpolyvinylalcohol, Noethylcellulose Cyanoethylcellulose, cyanoethylsucrose, pullulan, carboxyl methyl cellulose, acrylonitrile-styrene-butadiene copolymer, polyimide Or mixtures thereof.
- the inorganic particles may be inorganic particles having a dielectric constant of 5 or more, inorganic particles having a lithium ion transfer ability, or a mixture thereof.
- the inorganic particles having a dielectric constant of 5 or more include BaTiO 3 , Pb (Zr, Ti) O 3 (PZT), Pb 1-x La x Zr 1-y Ti y O 3 (PLZT), PB (Mg 3 Nb 2/3 ) O 3 -PbTiO 3 (PMN-PT), hafnia (HfO 2 ), SrTiO 3 , SnO 2 , CeO 2 , MgO, NiO, CaO, ZnO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , TiO 2, SiC Or mixtures thereof.
- the inorganic particles having the lithium ion transfer ability are lithium phosphate (Li 3 PO 4 ), lithium titanium phosphate (Li x Ti y (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3), lithium aluminum titanium phosphate (Li x Al y Ti z (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 3), (LiAlTiP) x O y series glass (0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 13), lithium lanthanum titanate (Li x La y TiO 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3), lithium germanium thiophosphate (Li x Ge y P z S w , 0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1, 0 ⁇ w ⁇ 5), lithium nitride (Li x N
- the organic particles are polystyrene, polyethylene, melamine resin, phenol resin, cellulose, cellulose modified body, polypropylene, polyester, polyphenylene sulfide, poly aramid, polyamideimide, polyimide, butyl acrylate and ethyl methacryl. Copolymers of the rates or mixtures thereof.
- the average particle diameter of the inorganic particles and the organic particles may be independently 0.001 to 10 ⁇ m.
- the method may further include winding and slitting the composite separator.
- Before the coating of the slurry for forming the porous coating layer may not include the step of heat setting and winding and slitting.
- the method may further include packaging the composite separator in which the winding and slitting are completed.
- a separator for an electrochemical device manufactured by the above-described manufacturing method.
- the separator including a cathode, an anode, and a separator interposed between the cathode and the anode, the separator is provided with an electrochemical device which is the separator for the electrochemical device described above.
- the electrochemical device may be a lithium secondary battery.
- the heat-setting was carried out between the conventional plasticizer extraction process and slurry coating process by manufacturing the separator in the order of extrusion process, stretching process, plasticizer extraction process, slurry coating process, and heat setting process
- the steps of / winding and slitting / unwinding can be drastically omitted.
- various properties such as improving the physical properties of the composite membrane, reduction of production cost, high quality, improvement of production yield, implementation of ultra-wide coating, use of space, etc. It can have an advantage.
- the heat setting is performed at a higher temperature than the conventional heat setting temperature, thereby improving mechanical and thermal performance and having excellent breathability.
- Membranes can be provided, and the heat-setting oven can be compactly shortened, saving space, processing and production costs.
- the heat setting step is omitted before the slurry coating step, it is possible to use the heat setting oven and the drying oven separately at the same time, thereby simultaneously using space and reducing costs.
- the polyolefin film since heat applied in the heat setting process is transferred to the polyolefin film through the porous coating layer, the polyolefin film has a thinner diameter of fibrils, thereby increasing the fibrilar number density per unit area and forming a porous coating layer.
- the interfacial contact area with the coating slurry is increased, thereby making it easier to maintain the physical form of the polyolefin film, thereby improving the heat shrinkage rate of the composite separator and improving the peel strength of the coating layer.
- FIG. 1 is a conceptual diagram showing a conventional process for producing a separator for an electrochemical device.
- FIG. 2 is a conceptual diagram illustrating a method of manufacturing a separator for an electrochemical device according to an embodiment of the present invention.
- Method for producing a separator for an electrochemical device the step of extruding a resin composition containing a polyolefin and a plasticizer; Stretching the extruded resin composition to obtain a polyolefin film; Extracting the plasticizer from the obtained polyolefin film to obtain a porous polyolefin film; Coating a slurry for forming a porous coating layer on at least one surface of the porous polyolefin film; And heat-setting the slurry-coated porous polyolefin film to obtain a composite separator in which a porous coating layer is formed.
- FIG. 2 is a conceptual diagram showing a method for manufacturing a separator for an electrochemical device according to an embodiment of the present invention.
- the method of manufacturing a separator for an electrochemical device may further include winding and slitting the composite separator in which heat setting is completed to obtain a final product.
- the method may further include packing the composite separator in which the winding and slitting are completed.
- the manufacturing method of the separator for an electrochemical device compared with the conventional manufacturing method shown in Figure 1, before the step of coating the slurry for forming the porous coating layer and the step of heat setting and winding and It does not include slitting.
- the separator by manufacturing the separator in the order of extrusion process, stretching process, plasticizer extraction process, slurry coating process, and heat setting process, the plasticizer as in the conventional manufacturing method shown in FIG. Since the heat setting step, the winding and slitting step, and the unwinding step are not required after the extraction step, these steps can be omitted dramatically.
- the polyolefin is not particularly limited as long as it is commonly used in the art.
- specific examples of such polyolefins include polyethylene such as high density polyethylene (HDPE), low density polyethylene (LDPE), linear low density polyethylene (LLDPE), ultra high molecular weight polyethylene (UHMWPE), and the like; Polypropylene; Polybutylene; Polypentene: polyhexene: polyoctene: one or more copolymers of ethylene, propylene, butene, pentene, 4-methylpentene, hexene, octene, or mixtures thereof.
- polyethylene such as high density polyethylene (HDPE), low density polyethylene (LDPE), linear low density polyethylene (LLDPE), ultra high molecular weight polyethylene (UHMWPE), and the like
- Polypropylene Polybutylene
- Polypentene polyhexene: polyoctene: one or more copolymers of ethylene, propylene, butene, pentene
- the plasticizer is not particularly limited as long as it is commonly used in the art.
- Non-limiting examples of such plasticizers include phthalic acid esters such as dibutyl phthalate, dihexyl phthalate and dioctyl phthalate; Aromatic ethers such as diphenyl ether and benzyl ether; Fatty acids having 10 to 20 carbon atoms, such as palmitic acid, stearic acid, oleic acid, linoleic acid, and linolenic acid; Fatty acid alcohols having 10 to 20 carbon atoms such as palmitic alcohol, stearic acid alcohol, and oleate alcohol; Palmitic acid mono-, di-, or triesters, stearic acid mono-, di-, or triesters.
- One double-bonded saturated or unsaturated fatty acid or unsaturated fatty acid having 4 to 26 carbon atoms in the fatty acid group such as oleic mono-, di- or triester, linoleic acid mono-, di- or triester, substituted by epoxy Or fatty acid esters in which two or more fatty acids have 1 to 8 hydroxyl groups and are ester-bonded with alcohols having 1 to 10 carbon atoms.
- plasticizer may be used as a mixture containing two or more of the above-described components.
- the weight ratio of the polyolefin to the plasticizer may be 80:20 to 10:90, preferably 70:30 to 20:80, preferably 50:50 to 30:70.
- the weight ratio is greater than 80:20 and the content of polyolefin is increased, the porosity decreases and the pore size decreases, the interconnectivity between pores decreases so that the permeability is greatly decreased, and the viscosity of the polyolefin solution rises to increase the extrusion load.
- the weight ratio is less than 10:90 and the content of polyolefin is decreased, the kneading property of the polyolefin and the plasticizer is lowered, so that the polyolefin is extruded in a gel form without thermodynamic kneading into the plasticizer, and thus the breakage and thickness of the polyolefin are not increased. It may cause problems such as uniformity, and the strength of the prepared separator may be lowered.
- melt kneading is carried out by a screw extruder such as a single screw extruder, a twin screw extruder, a kneader, a mixer, or the like, and is extruded from a T-type die or an annular die.
- the kneaded / extruded melt can be solidified by compression cooling. Examples of the cooling method include a method of directly contacting a cooling medium such as cold air or cooling water, or a method of contacting a roll or press machine cooled with a refrigerant.
- the extruded resin composition is stretched to obtain a polyolefin film.
- the stretching method may be carried out by conventional methods known in the art, non-limiting examples include MD (longitudinal) uniaxial stretching by a roll stretching machine, TD (lateral direction) uniaxial stretching by a tenter, roll stretching machine and tenter, Or sequential biaxial stretching by a combination of a tenter and a tenter, simultaneous biaxial stretching by a simultaneous biaxial tenter or inflation molding, and the like.
- the extruded resin composition may be uniaxially stretched one or more times in the MD direction or the TD direction, or biaxially stretched one or more times in the MD direction and the TD direction.
- the stretching ratio is 3 times or more, preferably 5 to 10 times, respectively in the longitudinal direction and the transverse direction, and the total stretching ratio (total plane magnification) can be 20 times or more, preferably 20 to 80 times.
- the orientation in one direction may not be sufficient, and at the same time, the balance of physical properties between the longitudinal and transverse directions may be broken, leading to a decrease in tensile strength and puncture strength.
- the total draw ratio is less than (20) times, unstretched, pore formation may not occur, and if it exceeds (80) times, breakage occurs during stretching, and the shrinkage of the final film may be increased. have.
- the stretching temperature may vary depending on the melting point of the polyolefin used and the concentration and type of the plasticizer.
- the stretching temperature is selected in a temperature range in which 30 to 80% by weight of the crystal part of the polyolefin in the film is melted. It is suitable.
- the stretching temperature is selected in a temperature range lower than the melting temperature of 30% by weight of the crystalline portion of the polyolefin in the sheet molding, there is no softness of the film, the stretchability is worsened and the breakage is more likely to occur when stretching, and at the same time unstretched Occurs.
- the stretching temperature is selected in the temperature range higher than the melting temperature of 80% by weight of the crystal portion, the stretching is easy and less unstretched, but the thickness deviation occurs due to partial overstretching, the orientation effect of the resin is less This will greatly fall.
- the degree of melting of the crystal portion with temperature can be obtained from differential scanning calorimeter (DSC) analysis of the film molding.
- the plasticizer is then extracted from the stretched film to obtain a porous polyolefin film. Specifically, the plasticizer in the stretched film is extracted using an organic solvent and dried.
- the extraction solvent used for the extraction of the plasticizer is preferably a poor solvent for the polyolefin, a good solvent for the plasticizer, and has a boiling point lower than the melting point of the polyolefin, so that drying is preferable.
- extraction solvents include hydrocarbons such as n-hexane and cyclohexane, halogenated hydrocarbons such as methylene chloride, 1,1,1-trichloroethane and fluorocarbons, alcohols such as ethanol and isopropanol, Ketones, such as acetone and 2-butanone, are mentioned.
- the content of residual plasticizer during extraction should preferably be 1% by weight or less. If the residual plasticizer exceeds 1% by weight, the physical properties decrease and the permeability of the porous membrane decreases.
- the amount of residual plasticizer may be influenced by the extraction temperature and extraction time, and the extraction temperature is preferably high in order to increase the solubility of the plasticizer and the organic solvent. However, the temperature is preferably 40 ° C. or lower in consideration of the safety problem due to the boiling of the organic solvent. . If the extraction temperature is below the freezing point of the plasticizer, the extraction efficiency is greatly reduced, so it must be higher than the freezing point of the plasticizer.
- the extraction time depends on the thickness of the porous polyolefin film to be produced, but in the case of 10 to 30 ⁇ m thickness, 2 to 4 minutes is suitable.
- the thickness of the porous polyolefin film obtained above is not particularly limited, but is preferably 5 to 50 ⁇ m, and the pore size and pore present in the porous substrate are also not particularly limited, but are 0.001 to 50 ⁇ m and 10 to 99%, respectively. desirable.
- a slurry for forming a porous coating layer should be prepared first, and the slurry is prepared by dispersing a binder polymer together with at least one of inorganic particles and organic particles in a solvent. That is, the slurry may include inorganic particles alone, organic particles alone, or inorganic particles and organic particles at the same time.
- the inorganic particles are not particularly limited as long as they are electrochemically stable. That is, the inorganic particles that can be used in the present invention are not particularly limited as long as the oxidation and / or reduction reactions do not occur in the operating voltage range (for example, 0 to 5 V on the basis of Li / Li + ) of the applied electrochemical device. In particular, in the case of using the inorganic particles having the ion transport ability, it is possible to improve the performance by increasing the ion conductivity in the electrochemical device.
- the ionic conductivity of the electrolyte may be improved by contributing to an increase in the dissociation degree of the electrolyte salt such as lithium salt in the liquid electrolyte.
- Non-limiting examples of the inorganic particles include high dielectric constant inorganic particles having a dielectric constant of 5 or more, preferably 10 or more, inorganic particles having a lithium ion transfer ability, or a mixture thereof.
- Non-limiting examples of inorganic particles having a dielectric constant of 5 or more include BaTiO 3 , Pb (Zr, Ti) O 3 (PZT), Pb 1-x La x Zr 1-y Ti y O 3 (PLZT), PB (Mg 3 Nb 2/3 ) O 3 -PbTiO 3 (PMN-PT), Hafnia (HfO 2 ), SrTiO 3 , SnO 2 , CeO 2 , MgO, NiO, CaO, ZnO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , TiO 2, SiC Or mixtures thereof.
- the term 'inorganic particles having lithium ion transporting ability' refers to inorganic particles containing lithium elements but having a function of transferring lithium ions without storing lithium, and are not limited to inorganic particles having lithium ion transporting ability.
- Typical examples include lithium phosphate (Li 3 PO 4 ), lithium titanium phosphate (Li x Ti y (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3), and lithium aluminum titanium phosphate (Li x Al y Ti z (LiAlTiP) x O y series such as (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 3), 14Li 2 O-9Al 2 O 3 -38TiO 2 -39P 2 O 5, etc.
- Lithium germanium thiophosphate such as 4 (Li x Ge y P z S w , 0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1, 0 ⁇ w ⁇ 5), lithium such as Li 3 N SiS 2 series glass (Li x Si y S z , 0 ⁇ x ⁇ ) such as nitride (Li x N y , 0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 2), Li 3 PO 4 -Li 2 S-SiS 2, etc.
- LiI P 2 S 5 series glass Li x P y S z , 0 ⁇ x ⁇ 3, 0 ⁇ y ⁇ 3, 0 ⁇ z ⁇ 7, such as Li 2 SP 2 S 5 , or a mixture thereof.
- Organic particles contained in the slurry are advantageous in terms of air permeability, heat shrinkability, peel strength, and excellent binding property with the binder polymer.
- Non-limiting examples of organic particles that can be used in the slurry for forming the porous coating layer include polystyrene, polyethylene, melamine-based resin, phenol-based resin, cellulose, cellulose modified body (carboxymethyl cellulose, etc.), polypropylene, polyester (polyethylene tere). Phthalate, polyethylene naphthalate, polybutylene terephthalate, etc.), polyphenylene sulfide, polyaramid, polyamideimide, polyimide, copolymer of butyl acrylate and ethyl methacrylate (butyl acrylate and ethyl methacrylate) Particle
- the organic particles may be composed of two or more kinds of polymers.
- the size of the inorganic particles or organic particles is not limited, but may be independently 0.001 to 10 ⁇ m in terms of forming a coating layer having a uniform thickness and having an appropriate porosity.
- the binder polymer used in the slurry for forming the porous coating layer is not particularly limited as long as it can perform a function of stably connecting the inorganic particles or the organic particles, and non-limiting examples include polyvinylidene fluoride-hexafluoro.
- Propylene polyvinylidene fluoride-co-hexafluoropropylene
- polyvinylidene fluoride-co-trichloroethylene polymethylmethacrylate, polybutylacrylate, polyacrylonitrile (polacrylonitrile, polyvinylpyrrolidone, polyvinylacetate, ethylene vinyl co-vinyl acetate, polyethylene oxide, cellulose acetate, cellulose acetate butyrate (cellulose acetate butyrate, cellulose acetate propionate, cyanoethylpullulan, cyanoethylpolyvinylalcohol, cyanoethylcellulose, cyanoethylsucrose, Pullulan, carboxyl methyl cellulose, acrylonitrile-styrene-butadiene copolymer, polyimide, and the like, each of which may be used alone or among them. Two or more kinds can be mixed and used.
- the composition ratio of the particles and the binder polymer in the slurry for forming the porous coating layer may range from 50:50 to 99: 1 by weight or may be from 70:30 to 95: 5, for example.
- the thermal stability of the separator may be improved, and the voids formed between the particles may not be formed sufficiently, resulting in a decrease in pore size and porosity, which may result in deterioration of final cell performance. have.
- the peeling resistance of the porous coating layer may be weakened.
- the particles and the binder polymer may be uniformly dispersed, and then, may be easily removed.
- solvents include acetone, tetrahydrofuran, methylene chloride, chloroform, dimethylformamide, N-methyl-2-pyrrolidone ( N-methyl-2-pyrrolidone, NMP), cyclohexane, water, or a mixture thereof.
- the slurry for forming the porous coating layer is coated on at least one surface of the porous polyolefin film, and the specific method of coating may use a conventional coating method known in the art, for example, dip coating, die coating, Various methods such as roll coating, comma coating, or a mixture thereof can be used.
- the porous coating layer may be selectively formed on both sides or only one side of the porous polyolefin film.
- the slurry-coated porous polyolefin film is heat-set to obtain a composite separator in which a porous coating layer is formed.
- the heat setting is a process of fixing the film and applying heat to forcibly grasp the film to be shrunk to remove residual stress.
- the higher the heat setting temperature is preferable because the shrinkage is reduced, but when the heat setting temperature is too high, the polyolefin film is partially melted, so that the formed micropores may be blocked and the permeability may be lowered.
- the plasticizer after stretching to a polyolefin film, the plasticizer is extracted and subsequently coated with a slurry for forming a porous coating layer, so that the heat setting is carried out, unlike the conventional process of extracting and heat setting the plasticizer after stretching to a polyolefin film, Since heat setting is performed on the coated slurry rather than the polyolefin film, heat is not directly applied to the polyolefin film.
- the thickness of the fibril of the polyethylene substrate adjacent to the porous coating layer is thinner than that of the conventional fibrillated polyolefin film. Accordingly, the fibrilar number density per unit area of the surface of the porous film adjacent to the porous coating layer is increased, thereby increasing the interfacial contact area with the coating slurry, and the glass transition temperature (T g ) or melting point (T) of the coating slurry.
- T g glass transition temperature
- T melting point
- the temperature of the heat setting is preferably adjusted to Tm-1 ° C or lower, where Tm corresponds to the melting point of the polyolefin.
- the temperature of the heat setting can be carried out at a temperature of 131 to 135 °C, preferably (131) to (133) °C, the heat setting temperature is such
- the range is satisfied, structural stability may be secured while thermal binding properties of the porous coating layer and the porous polyolefin film may be improved, and thermal mechanical properties may be improved.
- the heat setting may be performed using a heat source directed in a direction perpendicular to the surface of the slurry coated on the porous polyolefin film.
- the binder polymer in the coated slurry is likely to be rearranged in a direction perpendicular to the surface of the porous polyolefin film.
- a coating layer structure that facilitates movement of lithium ions is formed in the porous coating layer, and the lithium ions can communicate with pores formed in the porous polyolefin film.
- the binder polymer between the particles or the binder polymer not fully bonded to the particles may also be rearranged due to recrystallization by a high temperature heat source, thereby greatly reducing the resistance by the binder polymer.
- This increased tendency for the binder polymer to be placed in the vertical direction is particularly effective in the case of a binder polymer which is not well dispersed in a solvent such as cyanoethyl polyvinyl alcohol to form a dense film on the porous polyolefin film. to be.
- the thickness of the porous coating layer thus formed is not particularly limited, but may be in the range of 0.01 to 20 ⁇ m, and the pore size and porosity are also not particularly limited, but the pore size may be in the range of 0.001 to 10 ⁇ m, and the porosity is 10 to 99%. It can be a range.
- the pore size and porosity depend mainly on the size of the particles used. For example, when using particles having a particle diameter of 1 ⁇ m or less, the pores formed also exhibit approximately 1 ⁇ m or less.
- the porous coating layer is bound to each other by the binder polymer in the state that the particles are filled and in contact with each other, thereby forming an interstitial volume between the particles, the interstitial volume between the particles ( Interstitial Volume) becomes an empty space to form pores.
- the binder polymer is attached to each other so that the particles remain bound to each other, for example, the binder polymer is connected and fixed between the particles.
- the pores of the porous coating layer is a pore formed by the interstitial volume between the particles becomes an empty space, which is applied to the particles substantially interviewed in the closed packed or densely packed by the particles (particle). It is a space defined by.
- Such a pore structure may be filled with an electrolyte solution to be injected later, and thus the filled electrolyte may provide a path through which lithium ions essential to operate a battery through pores of the porous coating layer.
- the manufacturing method of the separator according to an embodiment of the present invention unlike the conventional manufacturing method shown in Figure 1, after the plasticizer extraction process heat setting process, winding and slitting process, unwinding process It is not necessary.
- the winding process refers to a step of winding a composite separator obtained after slurry coating and heat setting on a porous polyolefin film obtained through the extrusion / extension / extraction step on a roller
- the slitting process refers to a composite separator. Refers to the step of cutting unnecessary portions of both ends during winding.
- the winding and slitting process after the heat setting of the porous polyolefin film and the unwinding process of unwinding the film wound up again for slurry coating are necessary, and again after the slurry coating and drying process, the winding and slitting process is required again. The process was followed by a final packaging step.
- the yield can be increased by preventing the problem that the porous polyolefin film is partially lost in accordance with the winding and slitting process have.
- an electrochemical device including a cathode, an anode, and a separator interposed between the cathode and the anode, wherein the separator is an electrochemical device which is a separator for the electrochemical device described above.
- Such an electrochemical device may be manufactured according to a conventional method known in the art, and for example, may be manufactured by injecting an electrolyte after assembling the separator through the aforementioned separator between the cathode and the anode. have.
- the electrode to be applied together with the separator is not particularly limited, and may be manufactured in a form in which an electrode active material is bound to an electrode current collector according to conventional methods known in the art.
- Non-limiting examples of the cathode active material of the electrode active material may be a conventional cathode active material that can be used in the cathode of the conventional electrochemical device, in particular lithium manganese oxide, lithium cobalt oxide, lithium nickel oxide, lithium iron oxide or a combination thereof It is preferable to use one lithium composite oxide.
- Non-limiting examples of anode active materials include conventional anode active materials that can be used for the anodes of conventional electrochemical devices, in particular lithium metal or lithium alloys, carbon, petroleum coke, activated carbon, Lithium adsorbents such as graphite or other carbons are preferred.
- Non-limiting examples of the cathode current collector is a foil made by aluminum, nickel or a combination thereof, and non-limiting examples of the anode current collector by copper, gold, nickel or a copper alloy or a combination thereof. Foils produced.
- Electrolyte that may be used in one embodiment of the present invention is A + B - A salt of the structure, such as, A + comprises a Li +, Na +, an alkali metal cation or an ion composed of a combination thereof, such as K + B - it is PF 6 -, BF 4 -, Cl -, Br -, I -, ClO 4 -, AsF 6 -, CH 3 CO 2 -, CF 3 SO 3 -, N (CF 3 SO 2) 2 -, C Salts containing ions consisting of anions such as (CF 2 SO 2 ) 3 - or a combination thereof are propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC), dipropyl Carbonate (DPC), dimethylsulfoxide, acetonitrile, dimethoxyethane, diethoxyethane, tetrahydrofuran, N-methyl-2-pyrrolidone (N
- the electrolyte injection may be performed at an appropriate stage of the battery manufacturing process, depending on the manufacturing process and the required physical properties of the final product. That is, it may be applied before the battery assembly or at the end of battery assembly.
- a lamination (stacking) and a folding process of the separator and the electrode may be performed in addition to the general winding process.
- High density polyethylene having a weight average molecular weight of 500,000 as polyolefin and liquid paraffin having a kinematic viscosity of 68.00 cSt as a plasticizer were extruded at a temperature of 210 ° C. using a weight ratio of 35:65.
- liquid paraffin, which is a plasticizer was extracted at 2 M / min using methylene chloride as an extraction solvent, thereby obtaining a porous polyolefin film having an average pore size of 0.04 mu m.
- Al 2 O 3 particles / cyanoethyl polyvinyl alcohol (Cyano resin CR-V, Shin-Etsu Chemical, Ltd.) / PVDF-HFP (LBG2, Arkema) having an average particle diameter of 0.5 ⁇ m as the slurry for forming the porous layer. , Inc.) / Acetone were prepared by mixing to have a weight ratio of 13.5 / 0.225 / 1.275 / 85.
- the slurry was coated on one surface of the porous polyolefin film completed until the plasticizer extraction process with a thickness of 3.5 ⁇ m, and then heat-fixed at 5 m / min at 132.5 ° C. to prepare a separator having a thickness of 14.5 ⁇ m with a porous coating layer.
- the porous coating layer of the obtained separator has an average pore size of 0.4 ⁇ m and an average porosity of 55%.
- a slurry for forming a porous layer As a slurry for forming a porous layer (Xeon, PX9022), organic particles composed of a crosslinked polymer compound of butyl acrylate and ethyl methacrylate having an average particle diameter of 0.5 ⁇ m, a binder (polybutyl acrylate), and a dispersant (carboxymethyl cellulose ) And a solvent prepared with ultrapure water at a weight ratio of 18 / 1.5 / 0.5 / 80, and coating was performed on both sides of the porous polyethylene film with a coating thickness of 4.0 ⁇ m, except that the heat setting temperature was 133 ° C.
- a separator for an electrochemical device was prepared in the same manner as in Example 1.
- the porous coating layer of the obtained separator has an average pore size of 0.5 ⁇ m and an average porosity of 61%.
- Example 2 After heat-setting the same polyolefin film as used in Example 1 at 130 ° C., the same slurry for forming a porous coating layer as used in Example 1 was coated on one surface thereof with a thickness of 3.5 ⁇ m, and then 70 M / min at 70 ° C. It was dried under the conditions to prepare a separator for an electrochemical device.
- Example 2 After heat-setting the same porous polyolefin film as used in Example 2 at 130 ° C., the slurry used in Example 2 and the slurry for forming the porous coating layer were coated on both sides with a thickness of 4.0 ⁇ m, and then at 70 ° C. A separator for an electrochemical device was prepared by drying under the condition of 5 M / min.
- Example 2 After heat-setting the same polyolefin film used in Example 1 at 130 ° C., the same slurry for forming a porous coating layer as used in Example 1 was coated on one surface thereof to a thickness of 3.5 ⁇ m, and 5 M / min at 132.5 ° C. Heat-setting was again performed under the conditions to prepare a separator for an electrochemical device.
- Extrusion was carried out at 210 ° C. in the same manner as used in Example 1, followed by annealing at 110 ° C.
- the same porous coating layer forming slurry as used in Example 1 was coated on the annealed film to a thickness of 3.5 ⁇ m, and stretched at 115 ° C. at a magnification of 7 times. Thereafter, the extraction was performed in the same manner as in Example 1, and heat-setting was again performed at 132.5 ° C. under the condition of 5 M / min to prepare a separator for an electrochemical device.
- the separator prepared as described above was uncoated to be used as a separator because the coating layer was peeled off while being stretched after coating.
- Example 1 (Existing Process: Heat Setting ⁇ Coating)
- Example 1 (Improvement process: coating ⁇ heat setting) division fabric Composite membrane Composite membrane Oven Opening oven Coating Drying Oven Opening oven Oven length M 5 5
- Aeration time Sec / 100ml 170 240 200 The tensile strength MD Kg / cm 2 1800 1800 2300 TD 1700 1700 2150 Heat Shrinkage (120 °C / 1hr) MD Kg / cm 2 10 7 6 TD 10 5 3 Moisture Content (120 °C / 5min) ppm - 825 770
- Example 1 when comparing the Example 1 and Comparative Example 1 using the same raw material only in the order of the heat setting process, Example 1 is coated with a slurry containing inorganic particles after extracting the plasticizer from the polyolefin film It can be seen that the tensile strength and the heat shrinkage rate are superior to that of Comparative Example 1.
- the improvement in performance such as the improvement of tensile strength and the reduction of heat shrinkage, by performing a process of heat-setting the slurry after coating the extraction fabric, the conventional method of performing a slurry operation after performing the slurry coating after heat setting Compared with (Comparative 1), it is believed that the result is that the heat setting is performed at a higher temperature.
- the length of the heat setting oven can be further reduced, there is an advantage in space utilization, thereby not only reducing the production cost, but also due to drying at a temperature higher than 130 °C
- the low moisture content has the advantage of being applicable to batteries sensitive to moisture.
- Example 2 (Improvement process: coating ⁇ heat setting) division fabric Composite membrane Composite membrane Oven Opening oven Coating Drying Oven Opening oven Oven length M 5 5 5
- the tensile strength MD Kg / cm 2 1800 1850 2300 TD 1400 1450 1800 Heat Shrinkage (120 °C / 1hr) MD Kg / cm2 7 5 4 TD 5 3 2 Moisture Content (120 °C / 5min) ppm - 910 898
- Example 1 (Improvement process: coating ⁇ heat setting) division fabric Composite membrane Composite membrane Oven Heat setting oven Coating Drying Oven Heat setting oven Oven length M 5 5 5 One Oven temperature °C 130 132.5 132.5 Composite membrane thickness ⁇ m 11.0 14.5 14.5 Aeration time Sec / 100ml 170 255 200 The tensile strength MD Kg / cm 2 1800 1800 2300 TD 1700 1750 2150 Heat Shrinkage (120 °C / 1hr) MD Kg / cm 2 10 7 6 TD 10 4 3 Moisture Content (120 °C / 5min) ppm - 735 770
- Example 3 a composite separator was prepared under the same coating conditions as in Example 1 on one surface of a conventional 130 ° C. heat-set fabric.
- the fabric is heat-set (annealed) prior to slurry coating, the fibril binding is already completed.
- the mechanical strength and the thermal characteristics are not significantly improved because the coarse fibrillation is not easy to re-fix even if the heat setting is performed again at a temperature below Tm.
- the binding force between the porous coating layer and the porous polyolefin film is also not formed, it is difficult to exhibit excellent physical properties as in Example 1.
Abstract
Description
조건 | 비교예 1(기존공정: 열고정 → 코팅) | 실시예 1(개선공정:코팅 → 열고정) | |||
구분 | 원단 | 복합막 | 복합막 | ||
오븐 | 열고정오븐 | 코팅건조오븐 | 열고정오븐 | ||
오븐 길이 | M | 5 | 5 | 1 | |
오븐온도 | ℃ | 130 | 70 | 132.5 | |
복합 분리막 두께 | ㎛ | 11.0 | 14.5 | 14.5 | |
통기시간 | Sec/100ml | 170 | 240 | 200 | |
인장강도 | MD | Kg/cm2 | 1800 | 1800 | 2300 |
TD | 1700 | 1700 | 2150 | ||
열수축율(120℃/1hr) | MD | Kg/cm2 | 10 | 7 | 6 |
TD | 10 | 5 | 3 | ||
수분 함량(120℃/5min) | ppm | - | 825 | 770 |
조건 | 비교예 2(기존공정: 열고정 → 코팅) | 실시예 2(개선공정:코팅 → 열고정) | |||
구분 | 원단 | 복합막 | 복합막 | ||
오븐 | 열고정오븐 | 코팅건조오븐 | 열고정오븐 | ||
오븐 길이 | M | 5 | 5 | 1 | |
오븐온도 | ℃ | 130 | 70 | 133 | |
복합 분리막 두께 | ㎛ | 12.0 | 20.0 | 20.0 | |
통기시간 | Sec/100ml | 230 | 340 | 270 | |
인장강도 | MD | Kg/cm2 | 1800 | 1850 | 2300 |
TD | 1400 | 1450 | 1800 | ||
열수축율(120℃/1hr) | MD | Kg/cm2 | 7 | 5 | 4 |
TD | 5 | 3 | 2 | ||
수분 함량(120℃/5min) | ppm | - | 910 | 898 |
조건 | 비교예 3(기존공정: 열고정 →코팅) | 실시예 1(개선공정:코팅 → 열고정) | |||
구분 | 원단 | 복합막 | 복합막 | ||
오븐 | 열고정 오븐 | 코팅건조 오븐 | 열고정 오븐 | ||
오븐 길이 | M | 5 | 5 | 1 | |
오븐 온도 | ℃ | 130 | 132.5 | 132.5 | |
복합 분리막 두께 | ㎛ | 11.0 | 14.5 | 14.5 | |
통기시간 | Sec/100ml | 170 | 255 | 200 | |
인장강도 | MD | Kg/cm2 | 1800 | 1800 | 2300 |
TD | 1700 | 1750 | 2150 | ||
열수축율(120℃/1hr) | MD | Kg/cm2 | 10 | 7 | 6 |
TD | 10 | 4 | 3 | ||
수분 함량(120℃/5min) | ppm | - | 735 | 770 |
Claims (21)
- 폴리올레핀과 가소제를 함유하는 수지 조성물을 압출하는 단계;압출된 상기 수지 조성물을 연신하여 폴리올레핀 필름을 수득하는 단계;수득된 상기 폴리올레핀 필름으로부터 상기 가소제를 추출하여 다공성 폴리올레핀 필름을 수득하는 단계;상기 다공성 폴리올레핀 필름의 적어도 일 면에 다공성 코팅층 형성용 슬러리를 코팅하는 단계; 및상기 슬러리가 코팅된 다공성 폴리올레핀 필름을 열고정하여 다공성 코팅층이 형성된 복합 분리막을 수득하는 단계를 포함하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 압출된 상기 수지 조성물의 연신은 MD 방향 또는 TD 방향으로 1회 이상의 일축 연신을 하거나, MD 방향 및 TD 방향으로 1회 이상 이축 연신을 하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 열고정의 온도는, Tm - 1℃ 이하이고, 이때 Tm은 상기 폴리올레핀의 융점인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 열고정의 온도는 131℃ 내지 134℃인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 열고정은 상기 다공성 폴리올레핀 필름에 코팅된 슬러리의 표면에 대하여 수직 방향으로 향하는 열원을 이용하여 실시되는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 폴리올레핀은 폴리에틸렌; 폴리프로필렌; 폴리부틸렌; 폴리펜텐: 폴리헥센: 폴리옥텐: 에틸렌, 프로필렌, 부텐, 펜텐, 4-메틸펜텐, 헥센, 옥텐 중 1종 이상의 공중합체, 또는 이들의 혼합물을 포함하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 가소제는 파라핀 오일, 광유, 왁스, 대두유, 프탈산 에스테르류, 방향족 에테르류, 탄소수 10 내지 20개의 지방산류; 탄소수 10 내지 20개의 지방산알코올류; 및 지방산 에스테르류로 이루어진 군에서 선택되는 1종 이상을 포함하는 것을 특징으로 하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 다공성 폴리올레핀 필름의 두께는 5 내지 50 ㎛이고, 기공 크기 및 기공도는 각각 0.01 내지 50 ㎛ 및 10 내지 95%인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 다공성 코팅층 형성용 슬러리는, 무기물 입자 및 유기물 입자 중 1종 이상의 입자, 바인더 고분자 및 용매를 포함하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제9항에 있어서,상기 바인더 고분자는 폴리비닐리덴 플루오라이드-헥사플루오로프로필렌 (polyvinylidene fluoride-co-hexafluoropropylene), 폴리비닐리덴 플루오라이드-트리클로로에틸렌(polyvinylidene fluoride-co-trichloroethylene), 폴리메틸메타크릴레이트 (polymethylmethacrylate), 폴리부틸아크릴레이트(polybutylacrylate), 폴리아크릴로니트릴 (polyacrylonitrile), 폴리비닐피롤리돈 (polyvinylpyrrolidone), 폴리비닐아세테이트 (polyvinylacetate), 에틸렌 비닐 아세테이트 공중합체 (polyethylene-co-vinyl acetate), 폴리에틸렌옥사이드 (polyethylene oxide), 셀룰로오스 아세테이트 (cellulose acetate), 셀룰로오스 아세테이트 부티레이트 (cellulose acetate butyrate), 셀룰로오스 아세테이트 프로피오네이트 (cellulose acetate propionate), 시아노에틸풀루란 (cyanoethylpullulan), 시아노에틸폴리비닐알콜 (cyanoethylpolyvinylalcohol), 시아노에틸셀룰로오스 (cyanoethylcellulose), 시아노에틸수크로오스 (cyanoethylsucrose), 풀루란 (pullulan), 카르복실 메틸 셀룰로오스 (carboxyl methyl cellulose), 아크릴로니트릴스티렌부타디엔 공중합체 (acrylonitrile-styrene-butadiene copolymer), 폴리이미드(polyimide) 또는 이들의 혼합물인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제9항에 있어서,상기 무기물 입자는 유전율 상수가 5 이상, 리튬 이온 전달 능력을 갖는 무기물 입자 또는 이들의 혼합물인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제11항에 있어서,상기 유전율 상수가 5 이상인 무기물 입자가 BaTiO3, Pb(Zr,Ti)O3(PZT), Pb1-xLaxZr1-yTiyO3(PLZT), PB(Mg3Nb2/3)O3-PbTiO3(PMN-PT), 하프니아(HfO2), SrTiO3, SnO2, CeO2, MgO, NiO, CaO, ZnO, ZrO2, Y2O3, Al2O3, TiO2, SiC 또는 이들의 혼합물인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제11항에 있어서,상기 리튬 이온 전달 능력을 갖는 무기물 입자가 리튬포스페이트(Li3PO4), 리튬티타늄포스페이트(LixTiy(PO4)3, 0<x<2, 0<y<3), 리튬알루미늄티타늄포스페이트(LixAlyTiz(PO4)3, 0 <x<2, 0<y<1, 0<z<3), (LiAlTiP)xOy 계열 글래스(glass) (0<x<4, 0<y<13), 리튬란탄티타네이트(LixLayTiO3, 0<x<2, 0<y<3), 리튬게르마니움티오포스페이트(LixGeyPzSw, 0<x<4, 0<y<1, 0<z<1, 0<w<5), 리튬나이트라이드(LixNy, 0<x<4, 0<y<2), SiS2 계열 glass(LixSiySz, 0<x<3, 0<y<2, 0<z<4), P2S5 계열 glass(LixPySz, 0<x<3, 0<y<3, 0<z<7) 또는 이들의 혼합물인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제9항에 있어서,상기 유기물 입자가 폴리스티렌, 폴리에틸렌, 멜라민계 수지, 페놀계 수지, 셀룰로오스, 셀룰로오스 변성체, 폴리프로필렌, 폴리에스테르, 폴리페닐렌설파이드, 폴리아라미드, 폴리아미드이미드, 폴리이미드, 부틸아크릴레이트와 에틸메타아크릴레이트의 공중합체 또는 이들의 혼합물인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 무기물 입자 및 유기물 입자의 평균입경이 각각 독립적으로 0.001 내지 10 ㎛인 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 복합 분리막을 와인딩 및 슬리팅 하는 단계를 더 포함하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항에 있어서,상기 다공성 코팅층 형성용 슬러리를 코팅하는 단계 전에는 열고정하는 단계 및 와인딩 및 슬리팅 하는 단계를 포함하지 않는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제16항에 있어서,상기 와인딩 및 슬리팅이 완료된 복합 분리막을 포장하는 단계를 더 포함하는 것을 특징으로 하는 전기화학소자용 분리막의 제조방법.
- 제1항 내지 제18항 중 어느 한 항에 따른 방법에 의해 제조된 것을 특징으로 하는 전기화학소자용 분리막.
- 캐소드, 애노드, 및 캐소드와 애노드 사이에 개재된 분리막을 포함하는 전기화학소자에 있어서,상기 분리막은 제19항에 따른 전기화학소자용 분리막인 것을 특징으로 하는 전기화학소자.
- 제20항에 있어서,상기 전기화학소자는 리튬 이차전지인 것을 특징으로 하는 전기화학소자.
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KR20150050511A (ko) | 2015-05-08 |
EP3024061B1 (en) | 2018-12-05 |
CN105393383A (zh) | 2016-03-09 |
US10056589B2 (en) | 2018-08-21 |
EP3024061A1 (en) | 2016-05-25 |
TW201533104A (zh) | 2015-09-01 |
TWI557165B (zh) | 2016-11-11 |
JP2016523440A (ja) | 2016-08-08 |
EP3024061A4 (en) | 2017-02-22 |
JP6297685B2 (ja) | 2018-03-20 |
CN105393383B (zh) | 2019-02-01 |
US20160141574A1 (en) | 2016-05-19 |
KR101656413B1 (ko) | 2016-09-09 |
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