WO2018062253A1 - フィルム - Google Patents
フィルム Download PDFInfo
- Publication number
- WO2018062253A1 WO2018062253A1 PCT/JP2017/034911 JP2017034911W WO2018062253A1 WO 2018062253 A1 WO2018062253 A1 WO 2018062253A1 JP 2017034911 W JP2017034911 W JP 2017034911W WO 2018062253 A1 WO2018062253 A1 WO 2018062253A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- film
- copolymer
- mol
- vinylidene fluoride
- dielectric constant
- Prior art date
Links
- 230000015556 catabolic process Effects 0.000 claims abstract description 17
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical group FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 36
- 229920000642 polymer Polymers 0.000 claims description 24
- 239000003990 capacitor Substances 0.000 claims description 14
- 229920002313 fluoropolymer Polymers 0.000 claims description 11
- 239000004811 fluoropolymer Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 9
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 description 163
- 229920001577 copolymer Polymers 0.000 description 49
- 239000000178 monomer Substances 0.000 description 29
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 23
- 238000000034 method Methods 0.000 description 20
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- 239000010410 layer Substances 0.000 description 15
- 229920005989 resin Polymers 0.000 description 14
- 239000011347 resin Substances 0.000 description 14
- 239000000155 melt Substances 0.000 description 12
- 238000005259 measurement Methods 0.000 description 10
- 239000008188 pellet Substances 0.000 description 8
- 238000007740 vapor deposition Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 238000001125 extrusion Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000007334 copolymerization reaction Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 4
- 229910002113 barium titanate Inorganic materials 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- -1 polytetrafluoroethylene, tetrafluoroethylene Polymers 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 238000003851 corona treatment Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000009998 heat setting Methods 0.000 description 3
- 239000010954 inorganic particle Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000009832 plasma treatment Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 229920000193 polymethacrylate Polymers 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 3
- 239000011118 polyvinyl acetate Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000011437 continuous method Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 125000003709 fluoroalkyl group Chemical group 0.000 description 2
- 125000001475 halogen functional group Chemical group 0.000 description 2
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920006380 polyphenylene oxide Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012763 reinforcing filler Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920001218 Pullulan Polymers 0.000 description 1
- 239000004373 Pullulan Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 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
- 238000003306 harvesting Methods 0.000 description 1
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920003050 poly-cycloolefin Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B26/00—Optical devices or arrangements for the control of light using movable or deformable optical elements
- G02B26/004—Optical devices or arrangements for the control of light using movable or deformable optical elements based on a displacement or a deformation of a fluid
- G02B26/005—Optical devices or arrangements for the control of light using movable or deformable optical elements based on a displacement or a deformation of a fluid based on electrowetting
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
- H01B3/445—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds from vinylfluorides or other fluoroethylenic compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
- H01G4/186—Organic dielectrics of synthetic material, e.g. derivatives of cellulose halogenated
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/704—Piezoelectric or electrostrictive devices based on piezoelectric or electrostrictive films or coatings
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/857—Macromolecular compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/204—Di-electric
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/704—Crystalline
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/16—Capacitors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/32—Wound capacitors
Definitions
- the present invention relates to a film.
- Vinylidene fluoride homopolymer films and copolymer films of vinylidene fluoride and other monomers are known to have a high dielectric constant.
- Patent Document 1 describes a film obtained from a vinylidene fluoride resin composition comprising 95 to 30% by weight of a vinylidene fluoride resin and 5 to 70% by weight of a polyether as a film exhibiting excellent dielectric properties. ing.
- Patent Document 2 describes a high dielectric film formed using a fluororesin containing a total of 95 mol% or more of vinylidene fluoride units and tetrafluoroethylene units.
- Patent Document 3 forms a film of a tetrafluoroethylene-based resin containing vinylidene fluoride units and tetrafluoroethylene units in the range of 0/100 to 49/51 in terms of vinylidene fluoride units / tetrafluoroethylene units (molar ratio).
- a film for a film capacitor contained as a resin is described.
- An object of the present invention is to provide a film having high relative dielectric constant, volume resistivity, and dielectric breakdown strength in view of the above situation.
- the present invention is characterized in that a relative dielectric constant at a frequency of 1 kHz and 30 ° C. is 9 or more, a volume resistivity at 30 ° C. is 5E + 15 ⁇ ⁇ cm or more, and a dielectric breakdown strength is 500 V / ⁇ m or more. It is a film.
- the film preferably has a crystallinity of 60% or more.
- the film preferably has a half-value width of a crystal peak in X-ray diffraction of 0.5 to 1.5.
- the film preferably contains a polymer.
- the film preferably contains a fluoropolymer having a melting point of 180 ° C. or higher.
- the film preferably contains a fluoropolymer containing vinylidene fluoride units.
- the film preferably has a thickness of 1 to 100 ⁇ m.
- the film is preferably a high dielectric film or a piezoelectric film.
- the film can be suitably used for a film capacitor, an electrowetting device, or a piezoelectric panel.
- the film of this invention has the said structure, it has a high dielectric constant, a high volume resistivity, and a high dielectric breakdown strength.
- the film of the present invention has a relative dielectric constant of 9 or more at a frequency of 1 kHz and 30 ° C.
- the relative dielectric constant is preferably 10 or more.
- the film of the present invention has a volume resistivity at 30 ° C. of 5E + 15 ⁇ ⁇ cm or more, preferably 6E + 15 ⁇ ⁇ cm or more, more preferably 7E + 15 ⁇ ⁇ cm or more, still more preferably 8E + 15 ⁇ ⁇ cm or more, particularly preferably 9E + 15 ⁇ ⁇ cm or more. cm or more.
- the volume resistivity is most preferably 1E + 16 ⁇ ⁇ cm or more.
- the upper limit of the volume low efficiency may be 1E + 17 ⁇ ⁇ cm, or 5E + 17 ⁇ ⁇ cm.
- the volume resistivity is a sample obtained by depositing aluminum on one side of the film in a vacuum. Next, this sample was placed in a thermostatic chamber (30 ° C., 25% RH), and a voltage of 50 V / ⁇ m was applied to the sample with a digital superinsulator / microammeter, and the volume resistivity ( ⁇ ⁇ cm ).
- the film of the present invention has a dielectric breakdown strength of 500 V / ⁇ m or more, preferably 550 V / ⁇ m or more, and more preferably 600 V / ⁇ m or more.
- the dielectric breakdown strength may be 1000 V / ⁇ m or less, or 800 V / ⁇ m or less.
- the dielectric breakdown strength is measured by placing the film on the lower electrode, placing a weight of ⁇ 25 mm and a weight of 500 g as the upper electrode, increasing the voltage at both ends at 100 V / sec, and measuring the breaking voltage. The number of measurements is 50 points, the average value is calculated by removing the upper and lower 5 points, and the dielectric breakdown voltage is obtained by the value divided by the thickness.
- the film of this invention Since the film of this invention has the said structure, it has a high dielectric constant, a high volume resistivity, and a high dielectric breakdown strength. In actual operation, a high electric field of, for example, 150 V / um or more is applied to the capacitor element, but the film of the present invention is excellent in durability and insulation even in a high electric field region of 150 V / um or more, and High capacitor capacity and sufficient volume resistivity as a capacitor.
- the film of the present invention preferably has a crystallinity of 60% or more.
- As said crystallinity degree 70% or more is more preferable, and 80% or more is still more preferable.
- a plurality of the films are set in a sample holder, and this is used as a measurement sample.
- the degree of crystallinity is calculated from the area ratio of the crystalline part to the amorphous part of the diffraction spectrum obtained from the sample in the range of 10 to 40 ° with an X-ray diffractometer.
- the thickness of the film is less than 40 ⁇ m, the plurality of films are overlapped so that the total thickness is 40 ⁇ m or more.
- the film of the present invention preferably has a half-value width of a crystal peak in X-ray diffraction of 0.5 to 1.5.
- the above half width is obtained by decomposing a crystal peak and an amorphous halo from a spectrum obtained by an X-ray diffractometer using a peak separation method, and setting the height from the background to the peak top of the obtained crystal peak as h.
- the half width is calculated from the width of the crystal peak at the portion corresponding to h / 2.
- the film of the present invention preferably has a thickness of 100 ⁇ m or less, more preferably 30 ⁇ m or less, still more preferably 10 ⁇ m or less, and may be 1 ⁇ m or more.
- the thickness can be measured using a digital length measuring device.
- the thickness often used is 2 ⁇ m or more and 8 ⁇ m or less, or 2 ⁇ m or more and 5 ⁇ m or less.
- the film of the present invention preferably contains a polymer, and more preferably contains a fluoropolymer.
- the film of the present invention may be an organic film.
- Examples of the organic film include polyolefin polymers, polycycloolefin polymers, polyester polymers, polyamide polymers, polylactic acid polymers, polyimide polymers, polyetherimide polymers, urethane polymers, and epoxy polymers.
- Examples of the fluoropolymer include polytetrafluoroethylene, tetrafluoroethylene / ethylene copolymer, polyvinylidene fluoride, tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, and tetrafluoroethylene / hexafluoropropylene copolymer. It is done.
- Fluoropolymers containing vinylidene fluoride units are preferred because of their superior heat resistance and high dielectric properties. Vinylidene fluoride / tetrafluoroethylene copolymers, vinylidene fluoride / trifluoroethylene copolymers, vinylidene fluorides are preferred. / Hexafluoropropylene copolymer and vinylidene fluoride / tetrafluoroethylene / hexafluoropropylene copolymer are more preferable.
- the fluoropolymer preferably has a melting point of 180 ° C. or higher, and the upper limit may be 320 ° C. A more preferred lower limit is 190 ° C and an upper limit is 280 ° C.
- a vinylidene fluoride / tetrafluoroethylene copolymer is more preferable.
- the copolymer exhibits superior heat resistance, and the difference between the dielectric constant at low temperature and the dielectric constant at high temperature is further reduced, so that the vinylidene fluoride unit / tetrafluoroethylene unit has a molar ratio of 5 / It is preferably 95 to 95/5, more preferably 10/90 to 90/10, further preferably 10/90 to 49/51, and more preferably 20/80 or more. 45/55 or less is even more preferable.
- the copolymer preferably further contains copolymerized units of ethylenically unsaturated monomers (excluding tetrafluoroethylene and vinylidene fluoride).
- the content of copolymerized units of the ethylenically unsaturated monomer may be 0 to 50% by mole, 0 to 40% by mole, or 0 to 30% by mole, based on the total copolymerized units. %, 0 to 15 mol%, and 0 to 5 mol%.
- the ethylenically unsaturated monomer is not particularly limited as long as it is a monomer copolymerizable with tetrafluoroethylene and vinylidene fluoride, but is ethylenic represented by the following formulas (1) and (2). It is preferably at least one selected from the group consisting of unsaturated monomers.
- CF 2 CF-ORf 1 (2)
- Rf 1 represents an alkyl group having 1 to 3 carbon atoms or a fluoroalkyl group having 1 to 3 carbon atoms.
- the copolymer is 55.0-90.0 mol% tetrafluoroethylene, 5.0-44.9 mol% vinylidene fluoride, and 0.1-10.0 mol% of formula (1):
- CX 1 X 2 CX 3 (CF 2 ) n X 4 (1)
- X 1 , X 2 , X 3 and X 4 are the same or different and represent H, F or Cl, and n represents an integer of 0 to 8, provided that tetrafluoroethylene and vinylidene fluoride are substituted. except.
- the ethylenically unsaturated monomer represented by the formula (1) is CH 2 ⁇ CH—C 4 F 9 , CH 2 ⁇ CH—C. It is preferably at least one monomer selected from the group consisting of 6 F 13 and CH 2 ⁇ CF—C 3 F 6 H. More preferably, the ethylenically unsaturated monomer represented by formula (1) is CH 2 ⁇ CH—C 4 F 9 , CH 2 ⁇ CH—C 6 F 13 and CH 2 ⁇ CF—C 3 F 6 H.
- Tetrafluoroethylene having at least one monomer selected from the group consisting of 55.0 to 80.0 mol% of a copolymer, 19.5 to 44.9 mol% vinylidene fluoride, and 0.1 to 0.6 mol% of an ethylenically unsaturated monomer represented by the formula (1), It is a copolymer containing the copolymer unit of this.
- the copolymer is 58.0-85.0 mol% tetrafluoroethylene, 10.0-41.9 mol% vinylidene fluoride, and 0.1 to 5.0 mol% of an ethylenically unsaturated monomer represented by the formula (1), A copolymer containing the copolymer unit may be used.
- the copolymer is 55.0-90.0 mol% tetrafluoroethylene, 9.2-44.2 mol% vinylidene fluoride, and 0.1 to 0.8 mol% of formula (2):
- CF 2 CF-ORf 1 (2)
- Rf 1 represents an alkyl group having 1 to 3 carbon atoms or a fluoroalkyl group having 1 to 3 carbon atoms.
- Rf 1 represents an alkyl group having 1 to 3 carbon atoms or a fluoroalkyl group having 1 to 3 carbon atoms.
- the copolymer is 55.0-90.0 mol% tetrafluoroethylene, 5.0-44.8 mol% vinylidene fluoride, 0.1 to 10.0 mol% of an ethylenically unsaturated monomer represented by the formula (1), and 0.1 to 0.8 mol% of an ethylenically unsaturated monomer represented by the formula (2), It is also preferable that it is a copolymer containing these copolymer units.
- the copolymer is 58.0-85.0 mol% tetrafluoroethylene, 9.5-39.8 mol% vinylidene fluoride, 0.1 to 5.0 mol% of an ethylenically unsaturated monomer represented by the formula (1), and 0.1 to 0.5 mol% of an ethylenically unsaturated monomer represented by the formula (2), A copolymer containing the copolymer unit may be used.
- the copolymer preferably has a melt flow rate (MFR) of 0.1 to 100 g / 10 min, and more preferably 0.1 to 50 g / 10 min.
- MFR melt flow rate
- the MFR is the mass (g / 10 minutes) of the polymer flowing out per 10 minutes from a nozzle having an inner diameter of 2 mm and a length of 8 mm under a 5 kg load at 297 ° C. in accordance with ASTM D3307-01.
- the copolymer preferably has a melting point of 180 ° C. or higher, and the upper limit may be 290 ° C. A more preferred lower limit is 190 ° C and an upper limit is 280 ° C.
- the melting point is measured using a differential scanning calorimeter in accordance with ASTM D-4591 at a heating rate of 10 ° C./min, and the temperature corresponding to the peak of the obtained endothermic curve is taken as the melting point.
- the copolymer preferably has a thermal decomposition starting temperature (1% mass loss temperature) of 360 ° C. or higher. A more preferred lower limit is 370 ° C. If the said thermal decomposition start temperature is in the said range, an upper limit can be 410 degreeC, for example.
- the thermal decomposition starting temperature is a temperature at which 1% by mass of the copolymer subjected to the heating test is decomposed, and the temperature of the copolymer subjected to the heating test using a differential thermal / thermogravimetric measuring device [TG-DTA] is used. It is a value obtained by measuring the temperature when the mass is reduced by 1% by mass.
- the copolymer preferably has a storage elastic modulus (E ′) at 170 ° C. of 60 to 400 MPa as measured by dynamic viscoelasticity.
- the storage elastic modulus is a value measured at 170 ° C. by dynamic viscoelasticity measurement. More specifically, a sample having a length of 30 mm, a width of 5 mm, and a thickness of 0.25 mm with a dynamic viscoelasticity device is in tension mode. It is a value measured under the conditions of a grip width of 20 mm, a measurement temperature of 25 ° C. to 250 ° C., a heating rate of 2 ° C./min, and a frequency of 1 Hz.
- a preferable storage elastic modulus (E ′) at 170 ° C. is 80 to 350 MPa, and a more preferable storage elastic modulus (E ′) is 100 to 350 MPa.
- the molding temperature is set to a temperature 50 to 100 ° C. higher than the melting point of the copolymer, and a film molded to a thickness of 0.25 mm at a pressure of 3 MPa is cut into a length of 30 mm and a width of 5 mm. Can be created.
- the copolymer may be a fluororesin.
- the film of the present invention contains the fluoropolymer or the copolymer, it may further contain another polymer.
- Other polymers include, for example, polycarbonate (PC), polyester, polyethylene terephthalate (PET), polyethylene naphthalate (PEN), silicone resin, polyether, polyvinyl acetate, polyethylene, polypropylene (PP) to increase flexibility.
- PVdF polyvinylidene fluoride
- VdF vinylidene fluoride
- HFP hexafluoropropylene copolymer
- poly (meth) acrylate epoxy resin, polyethylene oxide, polypropylene oxide , Polyphenylene oxide (PPO), polyphenylene sulfide (PPS), polyamide (PA), polyimide (PI), polyamideimide (PAI), PC, polystyrene, polybenzimidazo Such as Le (PBI) and the like, also odd polyamide terms to supplement the high dielectric, cyano pullulan, such as copper phthalocyanine polymer.
- polymers to be combined with the above copolymer from the point of high affinity with the above copolymer, from the group consisting of PVdF, VdF / HFP copolymer, poly (meth) acrylate and polyvinyl acetate At least one polymer selected is preferred.
- PVdF and VdF / HFP copolymers are particularly preferable because they can improve the mechanical strength without impairing the dielectric constant.
- Poly (meth) acrylate and polyvinyl acetate are particularly preferable from the viewpoint of improving mechanical strength and insulation resistance.
- the mass ratio of the copolymer to the other polymer is preferably 50/50 to 99/1, and more preferably 75/25 to 99/1.
- the film of this invention can also contain a silica from the point which becomes possible to prevent blocking of a film, without impairing the mechanical strength of a film.
- the blending amount is preferably 0.01 to 10 parts by mass, more preferably 0.1 parts by mass or more, and more preferably 5 parts by mass or less with respect to 100 parts by mass of the polymer. More preferably, it is 2 parts by mass or less.
- the film of the present invention may contain high dielectric inorganic particles, reinforcing fillers, affinity improvers and the like.
- high dielectric inorganic particles examples include barium titanate oxide particles and strontium titanate oxide particles.
- the high dielectric inorganic particles are preferably blended in an amount of 10 to 200 parts by mass with respect to 100 parts by mass of the polymer.
- the dielectric constant is improved, but an increase in dielectric loss and a decrease in withstand voltage are observed. Therefore, the upper limit of the content of the barium titanate-based oxide particles is about 200 parts by mass with respect to 100 parts by mass of the polymer. Further, the content of the barium titanate-based oxide particles is preferably 10 parts by mass or more from the viewpoint of the effect of improving the dielectric constant.
- strontium titanate-based oxide particles is preferable because an increase in dielectric constant and a decrease in dielectric loss are observed. On the other hand, since the withstand voltage is lowered, it is better not to blend when an improvement in withstand voltage is required.
- Examples of the reinforcing filler include silicon carbide, silicon nitride, magnesium oxide, potassium titanate, glass, alumina, and boron compound particles or fibers.
- affinity improver examples include coupling agents, functional group-modified polyolefins, styrene-modified polyolefins, functional group-modified polystyrenes, polyacrylimides, cumylphenols, and the like within the range that does not impair the effects of the present invention. May be included. It is more preferable that these components are not included from the point of withstand voltage.
- the film of the present invention has a change rate calculated from the following equation of ⁇ 8 to + 8% from a relative permittivity A at a frequency of 1 kHz and 30 ° C. and a relative permittivity B at a frequency of 1 kHz and 150 ° C. Is preferred.
- the rate of change is more preferably ⁇ 7 to + 7%, and further preferably ⁇ 6 to + 6%.
- the rate of change may be -2.0% or less + 2.0% or more.
- Rate of change (%) (BA) / A ⁇ 100
- the film of the present invention preferably has a dielectric loss tangent of 7% or less at a frequency of 1 kHz and 150 ° C., more preferably 6% or less.
- the dielectric loss tangent is measured using an LCR meter.
- the film of the present invention preferably has a tensile elastic modulus at 25 ° C. in the longitudinal direction (MD) of 800 MPa or more, and more preferably 900 MPa or more.
- the tensile elastic modulus can be measured according to ASTM D1708.
- the film of the present invention may have an elastic modulus at 25 ° C. in the longitudinal direction (MD) of 800 MPa or more and a thickness of 100 ⁇ m or less.
- the elastic modulus is more preferably 900 MPa or more.
- the thickness is more preferably 30 ⁇ m or less, further preferably 10 ⁇ m or less, and preferably 1 ⁇ m or more.
- the film of the present invention can be suitably produced by a production method including a step of obtaining a film by melt extrusion molding a polymer and a step of obtaining a stretched film by stretching the film.
- the melt extrusion molding can be performed at 250 to 380 ° C.
- the melt extrusion molding can also be performed using a melt extrusion molding machine, and the cylinder temperature is preferably 250 to 350 ° C and the die temperature is preferably 300 to 380 ° C. It is also preferable to raise the molding temperature stepwise. For example, it is also preferable to raise the molding temperature stepwise so that the cylinder portion is 300 ° C. and then heated to 330 ° C., and the T die portion is 340 ° C.
- the manufacturing method preferably includes a step of winding the film obtained by the extrusion molding with a roll.
- the temperature of the roll is preferably 0 to 180 ° C.
- the obtained film is stretched to obtain a stretched film.
- the stretching may be biaxial stretching.
- the film is stretched in the transverse direction (TD) perpendicular to the longitudinal direction (MD).
- the stretching ratio in the biaxial stretching is preferably 2 to 10 times, more preferably 3 times or more, and further preferably 3.5 times or more, in each of MD and TD.
- the above is particularly preferable.
- the stretching temperature in the biaxial stretching is preferably 0 to 200 ° C, more preferably 40 ° C or higher, and more preferably 120 ° C or lower.
- the stretching speed in the biaxial stretching is preferably 1E + 2 to 1E + 5% / min.
- the biaxial stretching may be simultaneous biaxial stretching.
- methods such as tenter biaxial stretching and tubular biaxial stretching can be employed, and tenter biaxial stretching is preferred.
- the stretching temperature in the biaxial stretching is preferably 0 to 200 ° C, more preferably 40 ° C or higher, and more preferably 120 ° C or lower.
- the stretching speed in the simultaneous biaxial stretching is preferably 1E + 2 to 1E + 5% / min.
- the simultaneous biaxial stretching method is a method of stretching a film by grasping an end (TD side) of a roll-shaped film with a clip and extending the clip interval in both the MD direction and the TD direction.
- the stretching can be performed using a batch type or continuous type stretching machine.
- the stretching can also be performed continuously as it is from film formation by melt extrusion.
- the manufacturing method preferably includes a step of heat-setting the obtained stretched film after the stretching.
- the heat setting temperature is preferably 100 to 250 ° C., more preferably 150 ° C. or more, and more preferably 200 ° C. or less.
- the heat setting time may be short, and may be 5 minutes or less for continuous stretching.
- the film of the present invention is suitable as a high dielectric film or a piezoelectric film.
- the film of the present invention is a piezoelectric film
- the film is preferably subjected to polarization treatment.
- the polarization treatment can be performed by corona discharge.
- the film is applied using a linear electrode; or the film is needle-shaped.
- the application can be performed by using an electrode.
- Heat treatment may be performed after the polarization treatment.
- the film of the present invention can also be suitably used for a film capacitor, an electrowetting device, or a piezoelectric panel.
- the film of the present invention can be suitably used as a high dielectric film for a film capacitor.
- the film capacitor may have the film of the present invention and an electrode layer provided on at least one surface of the film.
- the structure of the film capacitor for example, a laminated type in which electrode layers and high dielectric films are alternately laminated (Japanese Patent Laid-Open Nos. 63-181411, 3-18113, etc.) or a tape-like high dielectric Winding type in which a conductive film and an electrode layer are wound (disclosed in, for example, Japanese Patent Application Laid-Open No. 60-262414 in which electrodes are not continuously laminated on a high dielectric film, or electrodes on a high dielectric film And the like disclosed in Japanese Patent Laid-Open No. 3-286514, etc.) are continuously laminated.
- a wound film capacitor that has a simple structure and is relatively easy to manufacture, and in which a wound film capacitor is formed by continuously laminating electrode layers on a highly dielectric film, it is generally highly dielectric with electrodes laminated on one side. Two films are rolled up so that the electrodes do not come into contact with each other. If necessary, the film is rolled and fixed so as not to be loosened.
- an electrode layer is not specifically limited, Generally, it is a layer which consists of conductive metals, such as aluminum, zinc, gold
- the vapor-deposited metal film is not limited to a single layer, and for example, a method of forming a semiconductor aluminum oxide layer on an aluminum layer to provide moisture resistance to form an electrode layer (for example, JP-A-2-250306) If necessary, it may be multilayered.
- the thickness of the vapor-deposited metal film is not particularly limited, but is preferably in the range of 100 to 2,000 angstrom, more preferably 200 to 1,000 angstrom. When the thickness of the deposited metal film is within this range, the capacity and strength of the capacitor are balanced, which is preferable.
- the method for forming the film is not particularly limited, and for example, a vacuum vapor deposition method, a sputtering method, an ion plating method, or the like can be employed. Usually, a vacuum deposition method is used.
- Vacuum deposition methods include, for example, the batch method for molded products, the semi-continuous method used for long products, and the air-to-air method.
- the semi-continuous method is the mainstay. Has been done.
- the semi-continuous metal vapor deposition method is a method in which after vapor deposition and winding of a metal in a vacuum system, the vacuum system is returned to the atmospheric system, and the deposited film is taken out.
- the film surface can also be pretreated with a treatment for improving adhesion, such as corona treatment or plasma treatment.
- a treatment for improving adhesion such as corona treatment or plasma treatment.
- the thickness of the metal foil is not particularly limited, but is usually in the range of 0.1 to 100 ⁇ m, preferably 1 to 50 ⁇ m, more preferably 3 to 15 ⁇ m.
- the fixing method is not particularly limited, and for example, fixing and protecting the structure may be performed simultaneously by sealing with resin or enclosing in an insulating case or the like.
- the method for connecting the lead wires is not limited, and examples thereof include welding, ultrasonic pressure welding, heat pressure welding, and fixing with an adhesive tape.
- a lead wire may be connected to the electrode before it is wound.
- the opening may be sealed with a thermosetting resin such as urethane resin or epoxy resin to prevent oxidative degradation.
- the surface tension is 24 mJ / m 2 , but if not performed, the deposition is insufficient.
- the surface tension can be increased to about 26 to 40 mJ / m 2 and the vapor deposition state is also good.
- the plasma treatment can perform the same treatment. However, if the treatment conditions are too tight and the surface tension exceeds 40 mJ / m 2 , the surface condition deteriorates and the treatment is inappropriate.
- a fuse pattern may be incorporated for the purpose of protecting the device from damage due to film defects and improving reliability. Also, depending on the fuse pattern configuration, it is possible to minimize the decrease in capacitance due to destruction.
- the deposited film is slit to a width required for the capacitor, generally about 20 mm to 150 mm, using a slitter device.
- Metallicon electrodes are formed by melting and jetting a metal such as zinc (Zn) on both end faces of the wound element. Next, after drying the element at a high temperature and reduced pressure (120 ° C., Torr, 24 hours) using a vacuum oven furnace, the lead wire or the terminal is soldered or welded. Then, it inserts in a resin case or a metal case, and seals by the fixing method shown below.
- a metal such as zinc (Zn)
- the film of the present invention can be suitably used as a high dielectric film of an electrowetting device.
- the electrowetting device includes a first electrode, a second electrode, a conductive liquid movably disposed between the first electrode and the second electrode, a first electrode, and the conductive liquid.
- the film of the present invention (high dielectric film) disposed so as to insulate the first electrode from the second electrode may be included.
- a water repellent layer may be provided on the film of the present invention.
- an insulating liquid is held between the first electrode and the second electrode, and the conductive liquid and the insulating liquid may constitute two layers.
- the electrowetting device includes an optical element, a display device (display), a variable focus lens, a light modulation device, an optical pickup device, an optical recording / reproducing device, a developing device, a droplet manipulation device, and an analytical instrument (eg, sample analysis). Therefore, it can be used for chemical, biochemical, and biological analytical instruments) in which a minute conductive liquid needs to be moved.
- the film of the present invention can be suitably used as a piezoelectric film for a piezoelectric panel.
- the piezoelectric panel may include a first electrode, a film of the present invention (piezoelectric film), and a second electrode in this order.
- the first electrode is arranged directly or indirectly on one main surface of the film
- the second electrode is arranged directly or indirectly on the other main surface of the film.
- the piezoelectric panel can be used for a touch panel.
- the touch panel can be used for an input device.
- the input device having the touch panel can input based on the touch position, the touch pressure, or both.
- the input device having the touch panel can include a position detection unit and a pressure detection unit.
- the input device can be used for electronic devices (eg, mobile phones (eg, smart phones), personal digital assistants (PDAs), tablet PCs, ATMs, automatic ticket vending machines, and car navigation systems).
- electronic devices eg, mobile phones (eg, smart phones), personal digital assistants (PDAs), tablet PCs, ATMs, automatic ticket vending machines, and car navigation systems.
- An electronic device including the input device can be operated and operated based on a touch position, a touch pressure, or both.
- ferroelectrics such as energy harvesting such as vibration power generation, touch sensors, touch panels, tactile sensors, dielectric bolometers, film speakers, tactile feedback (haptics), or electrostrictive actuators. it can.
- the measurement temperature is set to (polymer melting point + 20) ° C., and 19 F-NMR measurement is performed. Depending on the integral value of each peak and the type of monomer, elemental analysis is appropriately combined. Asked.
- MFR Melt flow rate
- the film placed on the substrate was measured at room temperature using a thickness digital length measuring machine.
- a film in which a plurality of films having a degree of crystallinity of 40 ⁇ m or more are stacked is set in a sample holder and used as a measurement sample.
- the crystallinity was calculated from the area ratio of the crystalline part to the amorphous part of the diffraction spectrum obtained from the sample in the range of 10 to 40 ° with an X-ray diffractometer.
- Aluminum is vapor-deposited on both sides of the film in a relative dielectric constant vacuum to make a sample.
- the capacitance of this sample is measured with an LCR meter at 30 ° C. and a frequency of 1 kHz.
- the relative dielectric constant was calculated from each obtained capacitance.
- Aluminum is vapor-deposited on one side of the film in a volume resistivity vacuum to obtain a sample.
- this sample was placed in a thermostatic chamber (30 ° C., 25% RH), and a voltage of 50 V / ⁇ m was applied to the sample with a digital superinsulator / microammeter, and the volume resistivity ( ⁇ ⁇ cm ) was measured.
- a dielectric breakdown strength film was placed on the lower electrode, a weight of ⁇ 25 mm and a weight of 500 g was placed as the upper electrode, and the voltage was increased at both ends at 100 V / sec to measure the breakdown voltage.
- the number of measurements was 50 points, the average value was calculated by removing the upper and lower 5 points, and the dielectric breakdown strength was obtained by the value divided by the thickness.
- Example 1 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m. The film was subjected to a batch-type biaxial stretching apparatus and simultaneously stretched 3.0 times in the MD direction and 3.0 times in the TD direction to obtain a stretched film.
- Example 2 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m. The film was subjected to a batch-type biaxial stretching apparatus and simultaneously stretched 3.5 times in the MD direction and 3.5 times in the TD direction to obtain a stretched film.
- Example 3 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m. The film was subjected to a batch type biaxial stretching apparatus and simultaneously stretched 4.0 times in the MD direction and 4.0 times in the TD direction to obtain a stretched film.
- Example 4 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m.
- the film was subjected to a batch-type biaxial stretching apparatus, and simultaneously stretched 4.0 times in the MD direction and 4.0 times in the TD direction. After stretching, the film was heat-set in an atmosphere of 160 ° C. for 3 minutes to obtain a film.
- Example 5 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m. The film was subjected to a batch-type biaxial stretching apparatus and simultaneously stretched 4.5 times in the MD direction and 4.5 times in the TD direction to obtain a stretched film.
- Comparative Example 1 A pellet resin was formed into a film at 250 ° C. by a melt press to obtain a film having a film thickness of 100 ⁇ m.
- Comparative Example 2 The pellet resin was formed into a film with a melt extruder at 250 ° C. to obtain a film having a film thickness of 50 ⁇ m.
- Comparative Example 3 A vinylidene fluoride homopolymer was formed into a film by a melt extruder to obtain a film having a film thickness of 25 ⁇ m.
- Table 1 The properties and results of each pellet resin are shown in Table 1.
- Table 2 shows the measurement results of volume resistivity at 30 ° C. and 120 ° C. of Example 4 and Comparative Example 2, and their electric field dependency.
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Abstract
Description
比誘電率を高くするために、高誘電率材料を複合する方法もあるが、比誘電率の高い材料では水分吸着量が多くなり体積抵抗率の低下を引き起こす。また、主ポリマー材料と添加物の比誘電率の違いから絶縁破壊強さの低下を引き起こす為、高誘電率と体積抵抗率及び絶縁破壊強さのすべてを満足させる方法が求められていた。
上記比誘電率としては、10以上が好ましい。
上記比誘電率は、上記フィルムの表面にφ50mmのアルミ蒸着を実施し、その反対面にも全面にアルミ蒸着を実施してサンプルとし、LCRメーターを用いて容量(C)を測定し、容量、電極面積(S)、フィルムの厚み(d)から、式C=ε×ε0×S/d(ε0は真空の誘電率)で算出する値である。
上記絶縁破壊強さは、上記フィルムを下部電極に置き、上部電極としてφ25mm、重さ500gの分銅を置いて、両端に電圧を100V/secで増加させて、破壊する電圧を測定する。測定数は50点とし、上下5点を削除して平均値を算出し、厚みで除した値で絶縁破壊電圧を求める。
上記厚みは、デジタル測長機を用いて測定できる。よく使用される厚みは2μm以上8μm以下、又は2μm以上5μm以下である。
また、上記フルオロポリマーとしては、ポリテトラフルオロエチレン、テトラフルオロエチレン/エチレン共重合体、ポリフッ化ビニリデン、テトラフルオロエチレン/パーフロアルキルビニルエーテル共重合体、テトラフルオロエチレン/ヘキサフルオロプロピレン共重合体などが挙げられる。より優れた耐熱性と高誘電性を示すことから、ビニリデンフルオライド単位を含むフルオロポリマーが好ましく、ビニリデンフルオライド/テトラフルオロエチレン共重合体、ビニリデンフルオライド/トリフルオロエチレン共重合体、ビニリデンフルオライド/ヘキサフルオロプロピレン共重合体、ビニリデンフルオライド/テトラフルオロエチレン/ヘキサフルオロプロピレン共重合体がより好ましい。
上記共重合体は、より優れた耐熱性を示し、低温での誘電率と高温での誘電率との差が更に小さくなることから、ビニリデンフルオライド単位/テトラフルオロエチレン単位がモル比で5/95~95/5であることが好ましく、10/90~90/10であることがより好ましく、さらには10/90~49/51であることが好ましく、20/80以上であることがより好ましく、45/55以下であることが更により好ましい。
上記エチレン性不飽和単量体の共重合単位の含有量としては、全共重合単位に対して0~50%モル%であってよく、0~40モル%であってよく、0~30モル%であってよく、0~15モル%であってよく、0~5モル%であってよい。
(式中、X1、X2、X3及びX4は、同一又は異なって、H、F又はClを表し、nは0~8の整数を表す。但し、テトラフルオロエチレン及びビニリデンフルオライドを除く。)
(式中、Rf1は炭素数1~3のアルキル基又は炭素数1~3のフルオロアルキル基を表す。)
CH2=CF-(CF2)nX4 (3)
(式中、X4及びnは上記と同じ。)、及び、下記式(4):
CH2=CH-(CF2)nX4 (4)
(式中、X4及びnは上記と同じ。)
からなる群より選択される少なくとも1種であることが好ましく、CF2=CFCl、CH2=CFCF3、CH2=CH-C4F9、CH2=CH-C6F13、CH2=CF-C3F6H及びCF2=CFCF3からなる群より選択される少なくとも1種であることがより好ましく、CF2=CFCl、CH2=CH-C6F13及びCH2=CFCF3から選択される少なくとも1種であることが更に好ましい。
55.0~90.0モル%のテトラフルオロエチレン、
5.0~44.9モル%のビニリデンフルオライド、及び、
0.1~10.0モル%の式(1):
CX1X2=CX3(CF2)nX4 (1)
(式中、X1、X2、X3及びX4は、同一又は異なって、H、F又はClを表し、nは0~8の整数を表す。但し、テトラフルオロエチレン及びビニリデンフルオライドを除く。)
で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体であることが好ましい。
55.0~85.0モル%のテトラフルオロエチレン、
10.0~44.9モル%のビニリデンフルオライド、及び、
0.1~5.0モル%の式(1)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体である。
55.0~85.0モル%のテトラフルオロエチレン、
13.0~44.9モル%のビニリデンフルオライド、及び、
0.1~2.0モル%の式(1)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体である。
55.0~80.0モル%のテトラフルオロエチレン、
19.5~44.9モル%のビニリデンフルオライド、及び、
0.1~0.6モル%の式(1)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体であることである。
58.0~85.0モル%のテトラフルオロエチレン、
10.0~41.9モル%のビニリデンフルオライド、及び、
0.1~5.0モル%の式(1)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体であってもよい。
55.0~90.0モル%のテトラフルオロエチレン、
9.2~44.2モル%のビニリデンフルオライド、及び、
0.1~0.8モル%の式(2):
CF2=CF-ORf1 (2)
(式中、Rf1は炭素数1~3のアルキル基又は炭素数1~3のフルオロアルキル基を表す。)
で表されるエチレン性不飽和単量体、の共重合単位を含む共重合体であることも好ましい。
58.0~85.0モル%のテトラフルオロエチレン、
14.5~39.9モル%のビニリデンフルオライド、及び、
0.1~0.5モル%の式(2)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体である。
55.0~90.0モル%のテトラフルオロエチレン、
5.0~44.8モル%のビニリデンフルオライド、
0.1~10.0モル%の式(1)で表されるエチレン性不飽和単量体、及び、
0.1~0.8モル%の式(2)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体であることも好ましい。
55.0~85.0モル%のテトラフルオロエチレン、
9.5~44.8モル%のビニリデンフルオライド、
0.1~5.0モル%の式(1)で表されるエチレン性不飽和単量体、及び、
0.1~0.5モル%の式(2)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体である。
55.0~80.0モル%のテトラフルオロエチレン、
19.8~44.8モル%のビニリデンフルオライド、
0.1~2.0モル%の式(1)で表されるエチレン性不飽和単量体、及び、
0.1~0.3モル%の式(2)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体である。上記共重合体がこの組成を有する場合、低透過性に特に優れる。
58.0~85.0モル%のテトラフルオロエチレン、
9.5~39.8モル%のビニリデンフルオライド、
0.1~5.0モル%の式(1)で表されるエチレン性不飽和単量体、及び、
0.1~0.5モル%の式(2)で表されるエチレン性不飽和単量体、
の共重合単位を含む共重合体であってもよい。
測定サンプルは、例えば、成形温度を共重合体の融点より50~100℃高い温度に設定し、3MPaの圧力で厚さ0.25mmに成形したフィルムを、長さ30mm、巾5mmにカットすることで作成することができる。
変化率(%)=(B-A)/A×100
変化率(%)=(F-E)/E×100
上記誘電正接は、LCRメーターを用いて測定する。
上記引張弾性率は、ASTM D1708に準拠して測定できる。
上記溶融押出成形は、また、溶融押出成形機を使用して行うことができ、シリンダー温度を250~350℃、ダイ温度を300~380℃とすることが好ましい。また、成形温度を段階的に上げることも好ましい。例えば、シリンダー部を300℃とした後に330℃に昇温させ、Tダイ部を340℃とするように、成形温度を段階的に上げることも好ましい。
上記延伸は、二軸延伸であってもよい。
上記二軸延伸における延伸倍率は、MDおよびTDの各倍率で2~10倍であることが好ましく、3倍以上であることがより好ましく、3.5倍以上であることが更に好ましく、4倍以上であることが特に好ましい。
上記二軸延伸における延伸温度は、0~200℃であることが好ましく、40℃以上であることがより好ましく、120℃以下であることがより好ましい。
上記二軸延伸における延伸速度は、1E+2~1E+5%/分であることが好ましい。
上記二軸延伸の方法としては、テンター式二軸延伸、チューブラー式二軸延伸等の方法が採用でき、テンター式二軸延伸が好ましい。
上記二軸延伸における延伸温度は、0~200℃であることが好ましく、40℃以上であることがより好ましく、120℃以下であることがより好ましい。
上記同時二軸延伸における延伸速度は、1E+2~1E+5%/分であることが好ましい。
同時二軸延伸法は、ロール状フィルムの端部(TD側)をクリップで掴み、そのクリップ間隔がMD方向、TD方向の両方に広がることでフィルムを延伸する方法である。
上記熱固定の温度は、100~250℃であることが好ましく、150℃以上であることがより好ましく、200℃以下であることがより好ましい。熱固定時間は短時間で良く、連続延伸では5分以下で良い。
核磁気共鳴装置を用い、測定温度を(ポリマーの融点+20)℃として19F-NMR測定を行い、各ピークの積分値およびモノマーの種類によっては元素分析を適宜組み合わせて求めた。
示差走査熱量計を用い、ASTM D-4591に準拠して、昇温速度10℃/分にて熱測定を行い、得られた吸熱曲線のピークから融点を求めた。
MFRは、ASTM D3307-01に準拠し、297℃、5kg荷重下で内径2mm、長さ8mmのノズルから10分間あたりに流出するポリマーの質量(g/10分)をMFRとした。
デジタル測長機を用いて、基板に載せたフィルムを室温下にて測定した。
複数のフィルムを40μm以上になるよう重ねあわせたものをサンプルホルダーにセットしこれを測定サンプルとする。サンプルをX線回折装置にて10~40°の範囲で得られた回折スペクトルの結晶質部分と非晶質部分の面積比から結晶化度を算出した。
X線回折装置で得られたスペクトルをピーク分離法によって結晶ピークと非晶ハローを分離し、得られた結晶ピークのバックグラウンドからピークトップまでの高さをhとした際、h/2に当たる部分の結晶ピークの幅より半価幅を算出した。
真空中でフィルムの両面にアルミニウムを蒸着しサンプルとする。このサンプルをLCRメーターにて、30℃で、周波数1kHzでの静電容量を測定する。得られた各静電容量から比誘電率を算出した。
真空中でフィルムの片面にアルミニウムを蒸着しサンプルとする。次に、このサンプルを恒温槽内(30℃、25%RH)に設置してデジタル超絶縁計/微小電流計にて、50V/μmの電圧をサンプルに印加し、体積抵抗率(Ω・cm)を測定した。
フィルムを下部電極に置き、上部電極としてφ25mm、重さ500gの分銅を置いて両端に電圧を100V/secで増加させて破壊する電圧を測定した。測定数は50点とし、上下5点を削除して平均値を算出し、厚みで除した値で絶縁破壊強さを求めた。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。そのフィルムをバッチ式の二軸延伸装置にかけ、MD方向に3.0倍、TD方向に3.0倍に同時延伸して延伸フィルムを得た。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。そのフィルムをバッチ式の二軸延伸装置にかけ、MD方向に3.5倍、TD方向に3.5倍に同時延伸して延伸フィルムを得た。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。そのフィルムをバッチ式の二軸延伸装置にかけ、MD方向に4.0倍、TD方向に4.0倍に同時延伸して延伸フィルムを得た。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。そのフィルムをバッチ式の二軸延伸装置にかけ、MD方向に4.0倍、TD方向に4.0倍に同時延伸し、延伸後に160℃雰囲気下で3分間熱固定を行いフィルムを得た。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。そのフィルムをバッチ式の二軸延伸装置にかけ、MD方向に4.5倍、TD方向に4.5倍に同時延伸して延伸フィルムを得た。
ペレット樹脂を250℃で溶融プレスにて製膜し、フィルム厚100μmのフィルムを得た。
ペレット樹脂を250℃で溶融押出機にて製膜し、フィルム厚50μmのフィルムを得た。
ビニリデンフルオライド単独重合体を溶融押出機にて製膜し、フィルム厚25μmのフィルムを得た。
Claims (9)
- 周波数1kHz、30℃での比誘電率が9以上であり、
30℃での体積抵抗率が5E+15Ω・cm以上であり、
絶縁破壊強さが500V/μm以上である
ことを特徴とするフィルム。 - 結晶化度が60%以上である請求項1記載のフィルム。
- X線回折における結晶ピークの半価幅が0.5~1.5である請求項1又は2記載のフィルム。
- ポリマーを含む請求項1、2又は3記載のフィルム。
- 融点180℃以上のフルオロポリマーを含む請求項1、2、3又は4記載のフィルム。
- ビニリデンフルオライド単位を含むフルオロポリマーを含む請求項1、2、3、4又は5記載のフィルム。
- 厚みが1~100μmである請求項1、2、3、4、5又は6記載のフィルム。
- 高誘電性フィルム又は圧電フィルムである請求項1、2、3、4、5、6又は7記載のフィルム。
- フィルムコンデンサ、エレクトロウェッティングデバイス、又は、圧電パネルに使用される請求項1、2、3、4、5、6、7又は8記載のフィルム。
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CN113736195B (zh) * | 2021-09-03 | 2022-04-15 | 武汉理工大学 | 一种耐高温铁电聚合物基介电储能复合薄膜及其制备方法和应用 |
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JP2018135482A (ja) * | 2017-02-23 | 2018-08-30 | ダイキン工業株式会社 | フッ素樹脂フィルム |
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JP7245026B2 (ja) | 2017-10-31 | 2023-03-23 | 王子ホールディングス株式会社 | 樹脂フィルム、金属層一体型樹脂フィルム、及び、フィルムコンデンサ |
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Also Published As
Publication number | Publication date |
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CN109689746B (zh) | 2022-03-01 |
KR20190045245A (ko) | 2019-05-02 |
US20200032014A1 (en) | 2020-01-30 |
EP3508519A1 (en) | 2019-07-10 |
KR102282919B1 (ko) | 2021-07-28 |
EP3508519A4 (en) | 2020-05-06 |
US11479647B2 (en) | 2022-10-25 |
TWI684187B (zh) | 2020-02-01 |
JP6838609B2 (ja) | 2021-03-03 |
JPWO2018062253A1 (ja) | 2019-06-24 |
CN109689746A (zh) | 2019-04-26 |
TW201818427A (zh) | 2018-05-16 |
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