WO2017221783A1 - 積層フィルム - Google Patents
積層フィルム Download PDFInfo
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- WO2017221783A1 WO2017221783A1 PCT/JP2017/021943 JP2017021943W WO2017221783A1 WO 2017221783 A1 WO2017221783 A1 WO 2017221783A1 JP 2017021943 W JP2017021943 W JP 2017021943W WO 2017221783 A1 WO2017221783 A1 WO 2017221783A1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 235000008645 Chenopodium bonus henricus Nutrition 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000007611 bar coating method Methods 0.000 description 1
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical group C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- WLPXOECYEATUCV-UHFFFAOYSA-N cyclohexane-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1CCCC(C(Cl)=O)C1 WLPXOECYEATUCV-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- CCAFPWNGIUBUSD-UHFFFAOYSA-N diethyl sulfoxide Chemical compound CCS(=O)CC CCAFPWNGIUBUSD-UHFFFAOYSA-N 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical class O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- AJFDBNQQDYLMJN-UHFFFAOYSA-N n,n-diethylacetamide Chemical compound CCN(CC)C(C)=O AJFDBNQQDYLMJN-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000001225 nuclear magnetic resonance method Methods 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001447 polyvinyl benzene Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007761 roller coating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K5/00—Casings, cabinets or drawers for electric apparatus
- H05K5/02—Details
- H05K5/03—Covers
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
-
- 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
-
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
-
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/02—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08L101/04—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- 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
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
-
- 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
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/536—Hardness
-
- 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
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/208—Touch screens
-
- 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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- 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
- C08J2433/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
Definitions
- the present invention relates to a laminated film that can be suitably used as a display film, particularly as a cover film on the front surface of a flexible display.
- Such a display requires a film that replaces glass in order to reduce weight and prevent cracking due to bending or impact.
- a film that replaces the glass used for the front plate of the touch panel there is a demand for a film having a surface hardness that is not easily damaged, specifically a pencil hardness of 5H or more.
- Such a film needs to be compatible with not only the high transparency but also the bending resistance, which is a characteristic contrary to the above surface hardness.
- Patent Documents 1 to 4 propose a high-hardness film having a hard coat layer on a film of an acrylic resin, a polyester resin, or a triacetyl cellulose resin.
- Patent Documents 5 to 7 propose a thin film with high hardness.
- Patent Document 8 describes a wholly aromatic polyamide film. Although this is excellent in bending resistance, it cannot be said that the surface hardness of the film alone is sufficient.
- An object of the present invention is to provide a laminated film that realizes both bending resistance by expressing high surface hardness even in a thin film.
- a laminated film according to the present invention is a laminated film in which a cured layer containing a curable resin is laminated on at least one side of the film,
- the total thickness is 1-100 ⁇ m
- the light transmittance at a wavelength of 400 nm is 70% or more
- the Young's modulus when the surface of the cured layer is pushed in by 1 ⁇ m with a nanoindenter in the thickness direction is 5 GPa or more
- the deformation amount after applying a stress of 0.5 MPa for 30 minutes is 500 ppm or less.
- the present invention it is possible to provide a laminated film that realizes both bending resistance by expressing a high surface hardness even in a thin film, and can be suitably used particularly as a cover film on the front surface of a display.
- the laminated film of the present invention is a laminated film in which a layer containing a curable resin (hereinafter sometimes referred to as a cured layer) is laminated on at least one side of a base film, and the total thickness of the laminated film is 1 to 100 ⁇ m. is there.
- a layer containing a curable resin hereinafter sometimes referred to as a cured layer
- the total thickness of the laminated film is preferably from 5 to 80 ⁇ m, more preferably from the viewpoint of achieving a higher level of surface hardness and bending resistance, and more preferably from 10 to 50 ⁇ m.
- the curable resin contained in the cured layer is preferably a thermosetting resin or an ultraviolet curable resin, specifically, an organic silicone type, a polyol type, a melamine type, an epoxy type, a polyfunctional acrylate type, a urethane.
- resins such as organic resins, isocyanate resins, organic-inorganic hybrid materials which are composite materials of organic materials and inorganic materials, and silsesquioxane resins having a curable functional group. More preferred are epoxy-based, polyfunctional acrylate-based, organic-inorganic hybrid-based, and silsesquioxane-based resins. More preferred are polyfunctional acrylate-based, organic-inorganic hybrid-based, and silsesquioxane-based resins.
- polyfunctional acrylate-based and silsesquioxane-based resins used as the curable resin polyfunctional acrylate monomers, oligomers, urethane acrylate oligomers, alkoxysilanes, alkoxysilane hydrolysates, alkoxysilane oligomers, and the like are preferable.
- polyfunctional acrylate monomers include polyfunctional acrylates having two or more (meth) acryloyloxy groups in one molecule and modified polymers thereof. Specific examples include pentaerythritol tri (meth) acrylate and pentaerythritol.
- pentaerythritol triacrylate hexanemethylene diisocyanate urethane polymer can be used. These monomers can be used alone or in combination of two or more.
- Each cured layer preferably contains one or more kinds of particles.
- the particles may be either inorganic particles or organic particles, but it is preferable to contain inorganic particles in order to improve the surface hardness.
- the inorganic particles are not particularly limited, and examples thereof include metal and metalloid oxides, silicides, nitrides, borides, chlorides, and carbonates. Specifically, silica (SiO 2 ), aluminum oxide (Al 2 O 3 ), zinc oxide (ZnO), zirconium oxide (ZrO 2 ), titanium oxide (TiO 2 ), antimony oxide (Sb 2 O 3 ), and indium At least one particle selected from the group consisting of tin oxide (In 2 O 3 ) is preferred.
- the particle diameter is preferably 1 to 300 nm.
- the particle diameter is more preferably from 50 to 200 nm, and even more preferably from 100 to 150 nm, from the viewpoint that the surface hardness and the bending resistance are compatible at a higher level.
- the particles are preferably subjected to surface treatment.
- Surface treatment here refers to introducing a compound onto the particle surface by chemical bonding (including covalent bonding, hydrogen bonding ionic bonding, van der Waals bonding, hydrophobic bonding, etc.) and adsorption (including physical adsorption and chemical adsorption).
- the particle / resin mass ratio is more preferably 30/70 to 70/30, and even more preferably 40/60 to 60/40, since the surface hardness and the bending resistance are compatible at a higher level. .
- the cured layer preferably has a thickness of one side of 1 to 20 ⁇ m. More preferably, it is 1 to 10 ⁇ m. If the thickness of the hardened layer is thinner than 1 ⁇ m, the surface hardness may be lowered. Moreover, when the thickness of a hardened layer exceeds 10 micrometers, when a laminated
- the B layer is in contact with the film (A layer), and the C layer is B.
- B layer / A layer, C layer / B layer / A layer, B layer / A layer / B layer, C layer / B layer / A layer / B layer / C layer It is preferable to include any one of the laminated structures. More preferably, it includes any laminated structure of C layer / B layer / A layer, B layer / A layer / B layer, C layer / B layer / A layer / B layer / C layer.
- a method of diluting or dissolving a curable resin, particles or the like using an organic solvent, and applying the solution on a film with a metabar or a slit die can be cited. It can. Then, the cured layer of desired thickness is obtained by hardening the curable resin apply
- the curing method include thermal curing, ultraviolet irradiation, and photocuring by electron beam (EB) irradiation, but are not particularly limited.
- the organic solvent used for diluting or dissolving the curable resin is methanol, ethanol, isopropyl alcohol, acetone, methyl ethyl ketone, methyl isobutyl ketone, ethyl acetate, methyl acetate, butyl acetate, toluene, methylene chloride, butyro It is preferable that at least one is selected from cellulose.
- it may already be diluted with a solvent other than the organic solvent described above.
- concentration of an above described solvent shall be 30 mass% or more. When the concentration of the solvent is less than 30% by mass, whitening, curling, and wrinkling may occur on the film during coating.
- the laminated film preferably has an intermediate layer having a thickness of 0.5 to 6.0 ⁇ m between the base film and the cured layer, the electron density by SEM observation being different from that of the film and the cured layer.
- the difference in electron density is determined by reading the density difference of the SEM photograph with an image analyzer and binarizing it.
- middle layer expresses adhesive force between a base film and a hardened layer, and also becomes difficult to peel even when it bends repeatedly. If the intermediate layer is less than 0.5 ⁇ m, peeling may occur during repeated bending, and if it exceeds 6.0 ⁇ m, the hardness may be reduced.
- a solvent having a good solvent / poor solvent mass ratio of 15/85 to 50/50 is used as a solvent for forming the cured layer described later.
- the good solvent acetone, methyl ethyl ketone, methyl isobutyl ketone, n-methyl-2-pyrrolidone, butyrocellulose and the like are preferable
- the poor solvent ethanol, methanol, isopropyl alcohol, butyl acetate, ethyl acetate, methyl acetate, toluene And methylene chloride are preferred.
- the laminated film preferably has EA> EC and EB> EC.
- the elastic modulus of each layer is obtained by measuring the cross section of the laminate by a force volume method using an atomic force microscope (AFM).
- FAM atomic force microscope
- EA> EC and EB> EC can be achieved by using a solvent having a good solvent / poor solvent mass ratio of 15/85 to 50/50 as a solvent for forming a cured layer described later.
- a solvent having a good solvent / poor solvent mass ratio of 15/85 to 50/50 as a solvent for forming a cured layer described later.
- the good solvent acetone, methyl ethyl ketone, n-methyl-2-pyrrolidone, butyrocellulose and the like are preferable
- the poor solvent ethanol, methanol, isopropyl alcohol, butyl acetate, ethyl acetate, methyl acetate, toluene, methylene chloride and the like Is preferred.
- the laminated film preferably has an average roughness Ra of the cured layer surface of 1 to 10 nm. If Ra is less than 1 nm, the slipperiness of the surface may be poor and scratches may be formed. If Ra exceeds 10 nm, the protrusions may be shaved and scratches may occur.
- the average roughness Ra is more preferably 2 to 8 nm, and even more preferably 3 to 7 nm because scratches are less likely to be scratched.
- An average roughness Ra on the surface of the hardened layer can be 1 to 10 nm by adding particles having the above-mentioned particle diameter in the above-described content.
- the laminated film has a Young's modulus of 5 GPa or more when the surface of the cured layer is pressed by 1 ⁇ m in the thickness direction with a nanoindenter.
- the upper limit of the Young's modulus is not particularly defined, but is usually about 20 GPa. Since defects such as dents at the time of contact can be further suppressed, the Young's modulus when pushed in by 1 ⁇ m in the thickness direction with a nanoindenter is more preferably 6 GPa or more, and further preferably 7 GPa or more.
- Such Young's modulus can be achieved by using the above-described particle size and resin for the cured layer.
- the above Young's modulus is preferably satisfied for at least one of them, and it is more preferable that both the cured layers satisfy the above Young's modulus.
- the laminated film has a light transmittance of 70% or more at a wavelength of 400 nm.
- the light transmittance of light at a wavelength of 400 nm is less than 70%, the visibility may be lowered when used for a cover film.
- the upper limit of the light transmittance is 100%.
- the amount is more preferably 75% or more, and further preferably 80% or more.
- a polymer with suppressed absorption on the visible light low wavelength side for example, a polymer containing structural units represented by chemical formulas (I) to (IV) described later Can be achieved by using.
- the laminated film preferably has a yellowness (YI) of 5.0 or less. If the yellowness (YI) exceeds 5.0, the visibility may be lowered when used for a cover film. Since visibility improves more, it is more preferable that it is 4.0 or less, and it is further more preferable that it is 3.5 or less.
- the degree of yellowness (YI) can be reduced to 5.0 or less by introducing a structure in which a conjugated bond does not last long in the polymer forming the film. In particular, in the case of an aromatic system, it is preferable to introduce an electron-withdrawing substituent such as fluorine into the aromatic ring.
- the laminated film preferably has a glass transition temperature of 150 ° C. or higher. More preferably, the glass transition temperature is 200 ° C. or higher, and further preferably the glass transition temperature is 250 ° C. or higher. If the glass transition temperature is lower than 150 ° C., curling, cracking, or misalignment may occur when ITO is formed on the film for curing or when a thin film transistor (TFT) is formed.
- TFT thin film transistor
- the laminated film preferably has a haze of 5% or less. If the haze is greater than 5%, the brightness may decrease when the haze is incorporated into a display device. Since brightness becomes higher, 4% or less is more preferable, and 3% or less is more preferable. In order to reduce the haze to 5% or less, it can be achieved by reducing foreign matter in the film to reduce internal haze, smoothing the film surface, and reducing irregular reflection (external haze) on the surface.
- the laminated film preferably has a Young's modulus in at least one direction in the plane direction of the laminated film exceeding 5.0 GPa.
- the Young's modulus exceeds 5.0 GPa, not only does it contribute to improving surface hardness, but handling properties are also improved.
- the storage elastic modulus at 30 ° C. is 5.0 GPa or more. More preferably, the storage elastic modulus at 30 ° C. is 5.5 GPa or more, more preferably the storage elastic modulus at 30 ° C. is 6.0 GPa or more, and most preferably the storage elastic modulus at 30 ° C. is 7.0 GPa or more. .
- the Young's modulus in at least one direction in the plane direction of the laminated film is set to more than 5.0 GPa, for example, when a film used as a base material is formed into a laminated film by stretching in a film forming process and stretching molecular chains It is preferable because the Young's modulus can be improved.
- the draw ratio is preferably 1.05 to 10.00 times in at least one direction, and more preferably 1.05 to 8.00 times. More preferably, it is 1.05 to 5.00 times. If it is less than 1.05 times, the effect of stretching is difficult to obtain, and if it exceeds 10.00 times, the film may be broken. It is also preferable to stretch two orthogonal directions of the film.
- the laminated film has a deformation amount of 500 ppm or less after applying a stress of 0.5 MPa in at least one direction for 30 minutes. If it exceeds 500 ppm, the film may have streaks, flatness may deteriorate, or cracks may occur in the cured layer when it is repeatedly bent.
- the content is preferably 0 to 500 ppm, more preferably 0 to 300 ppm, and still more preferably 0 to 100 ppm.
- the stretching of the base film is preferably 1.05 to 10.00 times, more preferably 1.05 to 5.00 times in at least one direction. More preferably, it is 1.05 to 3.00 times. If it is less than 1.05 times, the effect of stretching is difficult to obtain, and if it exceeds 10.00 times, the film may be broken. It is also preferable to stretch two orthogonal directions of the film.
- the heat treatment temperature is preferably 250 to 340 ° C., more preferably 300 to 340 ° C.
- the polymer for the base film is preferably a polymer selected from polyamide, aromatic polyamide, and polyimide described later. For the cured layer, it is preferable to use the particles and the resin.
- a hardened layer by applying a coating made of a curable resin on a film substrate in the order of application, drying, and curing. Further, when two or more cured layers are formed on one side, it is preferably formed on a film substrate by sequential or simultaneous application.
- the sequential application means that a first cured layer is formed by applying, drying and curing one type of coating using a dip coating method, a roller coating method, a wire bar coating method, a gravure coating method or a die coating method.
- the second cured layer is formed by applying, drying and curing a coating agent different from the first type on the first cured layer.
- the simultaneous application is a method in which two or more kinds of coating agents are simultaneously applied, dried and cured using a multilayer slit die, and two or more cured layers are obtained by one application.
- Drying methods include heat transfer drying, drying with hot air, drying by infrared irradiation, drying by microwave irradiation, and drying is not particularly limited, but drying by hot air irradiation is preferable.
- Examples of the curing method include thermal curing by heat and curing by irradiating active energy rays such as an electron beam and ultraviolet rays.
- curing is preferably performed at a temperature of 23 to 200 ° C, more preferably 80 to 200 ° C.
- the oxygen concentration is preferably as low as possible, and is preferably cured in an inert gas atmosphere. If the oxygen concentration is high, curing may be insufficient.
- Examples of the ultraviolet lamp used when irradiating with ultraviolet rays include a discharge lamp method, a flash method, a laser method, and an electrodeless lamp method.
- the illuminance of the UV is preferably 100 to 3,000 mW / cm 2 , more preferably 200 to 2,000 mW / cm 2 . More preferably, it is 200 to 1,500 mW / cm 2 .
- the protective film here refers to a film having a slightly adhesive layer on at least one side. By sticking the protective film, curling that occurs when the cured layer is formed on only one surface can be suppressed, and uneven application can be suppressed when the opposite surface is applied.
- the laminated film includes a resin containing fluorine in the polymer structure in terms of achieving both light transmittance and mechanical properties such as Young's modulus in the thickness direction, and this resin is polyamide, aromatic polyamide, polyimide, aromatic polyimide, A film (base film) that is at least one resin selected from the group consisting of polyamideimide and aromatic polyamideimide is used, and a laminated film in which a cured layer is laminated on at least one side is preferable. More preferably, a polyamide or an aromatic polyamide containing fluorine in the polymer structure is used, and more preferably an aromatic polyamide containing fluorine in the polymer structure is used.
- the resin is other than polyamide, aromatic polyamide, polyimide, aromatic polyimide, polyamideimide, and aromatic polyamideimide
- the supporting force of the cured layer decreases, the Young's modulus in the thickness direction decreases, The interaction is small and the creep may increase.
- the cross-section test piece of the laminated film is made by resin embedding method or freezing method, etc., and the composition analysis is performed by infrared spectroscopic analysis (IR) using the cross-section piece. It can be confirmed whether or not fluorine is contained.
- IR infrared spectroscopic analysis
- aprotic polar solvent such as N-methyl-2-pyrrolidone (NMP) or dimethyl sulfoxide (DMSO)
- NMP N-methyl-2-pyrrolidone
- DMSO dimethyl sulfoxide
- IR infrared spectroscopy
- NMR nuclear magnetic resonance spectroscopy
- the laminated film is preferably a laminated film in which a cured layer is laminated on at least one surface of a base film containing structural units represented by the following chemical formulas (I) to (IV).
- R 1 and R 2 are —H, an aliphatic group having 1 to 5 carbon atoms, —CF 3 , —CCl 3 , —OH, —F, —Cl, —Br, —OCH 3 , a silyl group, or an aromatic ring
- a group containing Preferred is —CF 3 , —F, —Cl, or a group containing an aromatic ring.
- R 3 is a group containing Si, a group containing P, a group containing S, a halogenated hydrocarbon group, a group containing an aromatic ring, or a group containing an ether bond (however, a structure having these groups in the molecule) Units may be mixed).
- a group containing Si, a halogenated hydrocarbon group, a group containing an aromatic ring, or a group containing an ether bond is preferable. More preferably, it is a group containing Si.
- R 4 is an arbitrary group. Although not particularly limited, —H, —Cl, and —F are preferable.
- R 5 is an arbitrary aromatic group or an arbitrary alicyclic group. Although not particularly limited, phenyl, biphenyl, cyclohexane, and decalin are more preferable.
- a polyamide solution that is, a film-forming stock solution.
- a low-temperature solution polymerization method an interfacial polymerization method, a melt polymerization method, a solid-phase polymerization method, and the like can be used.
- a low temperature solution polymerization method that is, from carboxylic acid dichloride and diamine, it is synthesized in an aprotic organic polar solvent.
- Carboxylic acid dichlorides include terephthalic acid dichloride, 2-chloro-terephthalic acid dichloride, 2-fluoro-terephthalic acid dichloride, isophthalic acid dichloride, naphthalene dicarbonyl chloride, 4,4'-biphenyl dicarbonyl chloride, terphenyl dicarbonyl chloride, 1,4-cyclohexanedicarboxylic acid chloride, 1,3-cyclohexanedicarboxylic acid chloride, 2,6-decalin dicarboxylic acid chloride and the like can be mentioned, but 1,4-cyclohexanedicarboxylic acid chloride, terephthalic acid dichloride, 4,4 are preferable.
- '-Biphenyl dicarbonyl chloride, isophthalic acid dichloride, 2-chloro-terephthalic acid dichloride are used.
- diamine examples include 4,4′-diaminodiphenyl ether, 3,4′-diaminodiphenyl ether, 4,4′-diaminodiphenyl sulfone, 3,3′-diaminodiphenyl sulfone, and 2,2′-ditrifluoromethyl-4,4.
- Examples include -4,4'-diaminobiphenyl and 4,4'-diaminodiphenyl sulfone.
- Polyamide solution uses acid dichloride and diamine as monomers to produce hydrogen chloride as a by-product.
- inorganic neutralizers such as calcium hydroxide, calcium carbonate, lithium carbonate, and ethylene
- Organic neutralizers such as oxide, propylene oxide, ammonia, triethylamine, triethanolamine, diethanolamine are used.
- the reaction between isocyanate and carboxylic acid is carried out in an aprotic organic polar solvent in the presence of a catalyst.
- diamine and dicarboxylic acid dichloride When diamine and dicarboxylic acid dichloride are used as raw materials, they are amine terminals or carboxylic acid terminals depending on the composition ratio of the raw materials.
- the end capping may be performed with other amine, carboxylic acid chloride, or carboxylic acid anhydride.
- Compounds used for end-capping include benzoyl chloride, substituted benzoyl chloride, acetic anhydride, 5-norbornene-2,3-dicarboxylic anhydride, 4-ethynylaniline, 4-phenylethynylphthalic anhydride, maleic anhydride, etc. It can be illustrated.
- aprotic polar solvent used in the production of polyamide examples include sulfoxide solvents such as dimethyl sulfoxide and diethyl sulfoxide, formamide solvents such as N, N-dimethylformamide and N, N-diethylformamide, N, N -Acetamide solvents such as dimethylacetamide, N, N-diethylacetamide, pyrrolidone solvents such as N-methyl-2-pyrrolidone, N-vinyl-2-pyrrolidone, phenol, o-, m- or p-cresol, xylenol And phenolic solvents such as halogenated phenol and catechol, or hexamethylphosphoramide and ⁇ -butyrolactone, which are preferably used alone or as a mixture. Using families hydrocarbons are also possible. Furthermore, for the purpose of accelerating the dissolution of the polymer, 50% by mass or less of an alkali metal or alkaline earth metal salt can be added
- a base film made of polyamide, aromatic polyamide, or polyimide containing fluorine in the polymer structure may contain an inorganic or organic additive for the purpose of surface formation, processability improvement, and the like.
- additives for surface formation include inorganic particles such as SiO 2 , TiO 2 , Al 2 O 3 , CaSO 4 , BaSO 4 , CaCO 3 , carbon black, carbon nanotubes, fullerene, zeolite, and other metal fine powders.
- Preferred organic particles include, for example, particles made of an organic polymer such as crosslinked polyvinylbenzene, crosslinked acrylic, crosslinked polystyrene, polyester particles, polyimide particles, polyamide particles, and fluororesin particles, or the above organic polymer on the surface.
- organic polymer such as crosslinked polyvinylbenzene, crosslinked acrylic, crosslinked polystyrene, polyester particles, polyimide particles, polyamide particles, and fluororesin particles, or the above organic polymer on the surface.
- Inorganic particles that have been subjected to treatment such as coating may be mentioned.
- the film-forming stock solution prepared as described above is formed into a film by a so-called solution film-forming method.
- the solution casting method includes a dry-wet method, a dry method, a wet method, etc., and any method may be used, but here, the dry-wet method will be described as an example.
- the stock solution is extruded from a die onto a support such as a drum, an endless belt, or a support film to form a thin film, and then dried until the thin film layer has self-holding property. Drying conditions can be performed, for example, at 23 to 220 ° C. within 60 minutes. Further, the smoother the surface of the drum, endless belt, and support film used in this drying step, the smoother the surface.
- the film (sheet) that has been subjected to the dry process is peeled off from the support and introduced into the wet process, where desalting and solvent removal are performed, and further, stretching, drying, and heat treatment are performed to form a film.
- the heat treatment temperature is preferably 250 to 340 ° C., more preferably 280 to 340 ° C., and further preferably 300 to 320 ° C. in order to control mechanical properties such as creep. If it exceeds 340 ° C, the yellowness (YI) may increase.
- the heat treatment time is preferably 30 seconds or longer, more preferably 1 minute or longer, still more preferably 3 minutes or longer, more preferably 5 minutes or longer.
- the heat treatment is preferably performed in an inert atmosphere such as nitrogen or argon.
- a base film made of any one of polyamide, aromatic polyamide and polyimide containing fluorine in the polymer structure can be used as a laminated film.
- a method of laminating before a die or in a die and casting it on a support is used.
- Examples of a method of laminating in front of the die include a method of laminating using a laminating apparatus called a pinole, a composite tube, or a feed block.
- a method of laminating in the die a method using a multilayer die or a multi-manifold die can be mentioned.
- An organic solvent solution of a resin and an organic solvent solution of a polymer (resin composition) such as an aromatic polyamide often have different solution viscosities. Therefore, there is a possibility that it is difficult to obtain a good laminated structure by a method of laminating before a die such as pinol. For this reason, it is preferable to laminate using a multi-manifold base.
- the film production method is controlled in the longitudinal direction of the film (in the film-conveying direction; hereinafter referred to as MD) and in the width direction (in the longitudinal direction in the film plane). It is preferable that the film is stretched at a draw ratio of 1.05 to 10.00 times.
- the draw ratio in the MD direction is preferably 1.05 to 5.00 times, more preferably 1.05 to 3.00 times, still more preferably 1.05 to 2.00 times, and most preferably 1.05 to 1. 50 times.
- the draw ratio in the TD direction is preferably 1.05 to 5.00 times or less, more preferably 1.05 to 3.00 times, still more preferably 1.05 to 2.00 times, and most preferably 1.05 to 1. .50 times.
- the draw ratio in the TD direction is preferably 1.00 to 1.50 times the draw ratio in the MD direction. More preferably, it is 1.05 to 1.20 times, and most preferably 1.10 to 1.15 times.
- the film structure is determined by its raw materials.
- mass spectrometry analysis by a nuclear magnetic resonance method, spectroscopic analysis, or the like can be used.
- the laminated film of the present invention described above includes a display material, a display material substrate, a circuit board, a flexible printed circuit board (FPC), a photoelectric composite circuit board, an optical waveguide board, a semiconductor mounting board, a multilayer laminated circuit board, a transparent conductive film.
- Observation apparatus Electrolytic emission scanning electron microscope manufactured by JEOL Ltd. FE-SEM (JSM-6700F type) Observation magnification: 3,000 times Observation mode: LEI mode Acceleration voltage: 3 kV
- the laminate cross-sectional sample for observation was created using the following apparatus.
- Pencil hardness Using a HEIDON-14DR manufactured by Shinto Kagaku Co., Ltd., the hardness was measured at a temperature of 23 ° C. and a humidity of 65% RH. The measurement conditions are as follows. In addition, about the hardness of a pencil, it represents that it is hard in the following order shown below, 10B is the softest, and 9H is the hardest. Therefore, for example, “pencil hardness H or higher” means that the pencil hardness is any one of H, 2H, 3H,..., 9H.
- Pencil hardness 10B (soft) ... B, HB, F, H, 2H ... 9H (hard)
- Pencil hardness determination method If three of the five were intact, it was judged that the hardness was present. For example, after processing 5 scratches using H pencil, 2 scratches were confirmed, and after processing 5 scratches using 2H pencil, 3 scratches were observed If confirmed, the pencil hardness is H. Further, for example, after processing 5 scratches using a 2H pencil, if the number of scratches observed is 2 or less, the pencil hardness is determined to be at least 2H or more.
- Sample size short side 50mm x long side 100mm
- Sample installation Installation so that the position of 50 mm in the long side direction is the folding line (cylindrical contact part) Bending: 10 times
- Tr1 is the intensity of light that has passed through the sample
- Tr0 is the intensity of light that has passed through the air at the same distance except that it does not pass through the sample.
- UV measuring instrument U-3410 manufactured by Hitachi Instruments
- Wavelength range 300-800nm
- Measurement speed 120 nm / min
- Measurement mode Transmission
- Apparatus Turbidimeter NDH5000 (Nippon Denshoku Industries Co., Ltd.)
- Light source White LED 5V3W (rated)
- Light receiving element Si photodiode with V ( ⁇ ) filter
- Measurement light beam ⁇ 14 mm (incident aperture ⁇ 25 mm)
- Optical conditions Conforms to JIS-K7136 (2000)
- Viscoelasticity measuring apparatus EXSTAR6000 DMS (manufactured by Seiko Instruments Inc.) Measurement frequency: 1Hz Temperature increase rate: 5 ° C / min Temperature range: 25 to 380 ° C Holding time: 2 minutes Glass transition temperature (Tg): The temperature at the maximum peak value of Tan ⁇ was defined as the glass transition temperature.
- Viscoelasticity measuring apparatus EXSTAR6000 DMS (manufactured by Seiko Instruments Inc.) Measurement frequency: 1Hz Temperature increase rate: 5 ° C / min Temperature range: 25 to 380 ° C Retention time: 2 minutes
- Apparatus High-precision ultra-small hardness meter Tribodenter TI950 (manufactured by Hystron) Measuring method: Nano-indentation method Indenter: Diamond triangular pyramid indenter Measurement atmosphere: Room temperature / air
- Observation device scanning electron microscope FE-SEM (JSM-6700F type) manufactured by JEOL Ltd. Observation magnification: 3,000 times Observation mode: LEI mode Acceleration voltage: 3 kV
- the laminate cross-sectional sample for observation was created using the following apparatus.
- Observation device scanning probe microscope (NanoScope V Dimension Icon) manufactured by Bruker AXS Probe: Silicon cantilever Scanning mode: Force volume (contact mode) Sectioning: Cross section polisher (CP) processing
- the obtained polymer solution was cast on an endless belt having a mirror-like surface so that the final film thickness was 23 ⁇ m using a die.
- the cast polymer solution was heated with hot air at 130 ° C. for 6 minutes to evaporate the solvent, and peeled off from the endless belt while stretching 1.11 times in the longitudinal direction.
- the film which came out of the water tank was introduced into a tenter, stretched 1.29 times at 260 ° C., then relaxed 0.98 times at 340 ° C., and further heat treated at the same temperature to obtain a base film A1. It was.
- a base film A2 is formed by the same method as the base film A1, except that the thickness cast on the endless belt is increased so that the final film thickness is 40 ⁇ m. Got.
- the obtained polymer solution was cast on an endless belt having a mirror-like surface so that the final film thickness was 12.5 ⁇ m using a die.
- the cast polymer solution was heated with hot air at 130 ° C. for 6 minutes to evaporate the solvent, and peeled off from the endless belt while stretching 1.12 times in the longitudinal direction.
- the film from the water tank was introduced into a tenter, stretched 1.25 times at 260 ° C., then relaxed 0.985 times at 335 ° C., and further heat treated at the same temperature to obtain a base film A3. It was.
- the solution thus obtained was applied to a stainless steel plate and dried with hot air at 130 ° C. for 30 minutes, and then the film was peeled off from the stainless steel plate and fixed to the frame with a pin.
- the frame on which the film was fixed was placed in a vacuum oven, slowly heated from 100 ° C. to 300 ° C. for 2 hours, then gradually cooled and separated from the frame to obtain a polyamideimide film. Thereafter, as a final heat treatment step, the polyamide-imide film was further heat-treated at 300 ° C. for 30 minutes (thickness 50 ⁇ m).
- base film A5 was obtained in the same manner as the base film A4 except that the thickness applied to the stainless steel plate was such that the final film thickness was 20 ⁇ m. .
- the obtained polymer solution was cast on an endless belt having a mirror-like surface so that the final film thickness was 23 ⁇ m using a die.
- the cast polymer solution was heated with hot air of 130 ° C. for 6 minutes to evaporate the solvent, and peeled from the endless belt while stretching the length of 1.10 times. Subsequently, it introduce
- Example 1 Using the coating agent B1 on the surface of the base film A1 having a protective film having a thickness of 100 ⁇ m on one side (CT100 manufactured by Panac Co., Ltd.) that is not bonded, using a bar coater (# 6) (manufactured by Matsuo Sangyo Co., Ltd.). It was applied and dried at 100 ° C. for 2 minutes. Next, under a nitrogen atmosphere, ultraviolet rays of 320 mJ / cm 2 were irradiated to cure the coating film to obtain a film having a laminated structure of B1 layer / A1 layer / protective film.
- a protective film (CT100 manufactured by Panac Co., Ltd.) was bonded onto the B1 layer to obtain a film having a laminated structure of protective film / B1 layer / A1 layer / protective film.
- CT100 manufactured by Panac Co., Ltd.
- the protective film on the A1 layer side is peeled off, and the coating material B1 is applied onto the A1 layer using a bar coater (# 6) (manufactured by Matsuo Sangyo Co., Ltd.) and dried at 100 ° C.
- Example 2 Examples 2 to 15, Comparative Examples 2 to 4
- the base film and the curing agent coating solution were changed as shown in Table 1 or Table 2, and a laminated film with a cured layer was prepared in the same manner as in Example 1.
- Tables 1 and 2 show the results of measuring the physical properties of the obtained laminated film.
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Abstract
Description
総厚みが1~100μmであり、
波長400nmにおける光線透過率が70%以上であり、
前記硬化層の表面について厚み方向にナノインデンターで1μm押し込んだときのヤング率が5GPa以上であり、
0.5MPaの応力を30分かけた後の変形量が500ppm以下であることを特徴とするものからなる。
手法としては、フィルム基材上に硬化性樹脂からなる塗料を塗布、乾燥、硬化の順で製造することで硬化層を形成することが好ましい。また、片面に付き2層以上の硬化層を形成する際には、逐次または同時塗布によりフィルム基材上に形成することが好ましい。
芳香族ポリアミドを用いた積層体において、各層の厚みは下記の装置を用いて、積層体断面を観察し、その観察画像のスケールから各層の厚みを算出した。
観察倍率:3,000倍
観察モード:LEIモード
加速電圧:3kV
新東科学株式会社製 HEIDON-14DRを用いて、温度23℃、湿度65%RHにおいて測定した。測定条件を下記する。なお、鉛筆の硬度については、下記に示す次の順に硬いことを表し、10Bが最も柔らかく9Hが最も硬い。従って、例えば「鉛筆硬度H以上」とは、鉛筆硬度がH、2H、3H、・・・、9Hのいずれかであることを意味する。
角度:45°
傷付け速度:30mm/分
傷付け:10mm×5本
サンプル状態:ガラス板にフィルムをテープで貼り付けて実施。
鉛筆の硬度:10B(柔らかい)・・・B、HB、F、H、2H・・・9H(硬い)
鉛筆硬度決定方法:5本中、3本無傷であればその硬度を有していると判断した。例えば、Hの鉛筆を使用し5本の傷を付け処理をした後、2本の傷が確認され、次いで2Hの鉛筆を使用し5本の傷を付け処理をした後、3本の傷が確認された場合は、鉛筆硬度はHとする。また、例えば2Hの鉛筆を使用し5本の傷を付け処理をした後、観察される傷の数が2本以下である場合は、鉛筆硬度は少なくとも2H以上であると判断する。
オールグッド社製のJIS-K5600-5-1(1999)「フィルム屈曲試験」対応のマンドレルを用いて、以下のサンプルを折り曲げ、曲率半径Rを基準に判定した。
サンプル設置:長辺方向50mmの位置が折り曲げ線(円筒接触部)となるよう設置
折り曲げ:10回
良:R=2mmでキズ・筋・クラックが発生しないが、R=1mmでは発生
可:R=3mmでキズ・筋・クラックが発生しない、R=2mmでは発生
不可:R=3mmでキズ・筋・クラックが発生する
下記装置を用いて透過率を測定し、波長400nmのときの光線透過率を採用した。
透過率[%]=(Tr1/Tr0)×100
波長範囲:300~800nm
測定速度:120nm/分
測定モード:透過
分光式色彩計(日本電色工業株式会社製)を用いて、温度23℃、湿度65%RHにおいて測定した。試験片は4cm×5cmの試料を用いて、透過モードにより測定した。
下記測定器を用いて測定した。
光源:白色LED5V3W(定格)
受光素子:V(λ)フィルタ付Siフォトダイオード
測定光束:φ14mm(入射開口φ25mm)
光学条件:JIS-K7136(2000)に準拠
下記装置を用いて測定した。
測定周波数:1Hz
昇温速度:5℃/分
温度範囲:25~380℃
保持時間:2分
ガラス転移温度(Tg):Tanδの最大ピーク値の温度をガラス転移温度とした。
下記装置を用いて測定し、30℃における損失弾性(E’)を測定した。
測定周波数:1Hz
昇温速度:5℃/分
温度範囲:25~380℃
保持時間:2分
下記装置を用いて測定し、1μm押し込み時のヤング率を測定した。
測定方法:ナノインデンテーション法
使用圧子:ダイヤモンド製三角錐圧子
測定雰囲気:室温・大気
下記装置を用いて、<1><2><3>の順に張力をかけて長さを測定し、計算式にそって計算した。
サンプルサイズ:幅4mm、長さ:20mm
温度:23℃
<1>0.1MPa-30分:低張力下で初期の長さを測定
<2>0.5MPa-30分:高張力で変形を加える
<3>0.1MPa-30分:張力を取り除いた後に一定となった長さを測定
変形量(ppm)=(L2-L1)/L1×1,000,000
下記の装置を用いて、積層体断面を観察し、硬化層とフィルムの間に存在する電子密度が硬化層及びフィルムと異なる領域の厚みを計算した。
観察倍率:3,000倍
観察モード:LEIモード
加速電圧:3kV
下記の装置を用いて、AFMフォースボリューム法にて積層体断面の弾性率を測定した。測定は23℃、65%RH、大気中にて実施した。
探針:シリコンカンチレバー
走査モード:フォースボリューム(コンタクトモード)
断面出し:クロスセクションポリッシャ(CP)加工
粒子としてシリカ粒子(日産化学工業株式会社製 オルガノシリカゾル)、樹脂として多官能アクリレート(日本化薬株式会社製 KAYARAD PET30)を使用し、粒子の粒径、粒子の表面処理、溶媒を表1の通り変化させ、硬化層塗剤を作成した。
撹拌機(撹拌翼の形状は3枚後退翼)を備えた1,000Lのグラスライニング製の反応槽に、ジアミン1を19.90kg、ジアミン2を3.85kg、無水臭化リチウムを7.00kg、N-メチル-2-ピロリドンを433.00kg入れ、窒素雰囲気下で0℃に冷却、攪拌しながら30分かけて酸ジクロライド2を総量4.33kg、5回に分けて添加した。90分間攪拌した後に酸ジクロライド1を総量12.46kg、10回に分けて添加した。1時間攪拌した後、反応で発生した塩化水素を炭酸リチウムで中和して、ポリマー濃度7質量%のポリマー溶液を得た。
エンドレスベルト上に流延する厚みを、最終フィルム厚みが40μmとなるように厚くした以外は、基材フィルムA1と同様の方法で製膜し、基材フィルムA2を得た。
撹拌機(撹拌翼の形状は3枚後退翼)を備えた1,000Lのグラスライニング製の反応槽に、ジアミン1を28.40kg、無水臭化リチウムを8.00kg、N-メチル-2-ピロリドンを424.00kg入れ、窒素雰囲気下、0℃に冷却、攪拌しながら30分かけて酸ジクロライド3を総量7.22kg、12回に分けて添加した。90分間攪拌した後に酸ジクロライド1を総量10.74kg、12回に分けて添加した。1時間攪拌した後、反応で発生した塩化水素を炭酸リチウムで中和して、ポリマー濃度8質量%のポリマー溶液を得た。
反応器として、攪拌器、窒素注入装置、滴下漏斗、温度調節器および冷却器を取り付けた1.5Lの反応器に窒素を通過させながらN,N-ジメチルアセトアミド(DMAc)769gを充填し、反応器の温度を25℃に合わせた後、ジアミン1を64.046g溶解し第1溶液を得て、この第1溶液を25℃に維持した。第1溶液に酸無水物1を8.885g、及び酸無水物2を17.653g投入した後、一定の時間攪拌して溶解および反応させて第2溶液を得た。この際、第2溶液の温度は25℃に維持した。そして、酸クロライド1を24.362g添加し、固形分の濃度が13質量%のポリアミド酸溶液を得た。
ステンレス板に塗布する厚みを、最終フィルム厚みが20μmとなるようにした以外は、基材フィルムA4と同様の方法で製膜し、基材フィルムA5を得た。
反応器として、攪拌器、窒素注入装置、滴下漏斗、温度調節器および冷却器を取り付けた1.5Lの反応器に窒素を通過させながらN,N-ジメチルアセトアミド(DMAc)769gを充填し、反応器の温度を25℃に合わせた後、ジアミン3を64.046g、及びジアミン4を64.046g溶解し第1溶液を得て、この第1溶液を25℃に維持した。第1溶液に酸無水物3を8.885gを投入した後、一定の時間攪拌して溶解および反応させて第2溶液を得た。
撹拌機(撹拌翼の形状は3枚後退翼)を備えた1,000Lのグラスライニング製の反応槽に、ジアミン1を43.90kg、N-メチル-2-ピロリドンを645.70kg入れ、窒素雰囲気下、0℃に冷却、攪拌しながら30分かけて酸ジクロライド4を総量31.74kg、連続的に滴下して添加した。1時間攪拌した後、反応で発生した塩化水素を炭酸リチウムで中和して、ポリマー濃度9質量%のポリマー溶液を得た。
片面に厚み100μmの保護フィルム(パナック社製CT100)を有する基材フィルムA1の保護フィルムが貼合されていない面に、塗剤B1をバーコーター(#6)(松尾産業社製)を用いて塗布し、100℃で2分間乾燥した。次いで、窒素雰囲気下において、320mJ/cm2の紫外線を照射し塗膜を硬化させ、B1層/A1層/保護フィルムの積層構成のフィルムを得た。次いで、B1層上に保護フィルム(パナック社製CT100)を貼合し、保護フィルム/B1層/A1層/保護フィルムの積層構成のフィルムを得た。次いで、A1層側の保護フィルムを剥離し、A1層上に塗剤B1をバーコーター(#6)(松尾産業社製)を用いて塗布し、100℃で2分間乾燥させた後に、窒素雰囲気下において、320mJ/cm2の紫外線を照射し塗膜を硬化させ、保護フィルム/B1層/A1層/B1層の積層構成のフィルムを得た。最後に保護フィルムを剥離し、積層フィルムを得た。得られた積層フィルムの各物性を測定した結果を表1に示す。
実施例1において、基材フィルム及び硬化剤塗液を表1あるいは表2の通りに変更して、実施例1と同様に硬化層付き積層フィルムを作成した。得られた積層フィルムの各物性を測定した結果を表1および表2に示す。
基剤フィルム単独の特性を表2に示す。
Claims (9)
- フィルムの少なくとも片面に硬化性樹脂を含有する硬化層を積層した積層フィルムであって、
総厚みが1~100μmであり、
波長400nmにおける光線透過率が70%以上であり、
前記硬化層の表面について厚み方向にナノインデンターで1μm押し込んだときのヤング率が5GPa以上であり、
0.5MPaの応力を30分かけた後の変形量が500ppm以下であることを特徴とする積層フィルム。 - 前記光線透過率が70~100%であり、
前記ヤング率が5~20GPaであり、
前記変形量が0~500ppmである、請求項1に記載の積層フィルム。 - ガラス転移温度が150℃以上である、請求項1または2に記載の積層フィルム。
- 前記総厚みが10~50μmであり、前記硬化層の厚みが1~10μmである、請求項1~3のいずれかに記載の積層フィルム。
- フィルムと硬化層の間に、0.5μm以上6μm以下の厚みを有する中間層が設けられている、請求項1~4のいずれかに記載の積層フィルム。
- 前記硬化層の表面が、1~10nmの平均粗さRaを有する、請求項1~5のいずれかに記載の積層フィルム。
- 粘弾性測定装置を用いて30℃で測定した貯蔵弾性率が5GPa以上である、請求項1~6のいずれかに記載の積層フィルム。
- ポリマー構造中にフッ素含有樹脂を含み、該フッ素含有樹脂がポリアミド、芳香族ポリアミド、ポリイミド、芳香族ポリイミド、ポリアミイミドおよび芳香族ポリアミドイミドからなる群から選ばれる少なくとも1種の樹脂である、請求項1~7のいずれかに記載の積層フィルム。
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Also Published As
Publication number | Publication date |
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JP6939556B2 (ja) | 2021-09-22 |
EP3476592A4 (en) | 2020-02-26 |
TW201819169A (zh) | 2018-06-01 |
TWI738801B (zh) | 2021-09-11 |
CN109311287B (zh) | 2021-08-24 |
CN109311287A (zh) | 2019-02-05 |
EP3476592A1 (en) | 2019-05-01 |
KR20190021318A (ko) | 2019-03-05 |
US10751980B2 (en) | 2020-08-25 |
EP3476592B1 (en) | 2023-06-14 |
JPWO2017221783A1 (ja) | 2019-04-11 |
US20190217587A1 (en) | 2019-07-18 |
KR102417461B1 (ko) | 2022-07-06 |
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