WO2015152075A1 - Corps stratifié barrière contre les gaz, élément de dispositif électronique, et dispositif électronique - Google Patents

Corps stratifié barrière contre les gaz, élément de dispositif électronique, et dispositif électronique Download PDF

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Publication number
WO2015152075A1
WO2015152075A1 PCT/JP2015/059726 JP2015059726W WO2015152075A1 WO 2015152075 A1 WO2015152075 A1 WO 2015152075A1 JP 2015059726 W JP2015059726 W JP 2015059726W WO 2015152075 A1 WO2015152075 A1 WO 2015152075A1
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Prior art keywords
gas barrier
layer
barrier laminate
thickness
electronic device
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PCT/JP2015/059726
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English (en)
Japanese (ja)
Inventor
渉 岩屋
公市 永元
智史 永縄
近藤　健
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リンテック株式会社
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Priority to JP2016511630A priority Critical patent/JP6544832B2/ja
Publication of WO2015152075A1 publication Critical patent/WO2015152075A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • 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
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin 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
    • 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
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/133345—Insulating layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/87—Passivation; Containers; Encapsulations
    • H10K59/873—Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/8791—Arrangements for improving contrast, e.g. preventing reflection of ambient light
    • H10K59/8792—Arrangements for improving contrast, e.g. preventing reflection of ambient light comprising light absorbing layers, e.g. black layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates
    • H10K77/111—Flexible substrates
    • 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
    • B32B2307/538—Roughness
    • 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
    • B32B2307/71—Resistive to light or to UV
    • 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
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • 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
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7246—Water vapor barrier
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Definitions

  • the present invention relates to a gas barrier laminate having a small thickness and excellent in ultraviolet blocking properties and gas barrier properties, an electronic device member comprising the gas barrier laminate, and an electronic device provided with the electronic device member.
  • Gas barrier films are widely used for liquid crystal displays and electroluminescence (EL) displays.
  • this gas barrier film a film having an ultraviolet blocking property and capable of reducing deterioration of an element or the like due to ultraviolet rays has been proposed.
  • Patent Document 1 includes a base material, an organic layer provided on the base material, and an inorganic layer provided on the organic layer, and the organic layer includes an electron beam curable resin, an ultraviolet ray, and the like.
  • a gas barrier film containing an absorber and a light stabilizer is described.
  • electronic devices have been made lighter and thinner, and gas barrier laminates used for electronic devices are also required to be thin.
  • an electron beam curable resin is used as a material for forming an organic layer containing an ultraviolet absorber or the like.
  • the reason for using an electron beam curable resin is that when an ultraviolet curable resin composition is used as a material for forming an organic layer, ultraviolet rays are absorbed by the ultraviolet absorber, so that the organic layer is sufficiently cured. It is stated that it is impossible.
  • the thickness of the organic layer is increased or the concentration of the ultraviolet absorber contained in the organic layer is increased. It was necessary to make it high.
  • a thin gas barrier laminate cannot be obtained, and in the latter case, since the ultraviolet ray is absorbed by the ultraviolet absorber, the organic layer may not be sufficiently cured.
  • the present invention has been made in view of such circumstances, and has a gas barrier laminate that is thin and excellent in ultraviolet blocking properties and gas barrier properties, a member for an electronic device comprising the gas barrier laminate, and the electronic device. It aims at providing an electronic device provided with a member.
  • the inventors of the present invention as a base material, a smoothing layer, and a gas barrier layer in which a gas barrier layer are laminated in this order, have the light transmittance at a wavelength of 360 nm as the base material.
  • the smoothing layer is made of a cured product of an ultraviolet curable resin composition, the thickness of the substrate (T 1 ), and the thickness of the smoothing layer (T 2 )
  • T 1 the thickness of the substrate
  • T 2 the thickness of the smoothing layer
  • gas barrier laminates (1) to (9), (10) electronic device members, and (11) electronic devices are provided.
  • a gas barrier laminate in which a substrate, a smoothing layer, and a gas barrier layer are laminated in this order, and the substrate comprises a resin film having a light transmittance of 3.0% or less at a wavelength of 360 nm,
  • the smoothing layer is made of a cured product of an ultraviolet curable resin composition, and the thickness of the substrate (T 1 ), the thickness of the smoothing layer (T 2 ), and the thickness of the gas barrier layer (T 3 )
  • a gas barrier laminate characterized by satisfying (1) and (2).
  • the arithmetic mean roughness (Ra) of the interface between the smoothing layer and the gas barrier layer is 5 nm or less, and the maximum cross-sectional height (Rt) of the roughness curve is 100 nm or less.
  • the substrate thickness (T 1 ) is 5 to 28 ⁇ m
  • the smoothing layer thickness (T 2 ) is 0.5 to 3 ⁇ m
  • the gas barrier layer thickness (T 3 ) is 0.05 to 0.3 ⁇ m.
  • the gas barrier laminate according to (1) The gas barrier laminate according to (1).
  • (6) The gas barrier laminate according to (1), further having a hard coat layer / base material / smoothing layer / gas barrier layer, which is a gas barrier laminate having a hard coat layer.
  • (7) The gas barrier laminate according to (1), wherein the thickness of the gas barrier laminate is 5 to 35 ⁇ m.
  • (8) The gas barrier laminate according to (1), wherein the water vapor permeability of the gas barrier laminate at a temperature of 40 ° C. and a relative humidity of 90% is 0.05 g / (m 2 ⁇ day) or less.
  • (9) The gas barrier laminate according to (1), wherein the light transmittance at a wavelength of 360 nm of the gas barrier laminate is 3.0% or less.
  • (1010) A member for an electronic device comprising the gas barrier laminate according to (1).
  • (11) An electronic device comprising the electronic device member according to (10).
  • a gas barrier laminate having a small thickness and excellent in ultraviolet blocking properties and gas barrier properties, an electronic device member comprising the gas barrier laminate, and an electronic device comprising the electronic device member.
  • Gas barrier laminate of the present invention is a gas barrier laminate in which a substrate, a smoothing layer, and a gas barrier layer are laminated in this order, and the substrate has a light transmittance at a wavelength of 360 nm.
  • the smoothing layer is made of a cured product of an ultraviolet curable resin composition
  • the thickness of the base material (T 1 ) the thickness of the smoothing layer (T 2 )
  • the thickness (T 3 ) of the gas barrier layer satisfies the above formulas (1) and (2).
  • the base material which comprises the gas-barrier laminated body of this invention consists of a resin film whose light transmittance in wavelength 360nm is 3.0% or less.
  • a resin film excellent in ultraviolet blocking properties that is, a “resin film having a light transmittance of 3.0% or less at a wavelength of 360 nm”.
  • the light transmittance at a wavelength of 360 nm of the resin film to be used is preferably 2.5% or less, and more preferably 2.0% or less.
  • the light transmittance at a wavelength of 360 nm can be measured using an ultraviolet spectrophotometer.
  • the resin film having an ultraviolet blocking property examples include a resin film containing a resin component and an ultraviolet absorber.
  • a resin component of the resin film polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyether sulfone, polyphenylene sulfide, acrylic resin, cycloolefin Based polymers, aromatic polymers, and the like.
  • These resin components can be used alone or in combination of two or more.
  • polyester, polyamide, polysulfone, polyether sulfone, polyphenylene sulfide, or cycloolefin-based polymer is more preferable, and polyester or cycloolefin-based polymer is more preferable because of excellent transparency and versatility.
  • polyester examples include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, and polyarylate.
  • cycloolefin polymers examples include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides thereof.
  • the ultraviolet absorber is not particularly limited as long as a resin film having a light transmittance of 3.0% or less at a wavelength of 360 nm can be obtained.
  • UV absorbers include salicylic acid UV absorbers such as pt-butylphenyl salicylate and p-octylphenyl salicylate; 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy Benzophenone ultraviolet absorbers such as -5-sulfobenzophenone, 2,2 ', 4,4'-tetrahydroxybenzophenone, bis (2-methoxy-4-hydroxy-5-benzoylphenyl) methane; 2- (2'- Hydroxy-5'-methylphenyl) benzotriazole, 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, 2,2'-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6- (2H-benzotriazol-2-y
  • the content of the ultraviolet absorber is preferably from 0.1 to 10% by mass, more preferably from 0.5 to 5% by mass, based on the resin component.
  • the resin film having ultraviolet blocking properties may contain various additives.
  • the additive include an antistatic agent, a stabilizer, an antioxidant, a plasticizer, a lubricant, a filler, and a color pigment. What is necessary is just to determine suitably content of these additives according to the objective.
  • the resin film having ultraviolet blocking properties can be obtained by preparing a resin composition containing a resin component and optionally various additives, and molding the resin composition into a film.
  • the forming method is not particularly limited, and a known film forming method such as a casting method or a melt extrusion method can be used.
  • the smoothing layer which comprises the gas-barrier laminated body of this invention consists of hardened
  • a smoothing layer reduces the unevenness
  • the base material contains an additive such as an ultraviolet absorber, it is possible to prevent these additives from bleeding out and diffusing into the gas barrier layer by providing a smoothing layer. The performance degradation can be avoided.
  • the ultraviolet curable resin composition usually contains a polymerizable compound and a photopolymerization initiator.
  • the polymerizable compound include polymerizable prepolymers and polymerizable monomers.
  • the polymerizable prepolymer includes a polyester oligomer having a hydroxyl group at both ends, a polyester acrylate prepolymer obtained by a reaction with (meth) acrylic acid, a low molecular weight bisphenol type epoxy resin or a novolac type epoxy resin, ) By reaction of epoxy acrylate prepolymer, polyurethane oligomer obtained by reaction with acrylic acid, urethane acrylate prepolymer, polyether polyol obtained by reaction of (meth) acrylic acid, and (meth) acrylic acid Examples thereof include a polyol acrylate prepolymer to be obtained.
  • Examples of the polymerizable monomer include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, and hydroxypivalic acid.
  • the active energy ray-curable resin composition may contain a polymer resin component that does not have reaction curability, such as an acrylic resin.
  • the viscosity of the composition can be adjusted by adding a polymer resin component.
  • a photoinitiator will not be specifically limited if a polymerization reaction is started by irradiation of an ultraviolet-ray.
  • the photopolymerization initiator include benzoin-based polymerization initiators such as benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin-n-butyl ether, and benzoin isobutyl ether; acetophenone, 4′-dimethylaminoacetophenone, 2,2 -Dimethoxy-2-phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- [ 4- (Methylthio) phenyl] -2-morpholino-propan-1-one, 2-hydroxy-1- ⁇ 4- [4- (2-hydroxy-2-methyl-propionyl) -
  • the ultraviolet curable resin composition may contain other components as long as the effects of the present invention are not hindered.
  • other components include an antistatic agent, a stabilizer, an antioxidant, a plasticizer, a lubricant, a filler, an inorganic filler, and a color pigment. What is necessary is just to determine these content suitably according to the objective.
  • the method for forming the smoothing layer is not particularly limited.
  • an ultraviolet curable resin composition and, if necessary, a coating liquid containing a solvent is prepared, and then this coating liquid is coated on a substrate by a known method, and the obtained coating film Is cured to form a smoothing layer made of a cured product of the ultraviolet curable resin composition.
  • the solvent for the coating solution examples include aromatic hydrocarbon solvents such as benzene and toluene; ester solvents such as ethyl acetate and butyl acetate; ketone solvents such as acetone, methyl ethyl ketone and methyl isobutyl ketone; n-pentane, n- And aliphatic hydrocarbon solvents such as hexane and n-heptane; and alicyclic hydrocarbon solvents such as cyclopentane and cyclohexane. These solvents can be used alone or in combination of two or more.
  • Examples of the coating method include a bar coating method, a spin coating method, a dipping method, a roll coating, a gravure coating, a knife coating, an air knife coating, a roll knife coating, a die coating, a screen printing method, a spray coating, and a gravure offset method.
  • drying method When the coating film is dried, conventionally known drying methods such as hot air drying, hot roll drying, and infrared irradiation can be adopted as the drying method.
  • the drying temperature is usually in the range of 60 to 130 ° C.
  • the drying time is usually several seconds to several tens of minutes.
  • Curing of the coating film can be performed by irradiating with ultraviolet rays from the surface of the coating film (side where the substrate does not exist).
  • a light source such as an ultrahigh pressure mercury lamp, a high pressure mercury lamp, a low pressure mercury lamp, a carbon arc, a black light lamp, a metal halide lamp, or the like can be used.
  • No particular restrictions on the quantity of ultraviolet light it is usually 100mJ / cm 2 ⁇ 1,000mJ / cm 2.
  • the irradiation time is usually several seconds to several hours, and the irradiation temperature is usually room temperature (20 ° C.) to 100 ° C.
  • the arithmetic mean roughness (Ra) of the surface of the smoothing layer is preferably 5 nm or less, more preferably 0.1 to 4 nm, and the maximum cross-sectional height (Rt) of the roughness curve is preferably 100 nm or less.
  • the thickness is preferably 1 to 100 nm, more preferably 20 to 80 nm, and particularly preferably 30 to 65 nm.
  • Gas barrier layer which comprises the gas barrier laminated body of this invention is a layer which has the characteristic (gas barrier property) which suppresses permeation
  • the gas barrier layer for example, a layer obtained by subjecting an inorganic vapor deposition film or a layer containing a polymer compound (hereinafter, also referred to as “polymer layer”) to a modification treatment [in this case, the gas barrier layer is In addition, it means not only a region modified by ion implantation treatment or the like, but a “polymer layer including a modified region”. ] Etc. are mentioned.
  • the inorganic vapor deposition film examples include vapor deposition films of inorganic compounds and metals.
  • inorganic oxides such as silicon oxide, aluminum oxide, magnesium oxide, zinc oxide, indium oxide and tin oxide
  • inorganic nitrides such as silicon nitride, aluminum nitride and titanium nitride
  • inorganic carbides Inorganic sulfides
  • inorganic oxynitrides such as silicon oxynitride
  • Examples of the raw material for the metal vapor deposition film include aluminum, magnesium, zinc, and tin. These can be used singly or in combination of two or more. Among these, an inorganic vapor-deposited film using an inorganic oxide, inorganic nitride or metal as a raw material is preferable from the viewpoint of gas barrier properties, and further, an inorganic material using an inorganic oxide or inorganic nitride as a raw material from the viewpoint of transparency. A vapor deposition film is preferred.
  • a PVD (physical vapor deposition) method such as a vacuum vapor deposition method, a sputtering method, or an ion plating method, a thermal CVD (chemical vapor deposition) method, a plasma CVD method, a photo CVD method, etc.
  • the CVD method is mentioned.
  • the thickness of the inorganic vapor deposition film varies depending on the inorganic compound to be used, but is preferably in the range of 50 to 300 nm, more preferably 50 to 200 nm from the viewpoint of gas barrier properties and handling properties.
  • the polymer compound used includes silicon-containing polymer compounds such as polyorganosiloxane and polysilazane compounds, polyimide, polyamide, polyamideimide, polyphenylene ether, polyether Examples include ketones, polyether ether ketones, polyolefins, polyesters, polycarbonates, polysulfones, polyether sulfones, polyphenylene sulfides, polyarylates, acrylic resins, cycloolefin polymers, and aromatic polymers. These polymer compounds can be used alone or in combination of two or more.
  • a silicon-containing polymer compound is preferable as the polymer compound because a gas barrier layer having better gas barrier properties can be formed.
  • silicon-containing polymer compounds include polysilazane compounds, polycarbosilane compounds, polysilane compounds, and polyorganosiloxane compounds.
  • a polysilazane compound is preferable because a gas barrier layer having excellent gas barrier properties can be formed even if it is thin.
  • the polysilazane compound is a polymer compound having a repeating unit containing —Si—N— bond (silazane bond) in the molecule. Specifically, the formula (1)
  • the compound which has a repeating unit represented by these is preferable.
  • the number average molecular weight of the polysilazane compound to be used is not particularly limited, but is preferably 100 to 50,000.
  • n represents arbitrary natural numbers.
  • Rx, Ry, and Rz each independently represent a hydrogen atom, an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, unsubstituted or substituted Represents a non-hydrolyzable group such as an aryl group having a group or an alkylsilyl group;
  • alkyl group of the unsubstituted or substituted alkyl group examples include a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, a t-butyl group, Examples thereof include alkyl groups having 1 to 10 carbon atoms such as n-pentyl group, isopentyl group, neopentyl group, n-hexyl group, n-heptyl group and n-octyl group.
  • Examples of the unsubstituted or substituted cycloalkyl group include cycloalkyl groups having 3 to 10 carbon atoms such as a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, and a cycloheptyl group.
  • alkenyl group of an unsubstituted or substituted alkenyl group examples include, for example, a vinyl group, 1-propenyl group, 2-propenyl group, 1-butenyl group, 2-butenyl group, 3-butenyl group and the like having 2 to 2 carbon atoms. 10 alkenyl groups are mentioned.
  • substituents for the alkyl group, cycloalkyl group and alkenyl group include halogen atoms such as fluorine atom, chlorine atom, bromine atom and iodine atom; hydroxyl group; thiol group; epoxy group; glycidoxy group; (meth) acryloyloxy group
  • halogen atoms such as fluorine atom, chlorine atom, bromine atom and iodine atom
  • hydroxyl group such as hydroxyl group; thiol group; epoxy group; glycidoxy group; (meth) acryloyloxy group
  • An unsubstituted or substituted aryl group such as a phenyl group, a 4-methylphenyl group, and a 4-chlorophenyl group;
  • aryl group of an unsubstituted or substituted aryl group examples include aryl groups having 6 to 10 carbon atoms such as a phenyl group, a 1-naphthyl group, and a 2-naphthyl group.
  • substituent of the aryl group examples include halogen atoms such as fluorine atom, chlorine atom, bromine atom and iodine atom; alkyl groups having 1 to 6 carbon atoms such as methyl group and ethyl group; carbon numbers such as methoxy group and ethoxy group 1-6 alkoxy groups; nitro groups; cyano groups; hydroxyl groups; thiol groups; epoxy groups; glycidoxy groups; (meth) acryloyloxy groups; unsubstituted phenyl groups, 4-methylphenyl groups, 4-chlorophenyl groups, etc.
  • alkylsilyl group examples include trimethylsilyl group, triethylsilyl group, triisopropylsilyl group, tri-t-butylsilyl group, methyldiethylsilyl group, dimethylsilyl group, diethylsilyl group, methylsilyl group, and ethylsilyl group.
  • Rx, Ry, and Rz a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, or a phenyl group is preferable, and a hydrogen atom is particularly preferable.
  • Examples of the polysilazane compound having a repeating unit represented by the formula (1) include inorganic polysilazanes in which Rx, Ry, and Rz are all hydrogen atoms, and organic polysilazanes in which at least one of Rx, Ry, and Rz is not a hydrogen atom. It may be.
  • a modified polysilazane compound can also be used as the polysilazane compound.
  • the modified polysilazane include, for example, JP-A-62-195024, JP-A-2-84437, JP-A-63-81122, JP-A-1-138108, and JP-A-2-175726.
  • JP-A-5-238827, JP-A-5-238827, JP-A-6-122852, JP-A-6-306329, JP-A-6-299118, JP-A-9-31333 Examples thereof include those described in Kaihei 5-345826 and JP-A-4-63833.
  • the polysilazane compound perhydropolysilazane in which Rx, Ry, and Rz are all hydrogen atoms is preferable from the viewpoint of easy availability and the ability to form an ion-implanted layer having excellent gas barrier properties.
  • a polysilazane compound a commercially available product as a glass coating material or the like can be used as it is.
  • the polysilazane compounds can be used alone or in combination of two or more.
  • the polymer layer may contain other components in addition to the polymer compound described above as long as the object of the present invention is not impaired.
  • other components include a curing agent, an anti-aging agent, a light stabilizer, and a flame retardant.
  • the content of the polymer compound in the polymer layer is preferably 50% by mass or more and more preferably 70% by mass or more because a gas barrier layer having better gas barrier properties can be obtained.
  • the thickness of the polymer layer is not particularly limited, but is preferably in the range of 50 to 300 nm, more preferably 50 to 200 nm. In the present invention, even if the thickness of the polymer layer is nano-order, a gas barrier laminate having a sufficient gas barrier property can be obtained.
  • the method for forming the polymer layer is not particularly limited. For example, preparing a polymer layer forming solution containing at least one polymer compound, optionally other components, a solvent, etc., and then applying this polymer layer forming solution by a known method, A polymer layer can be formed by drying the obtained coating film.
  • Solvents used for the polymer layer forming solution include aromatic hydrocarbon solvents such as benzene and toluene; ester solvents such as ethyl acetate and butyl acetate; ketone solvents such as acetone, methyl ethyl ketone and methyl isobutyl ketone; n- And aliphatic hydrocarbon solvents such as pentane, n-hexane, and n-heptane; and alicyclic hydrocarbon solvents such as cyclopentane and cyclohexane. These solvents can be used alone or in combination of two or more.
  • Coating methods for the polymer layer forming solution include bar coating, spin coating, dipping, roll coating, gravure coating, knife coating, air knife coating, roll knife coating, die coating, screen printing, spray coating, and gravure. Examples include an offset method.
  • drying the formed coating film As a method for drying the formed coating film, conventionally known drying methods such as hot air drying, hot roll drying, and infrared irradiation can be employed.
  • the heating temperature is usually in the range of 60 to 130 ° C.
  • the heating time is usually several seconds to several tens of minutes.
  • Examples of the polymer layer modification treatment include ion implantation treatment, plasma treatment, and ultraviolet irradiation treatment.
  • the ion implantation process is a method of modifying the polymer layer by implanting ions into the polymer layer, as will be described later.
  • the plasma treatment is a method for modifying the polymer layer by exposing the polymer layer to plasma.
  • plasma treatment can be performed according to the method described in Japanese Patent Application Laid-Open No. 2012-106421.
  • the ultraviolet irradiation treatment is a method for modifying the polymer layer by irradiating the polymer layer with ultraviolet rays.
  • the ultraviolet modification treatment can be performed according to the method described in JP2013-226757A.
  • the ion implantation treatment is preferable because the gas barrier layer can be efficiently modified to the inside without roughening the surface of the polymer layer and more excellent in gas barrier properties.
  • ions implanted into the polymer layer ions of rare gases such as argon, helium, neon, krypton, and xenon; ions of fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, sulfur, etc .; methane, ethane, etc.
  • rare gases such as argon, helium, neon, krypton, and xenon
  • fluorocarbon hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, sulfur, etc .
  • Ion of alkane gases such as ethylene and propylene
  • Ions of alkadiene gases such as pentadiene and butadiene
  • Ions of alkyne gases such as acetylene
  • Aromatic carbonization such as benzene and toluene
  • Examples include ions of hydrogen-based gases; ions of cycloalkane-based gases such as cyclopropane; ions of cycloalkene-based gases such as cyclopentene; ions of metals; ions of organosilicon compounds. These ions can be used alone or in combination of two or more.
  • ions of rare gases such as argon, helium, neon, krypton, and xenon are preferable because ions can be more easily implanted and a gas barrier layer having better gas barrier properties can be obtained.
  • the ion implantation amount can be appropriately determined according to the purpose of use of the gas barrier laminate (necessary gas barrier properties, transparency, etc.).
  • Examples of the method of implanting ions include a method of irradiating ions accelerated by an electric field (ion beam), a method of implanting ions in plasma, and the like.
  • the latter method of implanting plasma ions is preferable because the desired barrier layer can be easily obtained.
  • plasma is generated in an atmosphere containing a plasma generation gas such as a rare gas, and a negative high voltage pulse is applied to the polymer layer, whereby ions (positive ions) in the plasma are It can be performed by injecting into the surface portion of the polymer layer.
  • a plasma generation gas such as a rare gas
  • the thickness of the region into which ions are implanted can be controlled by implantation conditions such as ion type, applied voltage, and processing time, and is determined according to the thickness of the polymer layer, the purpose of use of the laminate, etc. Usually, it is 10 to 300 nm.
  • the gas barrier laminate of the present invention comprises the base material, the smoothing layer and the gas barrier layer laminated in this order, and the thickness (T 1 ) of the base material and the thickness of the smoothing layer ( T 2 ) and the gas barrier layer thickness (T 3 ) satisfy the following formulas (1) and (2).
  • the gas barrier laminate of the present invention since a resin film having ultraviolet blocking properties is used as the substrate, it is not necessary to include an ultraviolet absorber in the smoothing layer. Therefore, since it is not necessary to increase the thickness of the smoothing layer in order to obtain sufficient ultraviolet blocking properties, the thickness of the smoothing layer can be sufficiently reduced. Moreover, since it is not necessary to laminate
  • the curability of the smoothing layer is not lowered by the absorption of ultraviolet rays by the ultraviolet absorber.
  • the smoothing layer can be sufficiently cured by irradiating ultraviolet rays, and as a result, a gas barrier laminate having excellent gas barrier properties can be obtained.
  • the lower limit value of T 1 + T 2 + T 3 is usually 5 ⁇ m.
  • the substrate thickness (T 1 ), smoothing layer thickness (T 2 ), and gas barrier layer thickness (T 3 ) are preferably 5 to 28 ⁇ m, 0.5 to 3 ⁇ m, and 0.05 to 0.3 ⁇ m, respectively. More preferably, T 1 is 20 to 28 ⁇ m, T 2 is 0.5 to 2 ⁇ m, and T 3 is 0.05 to 0.2 ⁇ m.
  • the thickness of each layer can be measured by the method described in the examples.
  • the gas barrier laminate of the present invention may have a layer other than the substrate, the smoothing layer, and the gas barrier layer.
  • layers other than the base material, the smoothing layer, and the gas barrier layer include a hard code layer, a conductor layer, a shock absorbing layer, an adhesive layer, and a process sheet.
  • the process sheet has a role of protecting the gas barrier laminate when the laminate is stored, transported, etc., and is peeled off when the gas barrier laminate is used.
  • the arrangement of these layers is not particularly limited as long as the layer configuration of the base material / smoothing layer / gas barrier layer is maintained.
  • the layer structure of the gas barrier laminate of the present invention include the following.
  • the gas barrier laminate of (ii) is the side where the smoothing layer of the base material is formed. It has a hard coat layer on the opposite surface.
  • the ultraviolet absorber can be prevented from bleeding out, and by imparting scratch resistance, it can be avoided that the ultraviolet blocking property due to the substrate being damaged is deteriorated.
  • the thickness of the hard coat layer is preferably 0.5 to 3 ⁇ m, more preferably 0.5 to 2.5 ⁇ m.
  • the gas barrier laminate of the present invention can be produced, for example, by the following method.
  • a gas barrier layer having a layer structure of base material / smoothing layer / gas barrier layer can be obtained by forming a gas barrier layer on the obtained smoothing layer using the method described above. .
  • a hard coat layer is formed on one surface of the base material, and then the other surface of the base material
  • a smoothing layer is formed using the method described above.
  • a gas barrier layer having a layer configuration of hard coat layer / base material / smoothing layer / gas barrier layer is formed on the obtained smoothing layer by forming a gas barrier layer using the method described above.
  • each layer can be formed in the order of a smoothing layer, a hard coat layer, and a gas barrier layer, or each layer can be formed in the order of a smoothing layer, a gas barrier layer, and a hard coat layer to obtain a gas barrier laminate.
  • the hard coat layer can be formed by the same method as that for forming the smoothing layer, using the same material as that of the smoothing layer.
  • the gas barrier laminate of the present invention has a layer other than the base material, the smoothing layer, the gas barrier layer, and the hard coat layer, the above-described production method can be performed by appropriately adding necessary steps. A gas barrier laminate can be obtained.
  • the thickness of the gas barrier laminate of the present invention is not particularly limited, but is preferably 5 to 35 ⁇ m, more preferably 10 to 34 ⁇ m, and still more preferably 20 to 33 ⁇ m.
  • the gas barrier layered product of the present invention is preferably 0.05g / (m 2 ⁇ day) or less, more preferably 0.04g / (m 2 ⁇ day ) Or less, and more preferably 0.03 g / (m 2 ⁇ day) or less.
  • the water vapor transmission rate can be measured by the method described in the examples.
  • the light transmittance at a wavelength of 360 nm of the gas barrier laminate of the present invention is preferably 3.0% or less, preferably 2.5% or less, and more preferably 2.0% or less.
  • the lower limit of the light transmittance is usually 0.01% or more. Since it has these characteristics, the gas barrier laminate of the present invention is excellent in gas barrier properties and ultraviolet blocking properties, and is suitably used as a member for electronic devices.
  • the electronic device member of the present invention comprises the gas barrier laminate of the present invention. Since the electronic device member of the present invention has excellent gas barrier properties, it is possible to prevent deterioration of the element due to gas such as water vapor. Moreover, since it is excellent in ultraviolet-blocking property, deterioration of the element by ultraviolet irradiation can be prevented. Therefore, the electronic device member of the present invention is suitable as a display member such as a liquid crystal display or an EL display.
  • the electronic device of the present invention includes the electronic device member of the present invention. Specific examples include a liquid crystal display, an organic EL display, an inorganic EL display, electronic paper, and a solar battery. Since the electronic device of the present invention includes the electronic device member comprising the gas barrier laminate of the present invention, it is thin, lightweight, and excellent in durability against water vapor and ultraviolet rays.
  • -Substrate (1) Polyethylene terephthalate film (manufactured by Teijin DuPont, resin film containing an ultraviolet absorber, trade name: Teijin Tetron film HB3, thickness: 25 ⁇ m, light transmittance at a wavelength of 360 nm: 1.6%)
  • -Substrate (2) Polyethylene terephthalate film (Mitsubishi Plastics, trade name: PET25 T-100, thickness: 25 ⁇ m, light transmittance at a wavelength of 360 nm: 89%)
  • Production Example 3 In Production Example 2, a smoothing layer forming solution (3) was prepared in the same manner as in Production Example 2 except that the blending amount of the ultraviolet absorber was changed to 8 parts.
  • Example 1 On the base material (1), the smoothing layer forming solution (1) obtained in Production Example 1 was applied by the bar coating method, and the obtained coating film was heated and dried at 70 ° C. for 1 minute, and then irradiated with UV light. UV light irradiation is performed using a line (high pressure mercury lamp, line speed, 20 m / min, integrated light quantity 100 mJ / cm 2 , peak intensity 1.466 W, number of passes 2 times), and a smoothing layer (1) having a thickness of 1 ⁇ m is applied. Formed.
  • a line high pressure mercury lamp, line speed, 20 m / min, integrated light quantity 100 mJ / cm 2 , peak intensity 1.466 W, number of passes 2 times
  • perhydropolysilazane manufactured by AZ Electronic Materials, trade name: AZNL110A-20
  • AZNL110A-20 perhydropolysilazane
  • the smoothing layer (1) by a spin coating method, and the resulting coating film was heated at 120 ° C. for 2 minutes.
  • a perhydropolysilazane layer was formed.
  • argon (Ar) is ion-implanted on the surface of the perhydropolysilazane layer using a plasma ion implantation apparatus to form a gas barrier layer, and the base material (1) / smoothing layer (1)
  • a gas barrier laminate 1 having a layer structure of / gas barrier layer was obtained.
  • the plasma ion implantation apparatus and plasma ion implantation conditions used for forming the gas barrier layer are as follows.
  • RF power supply Model number “RF” 56000
  • JEOL high voltage pulse power supply “PV-3-HSHV-0835”, Kurita Manufacturing Co., Ltd.
  • Plasma generated gas Ar ⁇ Gas flow rate: 100sccm ⁇ Duty ratio: 0.5% ⁇ Repetition frequency: 1000Hz ⁇ Applied voltage: -10kV ⁇ RF power supply: frequency 13.56 MHz, applied power 1000 W -Chamber internal pressure: 0.2 Pa ⁇ Pulse width: 5 ⁇ sec ⁇ Processing time (ion implantation time): 5 minutes ⁇ Conveying speed: 0.2 m / min
  • Example 2 The hard coat layer forming solution obtained in Production Example 1 was applied to the surface of the base material (1) of the gas barrier laminate 1 obtained by the method described in Example 1 by the bar coating method. After the coating film is heated and dried at 70 ° C. for 1 minute, UV light irradiation is performed using a UV light irradiation line (high pressure mercury lamp, line speed, 20 m / min, integrated light quantity 100 mJ / cm 2 , peak intensity 1.466 W, pass The gas barrier laminate 2 having a layer structure of hard coat layer / base material (1) / smoothing layer (1) / gas barrier layer was obtained by forming a hard coat layer having a thickness of 2 ⁇ m twice.
  • a UV light irradiation line high pressure mercury lamp, line speed, 20 m / min, integrated light quantity 100 mJ / cm 2 , peak intensity 1.466 W
  • Example 1 In Example 1, in place of the substrate (1), the substrate (2) / smoothing layer (1) / gas barrier layer was produced in the same manner as in Example 1 except that the substrate (2) was used. Thus, a gas barrier laminate 3 having a layer structure of was obtained.
  • Comparative Example 2 In Comparative Example 1, a smoothing layer forming solution (2) obtained in Production Example 2 was used in place of the smoothing layer forming solution (1). A gas barrier laminate 4 having a layer structure of material (2) / smoothing layer (2) / gas barrier layer was obtained.
  • Comparative Example 3 In Comparative Example 1, in place of the smoothing layer forming solution (1), the smoothing layer forming solution (3) obtained in Production Example 3 was used. A gas barrier laminate 5 having a layer structure of material (2) / smoothing layer (3) / gas barrier layer was obtained.
  • Comparative Example 4 In Comparative Example 2, the layer structure of the base material (2) / smoothing layer (2) / gas barrier layer was the same as in Comparative Example 2 except that the thickness of the smoothing layer (2) was changed to 10 ⁇ m. A gas barrier laminate 6 having the following was obtained.
  • UV transmittance The light transmittance at 360 nm of the gas barrier laminates 1 to 6 was measured using an ultraviolet / visible / near infrared spectrophotometer (UV-3600, manufactured by Shimadzu Corporation). The measurement results are shown in Table 1.
  • the gas barrier laminates 1 to 6 were subjected to an abrasion resistance test to evaluate the abrasion resistance.
  • the pencil hardness of the surface opposite to the side on which the smoothing layer and the gas barrier layer of the gas barrier laminate are laminated is JIS. Measurement was performed according to K5600-5-4, and the scratch resistance was evaluated according to the following criteria.
  • Table 1 shows the following.
  • the gas barrier laminates of Examples 1 and 2 satisfy the above formulas (1) and (2), are thin, and have excellent gas barrier properties and ultraviolet blocking properties. Furthermore, the gas barrier laminate of Example 2 has these characteristics and is excellent in scratch resistance.
  • the gas barrier laminates of Comparative Examples 1 and 2 satisfy the above-described formulas (1) and (2), but the base material does not have ultraviolet blocking properties, so that the ultraviolet blocking properties are inferior.
  • the smoothing layer contains the ultraviolet absorber
  • the gas barrier laminate of Comparative Example 2 is inferior in ultraviolet blocking property because the thickness of the smoothing layer is thin.
  • the gas barrier laminate of Comparative Example 3 is excellent in ultraviolet blocking property as a result of containing a large amount of ultraviolet absorber in the smoothing layer, but has a high water vapor transmission rate.
  • the gas barrier laminate of Comparative Example 4 is excellent in UV blocking properties, but does not satisfy the above formula (2), and the thickness of the gas barrier laminate is increased. Yes.
  • the smoothing layer is excessively thick with respect to the thickness of the base material, the gas barrier laminate may be curled.

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  • Mathematical Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Laminated Bodies (AREA)
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Abstract

La présente invention concerne un corps stratifié barrière contre les gaz, un élément de dispositif électronique qui comprend le corps stratifié barrière contre les gaz, et un dispositif électronique équipé de l'élément de dispositif électronique. Le corps stratifié barrière contre les gaz contient un matériau de base, une couche de nivellement, et une couche barrière contre les gaz qui sont stratifiées dans cet ordre, et est caractérisé en ce que : le matériau de base comprend un film de résine qui possède une transmittance de lumière à 360 nm de longueur d'onde égale ou inférieure à 3,0 % ; la couche de nivellement comprend un produit durci d'une composition de résine durcissable par rayons UV ; et l'épaisseur (T1) du matériau de base, l'épaisseur (T2) de la couche de nivellement, et l'épaisseur (T3) de la couche barrière contre les gaz satisfont à la formule (1) (Ｔ１＞Ｔ２＞Ｔ３) et à la formule (2) (Ｔ１＋Ｔ２＋Ｔ３＜３０μｍ). La présente invention propose un mince corps stratifié barrière contre les gaz qui possède des propriétés supérieures de protection contre les rayons UV et des propriétés supérieures de barrière contre les gaz, un élément de dispositif électronique qui comprend le corps stratifié barrière contre les gaz, et un dispositif électronique équipé de l'élément de dispositif électronique.
PCT/JP2015/059726 2014-03-31 2015-03-27 Corps stratifié barrière contre les gaz, élément de dispositif électronique, et dispositif électronique WO2015152075A1 (fr)

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