WO2015151976A1 - Stratifié faisant barrière contre les gaz, élément pour dispositif électronique et dispositif électronique - Google Patents

Stratifié faisant barrière contre les gaz, élément pour dispositif électronique et dispositif électronique Download PDF

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Publication number
WO2015151976A1
WO2015151976A1 PCT/JP2015/059232 JP2015059232W WO2015151976A1 WO 2015151976 A1 WO2015151976 A1 WO 2015151976A1 JP 2015059232 W JP2015059232 W JP 2015059232W WO 2015151976 A1 WO2015151976 A1 WO 2015151976A1
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gas barrier
layer
optical adjustment
barrier laminate
adjustment layer
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PCT/JP2015/059232
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English (en)
Japanese (ja)
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有紀 仁藤
悠太 鈴木
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リンテック株式会社
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Priority to JP2016511589A priority Critical patent/JP6694380B2/ja
Publication of WO2015151976A1 publication Critical patent/WO2015151976A1/fr

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    • 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
    • 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
    • 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
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/402—Coloured
    • 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
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/418—Refractive
    • 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
    • B32B2457/00—Electrical equipment
    • B32B2457/12—Photovoltaic modules
    • 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

Definitions

  • the present invention relates to a gas barrier laminate excellent in gas barrier properties and colorless transparency, an electronic device member comprising the gas barrier laminate, and an electronic device including the electronic device member.
  • an inorganic compound layer (gas barrier layer) is formed on a transparent plastic film instead of a glass plate in order to achieve thinning, weight reduction, and flexibility.
  • a so-called gas barrier film is used.
  • Patent Document 1 discloses a high-oxidation degree silicon oxide layer having a value of x of SiO x of 1.8 or more on one side or both sides of a base material made of a plastic film by a dry coating method.
  • a low oxide silicon oxide layer having a value of x of SiO x of 1.0 to 1.6 is provided on the silicon oxide layer.
  • oxygen, nitrogen, argon, or helium of oxygen, nitrogen, argon, or helium is provided on the surface of the low oxide silicon oxide layer.
  • a transparent gas barrier laminated film is described in which a polymer layer is laminated on the plasma-treated surface of the low-oxidation silicon oxide layer after performing a plasma treatment with one kind or two or more kinds of gases.
  • Patent Document 2 describes a transparent gas barrier substrate in which a silicon oxynitride layer and a silicon nitride layer are laminated in this order on one surface or both surfaces of a transparent resin substrate.
  • JP 2004-351832 A Japanese Patent Laid-Open No. 2007-062305
  • the present invention has been made in view of such circumstances, and has a gas barrier laminate excellent in gas barrier properties and colorless transparency, an electronic device member comprising the gas barrier laminate, and an electronic device including the electronic device member.
  • the purpose is to provide a device.
  • the present inventors have conceived a gas barrier laminate in which an optical adjustment layer is laminated on a base material and a gas barrier layer, and intensively studied this gas barrier laminate.
  • the gas barrier layer and the optical adjustment layer are formed adjacent to each other, the gas barrier layer and the optical adjustment layer are layers having a specific refractive index, and b in the CIE L * a * b * color system.
  • a gas barrier laminate having a value in a specific range was found to be excellent in both colorless transparency and gas barrier properties, and the present invention was completed.
  • the following gas barrier laminates (1) to (8), an electronic device member (9), and an electronic device (10) are provided.
  • a base material, a gas barrier layer and an optical adjustment layer are laminated in this order, and the gas barrier layer and the optical adjustment layer are adjacent to each other, wherein the gas barrier layer has a refractive index of 1.55 to 1.81, the refractive index of the optical adjustment layer is 1.20 to 1.60, and the b * value in the CIE L * a * b * color system defined in JIS Z 8729-1994 is ⁇
  • a gas barrier laminate having a range of 1.00 to 1.00.
  • the gas barrier layer has a thickness of 10 nm to 10 ⁇ m.
  • a gas barrier laminate excellent in gas barrier properties and colorless transparency 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 gas barrier layer, and an optical adjustment layer are laminated in this order, and the gas barrier layer and the optical adjustment layer are adjacent to each other,
  • the refractive index of the gas barrier layer is 1.55 to 1.81
  • the refractive index of the optical adjustment layer is 1.20 to 1.60
  • b * b * values in color system characterized in that in the range of -1.00 to 1.00.
  • the base material constituting the gas barrier laminate of the present invention is not particularly limited as long as it can carry a gas barrier layer and an optical adjustment layer and is transparent.
  • a transparent base material means the base material which permeate
  • the light transmittance at 380 to 780 nm of the substrate is preferably 80% or more, and more preferably 85% or more.
  • the thickness of the substrate is not particularly limited and may be determined according to the purpose of the gas barrier laminate.
  • the thickness of the substrate is usually 0.5 to 500 ⁇ m, preferably 1 to 100 ⁇ m.
  • Resin components of the resin film include polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, acrylic resin, cycloolefin Examples thereof include polymers and aromatic polymers.
  • 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.
  • polyamide examples include wholly aromatic polyamide, nylon 6, nylon 66, nylon copolymer, and the like.
  • cycloolefin polymers include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides thereof. Specific examples thereof include Apel (an ethylene-cycloolefin copolymer manufactured by Mitsui Chemicals), Arton (a norbornene polymer manufactured by JSR), Zeonoa (a norbornene polymer manufactured by Nippon Zeon), and the like. .
  • Apel an ethylene-cycloolefin copolymer manufactured by Mitsui Chemicals
  • Arton a norbornene polymer manufactured by JSR
  • Zeonoa a norbornene polymer manufactured by Nippon Zeon
  • the resin film may contain various additives as long as the effects of the present invention are not hindered.
  • the additive include an ultraviolet absorber, an antistatic agent, a stabilizer, an antioxidant, a plasticizer, a lubricant, and a coloring pigment. What is necessary is just to determine suitably content of these additives according to the objective.
  • the resin film 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 molding method is not particularly limited, and a known method such as a casting method or a melt extrusion method can be used.
  • the 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 examples include a layer containing an inorganic compound such as an inorganic oxide, an inorganic oxynitride, an inorganic oxycarbide, an inorganic oxynitride carbide, or a metal.
  • the gas barrier layer preferably contains at least one selected from the group consisting of inorganic oxides, inorganic oxynitrides, inorganic oxycarbides, and inorganic oxynitride carbides.
  • an inorganic vapor-deposited film or a layer containing a polymer compound obtained by modifying treatment [in this case, the gas barrier layer]
  • polymer layer a polymer compound obtained by modifying treatment
  • the term “means a polymer layer including a modified region”, not only a region modified by ion implantation or the like. ] 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 from the viewpoint of gas barrier properties and handleability, it is preferably 10 to 2000 nm, more preferably 20 to 1000 nm, more preferably 30 to 500 nm, and still more preferably 40. It is in the range of ⁇ 200 nm.
  • the polymer compound used is a silicon-containing polymer compound, polyimide, polyamide, polyamideimide, polyphenylene ether, polyetherketone, polyetheretherketone, polyolefin, Examples thereof include polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin polymer, and aromatic polymer. 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 usually 20 nm to 10 ⁇ m, preferably 30 to 500 nm, more preferably 40 to 400 nm.
  • a gas barrier film having a sufficient gas barrier property can be obtained even if the layer containing the polymer compound is nano-order.
  • 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, ultraviolet irradiation treatment, and heat 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 in accordance with the purpose of use of the 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 and the purpose of use of the laminate. Usually, it is 10 to 400 nm.
  • the thickness of the gas barrier layer is usually 10 nm to 10 ⁇ m, preferably 10 to 2000 nm, more preferably 20 to 1000 nm.
  • the refractive index of the gas barrier layer is 1.55 to 1.81, preferably 1.60 to 1.67. When the refractive index of the gas barrier layer is less than 1.55, it is difficult to cause a problem that the gas barrier laminate is yellowish, so that it is not necessary to use the present invention. When the refractive index of the gas barrier layer exceeds 1.81, it becomes difficult to obtain a gas barrier laminate having b * of 1.00 or less.
  • the refractive index of the gas barrier layer may be in the above range, but is preferably larger than the refractive index of the optical adjustment layer described later.
  • the refractive index of the gas barrier layer and the refractive index of the optical adjustment layer have such a relationship, a gas barrier laminate having a b * of 1.00 or less can be easily obtained.
  • the refractive index means the refractive index of light having a wavelength of 590 nm measured at 23 ° C.
  • the optical adjustment layer constituting the gas barrier laminate of the present invention is a layer that adjusts the hue of the gas barrier laminate. Since the gas barrier layer usually has a high refractive index, a difference in refractive index from other adjacent layers becomes large, and light having a short wavelength is easily reflected at the interface between these layers. For this reason, the conventional gas barrier laminate has a tendency to be yellowish. Since the gas barrier laminate of the present invention has an optical adjustment layer adjacent to the gas barrier layer, yellowing is suppressed and excellent in colorless transparency.
  • Materials for the optical adjustment layer include cured products of curable compositions, polyester resins, polyurethane resins, acrylic resins, polycarbonate resins, vinyl chloride / vinyl acetate copolymers, polyvinyl butyral resins, and nitrocellulose resins.
  • Resins such as fluorine-based resins; inorganic materials such as inorganic oxides, inorganic oxynitrides, inorganic oxycarbides, and inorganic oxynitride carbides; Among them, cured products of curable compositions, polyester resins, polyurethane resins, acrylic resins, polycarbonate resins, vinyl chloride / vinyl acetate copolymers, polyvinyl butyral resins, nitrocellulose resins, fluorine resins, etc. Resins are preferred, and a layer made of a cured product of the curable composition is more preferred.
  • the optical adjustment layer is a layer composed of a cured product of the curable composition, in addition to the function of adjusting the hue of the gas barrier laminate, it is possible to impart scratch resistance to the gas barrier laminate.
  • the curable composition is a compound containing a curable component and can be cured by irradiation with active energy rays or heating.
  • examples of the curable component include a polymerizable prepolymer and a polymerizable monomer.
  • 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, )
  • 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 curable composition may contain a polymer resin component that does not itself have reaction curability, such as an acrylic resin.
  • the viscosity of the composition can be adjusted by adding a polymer resin component.
  • active energy rays examples include ultraviolet rays, electron beams, ⁇ rays, ⁇ rays, ⁇ rays, and the like.
  • ultraviolet rays are preferable as the active energy rays because they can be generated using a relatively simple apparatus.
  • the curable resin composition preferably contains a photopolymerization initiator.
  • 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) -
  • a photoinitiator can be used individually by 1 type or in combination of 2 or more types.
  • the content of the photopolymerization initiator is not particularly limited, but is usually 0.2 to 30% by mass, preferably 0.5 to 20% by mass with respect to the curable component.
  • the polymerizable prepolymer and the polymerizable monomer are contained as a curable component, a composition containing a thermal polymerization initiator, and a hydrolytic condensable compound as a curable component.
  • the composition etc. which contain are mentioned.
  • the thermal polymerization initiator is not particularly limited as long as it generates radicals by heating and initiates a polymerization reaction.
  • the thermal polymerization initiator include hydrogen peroxide; peroxodisulfates such as ammonium peroxodisulfate, sodium peroxodisulfate, and potassium peroxodisulfate; 2,2′-azobis (2-amidinopropane) dihydrochloride, 4,4 Azo compounds such as' -azobis (4-cyanovaleric acid), 2,2'-azobisisobutyronitrile, 2,2'-azobis (4-methoxy-2,4-dimethylvaleronitrile); benzoyl peroxide Organic peroxides such as lauroyl peroxide, peracetic acid, persuccinic acid, di-t-butyl peroxide, t-butyl hydroperoxide, cumene hydroperoxide, and the like.
  • a thermal polymerization initiator can be used individually by 1 type or in combination of 2 or more types.
  • the content of the thermal polymerization initiator is not particularly limited, but is usually 0.2 to 30% by mass, preferably 0.5 to 20% by mass with respect to the curable component.
  • hydrolytic condensable compound examples include silane compounds having a hydrolyzable organic group and oligomers thereof.
  • silane compound having a hydrolyzable group examples include tetramethoxysilane, tetraethoxysilane, tetra-n-propoxysilane, tetraisopropoxysilane, tetra-n-butoxysilane, tetraisobutoxysilane, tetra-s-butoxysilane, Tetraalkoxysilanes such as tetra-t-butoxysilane; trialkoxysilane hydrides such as trimethoxysilane hydride, triethoxysilane hydride, tripropoxysilane hydride; and the like.
  • These silane compounds can be used alone or in combination of two or more. Moreover, you may use together alkyl trialkoxysilane with these silane compounds.
  • the curable composition preferably contains a filler in addition to the curable component.
  • a filler By containing the filler, the refractive index of the optical adjustment layer can be efficiently controlled.
  • Examples of the filler include silica particles, metal oxide particles, polymer particles, and alkyl silicate particles.
  • Examples of the silica particles include colloidal silica, hollow silica, and reactive silica filler.
  • Examples of the metal oxide particles include particles of titanium oxide, zinc oxide, zirconium oxide, tantalum oxide, indium oxide, hafnium oxide, tin oxide, niobium oxide, and the like.
  • Polymer particles include poly (pentabromophenyl methacrylate), poly (pentabromophenyl acrylate), poly (2,4,6-tribromophenyl methacrylate), poly (1-naphthyl methacrylate), poly (2,6-dichloro).
  • Examples thereof include particles made of a polymer containing a halogen atom or an aromatic group such as styrene) or poly (2-chlorostyrene).
  • alkyl silicate particles the formula: R a —O [— ⁇ Si (OR b ) 2 ⁇ —O—] n —R a (wherein R a and R b represent an alkyl group having 1 to 10 carbon atoms). , N represents an integer of 1 or more).
  • silica particles or alkyl silicate particles are preferable because they are excellent in compatibility with the curable component and can efficiently control the refractive index of the optical adjustment layer.
  • a filler can be used individually by 1 type or in combination of 2 or more types.
  • the average particle diameter is preferably 2 to 1500 nm.
  • the content thereof is preferably 5 to 60% by mass, more preferably 10 to 50% by mass, based on the total solid content of the curable composition.
  • the curable composition may contain other components as long as the effects of the present invention are not hindered.
  • other components include leveling agents, antistatic agents, stabilizers, antioxidants, plasticizers, and lubricants. What is necessary is just to determine these content suitably according to the objective.
  • the method for forming the optical adjustment layer is not particularly limited.
  • a coating liquid containing a curable composition and, if necessary, a solvent is prepared. By doing so, an optical adjustment layer can be formed. Moreover, you may give a drying process before hardening a coating film as needed.
  • Solvents used for preparing the coating liquid 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 And aliphatic hydrocarbon solvents such as 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.
  • 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 active energy rays or heating in accordance with the curable composition used.
  • 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 can be used.
  • 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 to 100 ° C.
  • the thickness of the optical adjustment layer is usually 5 to 2500 nm, preferably 10 to 2000 nm.
  • the refractive index of the optical adjustment layer is 1.20 to 1.60, preferably 1.35 to 1.55.
  • the optical film thickness of the optical adjustment layer is usually 5 to 2000 nm, preferably 10 to 1500 nm.
  • a gas barrier laminate excellent in colorless transparency can be obtained by appropriately adjusting the optical film thickness of the optical adjustment layer within the above range.
  • b * is known to change periodically with respect to the change in the optical film thickness of the optical adjustment layer.
  • the present inventors have found that a gas barrier laminate having a b * value of ⁇ 1.00 to 1.00 can be obtained efficiently when the optical film thickness T of the
  • FIG. 1 shows the relationship between the optical film thickness of the optical adjustment layer and b * of the gas barrier laminate when the types of the base material and the gas barrier layer and the film thicknesses thereof are constant.
  • the horizontal axis represents the optical film thickness of the optical adjustment layer
  • the vertical axis represents b * of the gas barrier laminate.
  • the optical thickness of the optical adjustment layer is more than 760 nm
  • b * is the gas barrier laminate
  • b * is the gas barrier laminate
  • FIG. 1B shows an enlarged view of the optical film thickness in the range of 0 to about 900 nm in FIG. From FIG. 1B, in the range showing the periodic change (the optical film thickness of the optical adjustment layer is less than 760 nm), the range of the optical film thickness where b * of the gas barrier laminate is ⁇ 1 to 1 is It is as follows. Range 1: 30 to 100 nm, Range 2: 120 to 170 nm, Range 3: 280 to 310 nm, Range 4: 380 to 410 nm, Range 5: 520 to 550 nm, Range 6: 620 to 660 nm
  • FIG. 2 shows a graph in which the maximum value and the minimum value in the ranges 1 to 6 are plotted, and approximate lines of the maximum value and the minimum value are respectively shown.
  • the horizontal axis represents the range number
  • the vertical axis represents the optical film thickness of the optical adjustment layer.
  • the optical adjustment layer has an optical film thickness T (nm) of the following formula (1) or (2)
  • the gas barrier laminate of the present invention is a gas barrier laminate in which a base material, a gas barrier layer, and an optical adjustment layer are laminated in this order, and the gas barrier layer and the optical adjustment layer are adjacent to each other.
  • the gas barrier layer has a refractive index of 1.55 to 1.81
  • the optical adjustment layer has a refractive index of 1.20 to 1.60
  • the b * value in the * b * color system is in the range of -1.00 to 1.00.
  • the gas barrier laminate of the present invention may have one gas barrier layer or optical adjustment layer, or two or more layers.
  • the gas barrier laminate of the present invention may have a layer other than the base material, the gas barrier layer, and the optical adjustment layer.
  • layers other than the substrate, gas barrier layer, and optical adjustment layer there are a primer layer, a conductor layer, a shock absorbing layer, an adhesive layer, a hard coat layer, a process sheet, etc. for improving interlayer adhesion with the substrate. Can be mentioned.
  • seat has a role which protects a laminated body, when a laminated body is preserve
  • Examples of the layer structure of the gas barrier laminate of the present invention include, but are not limited to, the following.
  • (I) Optical adjustment layer / gas barrier layer / substrate ii) Optical adjustment layer / gas barrier layer / substrate / hard coat layer
  • Optical adjustment layer / gas barrier layer / optical adjustment layer / gas barrier layer / substrate iv) Optical adjustment layer / gas barrier layer / primer layer / base material
  • Optical adjustment layer / gas barrier layer / primer layer / base material Optical adjustment layer / gas barrier layer / primer layer / base material / hard coat layer
  • the gas barrier laminate of the present invention can be produced, for example, by the following method.
  • a gas barrier layer is formed on the substrate using the method described above.
  • an optical adjustment layer is formed on the obtained gas barrier layer using the method described above, whereby a gas barrier laminate having a layer configuration of optical adjustment layer / gas barrier layer / base material can be obtained. .
  • a gas barrier laminate having the layer configurations (ii) to (v) can be obtained by appropriately providing necessary steps.
  • the thickness of the gas barrier laminate of the present invention is not particularly limited, but is preferably 1 to 1000 ⁇ m, more preferably 10 to 500 ⁇ m, and still more preferably 50 to 100 ⁇ m.
  • the gas barrier layered product of the present invention is preferably 0.1g / (m 2 ⁇ day) or less, more preferably 0.05g / (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 b * value in the CIE L * a * b * color system defined by JIS Z 8729-1994 of the gas barrier laminate of the present invention is preferably ⁇ 1.00 to 1.00, more preferably -0.80 to 0.80.
  • the b * value represents the degree of yellow and blue when the color is digitized. If the b * value is positive, it is yellowish, and if it is negative, it is bluish. When the b * value is in the above range, the gas barrier laminate exhibits a hue that is more intermediate between yellow and blue.
  • the b * value can be controlled by providing an optical adjustment layer having an appropriate optical film thickness in accordance with the refractive index of the gas barrier layer to be formed.
  • the a * value in the CIE L * a * b * color system defined by JIS Z 8729-1994 of the gas barrier laminate of the present invention is preferably -1.00 to 1.00, more preferably. Is -0.80 to 0.80.
  • the a * value represents the degree of redness and greenness when the color is digitized. If the a * value is positive, it is reddish, if it is negative, This means that it is greenish. When the a * value is in the above range, the gas barrier laminate exhibits a hue between red and green.
  • Such a * value can be controlled by appropriately selecting the resin to be used and other components.
  • the b * value and a * value in the CIE L * a * b * color system defined in JIS Z 8729-1994 can be measured by the method described in the examples.
  • the gas barrier laminate of the present invention is suitably used as an electronic device member.
  • the electronic device member of the present invention comprises the gas barrier laminate of the present invention. Therefore, 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 colorless transparency, it 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 has excellent gas barrier properties.
  • Base material (1) Polyethylene terephthalate film (manufactured by Toyobo Co., Ltd., trade name: Cosmo Shine A4100, thickness 50 ⁇ m) -Polysilazane compound-based coating agent (1): (manufactured by Clariant Japan, trade name: Aquamica NL110-20, solid content 20%)
  • Curing component (1) Urethane acrylate oligomer (Arakawa Kogyo Co., Ltd., trade name: Beam Set 575VCB)
  • Filler (1) Hollow silica fine particles (manufactured by JGC Catalysts & Chemicals, trade name:
  • the refractive index of the gas barrier layer and the optical adjustment layer of the gas barrier laminate obtained in Examples and Comparative Examples is determined using an ellipsometer (manufactured by JA Woollam Japan, trade name: spectroscopic ellipsometry 2000U). It was measured.
  • Example 1 A polysilazane compound coating agent (1) is applied onto the substrate (1) by a spin coating method, and the resulting coating film is heated at 120 ° C. for 2 minutes to have a thickness of 150 nm and a polysilazane containing perhydropolysilazane. A layer was formed. Next, argon (Ar) was plasma ion-implanted on the surface of the polysilazane layer using a plasma ion implantation apparatus under the following conditions to form a gas barrier layer (refractive index: 1.62, thickness 150 nm). .
  • argon (Ar) was plasma ion-implanted on the surface of the polysilazane layer using a plasma ion implantation apparatus under the following conditions to form a gas barrier layer (refractive index: 1.62, thickness 150 nm).
  • the optical adjustment layer forming material (1) obtained in Production Example 1 was applied by a bar coating method, and the obtained coating film was dried at 70 ° C. for 1 minute, and then using a UV light irradiation line.
  • UV light irradiation 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
  • optical adjustment layer film thickness: 20 nm, optical film thickness) : 28 nm
  • the plasma ion implantation apparatus and ion implantation conditions used for forming the gas barrier layer are as follows.
  • RF power source JEOL Ltd., model number “RF” 56000
  • High voltage pulse power supply “PV-3-HSHV-0835” manufactured by Kurita Manufacturing Co., Ltd.
  • Chamber internal pressure 0.2 Pa
  • Plasma generation gas Argon gas flow rate: 100 sccm RF output: 1000W RF frequency: 1000Hz RF pulse width: 50 ⁇ sec RF delay: 25 ⁇ sec DC voltage: -6kV DC frequency: 1000Hz DC pulse width: 5 ⁇ sec DC delay: 50 ⁇ sec Duty ratio: 0.5% Processing time: 200 sec
  • Example 2 In Example 1, except that the optical adjustment layer forming material (2) was used instead of the optical adjustment layer forming material (1) to form an optical adjustment layer (film thickness: 50 nm, optical film thickness: 75 nm). A gas barrier laminate 2 was obtained in the same manner as in Example 1.
  • Example 3 A gas barrier laminate 3 was obtained in the same manner as in Example 1 except that the film thickness of the optical adjustment layer was changed to 90 nm (optical film thickness: 124 nm) in Example 1.
  • Example 4 A gas barrier laminate 4 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 120 nm (optical film thickness: 165 nm).
  • Example 5 In Example 1, in place of the optical adjustment layer forming material (1), the optical adjustment layer forming material (3) was applied, and the obtained coating film was cured by heating at 100 ° C. for 1 minute, thereby adjusting the optical adjustment.
  • a gas barrier laminate 5 was obtained in the same manner as in Example 1 except that a layer (film thickness: 200 nm, optical film thickness: 286 nm) was formed.
  • Example 6 the gas barrier laminate 6 was obtained in the same manner as in Example 1 except that the film thickness of the optical adjustment layer was changed to 220 nm (optical film thickness: 302 nm).
  • Example 7 A gas barrier laminate 7 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 280 nm (optical film thickness: 385 nm).
  • Example 8 A gas barrier laminate 8 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 295 nm (optical film thickness: 405 nm).
  • Example 9 A gas barrier laminate 9 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 380 nm (optical film thickness: 522n).
  • Example 10 In Example 1, the gas barrier laminate 10 was obtained in the same manner as in Example 1 except that the film thickness of the optical adjustment layer was changed to 390 nm (optical film thickness: 536 nm).
  • Example 11 A gas barrier laminate 11 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 460 nm (optical film thickness: 632 nm).
  • Example 12 A gas barrier laminate 12 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 475 nm (optical film thickness: 652 nm).
  • Example 13 A gas barrier laminate 13 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 555 nm (optical film thickness: 762 nm).
  • Example 2 A gas barrier laminate 15 was obtained in the same manner as in Example 5 except that the film thickness of the optical adjustment layer was changed to 70 nm (optical film thickness: 100 nm) in Example 5.
  • Example 3 A gas barrier laminate 16 was obtained in the same manner as in Example 2 except that the film thickness of the optical adjustment layer was changed to 150 nm (optical film thickness: 224 nm) in Example 2.
  • a gas barrier laminate 17 was obtained in the same manner as in Example 1, except that the film thickness of the optical adjustment layer was changed to 270 nm (optical film thickness: 371 nm).
  • Example 2 the gas barrier laminate 18 was obtained in the same manner as in Example 2 except that the film thickness of the optical adjustment layer was changed to 300 nm (optical film thickness: 448 nm).
  • Example 2 a gas barrier laminate 19 was obtained in the same manner as in Example 2 except that the film thickness of the optical adjustment layer was changed to 400 nm (optical film thickness: 597 nm).
  • Example 5 the gas barrier laminate 20 was obtained in the same manner as in Example 5 except that the film thickness of the optical adjustment layer was changed to 505 nm (optical film thickness: 723 nm).
  • Example 4 the gas barrier laminate was formed in the same manner as in Example 4 except that the DC voltage when forming the gas barrier layer was changed to ⁇ 9 kV and a gas barrier layer having a refractive index of 1.82 was formed. 21 was obtained.
  • Example 9 In Example 5, except that the optical adjustment layer forming material (4) was used instead of the optical adjustment layer forming material (3) to form an optical adjustment layer (film thickness: 178 nm, optical film thickness: 286 nm). A gas barrier laminate 22 was obtained in the same manner as in Example 5.
  • Comparative Example 1 In Comparative Example 1, the heating condition of the coating film of the polysilazane compound-based coating agent (1) was changed to 120 ° C. for 30 minutes, and a gas barrier layer having a refractive index of 1.54 was formed. A gas barrier laminate 23 was obtained in the same manner.
  • Table 1 shows the following.
  • the gas barrier laminates 1 to 13 of Examples 1 to 13 are excellent in gas barrier properties and suppressed yellowing.
  • the gas barrier laminates 14 to 22 of Comparative Examples 1 to 9 have a color value b * of less than ⁇ 1 or more than +1 and are yellowish or bluish.
  • the refractive index of the gas barrier layer is relatively low at 1.54, yellowing is suppressed without providing an optical adjustment layer.
  • the gas barrier laminate 21 of Comparative Example 8 since the refractive index of the gas barrier layer is as high as 1.82, it is difficult to set b * to 1.00 or less even if an optical adjustment layer is provided. . Further, the gas barrier laminate 22 of Comparative Example 9 does not function sufficiently as an optical adjustment layer because the refractive index of the optical adjustment layer is too high.
  • Range 1 Range 1 2: Range 2 3: Range 3 4: Range 4 5: Range 5 6: Range 6

Landscapes

  • Laminated Bodies (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

La présente invention concerne : un stratifié de faisant barrière contre les gaz formé par stratification d'un substrat, d'une couche barrière contre les gaz et d'une couche d'ajustement optique, dans cet ordre, ladite couche barrière contre les gaz étant adjacente à ladite couche d'ajustement optique, et ledit stratifié faisant barrière contre les gaz étant caractérisé en ce que l'indice de réfraction de la couche barrière contre les gaz est situé dans la plage allant de 1,55 à 1,81, l'indice de réfraction de la couche d'ajustement optique est situé dans la plage allant de 1,20 à 1,60, et la valeur b* dans le système couleur CIE L*a*b* spécifié conformément à la norme JIS Z 8729-1994 est située dans la plage allant de -1,00 à 1,00 ; un élément destiné à un dispositif électronique, ledit élément comprenant le stratifié faisant barrière contre les gaz ; et un dispositif électronique équipé dudit élément destiné à un dispositif électronique. La présente invention concerne ainsi un stratifié faisant barrière contre les gaz présentant d'excellentes propriétés de barrière contre les gaz et une transparence incolore, un élément destiné à un dispositif électronique, ledit élément comprenant le stratifié faisant barrière contre les gaz, et un dispositif électronique qui est équipé dudit élément destiné à un dispositif électronique.
PCT/JP2015/059232 2014-03-31 2015-03-25 Stratifié faisant barrière contre les gaz, élément pour dispositif électronique et dispositif électronique WO2015151976A1 (fr)

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WO2013035432A1 (fr) * 2011-09-08 2013-03-14 リンテック株式会社 Film de polysilazane modifié et procédé de fabrication d'un film barrière aux gaz
WO2013108487A1 (fr) * 2012-01-20 2013-07-25 リンテック株式会社 Film barrière contre les gaz et procédé de production d'un film barrière contre les gaz
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JP7100368B2 (ja) 2019-09-10 2022-07-13 尾池工業株式会社 ガスバリアフィルム

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