WO2013147093A1 - ガスバリアフィルム積層体、電子デバイス用部材、及び電子デバイス - Google Patents
ガスバリアフィルム積層体、電子デバイス用部材、及び電子デバイス Download PDFInfo
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- WO2013147093A1 WO2013147093A1 PCT/JP2013/059402 JP2013059402W WO2013147093A1 WO 2013147093 A1 WO2013147093 A1 WO 2013147093A1 JP 2013059402 W JP2013059402 W JP 2013059402W WO 2013147093 A1 WO2013147093 A1 WO 2013147093A1
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- gas barrier
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Images
Classifications
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- 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
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- 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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K30/80—Constructional details
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H—ELECTRICITY
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Definitions
- the present invention relates to a gas barrier film laminate excellent in gas barrier properties and bending resistance, an electronic device member comprising the gas barrier film laminate, and an electronic device comprising the electronic device member.
- a transparent plastic is used in place of a glass plate in order to realize a thin, lightweight, flexible and impact resistance.
- the use of films is being considered.
- the plastic film has a problem that it easily permeates water vapor, oxygen, and the like as compared with the glass plate, and easily causes deterioration of elements inside the electronic member.
- Patent Document 1 discloses a flexible display substrate in which a transparent gas barrier layer made of a metal oxide is laminated on a transparent plastic film.
- Patent Document 2 discloses a gas barrier laminate in which a plastic film and a resin layer containing polyorganosilsesquioxane as a main component are laminated on at least one surface of the plastic film.
- Patent Document 3 a transparent gas barrier layer is formed on a first transparent plastic film substrate, and a second transparent plastic film substrate is formed on the transparent gas barrier layer via a transparent adhesive layer. Disposed transparent films are disclosed.
- the applicant of the present application has previously proposed a laminate having a gas barrier layer formed of a material containing oxygen atoms, carbon atoms, and silicon atoms (WO2010 / 021326, WO2010 / 1001818, etc.).
- the laminates described in these documents are excellent in gas barrier properties.
- the present inventors further studied to obtain a laminate having excellent gas barrier properties, and devised a laminate in which at least two gas barrier films were laminated via an adhesive layer.
- the laminated body in which the gas barrier films are bonded to each other via the pressure-sensitive adhesive layer is bent, if the difference in thickness between the gas barrier films is large, peeling occurs remarkably at the interface between the gas barrier film and the pressure-sensitive adhesive layer. There was a case where floating occurred. This is considered to occur because bending stress concentrates at the interface between the gas barrier film and the pressure-sensitive adhesive layer due to the large difference in thickness between the gas barrier films.
- the present invention has been made in view of such a situation, and has a high gas barrier property and excellent bending resistance (it is difficult to lift when folded), and the gas barrier film laminate.
- An object of the present invention is to provide an electronic device member comprising a body, and an electronic device including the electronic device member.
- a gas barrier film laminate having excellent bending resistance can be obtained by providing a bonding layer in which adhesive layers are laminated adjacent to each other on both sides of a base film made of a synthetic resin of 000 to 10,000 MPa.
- the headline and the present invention were completed.
- the following gas barrier film laminates (1) to (11), an electronic device member (12), and an electronic device (13) are provided.
- a gas barrier film laminate comprising a pressure-sensitive adhesive layer laminated on both surfaces of a material film A, respectively.
- the value of (the thickness of the gas barrier film laminated on one surface of the bonding layer) / (the thickness of the gas barrier film laminated on the other surface of the bonding layer) is 0.05 to 1.
- the gas barrier film laminate according to (1), which is 0. (8) The gas barrier film laminate according to (1), wherein at least one of the gas barrier films has a base film B and at least one gas barrier layer provided on the base film B. body. (9) The gas barrier film laminate according to (8), wherein the gas barrier layer is a layer formed by implanting ions into a layer made of a polymeric silicon compound. (10) The gas barrier film laminate according to (8), wherein the gas barrier film is laminated so that the gas barrier layer is adjacent to the bonding layer. (11) The gas barrier film laminate according to (1), wherein the thickness is 100 ⁇ m or less. (12) An electronic device member comprising the gas barrier film laminate according to (1). (13) An electronic device comprising the electronic device member according to (12).
- the gas barrier film laminate of the present invention relaxes stress concentration due to bending at the interface between the gas barrier film on the thick film side and the joining layer when the laminate is folded by using the joining layer having the above characteristics, This solves the problem that peeling occurs at the interface between the gas barrier film on the thick film side and the pressure-sensitive adhesive layer, and floating occurs.
- the gas barrier film laminate of the present invention is suitable for electronic members such as solar cells, liquid crystal displays, and electroluminescence (EL) displays. Since the electronic device member of the present invention is composed of the gas barrier film laminate of the present invention that is excellent in gas barrier properties and bending resistance, electronic devices such as touch panels, electronic paper, organic / inorganic EL flexible displays, solar cells, etc. It can use suitably for etc.
- Gas barrier film laminate of the present invention is a gas barrier film laminate in which at least two gas barrier films are laminated via a joining layer, and the joining layer has a tensile modulus at 23 ° C. Is characterized in that an adhesive layer is laminated on both sides of a base film made of a synthetic resin of 3,000 to 10,000 MPa.
- the bonding layer used in the present invention is a base film made of a synthetic resin having a tensile elastic modulus at 23 ° C. of 3,000 to 10,000 MPa (hereinafter referred to as “base film A”.
- the pressure-sensitive adhesive layer is laminated on both sides of each other.
- the base film A is not particularly limited as long as it is made of a synthetic resin having a tensile elastic modulus at 23 ° C. of 3,000 to 10,000 MPa and can carry an adhesive layer.
- the tensile elastic modulus at 23 ° C. of the synthetic resin constituting the base film A is 3,000 to 10,000 MPa, preferably 3,000 to 5,000 MPa.
- the tensile elastic modulus is less than 3,000 MPa, floating tends to occur when the gas barrier film laminate is bent.
- the tensile elastic modulus exceeds 10,000 MPa, the flexibility of the gas barrier film laminate decreases.
- the tensile elastic modulus at 23 ° C. is measured according to JIS K7127.
- Examples of the synthetic resin constituting the base film A include polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, and polyphenylene sulfide.
- Examples include arylates, acrylic resins, cycloolefin polymers, and aromatic polymers. Among these, polyester or cycloolefin polymer is preferable because of its excellent transparency and versatility.
- polyester examples include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, and polyarylate.
- cycloolefin polymers include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides thereof.
- the thickness of the base film A is usually in the range of 0.5 to 25 ⁇ m, preferably 1 to 10 ⁇ m, more preferably 1 to 6 ⁇ m.
- the thickness of the base film A is 0.5 ⁇ m or more, the workability during production of the gas barrier film laminate is excellent.
- the thickness of the base film A is 25 ⁇ m or less, when the gas barrier film laminate is folded, it becomes difficult for floating to occur.
- the pressure-sensitive adhesive layer is provided adjacent to both surfaces of the base film A in order to maintain a laminated structure.
- the pressure-sensitive adhesive layer can be used without particular limitation as long as it does not peel off the gas barrier film or the base film A and has sufficient adhesive force.
- the types and thicknesses of the two pressure-sensitive adhesive layers may be the same or different.
- the thickness of the pressure-sensitive adhesive layer is usually 0.5 to 25 ⁇ m, preferably 1 to 10 ⁇ m, more preferably 1 to 6 ⁇ m.
- the thickness of the pressure-sensitive adhesive layer is 0.5 ⁇ m or more, a pressure-sensitive adhesive layer having sufficient adhesive force is formed, and when the gas barrier film laminate is bent, it is difficult for floating to occur.
- the thickness of the pressure-sensitive adhesive layer is 25 ⁇ m or less, it is advantageous in terms of productivity.
- the adhesive strength of the pressure-sensitive adhesive layer to be peeled off from the gas barrier film is preferably 2.0 N / 25 mm or more. Since the peel adhesive strength is 2.0 N / 25 mm or more, it has sufficient adhesive strength to the gas barrier film, and therefore, it is more difficult to lift when the gas barrier film laminate is folded.
- “180 ° peel adhesive strength of the pressure-sensitive adhesive layer to the gas barrier film” means that a polyester film is lined on one surface of the pressure-sensitive adhesive layer, as described in the Examples, and an adhesive strength test is performed. It is assumed that the adhesive strength is 180 ° peel adhesive strength measured according to JIS Z0237 (2000) with respect to the gas barrier film of this adhesive strength test adhesive film.
- the kind of adhesive is not particularly limited. In the present invention, known adhesives such as acrylic, rubber, polyester, urethane, and silicone can be used. Among these, an acrylic pressure-sensitive adhesive is preferable because excellent adhesive strength can be obtained.
- the acrylic pressure-sensitive adhesive is a pressure-sensitive adhesive mainly composed of an acrylic copolymer.
- An acrylic copolymer is a copolymer having a repeating unit derived from (meth) acrylic acid or (meth) acrylic acid ester. “(Meth) acrylic acid” means both acrylic acid and methacrylic acid, and “(meth) acrylic acid ester” means both acrylic acid ester and methacrylic acid ester.
- the acrylic copolymer may have a repeating unit other than the above as long as the effects of the present invention are not impaired.
- the acrylic copolymer preferably has both a repeating unit having a functional group capable of forming a crosslinked structure such as a carboxyl group, a hydroxyl group, an amino group, and an amide group and a repeating unit having no functional group.
- the monomers used for the production of the acrylic copolymer include acrylic monomers having a functional group, acrylic monomers having no functional group, and other monomers copolymerizable with these monomers. A monomer is mentioned.
- acrylic monomer having a functional group examples include acrylic monomers having a carboxyl group such as (meth) acrylic acid and 2-carboxyethyl (meth) acrylate; 2-hydroxyethyl (meth) acrylate, ( Such as 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3-hydroxybutyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, etc. And acrylic monomers having a hydroxyl group.
- acrylic monomers having a carboxyl group such as (meth) acrylic acid and 2-carboxyethyl (meth) acrylate; 2-hydroxyethyl (meth) acrylate, ( Such as 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3-hydroxybutyl (meth) acrylate, 4-hydroxybutyl (me
- acrylic monomers having a carboxyl group such as (meth) acrylic acid and 2-carboxyethyl (meth) acrylate are preferable, and (meth) acrylic acid is more preferable.
- acrylic monomers having a carboxyl group such as (meth) acrylic acid and 2-carboxyethyl (meth) acrylate are preferable, and (meth) acrylic acid is more preferable.
- These monomers can be used alone or in combination of two or more.
- acrylic monomer having no functional group examples include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, pentyl (meth) acrylate, (meth ) Straight chain such as hexyl acrylate, octyl (meth) acrylate, decyl (meth) acrylate, dodecyl (meth) acrylate, myristyl (meth) acrylate, palmityl (meth) acrylate, stearyl (meth) acrylate
- a monomer having a hydrocarbon group having 4 to 10 carbon atoms is preferable, and butyl (meth) acrylate is more preferable because an adhesive layer having excellent adhesiveness can be formed.
- These monomers can be used alone or in combination of two or more.
- monomers having a carboxyl group such as crotonic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid; (meth) acrylamide, N-methyl (meth) acrylamide, N-methylol (meta )
- monomers having an amide group such as acrylamide; acrylonitrile; styrene; vinyl acetate; vinylpyrrolidone and the like.
- the initiator used for the polymerization reaction is not particularly limited, and peroxide initiators such as benzoyl peroxide, lauroyl peroxide, methyl ethyl ketone peroxide, azobisisobutyronitrile, azobiscyanovaleric acid, azobiscyanopentane, etc. And azo initiators.
- the solvent used for the polymerization reaction is not particularly limited, and examples thereof include toluene, hexane, heptane, ethyl acetate, acetone, methyl ethyl ketone, and methanol.
- Known conditions can be adopted as the reaction conditions such as the temperature of the polymerization reaction and the reaction time.
- a crosslinking agent can be added to the acrylic pressure-sensitive adhesive.
- the cross-linking agent is a compound that reacts with the functional group to form a cross-link.
- limiting in particular in the crosslinking agent to be used An isocyanate type crosslinking agent, an epoxy-type crosslinking agent, etc. are mentioned. Of these, isocyanate-based crosslinking agents are preferred.
- the isocyanate-based crosslinking agent is not particularly limited, and a compound having two or more isocyanate groups in the molecule is used.
- isocyanate-based crosslinking agents include aromatic polyisocyanates such as tolylene diisocyanate, diphenylmethane diisocyanate, and xylylene diisocyanate; aliphatic polyisocyanates such as hexamethylene diisocyanate; isophorone diisocyanate.
- Cycloaliphatic polyisocyanates such as hydrogenated diphenylmethane diisocyanate; and their biurets, isocyanurates, and low molecules such as ethylene glycol, propylene glycol, neopentyl glycol, trimethylolpropane, castor oil, etc.
- the epoxy-based crosslinking agent a compound having two or more epoxy groups in the molecule is used.
- sorbitol tetraglycidyl ether trimethylolpropane triglycidyl ether, tetraglycidyl-1,3-bisaminomethylcyclohexane, tetra
- a crosslinking agent can be used individually by 1 type or in combination of 2 or more types.
- the amount of the crosslinking agent used is usually 0.01 to 10 parts by mass, preferably 0.05 to 5 parts by mass with respect to 100 parts by mass of the acrylic copolymer, although it depends on the type of the crosslinking agent.
- the acrylic pressure-sensitive adhesive is preferably used as a solvent-type pressure-sensitive adhesive.
- the solvent to be used is not particularly limited, and a known solvent can be used.
- the weight average molecular weight of the acrylic copolymer is usually 100,000 to 2,000,000, preferably 300,000 to 900,000.
- the weight average molecular weight can be adjusted by adding an amount of a polymerization initiator or a chain transfer agent.
- the said weight average molecular weight is the value of polystyrene conversion measured by the gel permeation chromatography (GPC) method.
- GPC gel permeation chromatography
- the method for producing the acrylic copolymer is not particularly limited, and a conventionally known method such as a solution polymerization method, an emulsion polymerization method, a suspension polymerization method, or a bulk polymerization method can be used. Among these, solution polymerization is desirable because polymerization is easy.
- the pressure-sensitive adhesive may contain conventionally known additives such as a tackifier, a filler, a pigment, and an ultraviolet absorber.
- a tackifier such as rosin resins and polyterpene resins, petroleum resins such as C5, C9, and dicyclopentadiene, and synthetic resins such as coumarone indene resin and xylene resin.
- the method for forming the pressure-sensitive adhesive layer is not particularly limited, and a conventionally known method can be used.
- a pressure-sensitive adhesive layer-forming composition is prepared by dissolving a pressure-sensitive adhesive component in an organic solvent such as toluene, ethyl acetate, methyl ethyl ketone, etc., and this composition is applied to a spin coating method, spray coating method, bar coating method, knife coating.
- a known coating method such as a coating method, a roll coating method, a blade coating method, a die coating method, or a gravure coating method
- the solvent is dried and removed from the obtained coating film, and heated if desired. Can be formed.
- the pressure-sensitive adhesive layer can also be formed by directly coating the base film A with the composition for forming a pressure-sensitive adhesive layer and drying the obtained coating film.
- the former method is preferable for efficiently producing the bonding layer.
- a conventionally known release sheet can be used as the release sheet.
- resin films such as polyethylene terephthalate and polypropylene; those obtained by removing the surface of these resin films with a silicone-based release agent or the like can be used.
- the bonding layer is formed by laminating the pressure-sensitive adhesive layer adjacent to both surfaces of the base film A, respectively.
- the thickness of the bonding layer is usually 75 ⁇ m or less, preferably 1.5 to 20 ⁇ m, more preferably 2.0 to 15 ⁇ m. When the thickness of the bonding layer is 75 ⁇ m or less, a gas barrier film laminate that is thin and excellent in bending resistance can be obtained.
- the bonding layer is bonded to one side of the base film A so that the surface of the base film A and the pressure-sensitive adhesive layer of the release film-attached pressure-sensitive adhesive layer face each other. It can obtain by sticking together on the other surface side so that the other surface of the base film A and the adhesive layer of an adhesive layer with a peeling film may oppose. In this case, a bonding layer with a release film is obtained.
- the bonding layer is obtained by directly coating the base film A with the composition for forming the pressure-sensitive adhesive layer, drying the obtained coating film, and placing the pressure-sensitive adhesive layer on one surface of the base film A.
- the composition for forming the pressure-sensitive adhesive layer is directly applied on the other surface of the base film A, and the obtained coating film is dried, so that the pressure-sensitive adhesive is formed on the other surface of the base film A. It can also be obtained by forming a layer.
- the former method is preferable from the viewpoint of efficiently producing the bonding layer.
- the gas barrier film used in the present invention is a film having a property of suppressing permeation of oxygen and water vapor (hereinafter referred to as “gas barrier property”).
- the gas barrier film used preferably has a water vapor transmission rate of 40 g or less and a relative humidity of 90%, preferably 1.0 g / m 2 / day or less, more preferably 0.5 g / m 2 / day or less. .
- a gas barrier film laminate having a high gas barrier property can be obtained.
- the thickness of the gas barrier film used in the present invention is usually 0.5 ⁇ m to 100 ⁇ m, preferably 1 ⁇ m to 50 ⁇ m, more preferably 5 ⁇ m to 30 ⁇ m.
- the gas barrier film laminate of the present invention at least two gas barrier films may have the same thickness, but the gas barrier film laminated on one surface of the bonding layer is the other of the bonding layers.
- the value of (the thickness of the gas barrier film laminated on one side of the bonding layer (thin film side)) / (the thickness of the gas barrier film laminated on the other side of the bonding layer (thick film side)) is 0.05 to 1.0, preferably 0.1 to 0.5, and more preferably 0.2 to 0.3.
- gas barrier film examples include a single layer film made of a synthetic resin, and a base film made of a synthetic resin (hereinafter sometimes referred to as “base film B”), either directly or via another layer.
- base film B a base film made of a synthetic resin
- Synthetic resins constituting the single layer film include polyvinyl alcohol, polyethylene terephthalate, ultra-low density polyethylene, polyvinyl chloride, polyvinylidene chloride, fluorine-based resin, polyamide-based resin, ethylene-vinyl alcohol copolymer, polyphenylene sulfide. , Single or two or more synthetic resins such as polyacrylonitrile.
- Examples of the material of the base film B include those exemplified above as the material of the base film A. Especially, since it is excellent in transparency and has versatility, a polyester, polyamide, or a cycloolefin type polymer is preferable, and a polyester or a cycloolefin type polymer is more preferable.
- 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 examples include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides thereof.
- the thickness of the base film B is usually in the range of 0.5 to 80 ⁇ m, preferably 1 to 40 ⁇ m, preferably 1 to 30 ⁇ m.
- the gas barrier layer in the gas barrier film is a layer having gas barrier properties.
- the gas barrier layer may be formed on one side of the base film B or may be formed on both sides of the base film B. Further, the gas barrier layer may be a single layer or a plurality of layers may be laminated.
- the material of the gas barrier layer is not particularly limited as long as it prevents the permeation of oxygen and water vapor, but a material having good transparency and good gas barrier properties is preferable.
- the material for the gas barrier layer examples include metals such as aluminum, magnesium, zinc, and tin; Inorganic oxides such as silicon oxide, aluminum oxide, magnesium oxide, zinc oxide, indium oxide and tin oxide; inorganic nitrides such as silicon nitride; inorganic carbides; inorganic sulfides; inorganic oxynitrides which are composites of these; inorganic Examples thereof include oxycarbides; inorganic nitride carbides; inorganic oxynitride carbides; polymer compounds;
- a method for forming the gas barrier layer is not particularly limited.
- a method for forming the above-described material on the base film B by a vapor deposition method, a sputtering method, an ion plating method, a thermal CVD method, a plasma CVD method, or the like a method in which a solution obtained by dissolving or dispersing the above-described material in an organic solvent is coated on the base film B by a known coating method, and the resulting coating film is appropriately dried to form a polymer compound. Examples include a method of forming the polymer layer by performing plasma treatment or ion implantation treatment.
- the thickness of the gas barrier layer is not particularly limited, but is usually 20 nm to 50 ⁇ m, preferably 30 nm to 1 ⁇ m, more preferably 40 to 500 nm.
- the gas barrier layer is preferably formed by performing ion implantation on a polymer layer composed of a polymer compound.
- the polymer layer composed of the polymer compound is modified by performing an ion implantation process, and the gas barrier property is improved.
- the gas barrier layer is preferably formed by implanting ions into a polymer layer composed of a polymer compound.
- the “gas barrier layer” does not mean only a portion modified by ion implantation, but means “a polymer layer having a portion modified by ion implantation”.
- Examples of the polymer compound constituting the polymer layer include silicon-based polymer compounds, polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, and polyether.
- Examples include sulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin polymer, aromatic polymer, and combinations of two or more of these polymers.
- a gas barrier layer having excellent gas barrier properties can be easily formed, a silicon-based polymer compound, polyester or acrylic resin is preferable, and a silicon-based polymer compound is more preferable.
- the silicon-based polymer compound may be an organic compound or an inorganic compound as long as it is a silicon-containing polymer.
- examples include polyorganosiloxane compounds, polycarbosilane compounds, polysilane compounds, polysilazane compounds, and the like.
- the polyorganosiloxane compound is a compound obtained by polycondensation of a silane compound having a hydrolyzable functional group.
- linear main chain structure is a structure represented by the following formula (a)
- ladder main chain structure is a structure represented by the following formula (b): a cage main chain structure
- each of Rx, Ry, and Rz independently represents a hydrogen atom, an unsubstituted or substituted alkyl group, an unsubstituted or substituted alkenyl group, an unsubstituted or substituted aryl group, etc. Represents a hydrolyzable group.
- the plurality of Rx in the formula (a), the plurality of Ry in the formula (b), and the plurality of Rz in the formula (c) may be the same or different. However, both Rx in the formula (a) are not hydrogen atoms.
- alkyl group of the unsubstituted or substituted alkyl group examples include, for example, methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, sec-butyl group, t-butyl group, n
- alkyl groups having 1 to 10 carbon atoms such as -pentyl group, isopentyl group, neopentyl group, n-hexyl group, n-heptyl group and n-octyl group.
- alkenyl group examples include alkenyl groups having 2 to 10 carbon atoms such as vinyl group, 1-propenyl group, 2-propenyl group, 1-butenyl group, 2-butenyl group and 3-butenyl group.
- substituent for the alkyl group and alkenyl group examples 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; And unsubstituted or substituted aryl groups such as 4-methylphenyl group and 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.
- Rx, Ry, and Rz a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, or a phenyl group is preferable, and an alkyl group having 1 to 6 carbon atoms is particularly preferable.
- polysiloxane-based compound As the polyorganosiloxane-based compound, a linear compound represented by the above formula (a) is preferable. From the viewpoint of easy availability and formation of a layer having excellent gas barrier properties, 2 in the above formula (a). Polydimethylsiloxane in which two Rx are both methyl group compounds is more preferable.
- the polyorganosiloxane compound can be obtained, for example, by a known production method in which a silane compound having a hydrolyzable functional group is polycondensed.
- the polycarbosilane compound is a polymer compound having a (—Si—C—) bond in the main chain in the molecule.
- a polycarbosilane type compound used for this invention what contains the repeating unit represented by following formula (d) is preferable.
- Rw and Rv each independently represent a hydrogen atom, a hydroxyl group, an alkyl group, an aryl group, an alkenyl group, or a monovalent heterocyclic group.
- a plurality of Rw and Rv may be the same or different.
- alkyl group, aryl group, and alkenyl group of Rw and Rv include the same groups as those exemplified as Rx and the like.
- These groups may have a substituent such as an alkyl group, an aryl group, an alkoxy group or an aryloxy group at an arbitrary position.
- R represents an alkylene group, an arylene group or a divalent heterocyclic group.
- alkylene group of R include alkylene groups having 1 to 10 carbon atoms such as a methylene group, an ethylene group, a propylene group, a trimethylene group, a tetramethylene group, a pentamethylene group, a hexamethylene group, and an octamethylene group.
- arylene group examples include arylene groups having 6 to 20 carbon atoms such as a phenylene group, a 1,4-naphthylene group, and a 2,5-naphthylene group.
- divalent heterocyclic group a divalent group derived from a 3- to 10-membered heterocyclic compound containing at least one hetero atom such as an oxygen atom, a nitrogen atom, or a sulfur atom in addition to a carbon atom is particularly preferable. There are no restrictions.
- the alkylene group, arylene group, and divalent heterocyclic group of R may have a substituent such as an alkyl group, an aryl group, an alkoxy group, or a halogen atom at an arbitrary position.
- Rw and Rv are each independently a hydrogen atom, an alkyl group or an aryl group, and more preferably include a repeating unit in which R is an alkylene group or an arylene group, Rw, More preferably, each Rv independently represents a hydrogen atom or an alkyl group, and R includes an alkylene group.
- the weight average molecular weight of the polycarbosilane compound having a repeating unit represented by the formula (d) is usually from 400 to 12,000.
- the method for producing the polycarbosilane compound is not particularly limited, and a conventionally known method can be adopted.
- the polysilane compound is a polymer compound having a (—Si—Si—) bond in the molecule.
- Examples of such polysilane compounds include compounds having at least one repeating unit selected from structural units represented by the following formula (e).
- Rq and Rr are the same or different and are a hydrogen atom, an alkenyl group, a cycloalkyl group, a cycloalkenyl group, an aryl group, a hydroxyl group, an alkoxy group, a cycloalkyloxy group, an aryloxy group, an aralkyloxy group.
- a group, an amino group optionally having a substituent, a silyl group, or a halogen atom is represented.
- alkyl group, alkenyl group, and aryl group of Rq and Rr examples include the same as those exemplified for Rx and the like.
- Examples of the cycloalkyl group include cycloalkenyl groups having 3 to 10 carbon atoms such as a cyclopentyl group, a cyclohexyl group, and a methylcyclohexyl group.
- Examples of the cycloalkenyl group include cycloalkenyl groups having 4 to 10 carbon atoms such as a cyclopentenyl group and a cyclohexenyl group.
- alkoxy group examples include alkoxy groups having 1 to 10 carbon atoms such as a methoxy group, an ethoxy group, a propoxy group, an isopropoxy group, a butoxy group, a t-butoxy group, and a pentyloxy group.
- cycloalkyloxy group examples include cycloalkyloxy groups having 3 to 10 carbon atoms such as a cyclopentyloxy group and a cyclohexyloxy group.
- Examples of the aryloxy group include aryloxy groups having 6 to 20 carbon atoms such as a phenoxy group and a naphthyloxy group.
- Examples of the aralkyloxy group include aralkyloxy groups having 7 to 20 carbon atoms such as benzyloxy group, phenethyloxy group, and phenylpropyloxy group.
- the amino group which may have a substituent is an amino group; an N-mono or N, N-disubstituted amino group substituted with an alkyl group, a cycloalkyl group, an aryl group, an aralkyl group, an acyl group, or the like. Is mentioned.
- silyl group examples include Si1-10 silanyl groups (preferably Si1-6 silanyl group) such as silyl group, disiranyl group, and trisilanyl group, substituted silyl groups (eg, alkyl group, cycloalkyl group, aryl group, aralkyl group, alkoxy group) A substituted silyl group substituted with a group, etc.).
- substituted silyl groups eg, alkyl group, cycloalkyl group, aryl group, aralkyl group, alkoxy group
- halogen atom examples include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom.
- the cycloalkyl group, cycloalkenyl group, alkoxy group, cycloalkyloxy group, aryloxy group, aralkyloxy group, silyl group may have a substituent such as a halogen atom, an alkyl group, an aryl group, or an alkoxy group. Good.
- a compound containing a repeating unit represented by the formula (e) is preferable.
- Rq and Rr are each independently A compound containing a repeating unit which is a hydrogen atom, a hydroxyl group, an alkyl group, an aryl group, an alkoxy group, an amino group or a silyl group is more preferable.
- Rq and Rr are each independently a hydrogen atom, More preferred are compounds containing a repeating unit which is an alkyl group or an aryl group.
- the form of the polysilane compound is not particularly limited, and may be a random copolymer, a block even if it is a homopolymer such as acyclic polysilane (linear polysilane, branched polysilane, network polysilane, etc.) or cyclic polysilane. Copolymers such as copolymers, alternating copolymers, and comb copolymers may also be used.
- the terminal group (terminal substituent) of the polysilane compound is a hydrogen atom, a halogen atom (chlorine atom, etc.), an alkyl group, a hydroxyl group, an alkoxy group, silyl It may be a group or the like.
- polysilane compound examples include polydialkylsilanes such as polydimethylsilane, poly (methylpropylsilane), poly (methylbutylsilane), poly (methylpentylsilane), poly (dibutylsilane), and poly (dihexylsilane).
- Homopolymers such as polydiarylsilanes such as poly (diphenylsilane), poly (alkylarylsilanes) such as poly (methylphenylsilane); dialkylsilanes such as dimethylsilane-methylhexylsilane copolymers and other dialkylsilanes Copolymer, arylsilane-alkylarylsilane copolymer such as phenylsilane-methylphenylsilane copolymer, dimethylsilane-methylphenylsilane copolymer, dimethylsilane-phenylhexylsilane copolymer, dimethylsilane-methylnaphtho And the like; Rushiran copolymer, methyl propyl silane - copolymers of alkyl aryl silane copolymer - dialkyl silane and methyl phenyl silane copolymer.
- the average degree of polymerization (for example, the number average degree of polymerization) of the polysilane compound is usually about 5 to 400, preferably about 10 to 350, and more preferably about 20 to 300.
- the weight average molecular weight of the polysilane compound is about 300 to 100,000, preferably 400 to 50,000, and more preferably about 500 to 30,000.
- polysilane compounds are known substances and can be produced using known methods.
- the polysilazane compound is a polymer compound having a (—Si—N—) bond in the molecule.
- Such polysilazane compounds include those represented by the formula (f)
- 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 an arbitrary natural number.
- Rm, Rp, and Rt each independently represent a non-hydrolyzable group such as a hydrogen atom, an alkyl group, a cycloalkyl group, an alkenyl group, an aryl group, or an alkylsilyl group.
- alkyl group, alkenyl group, and aryl group are the same as those exemplified for Rx and the like.
- Examples of the cycloalkyl group are the same as those exemplified for Rq and the like.
- alkylsilyl group examples include a trimethylsilyl group, a triethylsilyl group, a triisopropylsilyl group, a tri-t-butylsilyl group, a methyldiethylsilyl group, a dimethylsilyl group, a diethylsilyl group, a methylsilyl group, and an ethylsilyl group.
- Rm, Rp, and Rt 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 (f) include inorganic polysilazanes in which Rm, Rp, and Rt are all hydrogen atoms, and organic polysilazanes in which at least one of Rm, Rp, and Rt is not a hydrogen atom. It may be.
- inorganic polysilazane the following formula
- perhydropolysilazane having a linear structure, a branched structure and a cyclic structure in the molecule.
- organic polysilazane (I) — (Rm′SiHNH) — (Rm ′ represents the same alkyl group, cycloalkyl group, alkenyl group, aryl group or alkylsilyl group as Rm. The same applies to the following Rm ′).
- the organic polysilazane can be produced by a conventionally known method. For example, the following formula
- m represents 2 or 3
- X represents a halogen atom
- R 1 represents any of the substituents of Rm, Rp, Rt, Rm ′, Rp ′, and Rt ′ described above.
- the secondary amine, ammonia, and primary amine to be used may be appropriately selected according to the structure of the target polysilazane compound.
- a modified polysilazane compound can also be used as the polysilazane compound.
- the modified polysilazane include, for example, a polymetallosilazane containing a metal atom (the metal atom may be crosslinked), and repeating units of [(SiH 2 ) j (NH) h )] and [(SiH 2 ) i O] (wherein, j, h, i are each independently 1, 2 or 3.
- polysiloxazane JP 62-195024 discloses represented by)
- boron compound polysilazane Polyborosilazane produced by reacting polysilazane (Japanese Patent Laid-Open No.
- polymetallosilazane produced by reacting polysilazane and metal alkoxide Japanese Patent Laid-Open No. 63-81122, etc.
- inorganic silazane high polymer And modified polysilazanes such as JP-A-1-138108
- copolymerized silazanes obtained by introducing an organic component into polysilazane such as JP-A-2-175726
- Low-temperature ceramicized polysilazane Japanese Patent Laid-Open No.
- perhydropolysilazane with alcohol such as methanol or hexamethyldisilazane at the terminal N atom
- alcohol such as methanol or hexamethyldisilazane at the terminal N atom
- modified polysilazanes obtained by addition JP-A-5-345826, JP-A-4-63833
- inorganic polysilazane in which Rm, Rp, and Rt are all hydrogen atoms, and organic polysilazane in which at least one of Rm, Rp, and Rt is not a hydrogen atom are preferable and easily available. From the viewpoint of forming an injection layer having excellent gas barrier properties, inorganic polysilazane is more preferable.
- the polysilazane type compound can also use the commercial item marketed as a glass coating material etc. as it is.
- the polymer layer forming the gas barrier layer may contain other components in addition to the above-described polymer compound as long as the object of the present invention is not impaired.
- other components include curing agents, other polymers, anti-aging agents, light stabilizers, and flame retardants.
- 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 from the viewpoint of forming a gas barrier layer having excellent gas barrier properties.
- the method for forming the polymer layer is not particularly limited.
- a layer forming solution containing at least one kind of polymer compound, and optionally other components, a solvent, and the like may be formed on the substrate or desired by a known coating method.
- coating on the primer layer formed on the base material by and drying the obtained coating film moderately is mentioned.
- the coating apparatus known apparatuses such as a spin coater, a knife coater, and a gravure coater can be used.
- the coating film it is preferable to heat the coating film in order to dry the obtained coating film and improve the gas barrier property of the film.
- heating and drying methods conventionally known drying methods such as hot air drying, hot roll drying, and infrared irradiation can be employed.
- the heating temperature is usually 80 to 150 ° C.
- the heating time is usually several tens of seconds to several tens of minutes.
- the thickness of the formed polymer layer is not particularly limited, but is usually 20 nm to 1000 nm, preferably 30 to 500 nm, more preferably 40 to 200 nm. In the present invention, even if the thickness of the polymer layer is nano-order, a film having sufficient gas barrier performance can be obtained by implanting ions as will be described later.
- the amount of ions implanted into the polymer layer may be appropriately determined according to the purpose of use of the film to be formed (necessary gas barrier properties, transparency, etc.).
- ions to be implanted 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, propane, butane Ions of alkane gases such as ethylene, propylene, butene and pentene; ions of alkadiene gases such as pentadiene and butadiene; alkyne gases such as acetylene and methylacetylene Ions of aromatic hydrocarbon gases such as benzene, toluene, xylene, indene, naphthalene and phenanthrene; ions of cycloalkane gases such as cyclopropane and cyclohexane; cycloalkene gases such as cyclopentene and cyclohexene Like Down; gold, silver, copper, platinum, nickel, palladium, ions
- One kind of ion is preferred.
- the method of implanting ions is not particularly limited, and examples thereof include a method of irradiating ions accelerated by an electric field (ion beam), a method of implanting ions in plasma, and the like. Among them, in the present invention, the latter method of implanting plasma ions is preferable because a gas barrier film can be easily obtained.
- a method As the plasma ion implantation method, (A) a method in which ions existing in plasma generated using an external electric field are implanted into the surface portion of the polymer layer, or (B) the layer without using an external electric field.
- a method is preferred in which ions existing in plasma generated only by an electric field generated by a negative high voltage pulse applied to are implanted into the surface portion of the polymer layer.
- the pressure during ion implantation is preferably 0.01 to 1 Pa.
- the pressure during plasma ion implantation is in such a range, ions can be implanted easily and efficiently uniformly, and the target gas barrier layer can be efficiently formed.
- the processing operation is simple, and the processing time can be greatly shortened. Further, the entire layer can be processed uniformly, and ions in the plasma can be continuously injected into the surface portion of the layer with high energy when a negative high voltage pulse is applied. Furthermore, without requiring other special means such as radio frequency (hereinafter abbreviated as “RF”) or a high-frequency power source such as a microwave, By simply applying a negative high voltage pulse to the layer, a good quality ion-implanted layer can be uniformly formed on the surface of the layer.
- RF radio frequency
- a good quality ion-implanted layer can be uniformly formed on the surface of the layer.
- the pulse width when applying a negative high voltage pulse is preferably 1 to 15 ⁇ sec.
- the pulse width is in such a range, ions can be implanted more easily and efficiently and uniformly.
- the applied voltage when generating plasma is preferably -1 to -50 kV, more preferably -1 to -30 kV, and particularly preferably -5 to -20 kV. If ion implantation is performed at an applied voltage greater than ⁇ 1 kV, the ion implantation amount (dose amount) becomes insufficient, and desired performance cannot be obtained. On the other hand, if ion implantation is performed at a value smaller than ⁇ 50 kV, the film is charged at the time of ion implantation, and problems such as coloring of the film occur, which is not preferable.
- Examples of the ion species to be plasma ion implanted include those exemplified as the ions to be implanted.
- a plasma ion implantation apparatus is used when ions in plasma are implanted into the surface of the layer.
- a plasma ion implantation apparatus ( ⁇ ) a high-frequency power is superimposed on a feedthrough that applies a negative high-voltage pulse to a polymer layer (hereinafter also referred to as “ion-implanted layer”).
- ion-implanted layer a polymer layer
- a device that uniformly surrounds the periphery of the ion-implanted layer with plasma and attracts, implants, collides and deposits ions in the plasma Japanese Patent Laid-Open No.
- a plasma ion implantation apparatus that generates plasma using an external electric field such as a high-frequency power source such as a microwave and applies high voltage pulses to attract and inject ions in the plasma
- a plasma ion implantation apparatus that implants ions in plasma generated only by an electric field generated by applying a high voltage pulse without using an external electric field.
- the plasma ion implantation apparatus ( ⁇ ) or ( ⁇ ) because the processing operation is simple, the processing time can be greatly shortened, and it is suitable for continuous use.
- Examples of the method using the plasma ion implantation apparatus ( ⁇ ) and ( ⁇ ) include those described in International Publication WO2010 / 021326.
- the plasma generating means for generating plasma is also used by the high voltage pulse power source, other special means such as a high frequency power source such as RF and microwave are used.
- a high frequency power source such as RF and microwave.
- a portion that has been modified by ion implantation in the surface portion by generating a plasma simply by applying a negative high-voltage pulse without the need to inject ions in the plasma continuously into the surface portion of the polymer layer. It is possible to mass produce a gas barrier film having a polymer layer having a gas barrier layer, that is, a gas barrier layer.
- the thickness of the portion into which ions are implanted can be controlled by implantation conditions such as ion type, applied voltage, and processing time, and may be determined according to the thickness of the polymer layer, the purpose of use of the gas barrier film, etc. Usually, it is 10 to 1000 nm.
- the ion implantation can be confirmed by performing an elemental analysis measurement in the vicinity of 10 nm from the surface of the polymer layer using X-ray photoelectron spectroscopy (XPS).
- XPS X-ray photoelectron spectroscopy
- Gas barrier film laminate The gas barrier film laminate of the present invention is obtained by laminating at least two gas barrier films via the bonding layer.
- the shape of the gas barrier film laminate of the present invention is not particularly limited. For example, a sheet form etc. are mentioned.
- the number of gas barrier films to be laminated is not particularly limited as long as it is 2 or more.
- the number of laminated gas barrier films is usually 2-5.
- the method for bonding the gas barrier film and the bonding layer is not particularly limited, and the gas barrier film and the bonding layer can be bonded using a known method using an apparatus such as a laminator.
- the laminate configuration is not particularly limited as long as at least two gas barrier films are laminated via the bonding layer.
- the thickness of the gas barrier film laminate of the present invention is usually 100 ⁇ m or less, preferably 1 to 50 ⁇ m. When the thickness of the gas barrier film laminate is 100 ⁇ m or less, weight reduction of an electronic member using the gas barrier film laminate can be achieved.
- FIG. 1A An example of the gas barrier film laminated body of this invention is shown to Fig.1 (a), (b).
- the gas barrier film laminate 100A shown in FIG. 1A is configured so that the gas barrier layer 2a and the gas barrier layer 2b of the two gas barrier films 30a and 30b are adjacent to the bonding layer 20 (more specifically, the adhesion of the bonding layer 20).
- Layer structure laminated so as to be adjacent to the adhesive layers 4a and 4b base film B 1a / gas barrier layer 2a / adhesive layer 4a / base film A 3 / adhesive layer 4b / gas barrier layer 2b / base film) B 1b).
- the base layer 1a of the gas barrier film 30a is adjacent to the bonding layer 20 (more specifically, adjacent to the pressure-sensitive adhesive layer 4a of the bonding layer 20).
- the layer structure (gas barrier layer 2a /) is laminated so that the gas barrier layer 2b of the gas barrier film 30b is adjacent to the bonding layer 20 (more specifically, adjacent to the adhesive layer 4b of the bonding layer 20). It has base film B 1a / adhesive layer 4a / base film A 3 / adhesive layer 4b / gas barrier layer 2b / base film B 1b).
- At least one gas barrier film is laminated so that the gas barrier layer of the gas barrier film is adjacent to the bonding layer.
- the gas barrier layers of the two gas barrier films are laminated so as to be adjacent to the bonding layer.
- the method for laminating the at least two gas barrier films with a bonding layer interposed therebetween is not particularly limited, and a known method may be mentioned.
- the gas barrier film laminate 100A can be manufactured as follows.
- the adhesive layer 4 is formed on the peeling film 5, and the two peeling films 10 (10a, 10b) with an adhesive layer are produced.
- FIG. 2B after the adhesive layer 4a of the release film 10a with the adhesive layer and the base film A3 are bonded together, another sheet as shown in FIG.
- the method of bonding is not particularly limited, and examples thereof include a method using a known laminator.
- FIG. 2 (e) two sheets (30a, 30b) of a gas barrier film 30 having a base film B1 and a gas barrier layer 2 provided on the base film shown in FIG.
- the release film 5a of the laminate 20 ′ for bonding layer formation obtained by the above method is peeled off, and the gas barrier film 30a is applied to the exposed pressure-sensitive adhesive layer 4a surface.
- the release film 5b is peeled off, and another gas barrier film 30b is bonded at the exposed pressure-sensitive adhesive layer 4b surface with the gas barrier layer 2b.
- a gas barrier film laminate 100A can be obtained.
- the gas barrier film laminate of the present invention may be laminated with other layers such as a protective layer, a conductor layer, and a primer layer as desired.
- the position where other layers are stacked is not particularly limited.
- the other layer may be one or more of the same or different layers.
- the protective layer is required to have good transparency and good scratch resistance, and plays a role of protecting the gas barrier film laminate when an impact is applied from the outside.
- a protective layer is laminated
- the material constituting the protective layer is not particularly limited, and known materials can be used.
- a silicon-containing compound a polymerizable composition comprising a photopolymerizable compound comprising a photopolymerizable monomer and / or a photopolymerizable prepolymer, and a polymerization initiator that generates radicals at least in the visible light region; a polyester resin , Polyurethane resins (particularly polyacrylic polyols, polyester polyols, polyether polyols and isocyanate compounds) and acrylic resins, polycarbonate resins, vinyl chloride / vinyl acetate copolymers, polyvinyl butyral resins And resins such as nitrocellulose-based resins; alkyl titanates; ethyleneimine; These materials can be used alone or in combination of two or more.
- the protective layer is formed by applying a solution for forming a protective layer obtained by dissolving or dispersing the material constituting the protective layer in an appropriate solvent onto the layer to be laminated by a known method, and drying the obtained coating film. It can be formed by heating if desired.
- a normal wet coating method can be used as a method for applying the protective layer forming solution. Examples include dipping method, roll coating, gravure coating, knife coating, air knife coating, roll knife coating, die coating, screen printing method, spray coating, gravure offset method and the like.
- the coating film of the solution for forming the protective layer As a method for drying the coating film of the solution for forming the protective layer, conventionally known drying methods such as hot air drying, hot roll drying, and infrared irradiation can be employed.
- the thickness of the protective layer can be appropriately selected according to the purpose of the gas barrier film laminate, but is preferably 0.05 to 50 ⁇ m, more preferably 0.1 to 10 ⁇ m, and further preferably 0.2 to 5 ⁇ m.
- the scratch resistance is not sufficient, which is not preferable.
- the thickness is larger than 50 ⁇ m, curling due to distortion at the time of curing tends to occur, which is not preferable.
- Conductor layer examples of the material constituting the conductor layer include metals, alloys, metal oxides, electrically conductive compounds, and mixtures thereof. Specifically, tin oxide (ATO) doped with antimony; tin oxide (FTO) doped with fluorine; conductive such as tin oxide, zinc oxide, indium oxide, indium tin oxide (ITO), indium zinc oxide (IZO) Metal such as gold, silver, chromium and nickel; mixtures of these metals and conductive metal oxides; inorganic conductive materials such as copper iodide and copper sulfide; organic conductive materials such as polyaniline, polythiophene and polypyrrole Material, etc.
- ATO tin oxide
- FTO tin oxide
- FTO tin oxide
- conductive such as tin oxide, zinc oxide, indium oxide, indium tin oxide (ITO), indium zinc oxide (IZO) Metal such as gold, silver, chromium and nickel; mixtures of these metals
- the conductor layer may be formed by laminating a plurality of layers made of these materials.
- the method for forming the conductor layer include a vapor deposition method, a sputtering method, an ion plating method, a thermal CVD method, a plasma CVD method, and the like.
- the sputtering method is preferable because the conductor layer can be easily formed.
- the sputtering method introduces a discharge gas (such as argon) into a vacuum chamber, applies a high-frequency voltage or a direct current voltage between the target and the substrate to turn the discharge gas into plasma, and collides the plasma with the target material.
- a discharge gas such as argon
- This is a method of obtaining a thin film by skipping and attaching to a substrate.
- a target made of a material for forming the conductor layer is used as the target.
- the thickness of the conductor layer may be appropriately selected according to its use.
- the thickness is usually 10 nm to 50 ⁇ m, preferably 20 nm to 20 ⁇ m.
- the surface resistivity of the obtained conductor layer is usually 1000 ⁇ / ⁇ or less.
- the formed conductor layer may be patterned as necessary.
- the patterning method include chemical etching by photolithography and the like, physical etching using a laser and the like, vacuum deposition method using a mask, sputtering method, lift-off method, printing method, and the like.
- Primer layer plays the role which improves the interlayer adhesiveness of the base film B, a gas barrier layer, or another layer. By providing the primer layer, interlayer adhesion and surface smoothness can be improved. It does not specifically limit as a material which comprises a primer layer, A well-known thing can be used.
- a silicon-containing compound for example, a silicon-containing compound; a polymerizable composition comprising a photopolymerizable compound comprising a photopolymerizable monomer and / or a photopolymerizable prepolymer, and a polymerization initiator that generates radicals at least in the visible light region; a polyester resin , Polyurethane resins (particularly polyacrylic polyols, polyester polyols, polyether polyols and isocyanate compounds) and acrylic resins, polycarbonate resins, vinyl chloride / vinyl acetate copolymers, polyvinyl butyral resins And resins such as nitrocellulose-based resins; alkyl titanates; ethyleneimine; These materials can be used alone or in combination of two or more.
- a polyester resin Polyurethane resins (particularly polyacrylic polyols, polyester polyols, polyether polyols and isocyanate compounds) and acrylic resins, polycarbonate resins, vinyl chloride /
- a primer layer forming solution obtained by dissolving or dispersing the material constituting the primer layer in an appropriate solvent is applied to one side or both sides of the base material layer or other layers, and the resulting coating film is obtained.
- a normal wet coating method can be used as a method of applying the primer layer forming solution to the base film B or other layers. Examples include dipping method, roll coating, gravure coating, knife coating, air knife coating, roll knife coating, die coating, screen printing method, spray coating, gravure offset method and the like.
- the coating film of the primer layer forming solution As a method for drying the coating film of the primer layer forming solution, a conventionally known drying method such as hot air drying, hot roll drying, infrared irradiation or the like can be employed.
- the thickness of the primer layer is usually 10 to 1000 nm, preferably 20 to 4000 nm.
- the gas barrier film laminate of the present invention reduces the concentration of stress due to bending at the interface between the gas barrier film on the thick film side and the joining layer when the laminate is folded by using the joining layer having the characteristics described above. This solves the problem that peeling occurs at the interface between the gas barrier film on the thick film side and the pressure-sensitive adhesive layer, and floating occurs.
- the electronic device member of the present invention comprises the gas barrier film 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 has high light transmittance and excellent heat resistance, it is suitable as a member for electronic devices such as a display member such as a touch panel, a liquid crystal display and an EL display; a back sheet for solar cell;
- the electronic device of the present invention includes the electronic device member of the present invention.
- Specific examples include a touch panel, a liquid crystal display, an organic EL display, an inorganic EL display, electronic paper, a solar battery, and the like.
- a polyethylene terephthalate film (Mitsubishi Resin, PET25T-100, thickness 25 ⁇ m) is coated with a polysilazane compound [coating material containing perhydropolysilazane as a main component ( Clariant Japan Co., Ltd., Aquamica NL110-20)] was applied by spin coating and heated at 120 ° C. for 1 minute to form a polysilazane layer having a thickness of 150 nm and containing perhydropolysilazane on the PET film. .
- argon (Ar) was ion-implanted into the surface of the obtained polysilazane layer using a plasma ion implantation apparatus under the following conditions to form a gas barrier layer, thereby producing a gas barrier film A.
- 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.
- Plasma generation gas Ar Gas flow rate: 100sccm Duty ratio: 0.5%
- Applied voltage -6kV
- 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): 200 seconds
- a gas barrier film B was produced in the same manner as described above except that a polyethylene terephthalate film (PET film) (manufactured by Mitsubishi Plastics, Diafoil K205-6E, thickness 6 ⁇ m) was used as the base film B.
- PET film polyethylene terephthalate film
- Resin film 1 PET film (manufactured by Mitsubishi Plastics, trade name: Diafoil K100-2.0W, thickness 2 ⁇ m, tensile elastic modulus at 23 ° C., 3300 MPa)
- Resin film 2 Cycloolefin resin film (manufactured by JSR, trade name: Arton, thickness 5 ⁇ m, tensile modulus at 23 ° C., 4300 MPa)
- Resin film 3 Polysulfone resin film (manufactured by BASF, trade name: ULTRASON S3030, thickness 2 ⁇ m, tensile modulus at 23 ° C., 2400 MPa)
- Resin film 4 Polysulfone resin film (manufactured by BASF, trade name: ULTRASON S3030, thickness 5 ⁇ m, tensile modulus at 23 °
- Example 1 A pressure-sensitive adhesive composition A was applied to the release layer surface of a release film (SP-PET 381031 manufactured by Lintec Corporation) provided with a silicone release layer on one side of a 38 ⁇ m thick PET film by a comma direct coating method.
- the obtained coating film was dried at 100 ° C. for 1 minute to obtain a release film A with an adhesive layer having an adhesive layer with a thickness of 2 ⁇ m.
- the adhesive layer surface of the release film A with the adhesive layer and the resin film 1 are bonded together, and then the adhesive layer surface of the other release film A with the adhesive layer is bonded together to obtain the laminate A for forming the bonding layer. It was.
- One release film of the laminate A for bonding layer formation is peeled off, the exposed pressure-sensitive adhesive layer surface and the gas barrier layer surface of the gas barrier film A produced by the above method are bonded together, and then another release film is peeled off Then, the exposed pressure-sensitive adhesive layer surface and the gas barrier layer surface of the gas barrier film B were bonded together to produce a gas barrier film laminate A.
- Example 2 In Example 1, a gas barrier film laminate B was produced in the same manner as in Example 1 except that the resin film 2 was used instead of the resin film 1 as the base film of the bonding layer.
- the pressure-sensitive adhesive composition A was applied to the surface of the release layer of the release film (Lintec Corp., SP-PET381031) by the comma direct coating method, and the resulting coating film was dried at 100 ° C. for 1 minute to obtain a thickness.
- a release film B with an adhesive layer having a 6 ⁇ m adhesive layer was obtained.
- the release film was peeled off.
- the exposed pressure-sensitive adhesive layer surface and the gas barrier layer surface of the gas barrier film B were bonded together to produce a gas barrier film laminate C without the base film A.
- Comparative Example 2 In Comparative Example 1, the thickness of the pressure-sensitive adhesive layer was changed to 10 ⁇ m to obtain a release film C with a pressure-sensitive adhesive layer, and the gas barrier without the base film A was the same as in Comparative Example 1 except that this was used. A film laminate D was produced.
- Example 3 a gas barrier film laminate E was produced in the same manner as in Example 1 except that the resin film 3 was used instead of the resin film 1 as the base film of the bonding layer.
- Example 4 a gas barrier film laminate F was produced in the same manner as in Example 1 except that the resin film 4 was used instead of the resin film 1 as the base film of the bonding layer.
- the release film was peeled off, and the exposed pressure-sensitive adhesive layer surface and the gas barrier film surface of the gas barrier film A were bonded together and reciprocated once with a 2 kg roll to obtain a test piece. .
- the adhesive strength (N / 25 mm) at a peeling rate of 300 mm / min and 180 ° was measured according to JISZ0237. The measurement results are shown in Table 1.
- Table 1 shows the following.
- the gas barrier film laminates A and B obtained in Examples 1 and 2 are excellent in bending resistance.
- Comparative Examples 1 and 2 when only the pressure-sensitive adhesive layer is used as the bonding layer, the bending resistance is poor regardless of the thickness.
- Comparative Examples 3 and 4 when a base film made of a synthetic resin having a tensile elastic modulus at 23 ° C. of less than 3,000 MPa is used, the bending resistance is poor.
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Abstract
Description
スバリアフィルム積層体からなる電子デバイス用部材、及び前記電子デバイス用部材を備
える電子デバイスに関する。
レイ等の電子部材用の基板として、薄型化、軽量化、フレキシブル化や耐衝撃性等を実現
するために、ガラス板に代えて透明プラスチックフィルムを用いることが検討されている
。しかしながら、プラスチックフィルムは、ガラス板に比べて水蒸気や酸素等を透過しやすく、電子部材内部の素子の劣化を起こしやすいという問題があった。
特許文献2には、プラスチックフィルムと、該プラスチックフィルムの少なくとも一方の面に、ポリオルガノシルセスキオキサンを主成分とする樹脂層を積層してなるガスバリア性積層体が開示されている。
また、特許文献3には、第1の透明プラスチックフィルム基材の上に透明ガスバリア層が形成され、前記透明ガスバリア層の上に透明粘着剤層を介して、第2の透明プラスチックフィルム基材が配置されている透明フィルムが開示されている。
本発明者らは、さらにガスバリア性に優れる積層体を得るべく検討し、少なくとも2枚のガスバリアフィルムを、粘着剤層を介して積層した積層体を案出した。
しかしながら、粘着剤層を介してガスバリアフィルム同士を貼り合せた積層体は、折り曲げたときに、ガスバリアフィルム同士の厚みの差が大きい場合、顕著にガスバリアフィルムと粘着剤層との界面で剥離が生じ、浮きが発生することがあった。これは、ガスバリアフィルム同士の厚みの差が大きいことに起因して、ガスバリアフィルムと粘着剤層との界面で曲げ応力が集中するために起こるものと考えられる。
(1)少なくとも2枚のガスバリアフィルムが、接合層を介して積層されたガスバリアフィルム積層体であって、前記接合層が、23℃における引張弾性率が3,000~10000MPaの合成樹脂からなる基材フィルムAの両面に、それぞれ粘着剤層が隣接して積層されてなるものであることを特徴とするガスバリアフィルム積層体。
(2)前記基材フィルムAの厚みが0.5~25μmである、(1)に記載のガスバリアフィルム積層体。
(3)前記基材フィルムAの両面に積層された粘着剤層の厚みが、それぞれ、0.5~25μmである、(1)に記載のガスバリアフィルム積層体。
(4)前記粘着剤層の前記ガスバリアフィルムに対する180°ひきはがし粘着力が、2.0N/25mm以上である、(1)に記載のガスバリアフィルム積層体。
(5)前記接合層の厚みが75μm以下である、(1)に記載のガスバリアフィルム積層体。
(6)前記接合層の一方の面に積層されたガスバリアフィルムが、該接合層の他方の面に積層されたガスバリアフィルムよりも厚みが小さいものである、(1)に記載のガスバリアフィルム積層体。
(7)(前記接合層の一方の面に積層されたガスバリアフィルムの厚さ)/(前記接合層の他方の面に積層されたガスバリアフィルムの厚さ)の値が、0.05~1.0である、(1)に記載のガスバリアフィルム積層体。
(8)前記ガスバリアフィルムの少なくとも1枚が、基材フィルムBと、該基材フィルムB上に設けられた少なくとも1層のガスバリア層とを有するものである、(1)に記載のガスバリアフィルム積層体。
(9)前記ガスバリア層が、高分子ケイ素化合物からなる層にイオンが注入されて形成された層である、(8)に記載のガスバリアフィルム積層体。
(10)前記ガスバリアフィルムが、そのガスバリア層が前記接合層と隣接するように積層されたものである、(8)に記載のガスバリアフィルム積層体。
(11)厚みが100μm以下である、(1)に記載のガスバリアフィルム積層体。
(12)前記(1)に記載のガスバリアフィルム積層体からなる電子デバイス用部材。
(13)前記(12)に記載の電子デバイス用部材を備える電子デバイス。
本発明のガスバリアフィルム積層体は、太陽電池や、液晶ディスプレイ、エレクトロルミネッセンス(EL)ディスプレイ等の電子部材用に好適である。
本発明の電子デバイス用部材は、ガスバリア性及び耐折り曲げ性に優れる本発明のガスバリアフィルム積層体からなるものであるため、タッチパネル、電子ペーパー、有機・無機ELのフレキシブルディスプレイ、太陽電池等の電子デバイス等に好適に用いることができる。
本発明のガスバリアフィルム積層体は、少なくとも2枚のガスバリアフィルムが、接合層を介して積層されたガスバリアフィルム積層体であって、前記接合層が、23℃における引張弾性率が3,000~10,000MPaの合成樹脂からなる基材フィルムの両面に、それぞれ粘着剤層が隣接して積層されてなるものであることを特徴とする。
本発明に用いる接合層は、23℃における引張弾性率が3,000~10,000MPaの合成樹脂からなる基材フィルム(以下、接合層に用いられるこの基材フィルムを、「基材フィルムA」という。)の両面に、それぞれ粘着剤層が隣接して積層されてなるものである。
基材フィルムAを構成する合成樹脂の、23℃における引張弾性率は、3,000~10,000MPa、好ましくは、3,000~5,000MPaである。前記引張弾性率が3,000MPa未満のときは、ガスバリアフィルム積層体を折り曲げたときに、浮きが発生し易くなる。一方、前記引張弾性率が10,000MPaを超えると、ガスバリアフィルム積層体の屈曲性が低下する。
なお、23℃における引張弾性率は、JIS K7127に準じて測定されたものである。
トン、ポリオレフィン、ポリエステル、ポリカーボネート、ポリスルフォン、ポリエーテルスルフォン、ポリフェニレンスルフィド、ポリアリレート、アクリル系樹脂、シクロオレフィン系ポリマー、芳香族系重合体等が挙げられる。
これらの中でも、透明性に優れ、汎用性があることから、ポリエステル又はシクロオレフィン系ポリマーが好ましい。
シクロオレフィン系ポリマーとしては、ノルボルネン系重合体、単環の環状オレフィン系重合体、環状共役ジエン系重合体、ビニル脂環式炭化水素重合体、及びこれらの水素化物が挙げられる。
2つの粘着剤層の種類や厚みは、同一であってもよく、異なっていてもよい。
なお、本発明において、「前記粘着剤層の前記ガスバリアフィルムに対する180°ひきはがし粘着力」は、実施例で説明するように、粘着剤層の一方の面にポリエステルフィルムを裏打ちし、粘着力試験用粘着フィルムとし、この粘着力試験用粘着フィルムのガスバリアフィルムに対する、JIS Z0237(2000)に準じて測定される、180°ひきはがし粘着力を言うものとする。
粘着剤の種類は、特に制限されない。本発明においては、アクリル系、ゴム系、ポリエステル系、ウレタン系、シリコーン系などの公知の粘着剤を用いることができる。なかでも、優れた粘着力が得られることから、アクリル系粘着剤が好ましい。
アクリル系共重合体とは、(メタ)アクリル酸又は(メタ)アクリル酸エステル由来の繰り返し単位を有する共重合体である。「(メタ)アクリル酸」とは、アクリル酸とメタクリル酸の両方を意味し、「(メタ)アクリル酸エステル」とは、アクリル酸エステルとメタクリル酸エステルの両方を意味する。
また、アクリル系共重合体は、本発明の効果を阻害しない限り、上記以外の繰り返し単位を有するものであってもよい。
アクリル系共重合体の製造に用いる単量体としては、官能基を有するアクリル系単量体、官能基を有しないアクリル系単量体、及びこれらの単量体と共重合可能なその他の単量体が挙げられる。
これらのなかでも、(メタ)アクリル酸、(メタ)アクリル酸2-カルボキシエチル等のカルボキシル基を有するアクリル系単量体が好ましく、(メタ)アクリル酸がより好ましい。
これらの単量体は、一種単独で、あるいは二種以上を組み合わせて用いることができる
これらのなかでも、粘着性に優れる粘着剤層を形成することができることから、炭素数4~10の炭化水素基を有する単量体が好ましく、(メタ)アクリル酸ブチルがより好ましい。
これらの単量体は、一種単独で、あるいは二種以上を組み合わせて用いることができる。
重合反応に用いる開始剤は特に制限されず、ベンゾイルパーオキサイド、ラウロイルパーオキサイド、メチルエチルケトンパーオキサイド等の過酸化物系開始剤、アゾビスイソブチロニトリル、アゾビスシアノバレリン酸、アゾビスシアノペンタン等のアゾ系開始剤等が挙げられる。
重合反応の温度や反応時間等の反応条件は、公知の条件を採用することができる。
アクリル系粘着剤には、架橋剤を添加することができる。架橋剤とは、上記の官能基と反応して架橋を形成させる化合物である。架橋剤を用いる場合、用いる架橋剤に特に制限はなく、イソシアナート系架橋剤、エポキシ系架橋剤等が挙げられる。なかでも、イソシアナート系架橋剤が好ましい。
エポキシ系架橋剤としては、分子中に2個以上のエポキシ基を有する化合物が用いられ、例えば、ソルビトールテトラグリシジルエーテル、トリメチロールプロパントリグリシジルエーテル、テトラグリシジル-1,3-ビスアミノメチルシクロヘキサン、テトラグリシジル-m-キシレンジアミン、トリグリシジル-p-アミノフェノール等が挙げられる。
架橋剤は、一種単独で、あるいは二種以上を組み合わせて用いることができる。
架橋剤の使用量は、架橋剤の種類にもよるが、アクリル系共重合体100質量部に対し、通常0.01~10質量部、好ましくは、0.05~5質量部である。
アクリル系粘着剤は、溶剤型粘着剤として好ましく用いられる。用いる溶剤は特に制限されず、公知のものを使用することができる。
重量平均分子量は、重合開始剤の量や連鎖移動剤を添加することによって調節することができる。
なお、上記重量平均分子量は、ゲルパーミエーションクロマトグラフィー(GPC)法により測定したポリスチレン換算の値である。
アクリル系粘着剤を調製する際に、アクリル系共重合体は一種単独で、あるいは二種以上を組み合わせて用いることができる。
接合層は、その厚みは、通常75μm以下、好ましくは1.5~20μm、より好ましくは2.0~15μmの範囲である。接合層の厚みが75μm以下であることで、薄く、かつ、耐折り曲げ性に優れるガスバリアフィルム積層体を得ることができる。
本発明に用いるガスバリアフィルムは、酸素や水蒸気の透過を抑制する特性(以下、「ガスバリア性」という)を有するフィルムである。
用いるガスバリアフィルムは、水蒸気透過率が、40℃、相対湿度90%の雰囲気下で、1.0g/m2/day以下のものが好ましく、0.5g/m2/day以下のものがより好ましい。このような性能を有するガスバリアフィルムを用いることで、ガスバリア性の高いガスバリアフィルム積層体を得ることができる。
従って、(接合層の一方の面に積層されたガスバリアフィルムの厚さ(薄膜側))/(該接合層の他方の面に積層されたガスバリアフィルムの厚さ(厚膜側))の値は、0.05~1.0であることが好ましく、0.1~0.5であることがより好ましく、0.2~0.3であることがさらに好ましい。
なかでも、透明性に優れ、汎用性があることから、ポリエステル、ポリアミド又はシクロオレフィン系ポリマーが好ましく、ポリエステル又はシクロオレフィン系ポリマーがより好ましい。
ポリアミドとしては、全芳香族ポリアミド、ナイロン6、ナイロン66、ナイロン共重合体等が挙げられる。
基材フィルムBは、その厚みは、通常0.5~80μm、好ましくは1~40μm、好ましくは1~30μmの範囲である。
ガスバリア層は基材フィルムBの片面に形成されていても、基材フィルムBの両面に形成されていてもよい。また、ガスバリア層は単層であってもよく、複数層積層されていてもよい。
酸化珪素、酸化アルミニウム、酸化マグネシウム、酸化亜鉛、酸化インジウム、酸化スズ等の無機酸化物;窒化珪素等の無機窒化物;無機炭化物;無機硫化物;これらの複合体である無機酸化窒化物;無機酸化炭化物;無機窒化炭化物;無機酸化窒化炭化物;高分子化合物;等が挙げられる。
なお、この場合、「ガスバリア層」とは、イオン注入により改質された部分のみを意味するのではなく、「イオン注入により改質された部分を有する高分子層」を意味する。
例えば、前記直鎖状の主鎖構造としては下記式(a)で表される構造が、ラダー状の主鎖構造としては下記式(b)で表される構造が、籠状の主鎖構造としては、例えば下記式(c)で表される構造が、それぞれ挙げられる。
Rのアルキレン基としては、メチレン基、エチレン基、プロピレン基、トリメチレン基、テトラメチレン基、ペンタメチレン基、ヘキサメチレン基、オクタメチレン基等の炭素数1~10のアルキレン基が挙げられる。
シクロアルケニル基としては、シクロペンテニル基、シクロヘキセニル基等の炭素数4~10のシクロアルケニル基が挙げられる。
シクロアルキルオキシ基としては、シクロペンチルオキシ基、シクロヘキシルオキシ基等の炭素数3~10のシクロアルキルオキシ基が挙げられる。
アラルキルオキシ基としては、ベンジルオキシ基、フェネチルオキシ基、フェニルプロピルオキシ基等の炭素数7~20のアラルキルオキシ基が挙げられる。
置換基を有していてもよいアミノ基としては、アミノ基;アルキル基、シクロアルキル基、アリール基、アラルキル基、アシル基等で置換されたN-モノ又はN,N-ジ置換アミノ基等が挙げられる。
ハロゲン原子としては、フッ素原子、塩素原子、臭素原子、ヨウ素原子等が挙げられる。
ポリシラン系化合物が非環状ポリシランである場合は、ポリシラン系化合物の末端基(末端置換基)は、水素原子であっても、ハロゲン原子(塩素原子等)、アルキル基、ヒドロキシル基、アルコキシ基、シリル基等であってもよい。
また、ポリシラン系化合物の重量平均分子量は、300~100,000、好ましくは400~50,000、さらに好ましくは500~30,000程度である。
Rm、Rp、Rtは、それぞれ独立して、水素原子、アルキル基、シクロアルキル基、アルケニル基、アリール基又はアルキルシリル基等の非加水分解性基を表す。
シクロアルキル基としては、前記Rq等で例示したのと同様のものが挙げられる。
無機ポリシラザンとしては、下記式
(i)-(Rm’SiHNH)-(Rm’は、Rmと同様のアルキル基、シクロアルキル基、アルケニル基、アリール基又はアルキルシリル基を表す。以下のRm’も同様である。)を繰り返し単位として、主として重合度が3~5の環状構造を有するもの、
(ii)-(Rm’SiHNRt’)-(Rt’は、Rtと同様のアルキル基、シクロアルキル基、アルケニル基、アリール基又はアルキルシリル基を表す。)を繰り返し単位として、主として重合度が3~5の環状構造を有するもの、
(iii)-(Rm’Rp’SiNH)-(Rp’は、Rpと同様のアルキル基、シクロアルキル基、アルケニル基、アリール基アルキルシリル基を表す。)を繰り返し単位として、主として重合度が3~5の環状構造を有するもの、
(iv)下記式で表される構造を分子内に有するポリオルガノ(ヒドロ)シラザン、
で表される繰り返し構造を有するポリシラザン等が挙げられる。
用いる2級アミン、アンモニア及び1級アミンは、目的とするポリシラザン系化合物の構造に応じて、適宜選択すればよい。
ケイ素アルコキシド付加ポリシラザン(特開平5-238827号公報)、グリシドール付加ポリシラザン(特開平6-122852号公報)、アセチルアセトナト錯体付加ポリシラザン(特開平6-306329号公報)、金属カルボン酸塩付加ポリシラザン(特開平6-299118号公報等)、
上記ポリシラザン又はその変性物に、アミン類及び/又は酸類を添加してなるポリシラザン組成物(特開平9-31333号公報)、ペルヒドロポリシラザンにメタノール等のアルコール或いはヘキサメチルジシラザンを末端N原子に付加して得られる変性ポリシラザン(特開平5-345826号公報、特開平4-63833号公報)等が挙げられる。
なお、ポリシラザン系化合物は、ガラスコーティング材等として市販されている市販品をそのまま使用することもできる。
本発明においては、高分子層の厚みがナノオーダーであっても、後述するようにイオンを注入することで、充分なガスバリア性能を有するフィルムを得ることができる。
これらのイオンは、一種単独で、あるいは二種以上を組み合わせて用いてもよい。
層に負の高電圧パルスを印加するだけで、層の表面部に良質のイオン注入層を均一に形成することができる。
前記(γ)及び(δ)のプラズマイオン注入装置を用いる方法については、国際公開WO2010/021326号公報に記載のものが挙げられる。
本発明のガスバリアフィルム積層体は、少なくとも2枚のガスバリアフィルムが、前記接合層を介して積層されてなるものである。
本発明のガスバリアフィルム積層体は、その厚みは、通常100μm以下、好ましくは1~50μmの範囲である。ガスバリアフィルム積層体の厚みが100μm以下であることで、それを用いた電子部材の軽量化等を達成することができる。
図1(a)に示すガスバリアフィルム積層体100Aは、2枚のガスバリアフィルム30a、30bの、ガスバリア層2aとガスバリア層2bが接合層20に隣接するように(より詳しくは、接合層20の粘着剤層4a、4bに隣接するように)積層された層構成(基材フィルムB 1a/ガスバリア層2a/粘着剤層4a/基材フィルムA 3/粘着剤層4b/ガスバリア層2b/基材フィルムB 1b)を有するものである。
このように、ガスバリア層が接合層と隣接することで、そのガスバリア層にはキズが発生し難くなり、水蒸気バリア性が低下しにくいガスバリアフィルム積層体を得ることができる。
次いで、図2(b)に示すように、粘着剤層付剥離フィルム10aの粘着剤層4aと基材フィルムA 3とを貼り合わせた後、図2(c)に示すように、もう1枚の粘着剤層付剥離フィルム10bの粘着剤層4bと基材フィルムA 3とを貼り合わせることで、接合層形成用積層体20’を得る。貼り合わせの方法は特に限定されず、例えば、公知のラミネーターを使用する方法が挙げられる。
次いで、図2(e)に示すように、上記方法で得られた接合層形成用積層体20’の剥離フィルム5aを剥離して、露出した粘着剤層4a面に、ガスバリアフィルム30aをガスバリア層2aで貼り合わせた後、図2(f)に示すように、剥離フィルム5bを剥離して、露出した粘着剤層4b面に、もう1枚のガスバリアフィルム30bをガスバリア層2bで貼り合わせることで、ガスバリアフィルム積層体100Aを得ることができる。
保護層としては、透明性がよく、耐擦傷性が良好なことが要件であり、外部から衝撃が加わった場合に、ガスバリアフィルム積層体を保護する役割を担うものである。
保護層が積層される位置は、特に限定されないが、ガスバリアフィルム積層体の最外層に積層されることが好ましい。
導電体層を構成する材料としては、金属、合金、金属酸化物、電気伝導性化合物、これらの混物等が挙げられる。具体的には、アンチモンをドープした酸化スズ(ATO);フッ素をドープした酸化スズ(FTO);酸化スズ、酸化亜鉛、酸化インジウム、酸化インジウムスズ(ITO)、酸化亜鉛インジウム(IZO)等の導電性金属酸化物;金、銀、クロム、ニッケル等の金属;これら金属と導電性金属酸化物との混合物;ヨウ化銅、硫化銅等の無機導電性物質;ポリアニリン、ポリチオフェン、ポリピロール等の有機導電性材料;等が挙げられる。
導電体層の形成方法としては、例えば、蒸着法、スパッタリング法、イオンプレーティング法、熱CVD法、プラズマCVD法等が挙げられる。これらの中でも、簡便に導電体層が形成できることから、スパッタリング法が好ましい。
プライマー層は、基材フィルムBとガスバリア層、またはその他の層との層間密着性を高める役割を果たす。プライマー層を設けることにより、層間密着性及び表面平滑性を向上させることができる。
プライマー層を構成する材料としては、特に限定されず、公知のものが使用できる。例えば、ケイ素含有化合物;光重合性モノマー及び/又は光重合性プレポリマーからなる光重合性化合物、及び少なくとも可視光域の光でラジカルを発生する重合開始剤を含む重合性組成物;ポリエステル系樹脂、ポリウレタン系樹脂(特にポリアクリルポリオール、ポリエステルポリオール、ポリエーテルポリオール等とイソシアネート化合物との2液硬化型樹脂)、アクリル系樹脂、ポリカーボネート系樹脂、塩化ビニル/酢酸ビニル共重合体、ポリビニルブチラール系樹脂、ニトロセルロース系樹脂等の樹脂類;アルキルチタネート;エチレンイミン;等が挙げられる。これらの材料は単独で、あるいは2種以上を組み合わせて用いることができる。
本発明の電子デバイス用部材は、本発明のガスバリアフィルム積層体からなることを特徴とする。従って、本発明の電子デバイス用部材は、優れたガスバリア性を有しているので、水蒸気等のガスによる素子の劣化を防ぐことができる。また、光の透過性が高く、耐熱性に優れるので、タッチパネル、液晶ディスプレイ、ELディスプレイ等のディスプレイ部材;太陽電池用バックシート;等の電子デバイス用の部材として好適である。
ブチルアクリレート(BA)及びアクリル酸(AA)を用いて得られたアクリル系共重合体〔質量比(BA:AA)=90:10、重量平均分子量550,000〕100質量部とイソシアナート系架橋剤(東洋インキ社製、BHS-8515、濃度37.5質量%)0.22質量部を混合し、メチルエチルケトンで希釈して、不揮発分濃度30質量%の粘着剤組成物Aを得た。
基材フィルムBとして、ポリエチレンテレフタレートフィルム(PETフィルム)(三菱樹脂社製、PET25T-100、厚さ25μm)に、ポリシラザン化合物〔ペルヒドロポリシラザンを主成分とするコーティング材(クラリアントジャパン社製、アクアミカNL110-20)〕をスピンコート法により塗布し、120℃で1分間加熱して、PETフィルム上に、厚さ150nmの層の、ペルヒドロポリシラザンを含むポリシラザン層を形成した。
次に、得られたポリシラザン層の表面に、プラズマイオン注入装置を用いて、下記の条件にて、アルゴン(Ar)をプラズマイオン注入して、ガスバリア層を形成して、ガスバリアフィルムAを作製した。
ガスバリア層を形成するために用いたプラズマイオン注入装置及びイオン注入条件は以下の通りである。
RF電源:日本電子社製、型番号「RF」56000
高電圧パルス電源:栗田製作所社製、「PV-3-HSHV-0835」
(プラズマイオン注入条件)
プラズマ生成ガス:Ar
ガス流量:100sccm
Duty比:0.5%
印加電圧:-6kV
RF電源:周波数 13.56MHz、印加電力 1000W
チャンバー内圧:0.2Pa
パルス幅:5μsec
処理時間(イオン注入時間):200秒
なお、(ガスバリアフィルムBの厚さ)/(ガスバリアフィルムAの厚さ)の値は、0.24であった。
接合層の基材フィルムAとして用いた樹脂フィルム及びその引張弾性率を以下に示す。
樹脂フィルム1:PETフィルム(三菱樹脂社製、商品名:ダイアホイルK100-2.0W、厚み2μm、23℃における引張弾性率、3300MPa)
樹脂フィルム2:シクロオレフィン系樹脂フィルム(JSR社製、商品名:アートン、厚み5μm、23℃における引張弾性率、4300MPa)
樹脂フィルム3:ポリサルホン系樹脂フィルム(BASF社製、商品名:ULTRASON S3030、厚み2μm、23℃における引張弾性率、2400MPa)
樹脂フィルム4:ポリサルホン系樹脂フィルム(BASF社製、商品名:ULTRASON S3030、厚み5μm、23℃における引張弾性率、2400MPa)
なお、23℃における引張弾性率は、引張試験機(オリエンテック社製、TENSILON RTA-100)を用いてJIS K7127に準拠して測定した。
厚さ38μmのPETフィルムの片面に、シリコーン剥離層を設けてなる剥離フィルム(リンテック社製、SP-PET381031)の剥離層表面に、粘着剤組成物Aをコンマダイレクトコート法にて塗布し、得られた塗膜を100℃で1分間乾燥して、厚みが2μmの粘着剤層を有する、粘着剤層付剥離フィルムAを得た。
粘着剤層付剥離フィルムAの粘着剤層面と樹脂フィルム1を貼り合わせ、次いで、もう1枚の粘着剤層付剥離フィルムAの粘着剤層面を貼り合わせて、接合層形成用積層体Aを得た。
接合層形成用積層体Aの剥離フィルムを1枚剥離して、露出した粘着剤層面と上記方法で作製したガスバリアフィルムAのガスバリア層面とを貼り合わせ、次に、もう一枚の剥離フィルムを剥離して、露出した粘着剤層面とガスバリアフィルムBのガスバリア層面とを貼り合わせて、ガスバリアフィルム積層体Aを作製した。
実施例1において、接合層の基材フィルムとして、樹脂フィルム1に代えて、樹脂フィルム2を用いたこと以外は、実施例1と同様にしてガスバリアフィルム積層体Bを作製した。
前記剥離フィルム(リンテック社製、SP-PET381031)の剥離層表面に、粘着剤組成物Aをコンマダイレクトコート法にて塗布し、得られた塗膜を100℃で1分間乾燥して、厚みが6μmの粘着剤層を有する粘着剤層付剥離フィルムBを得た。
次いで、ガスバリアフィルムAのガスバリア層面と、粘着剤層付剥離フィルムBの粘着剤層面とを貼り合わせた後、剥離フィルムを剥離した。
次に、露出した粘着剤層面と、ガスバリアフィルムBのガスバリア層面とを貼り合わせて、基材フィルムAを有しないガスバリアフィルム積層体Cを作製した。
比較例1において、粘着剤層の厚みを10μmに変更して粘着剤層付剥離フィルムCを得、これを用いたこと以外は、比較例1と同様にして、基材フィルムAを有しないガスバリアフィルム積層体Dを作製した。
実施例1において、接合層の基材フィルムとして、樹脂フィルム1に代えて、樹脂フィルム3を用いたこと以外は、実施例1と同様にしてガスバリアフィルム積層体Eを作製した。
実施例1において、接合層の基材フィルムとして、樹脂フィルム1に代えて、樹脂フィルム4を用いたこと以外は、実施例1と同様にしてガスバリアフィルム積層体Fを作製した。
実施例および比較例で用いた粘着剤層付剥離フィルムA~Cについて、粘着剤層面とポリエチレンテレフタレート(PET)フィルム(三菱樹脂社製、PET25T-100、厚さ25μm)とを貼り合わせ、これを、幅25mm長さ250mmの大きさに裁断し、試験用粘着フィルムを得た。
測定結果を第1表に示す。
実施例1、2及び比較例1~4で得られたガスバリアフィルム積層体A~Fを、ガスバリアフィルムAが外側になるように中央部分で折り曲げて、ラミネート装置(フジプラ社製、「LAMIPACKER LPC1502」)の2本のロール間を、ラミネート速度5m/min、圧力0.18MPa、温度23℃の条件で通した後、目視によりガスバリアフィルム積層体を観察した。評価基準を、以下に示す。
○:ガスバリアフィルム積層体に浮きが見られなかった。
×:ガスバリアフィルム積層体に浮きが見られた。
評価結果を第1表に示す。
実施例1、2で得られるガスバリアフィルム積層体A、Bは、耐折り曲げ性に優れている。
一方、比較例1、2で示されるように、接合層として、粘着剤層のみを用いる場合、その厚みに関わらず、耐折り曲げ性に劣っている。
また、比較例3、4で示されるように、23℃における引張弾性率が3,000MPa未満の合成樹脂からなる基材フィルムを用いる場合も、耐折り曲げ性に劣っている。
2,2a,2b・・・ガスバリア層
3・・・基材フィルムA
4,4a,4b・・・粘着剤層
5,5a,5b・・・剥離フィルム
10,10a,10b・・・粘着剤層付剥離フィルム
20・・・接合層
20’・・・接合層形成用積層体
30,30a,30b・・・ガスバリアフィルム
100A,100B・・・ガスバリアフィルム積層体
Claims (13)
- 少なくとも2枚のガスバリアフィルムが、接合層を介して積層されたガスバリアフィルム積層体であって、
前記接合層が、23℃における引張弾性率が3,000~10,000MPaの合成樹脂からなる基材フィルムAの両面に、それぞれ粘着剤層が隣接して積層されてなるものであることを特徴とするガスバリアフィルム積層体。 - 前記基材フィルムAの厚みが0.5~25μmである、請求項1に記載のガスバリアフィルム積層体。
- 前記基材フィルムAの両面に積層された粘着剤層の厚みが、それぞれ、0.5~25μmである、請求項1に記載のガスバリアフィルム積層体。
- 前記粘着剤層の前記ガスバリアフィルムに対する180°ひきはがし粘着力が、JIS Z0237(2000)に準じて測定して、2.0N/25mm以上である、請求項1に記載のガスバリアフィルム積層体。
- 前記接合層の厚みが75μm以下である、請求項1に記載のガスバリアフィルム積層体。
- 前記接合層の一方の面に積層されたガスバリアフィルムが、該接合層の他方の面に積層されたガスバリアフィルムよりも厚みが小さいものである、請求項1に記載のガスバリアフィルム積層体。
- (前記接合層の一方の面に積層されたガスバリアフィルムの厚さ)/(前記接合層の他方の面に積層されたガスバリアフィルムの厚さ)の値が、0.05~1.0である、請求項1に記載のガスバリアフィルム積層体。
- 前記ガスバリアフィルムの少なくとも1枚が、基材フィルムBと、該基材フィルムB上に設けられた少なくとも1層のガスバリア層とを有するものである、請求項1に記載のガスバリアフィルム積層体。
- 前記ガスバリア層が、高分子ケイ素化合物からなる層にイオンが注入されて形成された層である、請求項8に記載のガスバリアフィルム積層体。
- 前記ガスバリアフィルムが、そのガスバリア層が前記接合層と隣接するように積層されたものである、請求項8に記載のガスバリアフィルム積層体。
- 厚みが100μm以下である、請求項1に記載のガスバリアフィルム積層体。
- 請求項1に記載のガスバリアフィルム積層体からなる電子デバイス用部材。
- 請求項12に記載の電子デバイス用部材を備える電子デバイス。
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2013
- 2013-03-28 WO PCT/JP2013/059402 patent/WO2013147093A1/ja active Application Filing
- 2013-03-28 CN CN201380018327.5A patent/CN104220254B/zh active Active
- 2013-03-28 EP EP13768775.2A patent/EP2832539B1/en active Active
- 2013-03-28 TW TW102111080A patent/TWI576247B/zh active
- 2013-03-28 KR KR1020147027187A patent/KR102055111B1/ko active IP Right Grant
- 2013-03-28 JP JP2014508067A patent/JP6078051B2/ja active Active
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KR20160102181A (ko) * | 2013-12-26 | 2016-08-29 | 니폰 제온 가부시키가이샤 | 봉지 필름, 유기 전기발광 표시장치 및 유기 반도체 디바이스 |
JPWO2015099079A1 (ja) * | 2013-12-26 | 2017-03-23 | 日本ゼオン株式会社 | 封止フィルム、有機エレクトロルミネッセンス表示装置及び有機半導体デバイス |
US10374190B2 (en) | 2013-12-26 | 2019-08-06 | Zeon Corporation | Sealing film, organic electroluminescent display, and organic semiconductor device |
KR102393258B1 (ko) | 2013-12-26 | 2022-04-29 | 니폰 제온 가부시키가이샤 | 봉지 필름, 유기 전기발광 표시장치 및 유기 반도체 디바이스 |
JP2016038013A (ja) * | 2014-08-07 | 2016-03-22 | 大日本印刷株式会社 | 真空断熱材、真空断熱材用外装材、および断熱物品 |
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WO2018079429A1 (ja) * | 2016-10-28 | 2018-05-03 | リンテック株式会社 | 積層フィルム、電子デバイス用部材、及び電子デバイス |
JPWO2018079429A1 (ja) * | 2016-10-28 | 2019-09-19 | リンテック株式会社 | 積層フィルム、電子デバイス用部材、及び電子デバイス |
Also Published As
Publication number | Publication date |
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CN104220254A (zh) | 2014-12-17 |
EP2832539B1 (en) | 2016-05-04 |
CN104220254B (zh) | 2016-05-04 |
TWI576247B (zh) | 2017-04-01 |
US20150064429A1 (en) | 2015-03-05 |
EP2832539A4 (en) | 2015-10-28 |
EP2832539A1 (en) | 2015-02-04 |
TW201404601A (zh) | 2014-02-01 |
KR20140144690A (ko) | 2014-12-19 |
JP6078051B2 (ja) | 2017-02-08 |
KR102055111B1 (ko) | 2020-01-22 |
JPWO2013147093A1 (ja) | 2015-12-14 |
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