WO2017170547A1 - ガスバリア性積層体、電子デバイス用部材及び電子デバイス - Google Patents
ガスバリア性積層体、電子デバイス用部材及び電子デバイス Download PDFInfo
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- WO2017170547A1 WO2017170547A1 PCT/JP2017/012634 JP2017012634W WO2017170547A1 WO 2017170547 A1 WO2017170547 A1 WO 2017170547A1 JP 2017012634 W JP2017012634 W JP 2017012634W WO 2017170547 A1 WO2017170547 A1 WO 2017170547A1
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- gas barrier
- layer
- group
- barrier layer
- protective layer
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- 230000009467 reduction Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000000391 spectroscopic ellipsometry Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 1
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 125000000025 triisopropylsilyl group Chemical group C(C)(C)[Si](C(C)C)(C(C)C)* 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229960000834 vinyl ether Drugs 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/022—Mechanical properties
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
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- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
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- B32B2307/724—Permeability to gases, adsorption
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- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
- B32B2310/0806—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation
- B32B2310/0831—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation using UV radiation
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B2310/14—Corona, ionisation, electrical discharge, plasma treatment
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- B32B2383/00—Polysiloxanes
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/206—Organic displays, e.g. OLED
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/873—Encapsulations
- H10K59/8731—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/24983—Hardness
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
Definitions
- the present invention relates to a gas barrier laminate having excellent gas barrier properties even when bent, and an electronic device member comprising the gas barrier laminate, and an electronic device provided with the electronic device member.
- displays such as a liquid crystal display and an electroluminescence (EL) display have a gas barrier on a transparent plastic film instead of a glass plate as a substrate having electrodes in order to realize a reduction in thickness, weight, and flexibility.
- a so-called gas barrier film in which layers are laminated is used.
- Patent Document 1 proposes a molded body having a gas barrier layer made of a material containing oxygen atoms and silicon atoms.
- a gas barrier layer made of a material containing oxygen atoms and silicon atoms.
- the present invention has been made in view of the above-described prior art, and is a gas barrier laminate having excellent gas barrier properties that hardly generates cracks even when bent, and an electronic device member comprising the gas barrier laminate. And it aims at providing an electronic device provided with this member for electronic devices.
- the inventors of the present invention are gas barrier laminates in which a base material, a gas barrier layer, and a protective layer are laminated in this order, and the surface layer on the protective layer side of the gas barrier layer. Portion, the oxygen atom content rate, the nitrogen atom content rate, and the silicon atom content rate relative to the total amount of oxygen atoms, nitrogen atoms, and silicon atoms are specific values, and the protective layer at 25 ° C.
- the gas barrier laminate having a specific Young's modulus has been found to have excellent gas barrier properties because cracks are hardly generated in the gas barrier layer even when bent, and the present invention has been completed.
- the following gas barrier laminates [1] to [8], an electronic device member [9], and an electronic device [10] are provided.
- [1] A gas barrier laminate in which a substrate, a gas barrier layer, and a protective layer are laminated in this order directly or via another layer, In the surface layer portion on the protective layer side of the gas barrier layer, the oxygen atom existing ratio is 20 to 70%, the nitrogen atom existing ratio is 0 to 30%, The presence is 25-50%,
- the gas barrier laminate, wherein the protective layer has a Young's modulus at 25 ° C. of 5 ⁇ 10 9 Pa or more and 1 ⁇ 10 12 Pa or less.
- the gas barrier laminate of the present invention is less susceptible to cracking even when bent, has excellent gas barrier properties, and even when bonded to a device having a step, the excellent gas barrier properties decrease over a long period of time.
- a device having a step means a device in which various members for forming a device are stacked on a substrate and there is a step between the substrate and the various members. Since the gas barrier laminate of the present invention has a protective layer, it is excellent in gas barrier properties and shock absorption. That is, even when the gas barrier laminate is bonded to a device, the gas barrier layer does not generate cracks or cracks, and the gas barrier property is unlikely to deteriorate.
- the gas barrier laminate of the present invention is a gas barrier laminate in which a substrate, a gas barrier layer, and a protective layer are laminated in this order directly or via another layer,
- the oxygen atom existing ratio is 20 to 70%
- the nitrogen atom existing ratio is 0 to 30%
- the presence is 25-50%
- the Young's modulus at 25 ° C. of the protective layer is 5 ⁇ 10 9 Pa or more and 1 ⁇ 10 12 Pa or less.
- the gas barrier layer constituting the gas barrier laminate of the present invention is a layer having a characteristic (gas barrier property) that suppresses permeation of gases such as oxygen and water vapor.
- Examples of the gas barrier layer of the gas barrier laminate of the present invention include an inorganic vapor-deposited film and a layer obtained by subjecting a layer containing a polymer compound (hereinafter sometimes referred to as “polymer layer”) to a modification treatment. Can be mentioned.
- the gas barrier layer is preferably a layer obtained by subjecting the polymer layer to a modification treatment, and is a layer obtained by subjecting the polymer layer to a modification treatment,
- An unmodified portion of the polymer layer disposed on the side hereinafter, also referred to as “gas barrier layer (1)”
- a gas barrier layer (1 ) Is more preferably a gas barrier unit composed of a layer (hereinafter sometimes referred to as “gas barrier layer (2)”) disposed on the surface side opposite to the substrate side.
- the inorganic vapor deposition film examples include inorganic compound and metal vapor deposition films.
- inorganic oxides such as silicon oxide, aluminum oxide, magnesium oxide, zinc oxide, indium oxide, tin oxide, and titanium 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 alone or in combination of two or more.
- 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 more preferable.
- a PVD (physical vapor deposition) method such as a vacuum vapor deposition method, a sputtering method, or an ion plating method, a thermal CVD (chemical vapor deposition) method, a plasma CVD method, a photo CVD method, etc.
- the CVD method is mentioned.
- the thickness of the inorganic vapor deposition film varies depending on the inorganic compound to be used, but is preferably in the range of 50 to 300 nm, more preferably 50 to 200 nm, from the viewpoint of gas barrier properties and handling properties.
- the polymer compound used 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.
- the silicon-containing polymer compound include polysilazane compounds and 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 are each independently a hydrogen atom, an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, an unsubstituted or substituted group Represents a non-hydrolyzable group such as an aryl group having alkyl 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.
- Examples of the modified polysilazane include, for example, JP-A-62-195024, JP-A-2-84437, JP-A-63-81122, JP-A-1-138108, and JP-A-2-175726.
- JP-A-5-238827, JP-A-5-238827, JP-A-6-122852, JP-A-6-306329, JP-A-6-299118, JP-A-9-31333 Examples thereof include those described in Kaihei 5-345826 and JP-A-4-63833.
- the polysilazane compound perhydropolysilazane in which Rx, Ry, and Rz are all hydrogen atoms is preferable from the viewpoint of easy availability and the ability to form an ion-implanted layer having excellent gas barrier properties.
- a polysilazane compound a commercially available product as a glass coating material or the like can be used as it is.
- the polysilazane compounds can be used alone or in combination of two or more.
- the polymer layer may contain other components in addition to the polymer compound described above as long as the object of the present invention is not impaired.
- other components include a curing agent, an anti-aging agent, a light stabilizer, and a flame retardant.
- the content of the polymer compound in the polymer layer is preferably 50% by mass or more and more preferably 70% by mass or more because a gas barrier layer having better gas barrier properties can be obtained.
- the thickness of the polymer layer is not particularly limited, but is preferably in the range of 50 nm to 1 ⁇ m, more preferably 50 to 300 nm, and still more preferably 50 to 200 nm. In the present invention, even if the thickness of the polymer layer is nano-order, a gas barrier laminate having a sufficient gas barrier property can be obtained.
- the method for forming the polymer layer is not particularly limited. For example, preparing a polymer layer forming solution containing at least one polymer compound, optionally other components, a solvent, etc., and then applying this polymer layer forming solution by a known method, A polymer layer can be formed by drying the obtained coating film.
- Solvents used in 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 according to the purpose of use of the gas barrier laminate (necessary gas barrier properties, transparency, etc.).
- Examples of the method of implanting ions include a method of irradiating ions accelerated by an electric field (ion beam), a method of implanting ions in plasma, and the like.
- the latter method of implanting plasma ions is preferable because the desired barrier layer can be easily obtained.
- plasma is generated in an atmosphere containing a plasma generation gas such as a rare gas, and a negative voltage pulse is applied to the polymer layer, whereby ions (positive ions) in the plasma are increased. It can be performed by injecting into the surface of the molecular layer.
- a plasma generation gas such as a rare gas
- the thickness of the region into which ions are implanted can be controlled by implantation conditions such as ion type, applied voltage, and processing time, and is determined according to the thickness of the polymer layer, the purpose of use of the laminate, etc. Usually, it is 10 to 300 nm.
- the total amount of oxygen atoms, carbon atoms and silicon atoms in the surface layer portion on the protective layer side of the gas barrier layer (that is, the amount of oxygen atoms, nitrogen atoms and silicon atoms present)
- the presence ratio of oxygen atoms (when the total is 100%) is 20 to 70%, the presence ratio of nitrogen atoms is 0 to 30%, and the presence ratio of silicon atoms is 25 to 50%. From the viewpoint of exhibiting, it is preferable that the oxygen atom content is 15 to 65%, the nitrogen atom content is 5 to 25%, and the silicon atom content is 30 to 45%.
- the “surface layer portion of the gas barrier layer on the protective layer side” refers to the surface of the gas barrier layer on the protective layer side and a portion 10 nm in the depth direction from the surface. Further, when the gas barrier layer is the gas barrier unit, “the surface layer portion of the gas barrier layer (2) on the protective layer side” corresponds to “the surface layer portion of the gas barrier layer on the protective layer side”. The abundance ratio of oxygen atoms, nitrogen atoms and silicon atoms is measured by the method described in the examples.
- a modification treatment such as an ion implantation treatment, a plasma treatment, an ultraviolet irradiation treatment, or a heat treatment.
- the gas barrier layer is composed of a material containing at least an oxygen atom, a nitrogen atom and a silicon atom, and It is preferable that the existence ratio of oxygen atoms in the layer gradually decreases and the existence ratio of nitrogen atoms gradually increases from the surface on the protective layer side of the layer in the depth direction.
- the thickness of the “region in which the oxygen atom existence ratio gradually decreases and the nitrogen atom existence ratio gradually increases from the surface in the depth direction” is usually 5 to 100 nm, preferably 10 to 50 nm.
- the film density in the surface layer portion on the protective layer side of the gas barrier layer is preferably 2.4 to 4.0 g / cm 3 , and preferably 2.5 to 4.0 g. / Cm 3 is more preferable, and 2.6 to 4.0 g / cm 3 is particularly preferable.
- the film density can be calculated using an X-ray reflectivity method. X-rays are totally reflected when they are incident on the thin film on the substrate at a very shallow angle. When the angle of incident X-rays exceeds the total reflection critical angle, X-rays enter the thin film and are divided into transmitted waves and reflected waves at the thin film surface and interface, and the reflected waves interfere. By analyzing the total reflection critical angle, the density of the film can be obtained. Note that the thickness of the thin film can also be obtained from measurement while changing the incident angle and analyzing the interference signal of the reflected wave accompanying the change in the optical path difference.
- the film density can be measured by the following method. In general, it is known that the refractive index n of a substance with respect to X-rays and ⁇ of the real part of the refractive index n satisfy the following formulas 1 and 2.
- the r e is the electron classical radius (2.818 ⁇ 10 -15 m)
- N 0 is the Avogadro's number
- a wavelength of ⁇ is X-ray
- [rho is the density (g / cm 3)
- Zi , Mi and xi represent the atomic number, atomic weight and atomic number ratio (molar ratio) of the i-th atom, respectively
- fi ′ represents the atomic scattering factor (anomalous dispersion term) of the i-th atom.
- the total reflection critical angle ⁇ C is given by Equation 3 when ⁇ related to absorption is ignored.
- the density ⁇ can be obtained by the following equation 4 from the relationship between the equations 2 and 3.
- ⁇ C is a value that can be obtained from the X-ray reflectivity
- r e , N 0 , and ⁇ are constants
- Zi, Mi, and fi ′ are values specific to the constituent atoms.
- xi atomic number ratio (molar ratio)
- the film density in the surface layer portion on the protective layer side of the gas barrier layer is calculated by using Equation 4 after measuring the X-ray reflectivity by the method described in Examples.
- the gas barrier layer (when the gas barrier layer is the gas barrier unit, the gas barrier layer (2)) has a Young's modulus at 25 ° C. of 1 ⁇ 10 10 from the viewpoint that the effects of the present invention can be more easily obtained. It is preferable that it is Pa or more and 1 ⁇ 10 12 Pa or less.
- the Young's modulus of the gas barrier layer (when the gas barrier layer is the gas barrier unit, the gas barrier layer (2)) is preferably higher than the Young's modulus of the protective layer described later.
- the Young's modulus of the gas barrier layer (when the gas barrier layer is the gas barrier unit, the Young's modulus of the gas barrier layer (2)) is higher than the Young's modulus of the protective layer, a step portion or the like is applied to a device having a step. Even if stress is concentrated locally, cracking of the gas barrier layer can be prevented.
- the Young's modulus can be measured, for example, by the method described in the examples.
- the film density of the gas barrier layer (1) is higher than the film density of the protective layer described later. Since the film density of the gas barrier layer (1) is higher than the film density of the protective layer described later, cracks in the gas barrier layer may occur even when force is locally concentrated on the stepped portion when affixed to a device having a stepped portion. Can be prevented.
- the gas barrier laminate of the present invention further has a protective layer in addition to the gas barrier layer.
- the Young's modulus of the protective layer is 5 ⁇ 10 9 Pa or more and 1 ⁇ 10 12 Pa or less, preferably 8 ⁇ 10 9 Pa or more and 8 ⁇ 10 10 Pa or less.
- the material for forming the protective layer is not particularly limited.
- Resins, rubber-based materials, polyvinyl chloride and the like can be mentioned.
- silicon-containing polymer compounds, acrylic resins, olefin resins, silicone resins, and rubber materials are preferable, silicon-containing polymer compounds, acrylic resins, and olefin resins are more preferable, and silicon-containing polymer compounds. Is more preferable.
- silicon-containing polymer compounds examples 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.
- (meth) acrylic acid ester homopolymer As acrylic resin, (meth) acrylic acid ester homopolymer, copolymer containing two or more (meth) acrylic acid ester units, and (meth) acrylic acid ester and other functional monomers The thing containing at least 1 sort (s) chosen from the copolymer is mentioned.
- (Meth) acrylic acid means acrylic acid or methacrylic acid (the same shall apply hereinafter).
- the (meth) acrylic acid ester is preferably a (meth) acrylic acid ester having 1 to 20 carbon atoms in the ester portion because the Young's modulus of the protective layer can be easily within the specific range.
- a (meth) acrylic acid ester having 4 to 10 carbon atoms is more preferred.
- Examples of the (meth) acrylic acid ester having 4 to 10 carbon atoms include butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, and octyl (meth) acrylate. , 2-ethylhexyl (meth) acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, and the like.
- the functional monomer is a monomer having a functional group such as a hydroxyl group, a carboxyl group, an amino group, or an amide group.
- a functional group such as a hydroxyl group, a carboxyl group, an amino group, or an amide group.
- examples include hydroxyl group-containing monomers such as hydroxyethyl (meth) acrylate, amide group-containing monomers such as (meth) acrylamide, and carboxylic acid group-containing monomers such as (meth) acrylic acid.
- a (meth) acrylic acid ester homopolymer or copolymer (hereinafter, these may be collectively referred to as “(meth) acrylic acid ester (co) polymer”) is, for example, a solution polymerization method or emulsification. It can be obtained by a known polymerization method such as a polymerization method or a suspension polymerization method.
- the (meth) acrylic acid ester (co) polymer may be mixed with a crosslinking agent to form a crosslinked body at least partially.
- a crosslinking agent examples include: tolylene diisocyanate, hexamethylene diisocyanate and the like, or isocyanate-based crosslinking agents such as adducts thereof; epoxy-based crosslinking agents such as ethylene glycol glycidyl ether; hexa [1- (2-methyl) -aziridinyl ] Aziridine type crosslinking agents such as triphosphatriazine; Chelate type crosslinking agents such as aluminum chelate;
- 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 solid content of the (meth) acrylic acid ester (co) polymer.
- a crosslinking agent can be used individually by 1 type or in combination of 2 or more types.
- olefin resin examples include low density polyethylene, linear low density polyethylene, polypropylene, polybutene, ethylene vinyl acetate copolymer, ethylene (meth) acrylic acid copolymer, and ethylene (meth) acrylic acid ester copolymer. It is done.
- silicone resin examples include those containing dimethylsiloxane as a main component.
- rubber-based material examples include those mainly composed of isoprene rubber, styrene-butadiene rubber, polyisobutylene rubber, styrene-butadiene-styrene rubber and the like.
- the protective layer may be a laminate of layers made of these resins. Further, the protective layer made of such a resin may be a sheet formed by extrusion molding of a thermoplastic resin, or a sheet formed by curing a thin film of a curable resin by a predetermined means. Also good.
- the curable resin to be used for example, an energy ray-curable urethane acrylate or the like as a main agent, an acrylate monomer having a relatively bulky group such as isobornyl acrylate as a diluent, and a photopolymerization initiator as required. What is obtained from the resin composition which mix
- the protective layer contains other additives such as antioxidants, tackifiers, plasticizers, ultraviolet absorbers, colorants, antistatic agents and the like.
- a formation method of a protective layer For example, the layer (the adhesive etc.) which forms the said protective layer, and the layer which should laminate
- coating on top, drying the obtained coating film, and forming by heating etc. as needed is mentioned.
- a protective layer may be separately formed on the peeling substrate, and the obtained film may be transferred and laminated on the layer to be laminated.
- the thickness of the protective layer is usually 10 nm to 10 ⁇ m, preferably 30 nm to 1 ⁇ m, more preferably 40 nm to 600 nm.
- the base material layer constituting the gas barrier laminate of the present invention is not particularly limited as long as it can support the gas barrier layer.
- Examples of the base material layer include plate-like bodies, various containers, and various electronic device members.
- Examples of the plate-like body include a resin film, a sheet, and a plate.
- Examples of the various containers include food containers, beverage containers, cosmetic containers, clothing containers, pharmaceutical containers, food bottles, beverage bottles, edible oil bottles, seasoning bottles, and the like.
- Various electronic device members include organic EL elements, liquid crystal elements, quantum dot elements, electronic paper elements, organic solar cell elements, thin film batteries, organic thin film transistor elements, organic sensor elements, and micro electro mechanical sensor (MEMS) elements. Can be mentioned.
- either a single plate or a long plate can be used as the base material layer.
- “long” means that the shape is a strip shape whose longitudinal direction is longer (preferably 10 times or longer) than the width direction. In the following description, “long” may be omitted.
- a resin film is preferable as the base material layer.
- the length of the resin film (length in the longitudinal direction) is not particularly limited, but is usually 400 to 2000 m.
- the width (length in the width direction) of the resin film is not particularly limited, but is usually 450 to 1300 mm, preferably 530 to 1280 mm.
- the thickness of the resin film is not particularly limited, but is usually 1 to 100 ⁇ m, preferably 5 to 70 ⁇ m, more preferably 10 to 60 ⁇ 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 polymer And aromatic polymers. These resin components can be used alone or in combination of two or more.
- polyester, polyamide, polysulfone, polyethersulfone, polyphenylene sulfide, or cycloolefin polymer is more preferable, and polyester or cycloolefin polymer is more preferable because of excellent transparency and versatility.
- polyester examples include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, and polyarylate.
- cycloolefin polymers examples include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, and hydrides thereof.
- the 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, a filler, 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 predetermined components and molding it 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 laminate of the present invention is a laminate in which the substrate, gas barrier layer, and protective layer are laminated in this order directly or via other layers.
- other layers include an inorganic compound layer, a conductor layer, and a primer layer.
- the gas barrier laminate of the present invention may have a primer layer.
- the primer layer is usually provided between the base material layer and the gas barrier layer.
- unevenness on the surface of the base material layer is reduced, and the interlayer adhesion of the gas barrier laminate is improved.
- the surface roughness of the gas barrier layer can be adjusted efficiently.
- the active energy ray-curable resin composition is a composition that contains a polymerizable compound and can be cured by irradiation with active energy rays.
- the polymerizable compound include polymerizable prepolymers and polymerizable monomers.
- the polymerizable prepolymer includes a polyester oligomer having a hydroxyl group at both ends, a polyester acrylate prepolymer obtained by a reaction with (meth) acrylic acid, a low molecular weight bisphenol type epoxy resin or a novolac type epoxy resin, )
- epoxy acrylate prepolymer polyurethane oligomer obtained by reaction with acrylic acid, urethane acrylate prepolymer, polyether polyol obtained by reaction of (meth) acrylic acid, and (meth) acrylic acid
- examples thereof include a polyol acrylate prepolymer to be obtained.
- Examples of the polymerizable monomer include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, and hydroxypivalic acid.
- the active energy ray-curable resin composition may contain a polymer resin component that does not have reaction curability, such as an acrylic resin.
- the viscosity of the composition can be adjusted by adding a polymer resin component.
- 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.
- These polymerizable compounds can be used singly or in combination of two or more.
- the active energy ray curable resin composition (that is, the ultraviolet 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) -
- the active energy ray-curable resin composition may contain fine particles such as organic fine particles and inorganic fine particles.
- fine particles such as organic fine particles and inorganic fine particles.
- organic fine particles examples include polystyrene resins, styrene-acrylic copolymer resins, acrylic resins, amino resins, divinylbenzene resins, silicone resins, urethane resins, melamine resins, urea resins, phenolic resins, Examples thereof include fine particles made of benzoguanamine resin, xylene resin, polycarbonate resin, polyethylene resin, polyvinyl chloride resin, and the like. Among these, silicone fine particles made of a silicone resin are preferable.
- Examples of the inorganic fine particles include silica particles, metal oxide particles, and alkyl silicate particles.
- Examples of the silica particles include colloidal silica and hollow silica.
- 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.
- As the 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. These fine particles can be used singly or in combination of two or more.
- the shape of the fine particles is not particularly limited.
- fine particles having various shapes such as an amorphous shape and a true spherical shape can be used.
- the average particle diameter of the fine particles is usually 1 to 100 nm, preferably 1 to 20 nm.
- the average particle diameter of the fine particles can be measured by a laser diffraction / scattering method.
- the content of the fine particles is preferably 0.1 to 50% by mass, and more preferably 1 to 30% by mass in the solid content of the resin composition.
- the active energy ray-curable resin composition preferably contains a leveling agent.
- a leveling agent include siloxane compounds. Of these, compounds having a dialkylsiloxane skeleton such as polydimethylsiloxane and derivatives thereof are preferred.
- the content of the leveling agent is preferably 0.01 to 10% by mass, and 0.05 to 5% by mass in the solid content of the resin composition. More preferred.
- the active energy ray-curable resin composition may contain other components as long as the effects of the present invention are not hindered.
- other components include an antistatic agent, a stabilizer, an antioxidant, a plasticizer, a lubricant, and a coloring pigment. What is necessary is just to determine these content suitably according to the objective.
- the method for forming the primer layer is not particularly limited.
- an active energy ray-curable resin composition and, if necessary, a coating liquid containing a solvent was prepared, and then this coating liquid was coated on a substrate by a known method, and obtained.
- a hard coat layer composed of a cured product of the active energy ray-curable resin composition can be formed.
- 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.
- the coating film can be cured by irradiating the coating film with active energy rays.
- active energy rays include ultraviolet rays, electron beams, ⁇ rays, ⁇ rays, ⁇ rays, and the like. Among these, since it can generate
- ultraviolet rays are used as the active energy rays, light sources such as an ultrahigh pressure mercury lamp, a high pressure mercury lamp, a low pressure mercury lamp, a carbon arc, a black light lamp, and a metal halide lamp can be used as the ultraviolet ray source. No particular restrictions on the quantity of ultraviolet light, it is usually 100mJ / cm 2 ⁇ 1,000mJ / cm 2.
- the irradiation time is usually several seconds to several hours, and the irradiation temperature is usually 20 to 100 ° C.
- the thickness of the primer layer is usually 20 ⁇ m or less, preferably 0.5 to 20 ⁇ m, more preferably 1.0 to 10 ⁇ m.
- gas barrier laminate examples include those having the following layer structures (A) and (B), but are not limited thereto.
- the thickness of the gas barrier laminate of the present invention is not particularly limited, but is preferably 5 to 100 ⁇ m, more preferably 10 to 50 ⁇ m, and still more preferably 20 to 40 ⁇ 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. Lower limit no particular, is preferably as small, usually is 0.001g / (m 2 ⁇ day) or more.
- the water vapor transmission rate can be measured by the method described in the examples.
- the gas barrier laminate of the present invention has excellent gas barrier properties, it is suitably used as a member for electronic devices.
- the method for producing the gas barrier laminate of the present invention is not particularly limited.
- a primer layer is formed on the long base layer resin film as necessary by the above method, and then the gas barrier is formed by the above method.
- the gas barrier laminate of the present invention can be produced.
- the long shape means a sheet having a length of at least about 5 times the width direction of the sheet, preferably a length of 10 times or more, for example, wound in a roll shape. It has a length that can be stored or transported.
- the primer layer forming solution may be applied directly on the resin film for the substrate layer, or the primer layer forming solution is applied on the process substrate, and the coating film is applied to the substrate. After the resin films are stacked, the primer layer may be formed by curing the coating film. According to such a production method, the gas barrier laminate of the present invention can be produced efficiently when it is elongated.
- the electronic device member of the present invention comprises the gas barrier laminate of the present invention. Therefore, the electronic device member of the present invention has excellent gas barrier properties because cracks are hardly generated in the gas barrier layer even when it is bent. Since the member for electronic devices of the present invention is excellent in colorless transparency, it is suitable as a display member such as a liquid crystal display and 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 organic EL illumination, an inorganic EL display, an inorganic EL illumination, electronic paper, and a solar cell.
- Example 1 Perhydropolysilazane (manufactured by AZ Electronic Materials, "ZNL110A-20”) was used for non-priming of a polyethylene terephthalate (PET) film (Toyobo Co., Ltd., "Cosmo Shine A-4100") having a thickness of 50 ⁇ m. ) was applied and heated and cured at 120 ° C. for 2 minutes to form a polysilazane layer. The film thickness of the polysilazane layer was 200 nm.
- PET polyethylene terephthalate
- the plasma ion implantation apparatus and plasma ion implantation conditions used are as follows.
- RF power supply Model number “RF” 56000, JEOL high voltage pulse power supply: “PV-3-HSHV-0835”, Kurita Manufacturing Co., Ltd.
- plasma ion implantation conditions ⁇
- Plasma generated gas Ar ⁇ Gas flow rate: 100sccm ⁇ Duty ratio: 0.5% ⁇
- Repetition frequency 1000Hz ⁇
- Applied voltage -10kV ⁇
- RF power supply frequency 13.56 MHz
- applied power 1000 W -Chamber internal pressure 0.2 Pa
- Pulse width 5 ⁇ sec ⁇ Processing time (ion implantation time): 5 minutes
- Example 2 In Example 1, a gas barrier laminate 2 was obtained in the same manner as in Example 1 except that the plasma ion implantation condition “applied voltage” at the time of forming the gas barrier layer was ⁇ 15 kV.
- Example 3 In Example 1, a gas barrier laminate 3 was obtained in the same manner as in Example 1 except that a 300 nm silicon dioxide layer formed by sputtering was used as the protective layer.
- Example 4 In Example 1, a gas barrier laminate 4 was obtained in the same manner as in Example 1 except that the silicon oxynitride layer 200 nm formed by sputtering was used as the gas barrier layer.
- Example 1 a gas barrier laminate 1r was obtained in the same manner as in Example 1 except that the protective layer was not provided.
- Example 2 In Example 1, 20 parts by mass of an acrylic resin [urethane acrylate-based UV curable compound (SHIKOH UT-4692, manufactured by Nippon Synthetic Chemical Co., Ltd.)] on a gas barrier layer was dissolved in 100 parts by mass of methyl isobutyl ketone. A photopolymerization initiator (Irgacure 127, manufactured by BASF) was added by adding 3 parts by mass to 100 parts by mass of the solid content of the solution, and after heating and drying at 70 ° C.
- an acrylic resin urethane acrylate-based UV curable compound (SHIKOH UT-4692, manufactured by Nippon Synthetic Chemical Co., Ltd.)
- a photopolymerization initiator Irgacure 127, manufactured by BASF
- a UV light irradiation line Example 1 except that a protective layer was formed by irradiating with UV light (high pressure mercury lamp, line speed, 20 m / min, integrated light quantity 100 mJ / cm2, peak intensity 1.466 W, number of passes 2 times) In the same manner as described above, a gas barrier laminate 2r was obtained.
- the thickness of the protective layer was 300 nm.
- Example 3 In Example 1, 20 parts by mass of acrylic resin [tricyclodecane dimethanol diacrylate (A-DCP, manufactured by Shin-Nakamura Chemical Co., Ltd.)] was dissolved in 100 parts by mass of methyl isobutyl ketone on the gas barrier layer. A polymerization initiator (Irgacure 127, manufactured by BASF) was added by adding 3 parts by mass to 100 parts by mass of the solid content of the solution, and after heating and drying at 70 ° C. for 1 minute, a UV light irradiation line was used.
- a polymerization initiator Irgacure 127, manufactured by BASF
- Example 1 except that a protective layer was formed by applying 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). In the same manner as described above, a gas barrier laminate 3r was obtained. The thickness of the protective layer was 300 nm.
- the film thickness of the gas barrier laminate was measured using “Spectroscopic Ellipsometry 2000U” manufactured by JA Woollam Japan. The measurement was performed at 23 ° C. using light having a wavelength of 590 nm.
- Durability evaluation 1 assuming an actual electronic device was performed by a method of evaluating moisture ingress by fading of metallic calcium.
- Metal calcium is vapor-deposited on a glass substrate having a step, and a sealing material (rubber adhesive, trade name “TN-286”, manufactured by Matsumura Petrochemical Co., Ltd.) is formed on the protective layer of the gas barrier laminate to a thickness of 20 ⁇ m. It formed into a film and bonded so that the level
- the glass substrate has a size of 50 ⁇ 50 mm, and has a step of 200 ⁇ m in thickness of 15 ⁇ 15 mm in the center.
- the sample is observed after standing for 100 hours in an atmosphere of 23 ° C. and 50% RH. The case where there was no fading of metallic calcium was evaluated as “ ⁇ (good)”, and the case where fading occurred was evaluated as “x (bad)”. The results are shown in Table 1.
- Durability evaluation 2 was performed by the method of evaluating moisture ingress by fading of metallic calcium in the same manner as durability evaluation method 1.
- an adhesive material rubber adhesive, trade name “TN-286”, manufactured by Matsumura Petrochemical Co., Ltd.
- TN-286 manufactured by Matsumura Petrochemical Co., Ltd.
- SP-PET382150 thickness And a pressure-sensitive adhesive sheet was prepared.
- Metal calcium was vapor-deposited on a glass substrate (product name: Eagle XG, dimensions: 100 ⁇ 100 mm, manufactured by Corning), the release film of the adhesive tape was peeled off, and bonded and covered so as to cover the calcium surface.
- the film density in the surface layer part of the gas barrier layer was calculated using the above equation 4 based on the X-ray reflectivity measured under the following measurement conditions to obtain the total reflection critical angle ⁇ c.
- the measuring apparatus and measurement conditions are as follows.
- Measuring device Sample horizontal X-ray diffractometer for thin film evaluation "SmartLab", manufactured by Rigaku Corporation
- X-ray source Cu-K ⁇ 1 (wavelength: 1.54059 mm)
- Optical system Parallel beam optical system
- Incident side slit system Ge (220) 2 crystal, height limiting slit 5 mm, incident slit 0.05 mm
- Receiving side slit system receiving slit 0.10mm, solar slit 5 ° Detector; Scintillation counter Tube voltage and tube current; 45kV-200mA Scanning axis; 2 ⁇ / ⁇ Scan mode; continuous scan scan range; 0.1-3.0 deg. Scanning speed: 1 deg. / Min.
- Table 1 shows the following.
- the protective layer has an appropriate elastic modulus, and even when bent, the gas barrier layer is hardly cracked, and the deterioration of the gas barrier property can be suppressed.
- the gas barrier laminate 1r of Comparative Example 1 is not provided with a protective layer, when the gas barrier laminate 1r is bent, the gas barrier layer cracks and the gas barrier property is lowered.
- the gas barrier laminates 2r and 3r of Comparative Examples 2 and 3 have a low elastic modulus of the protective layer, the gas barrier layer is cracked when bent, and the gas barrier properties are lowered.
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Abstract
Description
しかしながら、この文献記載のガスバリア性を有する成形体を、段差を有するデバイスに貼合した場合、ガスバリア層にクラックが発生しやすく、その場合にガスバリア性が低下し、デバイスが劣化しやすいという問題があった。
〔1〕基材と、ガスバリア層と、保護層とがこの順に直接又は他の層を介して積層されたガスバリア性積層体であって、
前記ガスバリア層の保護層側の表層部における、酸素原子、窒素原子及びケイ素原子の存在量全体に対する酸素原子の存在割合が20~70%、窒素原子の存在割合が0~30%、ケイ素原子の存在割合が25~50%であり、
前記保護層の25℃におけるヤング率が、5×109Pa以上、1×1012Pa以下であることを特徴とするガスバリア性積層体。
〔2〕前記ガスバリア層の保護層側の表層部における膜密度が、2.4~4.0g/cm3である〔1〕に記載のガスバリア性積層体。
〔3〕前記ガスバリア層の25℃におけるヤング率が、1×1010Pa以上、1×1012Pa以下である〔1〕又は〔2〕に記載のガスバリア性積層体。
〔4〕前記ガスバリア層のヤング率が、前記保護層のヤング率より高いことを特徴とする〔1〕~〔3〕のいずれかに記載のガスバリア性積層体。
〔5〕前記ガスバリア層が、前記基材側に配置されてなるガスバリア層(1)と、前記ガスバリア層(1)の基材側とは反対側の面側に配置されてなるガスバリア層(2)とからなるガスバリア性ユニットからなることを特徴とする〔1〕又は〔2〕に記載のガスバリア性積層体。
〔6〕前記ガスバリア層(2)の25℃におけるヤング率が、1×1010Pa以上、1×1012Pa以下である〔5〕に記載のガスバリア性積層体。
〔7〕前記ガスバリア層(2)のヤング率が、前記保護層のヤング率より高いことを特徴とする〔5〕又は〔6〕に記載のガスバリア性積層体。
〔8〕前記ガスバリア層(1)の膜密度が、前記保護層の膜密度より高いことを特徴とする〔5〕~〔7〕のいずれかに記載のガスバリア性積層体。
〔9〕〔1〕~〔8〕のいずれかに記載のガスバリア性積層体からなる電子デバイス用部材。
〔10〕〔9〕に記載の電子デバイス用部材を備える電子デバイス。
ここで、段差を有するデバイスとは、基板上にデバイスを形成するための各種部材が積層され、基板と各種部材との間に段差があるデバイスを意味する。
本発明のガスバリア性積層体は、保護層を有するため、ガスバリア性及び衝撃吸収性に優れる。すなわち、ガスバリア性積層体をデバイスに貼合しても、ガスバリア層にクラックや割れが発生せず、ガスバリア性が低下し難いものである。
前記ガスバリア層の保護層側の表層部における、酸素原子、窒素原子及びケイ素原子の存在量全体に対する酸素原子の存在割合が20~70%、窒素原子の存在割合が0~30%、ケイ素原子の存在割合が25~50%であり、
前記保護層の25℃におけるヤング率が、5×109Pa以上、1×1012Pa以下であることを特徴とする。
本発明のガスバリア性積層体を構成するガスバリア層は、酸素や水蒸気等のガスの透過を抑制する特性(ガスバリア性)を有する層である。
無機化合物の蒸着膜の原料としては、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、酸化チタン等の無機酸化物;窒化ケイ素、窒化アルミニウム、窒化チタン等の無機窒化物;無機炭化物;無機硫化物;酸化窒化ケイ素等の無機酸化窒化物;無機酸化炭化物;無機窒化炭化物;無機酸化窒化炭化物等が挙げられる。
金属の蒸着膜の原料としては、アルミニウム、マグネシウム、亜鉛、及びスズ等が挙げられる。
これらは1種単独で、あるいは2種以上を組み合わせて用いることができる。
これらの中では、ガスバリア性の観点から、無機酸化物、無機窒化物又は金属を原料とする無機蒸着膜が好ましく、さらに、透明性の観点から、無機酸化物又は無機窒化物を原料とする無機蒸着膜がより好ましい。
これらの高分子化合物は1種単独で、あるいは2種以上を組合せて用いることができる。
ケイ素含有高分子化合物としては、ポリシラザン系化合物、ポリカルボシラン系化合物、ポリシラン系化合物、及びポリオルガノシロキサン系化合物等が挙げられる。なかでも、薄くても優れたガスバリア性を有するガスバリア層を形成できることから、ポリシラザン系化合物が好ましい。
Rx、Ry、Rzはそれぞれ独立して、水素原子、無置換若しくは置換基を有するアルキル基、無置換若しくは置換基を有するシクロアルキル基、無置換若しくは置換基を有するアルケニル基、無置換若しくは置換基を有する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。
また、本発明においては、ポリシラザン系化合物として、ポリシラザン変性物を用いることもできる。ポリシラザン変性物としては、例えば、特開昭62-195024号公報、特開平2-84437号公報、特開昭63-81122号公報、特開平1-138108号公報等、特開平2-175726号公報、特開平5-238827号公報、特開平5-238827号公報、特開平6-122852号公報、特開平6-306329号公報、特開平6-299118号公報、特開平9-31333号公報、特開平5-345826号公報、特開平4-63833号公報等に記載されているものが挙げられる。
これらの中でも、ポリシラザン系化合物としては、入手容易性、及び優れたガスバリア性を有するイオン注入層を形成できる観点から、Rx、Ry、Rzが全て水素原子であるペルヒドロポリシラザンが好ましい。
また、ポリシラザン系化合物としては、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。
ポリシラザン系化合物は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
高分子層中の高分子化合物の含有量は、より優れたガスバリア性を有するガスバリア層が得られることから、50質量%以上が好ましく、70質量%以上がより好ましい。
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、充分なガスバリア性を有するガスバリア性積層体を得ることができる。
これらの溶媒は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
イオン注入処理は、後述するように、高分子層にイオンを注入して、高分子層を改質する方法である。
プラズマ処理は、高分子層をプラズマ中に晒して、高分子層を改質する方法である。例えば、特開2012-106421号公報に記載の方法に従って、プラズマ処理を行うことができる。
紫外線照射処理は、高分子層に紫外線を照射して高分子層を改質する方法である。例えば、特開2013-226757号公報に記載の方法に従って、紫外線改質処理を行うことができる。
これらの中でも、高分子層の表面を荒らすことなく、その内部まで効率よく改質し、よりガスバリア性に優れるガスバリア層を形成できることから、イオン注入処理が好ましい。
これらのイオンは、1種単独で、あるいは2種以上を組み合わせて用いることができる。
これらの中でも、より簡便にイオンを注入することができ、より優れたガスバリア性を有するガスバリア層が得られることから、アルゴン、ヘリウム、ネオン、クリプトン、キセノン等の希ガスのイオンが好ましい。
ここで、「ガスバリア層の保護層側の表層部」とは、ガスバリア層の保護層側の表面、及び該表面から深さ方向に10nmの部分をいう。また、ガスバリア層が前記ガスバリア性ユニットである場合、「ガスバリア層(2)の保護層側の表層部」が「ガスバリア層の保護層側の表層部」に該当する。
酸素原子、窒素原子及びケイ素原子の存在割合の測定は、実施例において説明する方法で行う。
「表面から深さ方向に向かって、酸素原子の存在割合が漸次減少し、窒素原子の存在割合が漸次増加する領域」の厚さは、通常、5~100nm、好ましくは10~50nmである。
X線は、基板上の薄膜に対して非常に浅い角度で入射させると全反射される。入射X線の角度が全反射臨界角以上になると、薄膜内部にX線が侵入し薄膜表面や界面で透過波と反射波に分かれ、反射波は干渉する。全反射臨界角を解析することで、膜の密度を求めることができる。なお、入射角度を変えながら測定を行い、光路差の変化に伴う反射波の干渉信号の解析から、薄膜の膜厚も求めることができる。
膜密度は、以下の方法で測定することができる。
一般に、X線に対する物質の屈折率n、及び屈折率nの実部部分のδは、下記式1及び式2を満たすことが知られている。
ガスバリア層の保護層側の表層部における膜密度は、実施例において説明する方法でX線の反射率を測定し、式4を用いて算出する。
ガスバリア層(ガスバリア層が、前記ガスバリア性ユニットである場合には、ガスバリア層(2))のヤング率が保護層のヤング率より高いことにより、段差を有するデバイスに貼付した際に、段差部分等で局所的に応力が集中してもガスバリア層のクラックを防ぐことができる。
ヤング率は、例えば、実施例に記載された方法により測定することができる。
ガスバリア層(1)の膜密度が、後述する保護層の膜密度より高いことにより、段差を有するデバイスに貼付した際に、段差部分等で局所的に力が集中してもガスバリア層のクラックを防ぐことができる。
本発明のガスバリア性積層体は、前記ガスバリア層に加えて、さらに保護層を有する。保護層のヤング率は、5×109Pa以上、1×1012Pa以下、好ましくは、8×109Pa以上、8×1010Pa以下である。
このようなヤング率を有する保護層を設けることにより、保護性能に優れ、衝撃を受けても、ガスバリア層にクラックや割れが生じることがない、すなわち、ガスバリア層のクラックや割れによるガスバリア性の低下のおそれがないガスバリア性積層体を得ることができる。
これらの中でも、ケイ素含有高分子化合物、アクリル系樹脂、オレフィン系樹脂、シリコーン系樹脂、ゴム系材料が好ましく、ケイ素含有高分子化合物、アクリル系樹脂、オレフィン系樹脂がより好ましく、ケイ素含有高分子化合物がさらに好ましい。
なお、「(メタ)アクリル酸」は、アクリル酸又はメタクリル酸の意である(以下同様。)
炭素数が4~10の(メタ)アクリル酸エステルとしては、(メタ)アクリル酸ブチル、(メタ)アクリル酸ペンチル、(メタ)アクリル酸ヘキシル、(メタ)アクリル酸ヘプチル、(メタ)アクリル酸オクチル、(メタ)アクリル酸2-エチルヘキシル、(メタ)アクリル酸ノニル、(メタ)アクリル酸デシル等が挙げられる。
架橋剤としては、トリレンジイソシアネート、ヘキサメチレンジイソシアナート等、あるいはそれらのアダクト体等のイソシアネート系架橋剤;エチレングリコールグリシジルエーテル等のエポキシ系架橋剤;ヘキサ〔1-(2-メチル)-アジリジニル〕トリフオスファトリアジン等のアジリジン系架橋剤;アルミニウムキレート等のキレート系架橋剤;等が挙げられる。
また、ゴム系材料としては、イソプレンゴム、スチレン-ブタジエンゴム、ポリイソブチレンゴム、スチレン-ブタジエン-スチレンゴム等を主成分とするものが挙げられる。
さらに、このような樹脂からなる保護層としては熱可塑性樹脂を押出し成形によりシート化したものであってもよいし、硬化性樹脂を所定手段により薄膜化し、硬化してシート化したものであってもよい。
また、別途、剥離基材上に保護層を製膜し、得られた膜を、積層すべき層上に転写して積層してもよい。
本発明のガスバリア性積層体を構成する基材層は、ガスバリア層を担持できるものであれば、特に限定されない。
基材層の例としては、板状体、各種容器、および各種電子デバイス用部材が挙げられる。板状体としては、例えば、樹脂フィルム、シート、およびプレートが挙げられる。各種容器としては、食品用容器、飲料用容器、化粧品用容器、衣料用容器、医薬品容器、食品用ボトル、飲料用ボトル、食用油ボトル、調味料ボトル等のボトル等が挙げられる。
本発明において、「長尺」とは、その形状が、幅方向に比べて、長手方向が長い(好ましくは10倍以上の長さ)帯状であることを意味する。また、以下の説明において、「長尺の」を省略することがある。
樹脂フィルムの幅(幅方向の長さ)は、特に限定されないが、通常、450~1300mm、好ましくは530~1280mmである。
樹脂フィルムの厚みは、特に限定されないが、通常、1~100μm、好ましくは5~70μm、より好ましくは10~60μmである。
これらの樹脂成分は、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。
他の層としては、無機化合物層、導電体層、プライマー層等が挙げられる。
本発明のガスバリア性積層体は、プライマー層を有するものであってもよい。
プライマー層は、通常、基材層とガスバリア層の間に設けられる。プライマー層を設けることにより、基材層表面の凹凸が低減化され、ガスバリア性積層体の層間密着性が向上する。また、プライマー層を形成することで、ガスバリア層の表面粗さを効率よく調節することができる。
活性エネルギー線硬化型樹脂組成物は、重合性化合物を含有し、活性エネルギー線の照射により硬化し得る組成物である。
重合性化合物としては、重合性プレポリマーや重合性モノマーが挙げられる。
重合性プレポリマーとしては、両末端に水酸基を有するポリエステルオリゴマーと、(メタ)アクリル酸との反応により得られるポリエステルアクリレート系プレポリマー、低分子量のビスフェノール型エポキシ樹脂やノボラック型エポキシ樹脂と、(メタ)アクリル酸との反応により得られるエポキシアクリレート系プレポリマー、ポリウレタンオリゴマーと、(メタ)アクリル酸との反応により得られるウレタンアクリレート系プレポリマー、ポリエーテルポリオールと、(メタ)アクリル酸との反応により得られるポリオールアクリレート系プレポリマー等が挙げられる。
これらの重合性化合物は一種単独で、あるいは二種以上を組み合わせて用いることができる。
ここで、(メタ)アクリロイル基なる表記は、アクリロイル基及びメタクリロイル基の両方を含む意味である。
これらの重合性化合物は一種単独で、あるいは二種以上を組み合わせて用いることができる。
光重合開始剤の含有量は、特に限定されないが、通常、前記重合性化合物に対して、0.2~30質量%、好ましくは0.5~20質量%である。
シリカ粒子としては、コロイダルシリカ、中空シリカ等が挙げられる。
金属酸化物粒子としては、酸化チタン、酸化亜鉛、酸化ジルコニウム、酸化タンタル、酸化インジウム、酸化ハフニウム、酸化錫、酸化ニオブ等の粒子が挙げられる。
アルキルシリケート粒子としては、式:Ra-O〔-{Si(ORb)2}-O-〕n-Ra(式中、Ra及びRbは炭素数1~10のアルキル基を表し、nは1以上の整数を表す。)で示されるアルキルシリケートの粒子が挙げられる。
これらの中でも、シリカ粒子又はアルキルシリケート粒子が好ましい。
これらの微粒子は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
微粒子の平均粒径は、通常、1~100nm、好ましくは1~20nmである。微粒子の平均粒径は、レーザー回折/散乱法により測定することができる。
レベリング剤としては、シロキサン系化合物が挙げられる。なかでも、ポリジメチルシロキサンおよびその誘導体等のジアルキルシロキサン骨格を有する化合物が好ましい。
活性エネルギー線硬化型樹脂組成物がレベリング剤を含有する場合、レベリング剤の含有量は、前記樹脂組成物の固形分中、0.01~10質量%が好ましく、0.05~5質量%がより好ましい。
その他の成分としては、帯電防止剤、安定剤、酸化防止剤、可塑剤、滑剤、着色顔料等が挙げられる。これらの含有量は、目的に合わせて適宜決定すればよい。
これらの溶媒は1種単独で、あるいは2種以上を組み合わせて用いることができる。
活性エネルギー線としては、紫外線、電子線、α線、β線、γ線等が挙げられる。これらの中でも、比較的簡便な装置を用いて発生させることができることから、活性エネルギー線としては、電子線、紫外線が好ましく、紫外線がより好ましい。
活性エネルギー線として紫外線を用いる場合、紫外線源としては、超高圧水銀灯、高圧水銀灯、低圧水銀灯、カーボンアーク、ブラックライトランプ、メタルハライドランプ等の光源を用いることができる。紫外線の光量には特に制限はないが、通常100mJ/cm2~1,000mJ/cm2である。照射時間は、通常数秒~数時間であり、照射温度は、通常20~100℃である。
本発明のガスバリア性積層体としては、下記の(A)、(B)の層構造を有するものが挙げられるが、これらに限定されるものではない。
(A):基材層/ガスバリア層/保護層
(B):基材層/プライマー層/ガスバリア層/保護層
水蒸気透過率は、実施例に記載の方法により測定することができる。
例えば、ガスバリア性積層体を長尺状のガスバリアフィルムとする場合には、長尺状の基材層用樹脂フィルム上に、必要に応じて前記方法によりプライマー層を形成した後、前記方法によりガスバリア層を形成することにより本発明のガスバリア性積層体を製造することができる。
長尺状とは、シートの幅方向に対して、少なくとも5倍程度以上の長さを有するものをいい、好ましくは10倍もしくはそれ以上の長さを有し、例えばロール状に巻回されて保管又は運搬される程度の長さを有するものをいう。
このような製造方法によれば、本発明のガスバリア性積層体を長尺状にする場合に効率よく製造することができる。
本発明の電子デバイス用部材は、本発明のガスバリア性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、折り曲げてもガスバリア層にクラックが発生しにくく、すぐれたガスバリア性を有するものである。
本発明の電子デバイス用部材は、無色透明性に優れるので、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;等として好適である。
各例中の部及び%は、特に断りのない限り、質量基準である。
厚みが50μmの片面下塗り処理されたポリエチレンテレフタレート(PET)フィルム(東洋紡社製、「コスモシャインA-4100」)の非下塗り処理に、ペルヒドロポリシラザン(AZエレクトロニックマテリアルズ社製、「ZNL110A-20」)を、塗工し、これを120℃で2分間加熱硬化させることで、ポリシラザン層を形成した。ポリシラザン層の膜厚は200nmとした。
次いで、プラズマイオン注入装置を用いて、上記のポリシラザン層に下記条件にてプラズマイオン注入を行い、ポリシラザン層の表面を改質し、ガスバリア層(ガスバリア性ユニット)を得た。
さらに、得られたガスバリア層上に前記ペルヒドロポリシラザンを塗工し、これを120℃で2分間加熱硬化させることで保護層を形成した。保護層の膜厚は300nmとした。
得られたガスバリア性積層体1について各種測定を行った。測定結果を表1に示す。
(プラズマイオン注入装置)
RF電源:型番号「RF」56000、日本電子社製
高電圧パルス電源:「PV-3-HSHV-0835」、栗田製作所社製
(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%
・繰り返し周波数:1000Hz
・印加電圧:-10kV
・RF電源:周波 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):5分間
実施例1において、ガスバリア層形成時のプラズマイオン注入条件「印加電圧」を-15kVとした以外は、実施例1と同様にしてガスバリア性積層体2を得た。
実施例1において、保護層に、スパッタリング法にて製膜した二酸化ケイ素層300nmを用いた以外は、実施例1と同様にしてガスバリア性積層体3を得た。
実施例1において、ガスバリア層としてスパッタリング法にて製膜した酸窒化ケイ素層200nmを用いた以外は実施例1と同様にしてガスバリア性積層体4を得た。
実施例1において、保護層を設けないこと以外は、実施例1と同様にしてガスバリア性積層体1rを得た。
実施例1において、ガスバリア層上に、アクリル系樹脂〔ウレタンアクリレート系紫外線硬化型化合物(SHIKOH UT-4692、日本合成化学社製)〕20質量部をメチルイソブチルケトン100質量部に溶解させた後、光重合開始剤(Irgacure127、BASF社製)を、溶液の固形分100質量部に対し、3質量部添加したものを塗工し、これを70℃で1分間加熱乾燥した後、UV光照射ラインを用いてUV光照射を行い(高圧水銀灯、ライン速度、20m/分、積算光量100mJ/cm2、ピーク強度1.466W、パス回数2回)、保護層を形成させたこと以外は、実施例1と同様にしてガスバリア性積層体2rを得た。保護層の膜厚は300nmとした。
実施例1において、ガスバリア層上に、アクリル系樹脂〔トリシクロデカンジメタノールジアクリレート(A-DCP、新中村化学社製)〕20質量部をメチルイソブチルケトン100質量部に溶解させた後、光重合開始剤(Irgacure127、BASF社製)を、溶液の固形分100質量部に対し、3質量部添加したものを塗工し、これを70℃で1分間加熱乾燥した後、UV光照射ラインを用いてUV光照射を行い(高圧水銀灯、ライン速度、20m/分、積算光量100mJ/cm2、ピーク強度1.466W、パス回数2回)、保護層を形成させたこと以外は、実施例1と同様にしてガスバリア性積層体3rを得た。保護層の膜厚は300nmとした。
(水蒸気透過率の測定)
ガスバリア性積層体の水蒸気透過率を、mocon社製、「AQUATRAN-1」を用いて測定した。測定は40℃、相対湿度90%雰囲気下で行った。
下記に示す測定条件にて、ガスバリア層(イオン注入されて得られた層)の表層部における酸素原子、窒素原子及びケイ素原子の存在割合の測定を行った。
測定装置:「PHI Quantera SXM」アルバックファイ社製
X線源:AlKα
X線ビーム径:100μm
電力値:25W
電圧:15kV
取り出し角度:45°
真空度:5.0×10-8Pa
ガスバリア性積層体の膜厚を、ジェー・エー・ウーラム・ジャパン社製、「分光エリプソメトリー2000U」を用いて測定した。測定は、波長が590nmの光を用いて、23℃で行った。
ガスバリア層(1)、ガスバリア層(2)、及び保護層のヤング率を微小表面硬度計(ダイナミック超微小硬度計W201S、島津製作所社製)を使用して測定した。結果を表1に示す。
金属カルシウムの退色により水分進入を評価する方法にて、実際の電子デバイスを想定した耐久性評価1を実施した。段差を有するガラス基板上に金属カルシウムを蒸着し、ガスバリア性積層体の保護層上に封止材(ゴム系粘着剤、商品名「TN-286」、松村石油化学社製)を膜厚20μmとなるように製膜し、ガラス基板の段差を覆うように貼合した。ガラス基板は、50×50mmの寸法であり、中央部に15×15mmの大きさの厚さ200μmの段差を有している。23℃50%RHの雰囲気下で100時間静置後、サンプルを観察する。金属カルシウムの退色が無い場合を「○(良好)」、退色した場合を「×(不良)」として評価した。結果を表1に示す。
耐久性の評価方法1と同様に金属カルシウムの退色により水分進入を評価する方法にて、耐久性評価2を実施した。ガスバリア性積層体の保護層上に粘着材(ゴム系粘着剤、商品名「TN-286」、松村石油化学社製)を膜厚20μmとなるように製膜し剥離フィルム(SP-PET382150、厚さ38μm、リンテック社製)と貼り合わせ、粘着シートを作製した。ガラス基板(品名:イーグルXG、寸法:100×100mm、コーニング社製)上に金属カルシウムを蒸着し、粘着テープの剥離フィルムを剥離し、カルシウム面を覆うように貼合し、封止した。23℃50%RHの雰囲気下で100時間静置後、サンプルを観察する。金属カルシウムの退色が無い場合を「○(良好)」、退色した場合を「×(不良)」として評価した。結果を表1に示す。
ガスバリア層の表層部における膜密度は、下記に示す測定条件にてX線の反射率を測定して全反射臨界角度θcを求め、その値から、前記式4を用いて算出した。
測定装置:薄膜評価用試料水平型X線回折装置「SmartLab」、株式会社リガク製
測定条件:
X線源;Cu-Kα1(波長:1.54059Å)
光学系;並行ビーム光学系
入射側スリット系;Ge(220)2結晶、高さ制限スリット5mm、入射スリット0.05mm
受光側スリット系;受光スリット 0.10mm、ソーラースリット 5°
検出器;シンチレーションカウンター
管電圧・管電流;45kV-200mA
走査軸;2θ/θ
走査モード;連続スキャン
走査範囲;0.1-3.0deg.
走査速度;1deg./min.
サンプリング間隔;0.002°/step
なお、原子数比(xi)は、X線光電子分光測定により得られたガスバリア層の表層部における酸素原子、窒素原子及びケイ素原子の存在割合を用いた。
実施例1~4のガスバリア性積層体1~4は、保護層の弾性率が適度なものであり、折り曲げてもガスバリア層にクラックが発生しにくく、ガスバリア性の低下が抑制できている。
一方、比較例1のガスバリア性積層体1rは、保護層を設けていないため、折り曲げるとガスバリア層にクラックが入り、ガスバリア性が低下している。
比較例2、3のガスバリア性積層体2r、3rは、保護層の弾性率が低いため、折り曲げるとガスバリア層にクラックが入り、ガスバリア性が低下している。
Claims (10)
- 基材と、ガスバリア層と、保護層とがこの順に直接又は他の層を介して積層されたガスバリア性積層体であって、
前記ガスバリア層の保護層側の表層部における、酸素原子、窒素原子及びケイ素原子の存在量全体に対する酸素原子の存在割合が20~70%、窒素原子の存在割合が0~30%、ケイ素原子の存在割合が25~50%であり、
前記保護層の25℃におけるヤング率が5×109Pa以上、1×1012Pa以下であることを特徴とするガスバリア性積層体。 - 前記ガスバリア層の保護層側の表層部における膜密度が、2.4~4.0g/cm3である請求項1に記載のガスバリア性積層体。
- 前記ガスバリア層の25℃におけるヤング率が、1×1010Pa以上、1×1012Pa以下である請求項1又は2に記載のガスバリア性積層体。
- 前記ガスバリア層のヤング率が、前記保護層のヤング率より高いことを特徴とする請求項1~3のいずれかに記載のガスバリア性積層体。
- 前記ガスバリア層が、前記基材側に配置されてなるガスバリア層(1)と、前記ガスバリア層(1)の基材側とは反対側の面側に配置されてなるガスバリア層(2)とからなるガスバリア性ユニットからなることを特徴とする請求項1又は2に記載のガスバリア性積層体。
- 前記ガスバリア層(2)の25℃におけるヤング率が、1×1010Pa以上、1×1012Pa以下である請求項5に記載のガスバリア性積層体。
- 前記ガスバリア層(2)のヤング率が、前記保護層のヤング率より高いことを特徴とする請求項5又は6に記載のガスバリア性積層体。
- 前記ガスバリア層(1)の膜密度が、前記保護層の膜密度より高いことを特徴とする請求項5~7のいずれかに記載のガスバリア性積層体。
- 請求項1~8のいずれかに記載のガスバリア性積層体からなる電子デバイス用部材。
- 請求項9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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Publication number | Publication date |
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TW201805160A (zh) | 2018-02-16 |
EP3437855B1 (en) | 2022-07-20 |
JPWO2017170547A1 (ja) | 2019-02-07 |
EP3437855A1 (en) | 2019-02-06 |
KR20180129839A (ko) | 2018-12-05 |
JP7018872B2 (ja) | 2022-02-14 |
US20190088903A1 (en) | 2019-03-21 |
KR102330884B1 (ko) | 2021-11-25 |
EP3437855A4 (en) | 2019-11-20 |
TWI715750B (zh) | 2021-01-11 |
CN108883605A (zh) | 2018-11-23 |
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