WO2012032907A1 - 粘着シート、及び電子デバイス - Google Patents
粘着シート、及び電子デバイス Download PDFInfo
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- WO2012032907A1 WO2012032907A1 PCT/JP2011/068651 JP2011068651W WO2012032907A1 WO 2012032907 A1 WO2012032907 A1 WO 2012032907A1 JP 2011068651 W JP2011068651 W JP 2011068651W WO 2012032907 A1 WO2012032907 A1 WO 2012032907A1
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- WIPO (PCT)
- Prior art keywords
- sensitive adhesive
- pressure
- gas barrier
- layer
- adhesive sheet
- Prior art date
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- 229920006267 polyester film Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000007650 screen-printing Methods 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
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000013077 target material Substances 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
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-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
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/29—Laminated material
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/62—Nitrogen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J121/00—Adhesives based on unspecified rubbers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
-
- 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
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/16—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2421/00—Presence of unspecified rubber
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2433/00—Presence of (meth)acrylic polymer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
- C09J2483/006—Presence of polysiloxane in the substrate
-
- 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
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2848—Three or more layers
Definitions
- the present invention relates to an adhesive sheet and an electronic device provided with the adhesive sheet as an electronic device member.
- organic electronics has attracted attention as a technology that can form displays, circuits, batteries, etc. on flexible plastic substrates at low temperatures close to room temperature using coating and printing processes. It is being advanced.
- a light-emitting element used for a liquid crystal display or an electroluminescence (EL) display an organic EL element capable of high-luminance light emission by low-voltage direct current drive has attracted attention.
- EL electroluminescence
- use of a transparent plastic film as a substrate having electrodes has been studied in order to realize a reduction in thickness, weight, flexibility, and the like.
- this organic EL element has a problem that when it is driven for a certain period of time, light emission characteristics such as light emission luminance, light emission efficiency, and light emission uniformity are deteriorated compared to the initial stage. Possible causes of this problem include oxidation of the electrode due to oxygen or water vapor entering the organic EL element, modification of organic matter, oxidative decomposition of the organic material due to heat during driving, and the like.
- a plastic film used as a substrate has a problem that it easily transmits oxygen, water vapor, and the like, and easily deteriorates an organic EL element.
- an adhesive sheet for an organic device for example, an adhesive film using a polyisobutylene-based resin as an adhesive layer is disclosed (see Patent Document 2).
- the adhesive layer of Patent Document 2 is vulnerable to high temperatures, ultraviolet rays, and the like, and the organic EL elements and devices are exposed to high temperature or ultraviolet irradiation due to long-time driving or driving environment, so that the resin itself of the adhesive layer deteriorates.
- the performance of the adhesive film may be degraded and the organic EL element may be deteriorated accordingly.
- the present invention has been made in view of solving the above-described problems, and provides an adhesive sheet excellent in gas barrier properties, bending resistance, and transparency, and an electronic device including the adhesive sheet as a member for an electronic device. With the goal.
- the gas barrier layer constituting the pressure-sensitive adhesive sheet is composed of a material containing at least oxygen atoms and silicon atoms, and the ratio of oxygen atoms, nitrogen atoms and silicon atoms in the surface layer portion of the gas barrier layer, and It has been found that an adhesive sheet having a film density in a specific range can solve the above problems.
- a pressure-sensitive adhesive sheet having at least a gas barrier layer and a pressure-sensitive adhesive layer on a substrate, wherein the gas barrier layer is made of a material containing at least oxygen atoms and silicon atoms, and is a surface layer of the gas barrier layer
- the oxygen atom content ratio is 60 to 75%
- the nitrogen atom content ratio is 0 to 10%
- the silicon atom content ratio is 25 to 35% with respect to the total amount of oxygen atoms, nitrogen atoms, and silicon atoms.
- a pressure-sensitive adhesive sheet having a film density of 2.4 to 4.0 g / cm 3 in a surface layer portion of the gas barrier layer.
- the pressure-sensitive adhesive sheet according to the above [1], wherein the material constituting the gas barrier layer comprises a polysilazane compound.
- the polysilazane compound is perhydropolysilazane.
- the ions are ionized at least one gas selected from the group consisting of hydrogen, nitrogen, oxygen, argon, helium, neon, xenon, and krypton. .
- the pressure-sensitive adhesive sheet of the present invention is excellent in gas barrier properties, bending resistance, and transparency. Therefore, the adhesive sheet of this invention can be used suitably for electronic devices, such as a display and a solar cell.
- the pressure-sensitive adhesive sheet of the present invention has at least a gas barrier layer and a pressure-sensitive adhesive layer on a substrate.
- Drawing 1 is a figure showing an example of composition of an adhesive sheet of the present invention.
- the adhesive sheet of this invention has a base material, a gas barrier layer, and an adhesive layer at least, if an adhesive layer exists in the outermost layer, the order to laminate
- FIG. 1 (A1) there is a pressure-sensitive adhesive sheet 1 in which a gas barrier layer 3 is laminated on one side of a substrate 2 and a pressure-sensitive adhesive layer 4 is laminated on the gas barrier layer 3.
- the adhesive layer 4 is laminated
- the pressure-sensitive adhesive layer 4b is provided on the surface of the opposite base material, It is good also as the adhesive sheet 1b which has an adhesive layer on both surfaces.
- a pressure-sensitive adhesive is provided between two gas barrier layers 3a and 3b including a gas barrier layer 3a laminated on one side of the substrate 2a and a gas barrier layer 3b laminated on one side of the substrate 2b.
- the adhesive sheet 1c which provides the layer 4a and has the adhesive layers 4b and 4c on the opposite side to the surface in which the gas barrier layer of the base materials 2a and 2b was provided, respectively.
- the pressure-sensitive adhesive sheet 1c serves not only to bond the two gas barrier layers 3a and 3b to the pressure-sensitive adhesive layer 4a but also to absorb the shock and protect the gas barrier layers 3a and 3b when an impact is applied from the outside. be able to.
- “other layers” other than the base material, the gas barrier layer, and the pressure-sensitive adhesive layer may be provided.
- the position where other layers are laminated is not particularly limited, and is appropriately selected according to the role of each layer.
- (1) base material, (2) gas barrier layer, (3) pressure-sensitive adhesive layer, and (4) other layers constituting the pressure-sensitive adhesive sheet will be sequentially described.
- the substrate of the present invention is not particularly limited as long as it is a material other than the polysilazane compound and has a self-supporting property and meets the object of the present invention.
- a base material to be used for example, polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, A cycloolefin type polymer, an aromatic polymer, etc. are mentioned.
- polyester, polyamide, or cycloolefin polymer is preferable, and polyester or cycloolefin polymer is more preferable because of excellent transparency and versatility.
- the polyester polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polyarylate, and the like.
- the polyamide wholly aromatic polyamide, nylon 6, nylon 66, nylon copolymer and the like.
- cycloolefin polymers include norbornene polymers, monocyclic olefin polymers, cyclic conjugated diene polymers, vinyl alicyclic hydrocarbon polymers, hydrides thereof, and the like.
- Specific examples of products include Apel (ethylene-cycloolefin copolymer manufactured by Mitsui Chemicals), Arton (norbornene polymer manufactured by JSR), Zeonore (norbornene polymer manufactured by Nippon Zeon), and the like. It is done.
- the thickness of the substrate is not particularly limited, but is preferably 0.5 to 500 ⁇ m, more preferably 1 to 200 ⁇ m, and more preferably 10 to 100 ⁇ m.
- the gas barrier layer of the pressure-sensitive adhesive sheet of the present invention satisfies at least the following requirements (a) to (c).
- (A) It is comprised from the material containing an oxygen atom and a silicon atom at least.
- (B) The proportion of oxygen atoms present is 60 to 75%, the proportion of nitrogen atoms is 0 to 10%, and the presence of silicon atoms with respect to the total amount of oxygen atoms, nitrogen atoms and silicon atoms in the surface layer portion of the gas barrier layer. The proportion is 25 to 35%.
- the film density in the surface layer portion of the gas barrier layer is 2.4 to 4.0 g / cm 3 .
- the pressure-sensitive adhesive sheet of the present invention has excellent gas barrier properties because the permeability of gas such as water vapor is remarkably small.
- the water vapor transmission rate of the gas barrier layer is preferably 1.0 g / m 2 / day or less, more preferably 0.5 g / m 2 / day or less, and still more preferably 0.000 or less in an atmosphere of 40 ° C. and 90% relative humidity. 1 g / m 2 / day or less.
- the water vapor transmission rate can be measured using a known gas transmission rate measuring device, and in the present invention, it means a value measured by the method described in Examples (the same applies hereinafter).
- the pressure-sensitive adhesive sheet of the present invention is excellent in bending resistance, it is possible to maintain the gas barrier property even when folding or the like is performed. This can be confirmed from the fact that the partial gas barrier layer is not deteriorated and the water vapor transmission rate hardly decreases.
- the pressure-sensitive adhesive sheet of the present invention is excellent in maintaining gas barrier properties even after folding, as compared with the case where an inorganic film having the same thickness is laminated as a gas barrier layer.
- a polysilazane compound As a material satisfying the above requirement (a), a polysilazane compound is preferable from the viewpoint of improving gas barrier properties, bending resistance, and transparency.
- the polysilazane compound is a polymer having a repeating unit containing a —Si—N— bond in the molecule, and specifically includes a compound having a repeating unit represented by the formula (1).
- n represents an arbitrary natural number.
- Rx, Ry, and Rz each independently represent a hydrogen atom, an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, unsubstituted or substituted Represents a non-hydrolyzable group such as an aryl group having a group or an alkylsilyl group;
- alkyl group of the unsubstituted or substituted alkyl group examples include, 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.
- 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.
- Examples of the alkenyl group of an unsubstituted or substituted alkenyl group include, for example, a vinyl group, a 1-propylenyl group, a 2-propenyl group, a 1-butenyl group, a 2-butenyl group, and a 3-butenyl group. Examples include 2 to 10 alkenynyl groups.
- 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 the 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.
- substituents for these aryl groups there are 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 such as methoxy group and ethoxy group Nitro group; cyano group; hydroxyl group; thiol group; eboxy group; glycidoxy group; (meth) acryloyloxy group; unsubstituted phenyl group, 4-methylphenyl group, 4-chlorophenyl group, etc. Or the aryl group which has a substituent; etc. are mentioned.
- 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 more 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. There may be.
- the inorganic polysilazane is a perhydro having a linear structure having a repeating unit represented by the following formula (2), a molecular weight of 690 to 2000, and 3 to 10 SiH 3 groups in one molecule.
- Polysilazane (see Japanese Patent Publication No. 63-16325), perhydropolysilazane having a linear structure and a branched structure represented by the following formula (3), and perhydropolysilazane represented by the following formula (5) Examples thereof include perhydropolysilazane having a polysilazane structure, a linear structure, a branched structure and a cyclic structure in the molecule.
- Examples of the organic polysilazane include the following compounds (i) to (v).
- Rx ′ is an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, unsubstituted or substituted
- (Ii) — (Rx′SiHNRz ′) — (Rz ′) is an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, unsubstituted or A compound having a cyclic structure mainly having a degree of polymerization of 3 to 5 with a repeating unit of an aryl group having a substituent or an alkylsilyl group.
- Rx ′ and Ry ′ represent the same meaning as described above, e and f represent an arbitrary natural number, and Y 3 represents a hydrogen atom or a group represented by the following formula (8).
- the organic polysilazane can be produced by a conventionally known method. As a specific production method, for example, by reacting ammonia or a primary amine with a reaction product of a halogenosilane compound having an unsubstituted or substituted group represented by the following formula (9) and a secondary amine. Organic polysilazanes can be synthesized. Secondary amine and primary amine used, depending on the structure of the polysilazane compound of interest, may be selected.
- m represents 2 or 3
- X represents a halogen atom
- R 1 represents a substituent of any one of the aforementioned Rx, Ry, Rz, Rx ′, Ry ′, and Rz ′. .
- 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 ) g (NH) h )] and [(SiH 2 ) i O] (wherein g, h and i are each independently 1, 2 or 3), polysiloxazan (Japanese Patent Laid-Open No. 62-195024), and polysilazane with a poron compound.
- a polyborosilazane produced by reaction Japanese Patent Laid-Open No.
- a polymetallosilazane produced by reacting polysilazane and a metal alkoxide Japanese Patent Laid-Open No. 63-81122
- an inorganic silazane high polymer Modified polysilazanes (JP-A-1-138108, etc.), copolymerized silazanes obtained by introducing organic components into polysilazane (JP-A-2-175726, etc.), polysilazanes Low temperature ceramicized polysilazanes (JP-A-5-238827, etc.), silicon alkoxide-added polysilazanes (JP-A-5-238827), glycidol-added polysilazanes (specially) Kaihei 6-122852), acetylacetonato complex-added polysilazane (JP-A-6-306329), metal carboxylate-added polysilazane (JP-A-6-299118, etc.), these polys
- modified polysilazane obtained by adding alcohol such as methanol or hexamethyldisilazane to the terminal N atom to perhydropolysilazane ( JP-A-5-345 26, JP-A No. 4-63833 JP), and the like.
- the polysilazane compound inorganic polysilazane in which Rx, Ry, and Rz are all hydrogen atoms, and organic polysilazane in which at least one of Rx, Ry, and Rz is not a hydrogen atom are preferable, and easy availability and excellent gas barrier properties are obtained. From the viewpoint of forming a layer having an inorganic polysilazane, inorganic polysilazane is more preferable, and perhydropolysilazane is more preferable.
- the number average molecular weight of the polysilazane compound to be used is not particularly limited, but is preferably 100 to 50,000. In the present invention, the number average molecular weight (Mn) is a value calculated as a polystyrene conversion value by gel permeation chromatography (GPC method) (hereinafter the same).
- the polysilazane compound a commercially available product as a glass coating material or the like can be used as it is.
- the gas barrier layer may contain other components in addition to the polysilazane compound as long as the object of the present invention is not impaired. Examples of other components include curing agents, other polymers, anti-aging agents, light stabilizers, and flame retardants.
- the content of the polysilazane compound in the gas barrier layer is preferably 50% by mass or more, more preferably 70% by mass or more, in all materials constituting the gas barrier layer, from the viewpoint of forming a gas barrier layer having excellent gas barrier properties. Preferably it is 85 mass% or more, More preferably, it is substantially 100 mass%.
- the method for forming the gas barrier layer is not particularly limited.
- a gas barrier layer-forming solution containing at least one polysilazane compound, and optionally other components, a solvent, and the like is applied onto the substrate.
- the method of forming the obtained coating film by dry-drying moderately is mentioned. It does not specifically limit as a coating method, The method of using well-known coating apparatuses, such as a spin coater, a knife coater, and a gravure coater, is mentioned. Further, in order to improve gas barrier properties of the dried and the gas barrier layer of the resulting coating film, it is preferred to heat the coating. Heating is preferably performed at 80 to 150 ° C.
- the gas barrier layer can also be formed by bringing a plasma polymerizable silazane compound gas such as dimethyldisilazane, tetramethyldisilazane, hexamethyldisilazane, etc. into contact with the substrate and subjecting it to plasma polymerization treatment ( JP-A-9-143289).
- a plasma polymerizable silazane compound gas such as dimethyldisilazane, tetramethyldisilazane, hexamethyldisilazane, etc.
- the thickness of the formed gas barrier layer is preferably 20 nm to 100 ⁇ m, more preferably 30 to 500 nm, and still more preferably 40 to 200 nm.
- the adhesive sheet which has sufficient gas barrier performance can be obtained.
- the surface layer portion of the gas barrier layer in the present invention refers to the surface of the gas barrier layer and a region from the surface to a depth of 5 nm.
- the surface of the gas barrier layer includes the boundary surface when forming a boundary surface with another layer.
- the existence ratio of oxygen atoms, nitrogen atoms, and silicon atoms in the surface layer portion of the gas barrier layer is determined by performing elemental analysis of the surface layer portion of the gas barrier layer near 5 nm from the surface using X-ray photoelectron spectroscopy (XPS). Can be confirmed. Specifically, it is measured by the method described in the examples.
- the proportion of oxygen atoms present is 60 to 75%, the proportion of nitrogen atoms is 0 to 10%, and the presence of silicon atoms with respect to the total amount of oxygen atoms, nitrogen atoms and silicon atoms in the surface layer portion of the gas barrier layer of the present invention.
- the proportion is 25 to 35%, preferably the proportion of oxygen atoms is 60 to 72%, the proportion of nitrogen atoms is 0.1 to 8.0%, and the proportion of silicon atoms is 27 to 35%.
- the film density in the surface layer portion of the gas barrier layer of the present invention is 2.4 to 4.0 g / cm 3 from the viewpoint of improving gas barrier properties, bending resistance and transparency, but preferably 2.45 to 4 0.0 g / cm 3 , more preferably 2.5 to 4.0 g / cm 3 .
- the film density is less than 2.4 g / cm 3, a particular result gas barrier properties of the adhesive sheet is poor.
- the film density can be calculated using an X-ray reflectivity method (XRR).
- X-rays are totally reflected when they are incident on the thin film on the substrate at a very shallow angle.
- XRR X-ray reflectivity method
- XRR X-ray reflectivity method
- x-rays penetrate into the thin film and are divided into transmitted waves and reflected waves at the thin film surface and interface, and the reflected waves interfere.
- the density of the film can be obtained.
- 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 are expressed by the following equations 1 and 2.
- the r e is the electron classical radius (2.818 ⁇ 10 -15 m)
- a N o is Avogadro's number
- a wavelength of ⁇ is X-ray
- [rho is the density (g / cm 3)
- Z i , M i and x i respectively represent the atomic number, atomic weight and atomic number ratio (molar ratio) of the i-th atom
- f i ′ 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, and the density ⁇ can be obtained by Equation 4 from the relationship of Equations 2 and 3.
- ⁇ c is a value that can be obtained from the X-ray reflectivity
- r e , N o , and ⁇ are constants
- Z i , M i , and f i ′ are values specific to the constituent atoms.
- x i atomic number ratio (molar ratio)
- the result obtained from the XPS measurement is used.
- the film density in the surface part of the gas legislation layer is measured by the method described in Examples, and is obtained using Equation 4.
- the gas barrier layer of the present invention is preferably adjusted so as to satisfy the above requirements (b) and (c) by implanting ions. Therefore, it is preferable that ions are implanted into the gas barrier layer of the pressure-sensitive adhesive sheet of the present invention.
- the timing for implanting ions is not particularly limited. For example, there is a procedure in which a gas barrier layer is formed on a substrate and then ions are implanted into the gas barrier layer.
- Implanted ions include those obtained by ionizing rare gases such as argon, helium, neon, krypton, and xenon; ions obtained by ionizing gases such as fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, and sulfur. And metal ions such as gold, silver, copper, platinum, nickel, palladium, chromium, titanium, molybdenum, niobium, tantalum, tungsten, and aluminum.
- rare gases such as argon, helium, neon, krypton, and xenon
- ions obtained by ionizing gases such as fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, and sulfur.
- metal ions such as gold, silver, copper, platinum, nickel, palladium, chromium, titanium, molybdenum, niobium, tantalum, tungsten, and aluminum.
- a pressure-sensitive adhesive sheet that can be more easily injected and has particularly excellent gas barrier properties and transparency
- a gas in which at least one selected gas is ionized is preferable.
- the ion implantation amount is appropriately determined in consideration of the purpose of use of the pressure-sensitive adhesive sheet (necessary gas barrier properties, transparency, etc.).
- conditions for implanting ions known ones can be used, and examples include the conditions described in the examples.
- Examples of the ion implantation method include a method of irradiating ions accelerated by an electric field (ion beam), a method of implanting ions in plasma (plasma ion implantation method), and the like.
- plasma ion implantation method are preferable.
- a plasma is generated in an atmosphere containing a plasma generation gas, and a negative high voltage pulse is applied to the gas barrier layer, so that ions (positive ions) in the plasma are changed to the surface of the gas barrier layer. It can be performed by injecting into the part.
- the thickness of the portion into which ions are implanted can be controlled by the implantation conditions such as ion type, applied voltage, treatment time, etc., and may be determined according to the thickness of the gas barrier layer, the purpose of use of the adhesive sheet, and the like.
- the thickness of the portion into which ions are implanted is preferably 10 to 1000 nm, more preferably 10 to 500 nm, and still more preferably 10 to 250 nm.
- Adhesive layer It does not specifically limit as an adhesive which forms an adhesive layer, For example, what is used normally, for example, an acrylic adhesive, a rubber adhesive, a polyurethane adhesive, a silicone adhesive, etc. are mentioned.
- the acrylic pressure-sensitive adhesive is not particularly limited. For example, a (meth) acrylic acid ester homopolymer, a copolymer containing two or more (meth) acrylic acid ester units, and a (meth) acrylic acid ester and others. And those containing at least one selected from copolymers with functional monomers.
- “(Meth) acrylic acid” means acrylic acid or methacrylic acid (the same applies hereinafter).
- (meth) acrylic acid ester (meth) acrylic acid having 1 to 20 carbon atoms in the alkyl group is preferable, and butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, (meth ) Heptyl acrylate, octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, and the like.
- rubber-based pressure-sensitive adhesives include natural rubber, modified natural rubber obtained by graft polymerization of one or more monomers selected from (meth) acrylic acid alkyl ester, styrene, and (meth) acrylonitrile on natural rubber. And rubber adhesives made of styrene-butadiene rubber, acrylonitrile-butadiene rubber, methyl methacrylate-butadiene rubber, urethane rubber, polyisobutylene resin, polybutene resin, and the like.
- a rubber-based pressure-sensitive adhesive is preferable from the viewpoint of suppressing the permeation of water vapor from the end of the formed pressure-sensitive adhesive layer, and a pressure-sensitive adhesive containing a polyisobutylene resin is used. More preferably, a pressure-sensitive adhesive containing both a polyisobutylene resin and a polybutene resin is more preferable.
- the polyisobutylene-based resin is a resin having a polyisobutylene skeleton in the main chain or side chain, a resin having the following structural unit (a), and is a homopolymer of isobutylene, polyisobutylene, isobutylene and isoprene, isobutylene and n A copolymer of butene or isobutylene and butadiene, a halogenated butyl rubber obtained by brominating or chlorinating these copolymers, and the like.
- the polyisobutylene resin is a copolymer obtained from isobutylene and n-butene
- isobutylene is the maximum amount of monomer as a main component in the raw material monomers.
- Polyisobutylene resins may be used alone or in combination of two or more.
- the weight average molecular weight of the polyisobutylene resin is preferably 200,000 to 1,000,000, more preferably 250,000 to 800,000, still more preferably 300,000 to 500,000. If it is 200,000 or more, sufficient cohesive force of the adhesive composition can be obtained. Moreover, if it is 1 million or less, the cohesive force of the pressure-sensitive adhesive composition will not be too high, and sufficient wettability with the adherend will be obtained. Also, when preparing the pressure-sensitive adhesive, It can be dissolved sufficiently. Therefore, by selecting an appropriate molecular weight, the water vapor transmission rate is low, and high cohesion and wettability can be maintained. In addition, this weight average molecular weight (Mw) is a value in terms of polystyrene measured by gel permeation chromatography (GPC) method (hereinafter the same).
- Polybutene resin is a copolymer having a long-chain hydrocarbon molecular structure.
- the polybutene copolymer is a copolymer of isobutene, 1-butene, and 2-butene, and among these, an isobutene-1-butene copolymer is preferable.
- Polybutene resins may be used alone or in combination of two or more. This polybutene resin is well compatible with the polyisobutylene resin and appropriately plasticizes the polyisobutylene resin to improve the wettability with respect to the adherend and improve the adhesive properties, flexibility, holding power, etc. Is for.
- the weight average molecular weight of the polybutene resin is preferably 500 to 100,000, more preferably 1000 to 50,000, and still more preferably 3,000 to 10,000. If it is 500 or more, it is possible to prevent the possibility of adversely affecting the physical properties such as contamination of the adherend by separation as a low molecular component and increase of outgas generated at high temperature. Also, if 100,000 or less, it is possible to obtain a sufficient plasticizing effect, wetting of the adherend is sufficient.
- the weight average molecular weight is a value in terms of polystyrene as measured by gel permeation chromatography (GPC).
- the content of the polybutene resin is preferably 10 to 100 parts by mass, more preferably 15 to 100 parts by mass, and further preferably 25 to 100 parts by mass with respect to 100 parts by mass of the polyisobutylene resin.
- a hindered amine light stabilizer as a light stabilizer and a hindered phenol-based oxidation as an antioxidant.
- An inhibitor may be included. You may use a hindered amine light stabilizer and a hindered phenolic antioxidant individually or in combination of 2 or more types.
- hindered amine light stabilizer examples include dimethyl succinate-1- (2-hydroxyethyl) -4-hydroxy-2,2,6,6-tetramethylpiperidine polycondensate, poly [ ⁇ 6- (1,1,3,3? Tetramethylbutyl) amino-1,3,5?
- hindered phenol antioxidant examples include triethylene glycol-bis [3- (3-tert-butyl-5-methyl-4-hydroxyphenyl) propionate], 1,6-hexanediol-bis. [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], pentaerythrityl tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], 2 , 2-thio-diethylenebis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], octadecyl-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate N, N′-hexamethylenebis (3,5-di-tert-butyl-4-hydroxy-hydroxynnamamide, 1,3,5-trimethyl 2,4,6-tris (3,5-di-t-butyl-4-hydroxy
- the content of the hindered amine light stabilizer is preferably 0.25 to 1.0 part by weight, more preferably 0.4 to 1.0 part by weight, based on 100 parts by weight of the polyisobutylene resin.
- the content of the hindered phenol-based antioxidant is preferably 0.25 to 1.0 part by weight, more preferably 0.4 to 1.0 part by weight with respect to 100 parts by weight of the polyisobutylene resin. is there.
- the pressure-sensitive adhesive composition used in the present invention may further contain a cyclic olefin polymer.
- the cyclic olefin-based polymer is useful for the purpose of adjusting the viscosity at the time of coating, improving the flexibility due to the plastic effect, improving the initial adhesive force by improving the wettability, and increasing the cohesive force. Moreover, the point with a low water vapor transmission rate is also preferable.
- the cyclic olefin polymer is meant a polymer containing repeating units derived from cycloolefin monomers.
- the bonding mode of the cyclic olefin monomer is not particularly limited as long as a cyclic structure can be introduced into the main chain.
- Examples of the cyclic olefin polymer include those obtained by polymerizing the carbon-carbon unsaturated bond of the monomer, those obtained by addition polymerization of a cyclic conjugated diene, and more specifically, alicyclic having a norbornene ring. Ring-opening polymer obtained by ring-opening polymerization of an alicyclic monomer having a norbornene ring. Or addition polymerization of a monocyclic olefin monomer, or 1,4-addition polymerization of a cyclic conjugated diene monomer such as cyclopentadiene or cyclohexadiene, or a monocyclic olefin monomer.
- Examples include those obtained by copolymerizing a monomer and a cyclic conjugated diene monomer and a copolymerizable monomer other than the cyclic olefin. Further, these polymers may be further hydrogenated, and specific examples include so-called hydrogenated petroleum resins obtained by hydrogenating petroleum resins known as tackifiers. Examples of hydrogenated petroleum resins include partially hydrogenated resins having different hydrogenation rates, and fully hydrogenated resins. Compatibility with the polyisobutylene resin and the polybutene resin, water vapor transmission rate, high From the viewpoint of durability against wet heat and ultraviolet rays, a completely hydrogenated resin is preferred. In addition, you may use these cyclic olefin type polymers individually or in combination of 2 or more types.
- the weight average molecular weight of the cyclic olefin polymer is preferably from 200 to 5,000, more preferably from 500 to 3,000, from the viewpoints of adhesion, wetting with the adherend, and compatibility with the polyisobutylene resin.
- the content of the cyclic olefin polymer is preferably 10 to 300 parts by mass, more preferably 10 to 100 parts by mass with respect to 100 parts by mass of the polyisobutylene resin from the viewpoints of tackiness and wetting with the adherend. It is.
- the pressure-sensitive adhesive used in the present invention includes, as far as other additives are added, a light stabilizer, an antioxidant, an ultraviolet absorber, a resin stabilizer, a filler, a pigment, and an extender, as long as the adhesiveness is not impaired. Further, it may contain an antistatic agent, a tackifier, and the like. These additives may be used alone or in combination of two or more.
- the thickness of the pressure-sensitive adhesive layer is not particularly limited and may be appropriately selected depending on the use of the pressure-sensitive adhesive sheet, but is preferably 0.5 to 100 ⁇ m, more preferably 1 to 60 ⁇ m, and still more preferably 3 to 40 ⁇ m. It is. If it is 0.5 ⁇ m or more, good adhesive force can be obtained for the adherend, and if it is 100 ⁇ m or less, it is advantageous in terms of productivity and can be an easy-to-handle pressure-sensitive adhesive sheet.
- the pressure-sensitive adhesive composition can be produced by a known coating method as a solution in which the pressure-sensitive adhesive composition is dissolved in an organic solvent such as toluene, ethyl acetate, or methyl ethyl ketone.
- concentration of the solution is preferably 10 to 60% by mass, more preferably 10 to 30% by mass.
- Examples of the coating method include spin coating, spray coating, bar coating, knife coating, roll coating, blade coating, die coating, and gravure coating. After applying a solution in which the above-mentioned adhesive is dissolved in an organic solvent to the release layer surface of the substrate or release sheet by these coating methods, a temperature of 80 to 150 ° C. is used to prevent the solvent and low-boiling components from remaining. Can be heated and dried for 30 seconds to 5 minutes to form an adhesive layer.
- a release sheet can be further provided on the formed pressure-sensitive adhesive layer as desired.
- the adhesive sheet of this invention what laminated
- the release sheet may be in the outermost layer of the layer constituting the pressure-sensitive adhesive sheet, or the pressure-sensitive adhesive layer formed on the release sheet having releasability on both sides It may be in the form of being laminated and wound up as it is.
- the release sheet examples include paper substrates such as glassine paper, coated paper, and high-quality paper, laminated paper obtained by laminating a thermoplastic resin such as polyethylene or polypropylene on these paper substrates, and cellulose, starch A paper base material treated with polyvinyl alcohol, acrylic-styrene resin or the like, or a polyester film such as polyethylene terephthalate, polybutylene terephthalate or polyethylene naphthalate, a plastic film such as a polyolefin film such as polyethylene or polypropylene, and Examples include those obtained by applying a release agent to a film obtained by subjecting these plastic films to an easy adhesion treatment, and forming a release agent layer.
- release agent examples include rubber elastomers such as olefin resins, isoprene resins, butadiene resins, long chain alkyl resins, alkyd resins, fluorine resins, silicone resins, and the like.
- the thickness of the release agent layer formed on the substrate of the release sheet is not particularly limited. However, when a solution prepared by dissolving the release agent in the above organic solvent is applied on the substrate, it is preferably 0. .05 to 2.0 ⁇ m, more preferably 0.1 to 1.5 ⁇ m. On the other hand, when the release agent layer is formed using a thermoplastic resin such as polyethylene or polypropylene, the thickness of the release agent layer is preferably 3 to 50 ⁇ m, more preferably 5 to 40 ⁇ m.
- the water vapor transmission rate at a thickness of 50 ⁇ m of the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet of the present invention is preferably 25 g / m 2 / day or less, more preferably 10 g / m 2 / day or less in an atmosphere of 40 ° C. and relative humidity 90%. More preferably, it is 8 g / m 2 / day or less. If the water vapor transmission rate is 25 g / m 2 / day or less, water intrusion from the end of the pressure-sensitive adhesive layer can be prevented, so that it can also be suitably used for sealing organic EL elements. Further, the adhesive strength of the adhesive sheet of the present invention, even when a small thickness of the adhesive layer, has a high adhesive force.
- the adhesive strength of the adhesive sheet of the present invention is preferably 3N / 25 mm or more, more preferably 5N / 25 mm or more.
- the adhesive strength of the adhesive sheet of the present invention means a value measured by the method described in Example.
- the pressure-sensitive adhesive sheet of the present invention can be provided with other layers other than the above (1) to (3).
- examples of other layers include an inorganic compound layer, a shock absorbing layer, a conductor layer, and a primer layer.
- stacked is not specifically limited, According to the role of each layer, it selects suitably.
- An inorganic compound layer is a layer which consists of 1 type, or 2 or more types of an inorganic compound, and can further improve the gas barrier property of an adhesive sheet.
- the inorganic compound that constitutes the inorganic compound layer is generally capable of vacuum film formation and has a gas barrier property, such as an inorganic oxide, an inorganic nitride, an inorganic carbide, an inorganic sulfide, or a composite of these.
- gas barrier property such as an inorganic oxide, an inorganic nitride, an inorganic carbide, an inorganic sulfide, or a composite of these.
- examples thereof include nitrides, inorganic oxide carbides, inorganic nitride carbides, and inorganic oxynitride carbides.
- inorganic oxides, inorganic nitrides, and inorganic oxynitrides are preferable.
- Examples of inorganic oxides include metal oxides represented by the general formula: MOx.
- M represents a metal element.
- x has a different range depending on M. For example, if M is silicon (Si), 0.1 to 2.0, if aluminum (Al), 0.1 to 1.5, and if magnesium (Mg), 0.1 to 1.0, 0.1 to 1.0 for calcium (Ca), 0.1 to 0.5 for potassium (K), 0.1 to 2 for tin (Sn) 0.0, 0.1 to 0.5 for sodium (Na), 0.1 to 1.5 for boron (B), 0.1 to 2.0 for titanium (Ti), lead ( The value is in the range of 0.1 to 1.0 for Pb), 0.1 to 2.0 for zirconium (Zr), and 0.1 to 1.5 for yttrium (Y).
- silicon oxide in which M is silicon, aluminum oxide in aluminum, and titanium oxide in titanium are preferable, and silicon oxide is more preferable.
- the value of x is 1.0 to 2.0 when M is silicon and 0.5 to 1.5 when aluminum is used from the viewpoint of forming a layer having excellent transparency and the like. If so, the range of 1.3 to 2.0 is preferable.
- Examples of inorganic nitrides include metal nitrides represented by the general formula: MNy.
- M represents a metal element.
- silicon nitride where M is silicon, aluminum nitride which is aluminum, titanium nitride which is titanium, and tin nitride which is tin are preferable.
- Nitride (SiN) is more preferred.
- titanium 0.5 to 1.3 is preferable
- tin 0.5 to 1.3 is preferable.
- Examples of the inorganic oxynitrides include metal oxynitrides represented by the general formula: MOxNy.
- M represents a metal element.
- the metal oxide, a metal nitride and a metal oxynitride may also contain two or more metals.
- the method for forming the inorganic compound layer is not particularly limited, and examples thereof include a vapor deposition method, a sputtering method, an ion plating method, a thermal CVD method, a plasma CVD method, and a dynamic ion mixing method.
- a magnetron sputtering method is preferable because a laminate having an excellent gas barrier property can be easily obtained.
- the thickness of the inorganic compound layer is not particularly limited, but is preferably 10 to 1000 nm, more preferably 20 to 500 nm, and still more preferably 50 to 200 nm from the viewpoint of improving gas barrier properties.
- the shock absorbing layer is for preventing cracking when an impact is applied to the gas barrier layer or the inorganic compound layer, and the material for forming the shock absorbing layer is not particularly limited. Resins, urethane resins, silicone resins, olefin resins, rubber materials, and the like can be used. Among these, acrylic resins, silicone resins, and rubber materials are preferable.
- acrylic resins As acrylic resins, (meth) acrylic acid ester homopolymers, copolymers containing two or more (meth) acrylic acid ester units, and (meth) acrylic acid esters and other functional monomers are used as main components. What contains at least 1 sort (s) chosen from the copolymer with a monomer is mentioned.
- (meth) acrylic acid ester As the (meth) acrylic acid ester, (meth) acrylic acid having 1 to 20 carbon atoms in the ester portion is preferable, and (meth) acrylic acid ester having 4 to 10 carbon atoms in the ester portion is more preferable.
- Such (meth) acrylic acid esters include butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, (meth) Examples include 2-ethylhexyl acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, and the like.
- silicone resin examples include those containing dimethylsiloxane as a main component.
- the rubber-based material examples include materials mainly composed of isoprene rubber, styrene-butadiene rubber, polyisobutylene rubber, styrene-butadiene-styrene rubber and the like.
- the raw material which forms a shock absorption layer can also use what is marketed.
- the impact absorbing layer may contain other additives such as other components such as an antioxidant, a plasticizer, an ultraviolet absorber, a colorant, and an antistatic agent.
- the shock absorption layer containing the raw material which forms the said shock absorption layer, and other components, such as a solvent if desired, similarly to the formation method of an adhesive layer
- examples include a method in which a forming solution is applied onto a layer to be laminated, the obtained coating film is dried, and heated to form the film as necessary.
- a shock absorbing layer may be separately formed on the release substrate, and the obtained film may be transferred and stacked on the layer to be stacked.
- the thickness of the shock absorbing layer is usually 1 to 100 ⁇ m, preferably 5 to 50 ⁇ m.
- a conductor layer is a layer provided in order to give electroconductivity, when providing antistatic performance, or when using an adhesive sheet as an electrode.
- Examples of the material constituting the conductor layer include metals, alloys, metal oxides, electrically conductive compounds, and mixtures thereof.
- 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 Materials and the like.
- the conductor layer may be a laminate in which a plurality of layers made of these materials are laminated. Among these, in terms of transparency, a conductive metal oxide is preferable, and ITO is more preferable.
- Examples of 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 depending on the application and the like, but 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 with a base material layer, a gas barrier layer, an adhesive layer, or another layer.
- a pressure-sensitive adhesive sheet having excellent interlayer adhesion and surface smoothness can be obtained.
- the material constituting the primer 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; and ethyleneimine.
- These materials can be used alone or in combination of two or more.
- a primer layer forming solution obtained by dissolving or dispersing the material constituting the primer layer in an appropriate solvent is applied to one or both sides of the layer to be formed, and the resulting coating film is dried. It can be formed by heating if desired.
- a normal wet coating method can be used as a method for applying the primer layer forming solution to the layer to be formed. 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.
- 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.
- ion implantation may be performed on the obtained primer layer by a method similar to the method of implanting ions into the gas barrier layer described above. By performing ion implantation also on the primer layer, a pressure-sensitive adhesive sheet with better gas barrier properties can be obtained.
- the shape of the pressure-sensitive adhesive sheet of the present invention is not particularly limited, and examples thereof include a sheet shape. When used as an electronic device member to be described later, a sheet shape is preferable.
- the visible light transmittance of the pressure-sensitive adhesive sheet of the present invention at a wavelength of 550 nm is preferably 85% or more, more preferably 88% or more, and still more preferably 90% or more. If the visible light transmittance is 85% or more, it can be suitably used as an electronic device member to be described later, for example, as a sealing application in an organic EL element.
- permeability of an adhesive sheet can be measured using a well-known visible light transmittance
- the water vapor transmission rate of the entire pressure-sensitive adhesive sheet of the present invention having the gas barrier layer and the pressure-sensitive adhesive layer described above is preferably 1.0 g / m 2 / day or less, more preferably 0 in an atmosphere of 40 ° C. and a relative humidity of 90%. .5g / m 2 / day, more preferably not more than 0.1g / m 2 / day.
- the adhesive sheet of this invention is excellent in bending resistance as above-mentioned, even if it performs bending etc., gas barrier property can be maintained.
- the water vapor permeability of the entire pressure-sensitive adhesive sheet after the bending test described in the examples is preferably 1.0 g / m 2 / day or less, more preferably 0.5 g in an atmosphere of 40 ° C. and a relative humidity of 90%. / M 2 / day or less, more preferably 0.1 g / m 2 / day or less.
- the pressure-sensitive adhesive sheet of the present invention can be used as an electronic device member, for example, for sealing organic EL elements. Since the pressure-sensitive adhesive sheet of the present invention has excellent gas barrier properties and the like, for example, it is possible to prevent deterioration of organic EL elements and the like used in electronic devices.
- FIG. 2 the example of the organic EL element using the adhesive sheet of this invention is shown.
- the organic EL element 10 a structure 14 in which a transparent electrode, a hole transport layer, a light emitting layer, a back electrode, and the like are laminated on a glass substrate 12 is formed.
- the pressure-sensitive adhesive sheet 1 of the present invention has a configuration in which a gas barrier layer 3 and a pressure-sensitive adhesive layer 4 are laminated on a base material 2.
- the structure 14 is sealed.
- the organic EL element 10 is sealed by attaching the adhesive sheet 16 of the present invention after forming the structure 14 on the glass substrate 12. According to the pressure-sensitive adhesive sheet of the present invention, the element can be easily sealed.
- the electronic device of this invention is equipped with the adhesive sheet of this invention as a member for electronic devices. Since the pressure-sensitive adhesive sheet of the present invention has excellent gas barrier properties, transparency, bending resistance, etc., it can be used for various electronic devices. Examples of the electronic device of the present invention include a liquid crystal display, an organic EL display, an inorganic EL display, electronic paper, and a solar battery.
- Plasma ion implantation apparatus used XPS measurement apparatus, film density measurement apparatus by X-ray reflectivity method, bending test method, water vapor transmission rate measurement apparatus and measurement conditions, water vapor transmission test method at end of adhesive layer, adhesion
- the force measuring method and the visible light transmittance measuring device 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.
- the plasma ion implantation apparatus used is an apparatus for implanting ions using an external electric field. The conditions for plasma ion implantation are shown below.
- Plasma generated gas Ar ⁇ Gas flow rate: 100sccm ⁇ Duty ratio: 0.5% ⁇ Repetition frequency: 1000Hz ⁇ Applied voltage: -10kV -RF power supply: frequency 13.56 MHz, applied power 1000 W -Chamber internal pressure: 0.2 Pa ⁇ Pulse width: 5 ⁇ sec ⁇ Processing time (ion implantation time): 5 minutes ⁇ Conveying speed: 0.2 m / min
- XPS measuring device An XPS measurement device is measured by elemental analysis by X-ray photoelectron spectroscopy (XPS) to measure the abundance ratio of oxygen atoms, nitrogen atoms, and silicon atoms in the surface layer portion (around 5 nm from the surface) of the gas barrier layer. Used.
- the measurement equipment and measurement conditions are as follows. Measuring device: “PHI Quantera SXM”
- ULVAC-PHI X-ray source AlK ⁇ X-ray beam diameter: 100 ⁇ m
- Electric power value 25W Voltage: 15kV Extraction angle: 45 ° Degree of vacuum: 5.0 ⁇ 10 ⁇ 8 Pa
- the film density in the surface layer portion of the gas barrier layer was calculated from the total reflection critical angle ⁇ c obtained by measuring the X-ray reflectivity under the following measurement conditions.
- the measurement equipment and measurement conditions are as follows.
- Measuring device Sample horizontal X-ray diffractometer for thin film evaluation “SmartLab” manufactured by Rigaku Corporation Measurement conditions: 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
- Light receiving slit system Light 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; ldeg. / Min.
- the atomic ratio (x i in the above formula 4) used the abundance ratio of oxygen atoms, nitrogen atoms and silicon atoms in the surface layer portion of the gas para layer obtained by X-ray photoelectron spectroscopy measurement.
- Water vapor permeability measuring device and measurement conditions When the water vapor transmission rate is 0.01 g / m 2 / day or more, a water vapor transmission meter (manufactured by LYSSY, product name “L89-500”) is used, and the water vapor transmission rate is less than 0.01 g / m 2 / day.
- the water vapor transmission rate of the pressure-sensitive adhesive sheet (“water vapor transmission rate before bending” in Table 1) was measured under the conditions of 40 ° C. and relative humidity of 90% using “deltaperm” manufactured by TECHNOLOX. Further, the water vapor transmission rate of the pressure-sensitive adhesive sheet after the bending test (“water vapor transmission rate after bending” in Table 1) was also measured in the same manner.
- PET 6 ⁇ m polyethylene terephthalate film (manufactured by Mitsubishi Plastics, trade name“ K200-6E ”, thickness 6 ⁇ m) (hereinafter also referred to as“ PET 6 ⁇ m ”)” It stuck on both surfaces and measured by the structure of PET6micrometer / adhesive layer 50micrometer / PET6micrometer.
- the pressure-sensitive adhesive sheet for the water vapor permeation test at the edge of the pressure-sensitive adhesive was cut into a frame shape having an outer dimension of 60 mm ⁇ 60 mm and a width of 2 mm, the light release sheet was peeled off, and affixed to a 70 mm ⁇ 70 mm ⁇ 2 mm thick glass plate. Next, the heavy release sheet is peeled off, a humidity indicator seal (product name “RH-70”, manufactured by Asei Kogyo Co., Ltd.) is attached to the inside of the frame of the adhesive sheet, and then attached to another glass plate. The space was sealed with two glass plates and an adhesive sheet.
- a humidity indicator seal product name “RH-70”, manufactured by Asei Kogyo Co., Ltd.
- the prepared specimen was left in an atmosphere of 60 ° C. and a relative humidity of 90%, and then the humidity in the frame was evaluated.
- the humidity indicator used is colored from white to blue at a relative humidity of 70%, and the accuracy is ⁇ 5% RH (RH: relative humidity) at 25 ° C.
- the evaluation criteria are as shown below. ⁇ : No color change of humidity indicator seal ⁇ : There is a slight color change of humidity indicator seal
- the visible light transmittance (%) of the pressure-sensitive adhesive sheet was measured at a measurement wavelength of 550 nm using a visible light transmittance measuring device (manufactured by Shimadzu Corporation, “UV-3101PC”).
- Polysilazane compound A Coating material mainly composed of perhydropolysilazane (trade name “AQUAMICA NL110-20” manufactured by Clariant Japan Co., Ltd.)
- Polysilazane compound B a coating material mainly composed of a mixture of organopolysilazane compounds having a saturated hydrocarbon group (manufactured by Clariant Japan, trade name “tutoPromBright”)
- polysilazane compound A As a substrate, polysilazane compound A was applied by spin coating to a polyethylene terephthalate film (Mitsubishi Resin, “PET38 T-100”, thickness 38 ⁇ m, hereinafter referred to as “PET film”), and then at 120 ° C. for 1 minute. A 60 nm thick polysilazane layer containing perhydropolysilazane was formed on the PET film by heating. Next, argon (Ar) was plasma ion-implanted into the surface of the layer containing perhydropolysilazane using a plasma ion implantation apparatus to produce “a substrate with a gas barrier layer 1”.
- argon (Ar) was plasma ion-implanted into the surface of the layer containing perhydropolysilazane using a plasma ion implantation apparatus to produce “a substrate with a gas barrier layer 1”.
- a “base material with a gas barrier layer 11” was obtained in the same manner as in Production Example 2 except that oxygen (O 2 ) was used instead of argon as the plasma generation gas.
- a “base material with a gas barrier layer 12” was obtained in the same manner as in Production Example 2 except that helium (He) was used instead of argon as the plasma generation gas.
- a “base material with a gas barrier layer 13” was obtained in the same manner as in Production Example 2, except that neon (Ne) was used instead of argon as the plasma generation gas.
- Examples 1 to 22, Comparative Examples 1 to 3 Using the pressure-sensitive adhesive composition obtained as described above and the base material with a gas barrier layer obtained in Production Examples 1 to 17, the pressure-sensitive adhesive sheets of Examples 1 to 22 and Comparative Examples 1 to 3 were as follows. It produced as follows. Combinations of the pressure-sensitive adhesive composition and the base material with the gas barrier layer are as shown in Table 1.
- the pressure-sensitive adhesive compositions A to H are applied to the release surface of a light release sheet (trade name “SP-PET1031”, manufactured by Lintec Corporation) using a roll knife coater so that the film thickness after drying becomes 20 ⁇ m. And dried at 100 ° C. for about 1 minute to form an adhesive layer.
- the gas barrier layer surface of the substrate with the gas barrier layers 1 to 17 was laminated on the pressure-sensitive adhesive surface and bonded to obtain a pressure-sensitive adhesive sheet.
- the pressure-sensitive adhesive sheet of the example having the gas barrier layer satisfying the above requirements (A) to (C) has a low water vapor transmission rate and high compared to the pressure-sensitive adhesive sheets of Comparative Examples 1 to 3 that do not satisfy the requirement. It had gas barrier properties. Also, in the water vapor permeation test at the end of the pressure-sensitive adhesive layer, there was almost no water intrusion from the end of the pressure-sensitive adhesive layer, and the adhesive strength was sufficient. Further, after the bending test, the pressure-sensitive adhesive sheet of the example showed no occurrence of cracks in the gas barrier layer, but in Comparative Example 3 in which an inorganic film (silicon nitride film) was formed, the occurrence of cracks was seen. . In addition, the pressure-sensitive adhesive sheet of the example had a small increase in water vapor transmission rate as compared with Comparative Example 3, was excellent in bending resistance, and was also excellent in transparency.
- the pressure-sensitive adhesive sheet of the present invention is an organic transistor, organic memory, electrochromic electronic device, LCD, touch panel, electronic paper display, solar cell photoelectric conversion device, electrochemiluminescence device, thermoelectric conversion device, piezoelectric conversion device, etc. It is useful in various electronic devices.
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Abstract
Description
例えば、液晶ディスプレイやエレクトロルミネッセンス(EL)ディスプレイに用いられる発光素子として、低電圧直流駆動による高輝度発光が可能な有機EL素子が注目されている。これらのディスプレイには、薄型化、軽量化、フレキシブル化等を実現するために、電極を有する基板として、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。
また、フィルムの少なくとも一方の面にポリシラザン膜を形成し、該ポリシラザン膜にプラズマ処理を施して、ガスバリア性フィルムを製造する方法が開示されている(特許文献1参照)。しかしながら、このガスバリア性フィルムを基材として用いると、ガスバリア層にクラックが発生する等の問題を有している。
他に、有機デバイス用の粘着シートとして、例えば、ポリイソブチレン系の樹脂を接着層として用いる接着性フィルムが開示されている(特許文献2参照)。しかしながら、特許文献2の接着層は高温・紫外線等に弱く、有機EL素子やデバイスが長時間の駆動や駆動環境によって高温下又は紫外線照射下に曝されることによって、接着層の樹脂自体が劣化し、接着性フィルムの性能低下とそれに伴う有機EL素子の劣化を引き起こす可能性あるという問題を有している。
[1]基材上に、少なくともガスバリア層と粘着剤層とを有する粘着シートであって、前記ガスバリア層が、少なくとも、酸素原子及びケイ素原子を含む材料から構成されてなり、前記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量全体に対する、酸素原子の存在割合が60~75%、窒素原子の存在割合が0~10%、ケイ素原子の存在割合が25~35%であり、かつ、前記ガスバリア層の表層部における膜密度が、2.4~4.0g/cm3である、粘着シート。
[2]前記ガスバリア層を構成する材料が、ポリシラザン化合物よりなる、上記[1]に記載の粘着シート。
[3]前記ポリシラザン化合物が、ペルヒドロポリシラザンである、上記[2]に記載の粘着シート。
[4]前記ガスバリア層が、イオンが注入されてなる、上記[1]~[3]のいずれか1項に記載の粘着シート。
[5]前記イオンが、水素、窒素、酸素、アルゴン、ヘリウム、ネオン、キセノン、及びクリプトンからなる群から選ばれる少なくとも一種のガスがイオン化されたものである、上記[4]に記載の粘着シート。
[6]前記粘着剤層の厚み50μmにおける水蒸気透過率が、40℃、相対湿度90%の雰囲気下で、25g/m2/day以下である、上記[1]~[5]のいずれか1項に記載の粘着シート。
[7]前記粘着剤層を形成する粘着剤が、ゴム系粘着剤又はアクリル系粘着剤である、上記[1]~[6]のいずれか1項に記載の粘着シート。
[8]上記[1]~[7]のいずれか1項に記載の粘着シートを電子デバイス用部材として備えた、電子デバイス。
本発明の粘着シートは、基材上に、少なくともガスバリア層と粘着剤層を有する。図1は、本発明の粘着シートの構成の一例を示す図である。本発明の粘着シートは、少なくとも、基材、ガスバリア層、粘着剤層を有しているが、粘着剤層が最外層に存在すれば、積層する順序は特に問わない。例えば、図1の(A1)のように、基材2の片面にガスバリア層3を積層し、そのガスバリア層3の上に粘着剤層4が積層される粘着シート1が挙げられる。また、図1の(A2)の粘着シート1aのように、基材2の片面上に粘着剤層4を積層し、基材2の粘着剤層4の反対側にガスバリア層3を形成してもよい。
他にも、図1の(B)のように、基材2の片面にガスバリア層3、粘着剤層4aを積層した上で、反対側の基材の表面に粘着剤層4bを設けて、両面に粘着剤層を有する粘着シート1bとしてもよい。
さらに、図1の(C)のように、基材2aの片面に積層したガスバリア層3aと、基材2bの片面に積層したガスバリア層3bとの2つのガスバリア層3a、3bの間に粘着剤層4aを設け、基材2a、2bのガスバリア層が設けられた面とは反対側にそれぞれ粘着剤層4b、4cを有する粘着シート1cとしてもよい。この粘着シート1cは、粘着剤層4aが2つのガスバリア層3a、3bを接着するだけでなく、外部から衝撃が加わった場合に、衝撃を吸収し、ガスバリア層3a、3bを保護する役割を担うことができる。
なお、図1には示されていないが、基材、ガスバリア層、粘着剤層以外の「その他の層」を設けてもよい。その他の層が積層される位置は、特に限定されず、各層の役割に応じて適宜選択される。
以下、粘着シートを構成する(1)基材、(2)ガスバリア層、(3)粘着剤層、(4)その他の層について、順次説明する。
本発明の基材としては、ポリシラザン化合物以外の材料であって、自己支持性を有し、本発明の目的に合致するものであれば特に制限されない。用いる基材としては、例えば、ポリイミド、ポリアミド、ポリアミドイミド、ポリフェニレンエーテル、ポリエーテルケトン、ポリエーテルエーテルケトン、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、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。
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等が挙げられ、これらの市販品の具体例としては、アペル(三井化学社製のエチレン-シクロオレフィン共重合体)、アートン(JSR社製のノルボルネン系重合体)、ゼオノア(日本ゼオン社製のノルボルネン系重合体)等が挙げられる。
基材の厚みとしては、特に限定はされないが、好ましくは0.5~500μm、より好ましくは1~200μm、より好ましくは10~100μmである。
本発明の粘着シートのガスバリア層は、少なくとも以下の(a)~(c)の要件を満たす。
(a)少なくとも、酸素原子及びケイ素原子を含む材料から構成されてなる。
(b)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量全体に対する、酸素原子の存在割合が60~75%、窒素原子の存在割合が0~10%、ケイ素原子の存在割合が25~35%である。
(c)ガスバリア層の表層部における膜密度が、2.4~4.0g/cm3である。
上記要件(a)~(c)を具備するガスバリア層を用いることで、ガスバリア性、耐折り曲げ性、及び透明性に優れた粘着シートを得ることができる。
上記要件(a)を満たす材料として、ガスバリア性、耐折り曲げ性、及び透明性を向上させる観点から、ポリシラザン化合物が好ましい。
ポリシラザン化合物は、分子内に、-Si-N-結合を含む繰り返し単位を有する高分子であり、具体的には、式(1)で表される繰り返し単位を有する化合物が挙げられる。
無置換若しくは置換基を有するシクロアルキル基のシクロアルキル基としては、シクロブチル基、シクロペンチル基、シクロヘキシル基、シクロヘプチル基等の炭素数3~10のシクロアルキル基が挙げられる。
無置換若しくは置換基を有するアルケニル基のアルケニル基としては、例えば、ビニル基、1-プ口ペニル基、2-プロペニル基、1-ブテニル基、2-ブテニル基、3-ブテニル基等の炭素数2~10のアルケニニル基が挙げられる。
これらのアリール基の置換基としては、フッ素原子、塩素原子、臭素原子、ヨウ素原子等のハロゲン原子;メチル基、エチル基等の炭素数1~6のアルキル基;メトキシ基、エトキシ基等の炭素数1~6のアルコキシ基;ニトロ基;シアノ基;ヒドロキシル基;チオール基;エボキシ基;グリシドキシ基;(メタ)アクリロイルオキシ基;フェニル基、4-メチルフェニル基、4-クロロフェニル基等の無置換若しくは置換基を有するアリール基;等が挙げられる。
これらの中でも、Rx、Ry、Rzとしては、水素原子、炭素数1~6のアルキル基、又はフェニル基が好ましく、水素原子がより好ましい。
(i)-(Rx’SiHNH)-(Rx’は、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を表す。以下のRx’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化合物。
(ii)-(Rx’SiHNRz’)-(Rz’は、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化合物。
(iii)-(Rx’Ry’SiNH)-(Ry’は.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化合物。
(iv)下記式(6)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。
(v)下記式(7)で表される繰り返し構造を有するポリシラザン。
具体的な製造方法としては、例えば、下記式(9)で表される無置換若しくは置換基を有するハロゲノシラン化合物と2級アミンとの反応生成物に、アンモニア又は1級アミンを反応させることにより有機ポリシラザンを合成することができる。用いる2級アミン及び1級アミンは、目的とするポリシラザン化合物の構造に応じて、適宜選択すればよい。
用いるポリシラザン化合物の数平均分子量は、特に限定されないが、好ましくは100~50000である。なお、本発明において数平均分子量(Mn)は、ゲルパーミエーションクロマトグラフィー(GPC法)によりポリスチレン換算値として算出した値である(以下同じ)。
また、ガスバリア層は、ポリシラザン化合物の他に、本発明の目的を阻害しない範囲で他の成分を含んでいてもよい。他の成分としては、硬化剤、他の高分子、老化防止剤、光安定剤、難燃剤等が挙げられる。
ガスバリア層中のポリシラザン化合物の含有量は、優れたガスバリア性を有するガスバリア層を形成する観点から、ガスバリア層を構成する全材料中、好ましくは50質量%以上、より好ましくは70質量%以上、更に好ましくは85質量%以上、より更に好ましくは実質100質量%である。
塗工方法としては、特に限定されず、スピンコーター、ナイフコーター、グラビアコーター等の公知の塗工装置を使用する方法が挙げられる。
また、得られた塗膜の乾燥及びガスバリア層のガスバリア性向上のため、塗膜を加熱することが好ましい。加熱は80~150℃で数十秒から数十分行うことが好ましく、80~150℃で10秒~120分行うことがより好ましく、95~140℃で30秒~40分行うことが更に好ましく、95~140℃で60秒~30分行うことがより更に好ましい。
本発明におけるガスバリア層の表層部とは、ガスバリア層の表面、及び該表面から深さ方向に5nmまでの領域をいう。また、ガスバリア層の表面とは、他層との境界面を形成する場合、該境界面も含まれる。
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は、X線光電子分光分析(XPS)を用いて、表面から5nm付近のガスバリア層の表層部の元素分析測定を行うことによって確認することができる。具体的には、実施例において説明する方法で測定される。
本発明のガスバリア層の表層部における膜密度は、ガスバリア性、耐折り曲げ性、及び透明性を向上させる観点から、2.4~4.0g/cm3であるが、好ましくは2.45~4.0g/cm3、より好ましくは2.5~4.0g/cm3である。
当該膜密度が2.4g/cm3未満であると、特に粘着シートのガスバリア性が劣る結果となる。
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、以下の式1及び式2となることが知られている。
ガスパリア層の表属部における膜密度は、実施例において説明する方法で測定し、式4を用いて得られる。
イオンを注入する時機としては、特に限定されないが、例えば、基材上にガスバリア層を形成した後、該ガスバリア層にイオンを注入する手順が挙げられる。
これらの中でも、より簡便に注入することができ、特に優れたガスバリア性と透明性を有する粘着シートを得る観点から、水素、窒素、酸素、アルゴン、ヘリウム、ネオン、キセノン、及びクリプトンからなる群から選ばれる少なくとも一種のガスがイオン化されたものが好ましい。
なお、イオンの注入量は、粘着シートの使用目的(必要なガスバリア性、透明性等)等を考慮して適宜決定される。イオンを注入する条件としては、公知のもの用いることができ、例えば、実施例に記載の条件等が挙げられる。
プラズマイオン注入法は、例えば、プラズマ生成ガスを含む雰囲気下でプラズマを発生させ、ガスバリア層に負の高電圧パルスを印加することにより、該プラズマ中のイオン(陽イオン)を、ガスバリア層の表面部に注入して行うことができる。
イオンが注入される部分の厚みは、好ましくは10~1000nm、より好ましくは10~500nm、更に好ましくは10~250nmである。
粘着剤層を形成する粘着剤としては、特に限定されず、通常用いられるもの、例えば、アクリル系粘着剤、ゴム系粘着剤、ポリウレタン系粘着剤、シリコーン系粘着剤等が挙げられる。
アクリル系粘着剤としては、特に限定されず、例えば、(メタ)アクリル酸エステル単独重合体、2種以上の(メタ)アクリル酸エステル単位を含む共重合体、及び(メタ)アクリル酸エステルと他の官能性単量体との共重合体の中から選ばれた少なくとも1種を含有するものが挙げられる。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)。
(メタ)アクリル酸エステルとしては、アルキル基の炭素数が1~20の(メタ)アクリル酸が好ましく、(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。
ゴム系粘着剤としては、例えば、天然ゴム、天然ゴムに(メタ)アクリル酸アルキルエステル、スチレン、(メタ)アクリロニトリルから選ばれる1種又は2種以上の単量体をグラフト重合させた変性天然ゴム系粘着剤や、スチレン-ブタジエンゴム、アクリロニトリル-ブタジエンゴム、メタクリル酸メチル-ブタジエンゴム、ウレタンゴム、ポリイソブチレン系樹脂、ポリブテン樹脂等からなるゴム系粘着剤等が挙げられる。
これらの中でも、粘着剤層を形成する粘着剤として、形成される粘着剤層の端部からの水蒸気の透過を抑制する観点から、ゴム系粘着剤が好ましく、ポリイソブチレン系樹脂を含む粘着剤がより好ましく、ポリイソブチレン系樹脂とポリブテン樹脂とを共に含む粘着剤が更に好ましい。
ポリブテン樹脂は単独又は2種以上を併用して用いてもよい。このポリブテン樹脂は、前記ポリイソブチレン系樹脂と良好に相溶し、このポリイソブチレン系樹脂を適度に可塑化して、被着体に対する濡れ性を高め、粘着物性、柔軟性、保持力等を向上させるためのものである。
ポリブテン樹脂の含有量は、ポリイソブチレン系樹脂100質量部に対して、好ましくは10~100質量部、より好ましくは15~100質量部、更に好ましくは25~100質量部含む。
特定の重量平均分子量を有するポリイソブチレン系樹脂とポリブテン樹脂とを特定の量で含むことで、粘着力や凝集力と水蒸気透過率とがバランスよく、透明性にも優れた粘着剤層を形成し得る粘着剤組成物となる。
また、ヒンダードフェノール系酸化防止剤の含有量は、ポリイソブチレン系樹脂100質量部に対して、好ましくは0.25~1.0重量部、より好ましくは0.4~1.0質量部である。
本発明において、環状オレフィン系重合体とは、環状オレフィン系単量体由来の繰り返し単位を含有する重合体を意味する。環状オレフィン系単量体の結合様式は、主鎖中に環状構造を導入しうるものであれば特に限定されない。
環状オレフィン系重合体としては、該単量体の炭素-炭素不飽和結合を重合したもの、環状共役ジエンを付加重合したもの等が挙げられ、より具体的には、ノルボルネン環を有する脂環族系単量体を付加重合させたもの、環状オレフィン以外の共重合可能な単量体と共重合させたもの、ノルボルネン環を有する脂環族系単量体を開環重合させた開環重合体や、単環の環状オレフィン系単量体を付加重合させたもの、シクロペンタジエンやシクロヘキサジエン等の環状共役ジエン系単量体を1,4-付加重合させたもの、単環の環状オレフィン系単量体及び環状共役ジエン系単量体と環状オレフィン以外の共重合可能な単量体とを共重合させたもの等も挙げられる。
また、これらの重合体は、更に水素添加させたものを用いてもよく、具体的には、粘着付与剤として知られる石油樹脂を水素添加した、いわゆる水添石油樹脂等を挙げることができる。
水添石油樹脂としては、水添化率を異にする部分水添樹脂、及び完全水添樹脂を挙げることができ、前記ポリイソブチレン系樹脂及び前記ポリブテン樹脂との相溶性、水蒸気透過率、高湿熱や紫外線に対する耐久性の点から、完全水添樹脂が好ましい。
なお、これらの環状オレフィン系重合体は、単独又は2種以上を併用して用いてもよい。
環状オレフィン系重合体の含有量は、粘着性、被着体との濡れの観点から、ポリイソブチレン系樹脂100質量部に対して、好ましくは10~300質量部、より好ましくは10~100質量部である。
本発明の粘着剤層を形成する方法は、特に制限はなく公知の方法により製造できる。例えば、粘着剤組成物をトルエン、酢酸エチル、メチルエチルケトン等の有機溶剤に溶解した溶液として公知の塗工方法により製造することができる。この場合、当該溶液の濃度としては、好ましくは10~60質量%、より好ましくは10~30質量%である。
本発明の粘着シートにおいて、剥離シートが粘着シートを構成する層の最外層に位置するような形態であってもよいし、両面に離型性を持たせた剥離シートに、形成した粘着剤層上に積層してそのまま巻き取った形態であってもよい。
剥離剤としては、例えば、オレフィン系樹脂、イソプレン系樹脂、ブタジエン系樹脂等のゴム系エラストマー、長鎖アルキル系樹脂、アルキド系樹脂、フッ素系樹脂、シリコーン系樹脂等が挙げられる。
また、本発明の粘着シートの粘着力は、粘着剤層の厚みが薄い場合でも、高い粘着力を有する。本発明の粘着シートの粘着力は、好ましくは3N/25mm以上、より好ましくは5N/25mm以上である。なお、本発明の粘着シートの粘着力は、実施例に記載された方法により測定された値を意味する。
本発明の粘着シートは、上述の(1)~(3)以外のその他の層を設けることができる。その他の層としては、無機化合物層、衝撃吸収層、導電体層、プライマー層等が挙げられる。なお、その他の層が積層される位置は、特に限定されず、各層の役割に応じて適宜選択される。
(無機化合物層)
無機化合物層は、無機化合物の1種又は2種以上からなる層であり、粘着シートのガスバリア性をさらに向上させることができる。無機化合物層を構成する無機化合物としては、一般的に真空成膜可能で、ガスバリア性を有するもの、例えば無機酸化物、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等が挙げられる。本発明においては、これらの中でも、無機酸化物、無機窒化物、無機酸化窒化物が好ましい。
式中、Mは金属元素を表す。xはMによってそれぞれ範囲が異なり、例えば、Mがケイ素(Si)であれば0.1~2.0、アルミニウム(Al)であれば0.1~1.5、マグネシウム(Mg)であれば0.1~1.0、カルシウム(Ca)であれば0.1~1.0、カリウム(K)であれば0.1~0.5、スズ(Sn)であれば0.1~2.0、ナトリウム(Na)であれば0.1~0.5、ホウ素(B)であれば0.1~1.5、チタン(Ti)であれば0.1~2.0、鉛(Pb)であれば0.1~1.0、ジルコニウム(Zr)であれば0.1~2.0、イットリウム(Y)であれば、0.1~1.5の範囲の値である。
式中、Mは金属元素を表す。yはMによってそれぞれ範囲が異なり、Mがケイ素(Si)であればy=0.1~1.3、アルミニウム(Al)であればy=0.1~1.1、チタン(Ti)であればy=0.1~1.3、すず(Sn)であればy=0.1~1.3の範囲の値である。
式中、Mは金属元素を表す。x及びyの値は、Mによってそれぞれ範囲が異なる。すなわち、x、yは、例えば、Mがケイ素(Si)であればx=1.0~2.0、y=0.1~1.3、アルミニウム(Al)であればx=0.5~1.0、y=0.1~1.0、マグネシウム(Mg)であればx=0.1~1.0、y=0.1~0.6、カルシウム(Ca)であればx=0.1~1.0、y=0.1~0.5、カリウム(K)であればx=0.1~0.5、y=0.1~0.2、スズ(Sn)であればx=0.1~2.0、y=0.1~1.3、ナトリウム(Na)であればx=0.1~0.5、y=0.1~0.2、ホウ素(B)であればx=0.1~1.0、y=0.1~0.5、チタン(Ti)であればx=0.1~2.0、y=0.1~1.3、鉛(Pb)であればx=0.1~1.0、y=0.1~0.5、ジルコニウム(Zr)であればx=0.1~2.0、y=0.1~1.0、イットリウム(Y)であればx=0.1~1.5、y=0.1~1.0の範囲の値である。
なお、金属酸化物、金属窒化物及び金属酸化窒化物には、2種類以上の金属が含まれていてもよい。
衝撃吸収層は、前記ガスバリア層や、無機化合物層に衝撃が加わった際に、割れを防止するためのものであり、衝撃吸収層を形成する素材としては、特に限定されないが、例えば、アクリル系樹脂、ウレタン系樹脂、シリコーン系樹脂、オレフィン系樹脂、ゴム系材料等を用いることができる。これらの中でも、アクリル系樹脂、シリコーン系樹脂、ゴム系材料が好ましい。
(メタ)アクリル酸エステルとしては、エステル部分の炭素数が1~20の(メタ)アクリル酸が好ましく、エステル部分の炭素数が4~10の(メタ)アクリル酸エステルを用いることがより好ましい。このような(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。
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等が挙げられる。なお、衝撃吸収層を形成する素材は、市販されているものを使用することもできる。
また、衝撃吸収層には、各種添加剤、例えば、酸化防止剤、可塑剤、紫外線吸収剤、着色剤、帯電防止剤等の他の成分を含んでいてもよい。
衝撃吸収層の厚みは、通常1~100μm、好ましくは5~50μmである。
導電体層は、帯電防止性能を付与する場合や、粘着シートを電極として用いる場合に、導電性を持たせるために設けられる層である。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、これらの混合物等が挙げられる。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。導電体層は、これらの材料からなる層が複数積層されてなる積層体であってもよい。
これらの中でも、透明性の点から、導電性金属酸化物が好ましく、ITOがより好ましい。
プライマー層は、基材層、ガスバリア層、粘着剤層、あるい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に極めて優れる粘着シートを得ることができる。
本発明の粘着シートの波長550nmにおける可視光線透過率は、好ましくは85%以上、より好ましくは88%以上、更に好ましくは90%以上である。可視光線透過率が85%以上であれば、後述する電子デバイス用部材として、例えば、有機EL素子において封止用途として好適に用いることができる。なお、粘着シートの可視光透過率は、公知の可視光透過率測定装置を使用して測定することができ、本発明においては実施例に記載の方法にて測定された値を意味する。
また、上述のとおり、本発明の粘着シートは耐折り曲げ性に優れているため、折り曲げ等を行っても、ガスバリア性を維持できる。実施例に記載の折れ曲げ試験後の粘着シート全体の水蒸気透過率としては、40℃、相対湿度90%の雰囲気下で、好ましくは1.0g/m2/day以下、より好ましくは0.5g/m2/day以下、更に好ましくは0.1g/m2/day以下である。
本発明の粘着シートは、電子デバイス用部材として、例えば、有機EL素子の封止用途として用いることができる。本発明の粘着シートは優れたガスバリア性等を有するため、例えば、電子デバイスで用いている有機EL素子等の劣化を防ぐことができる。図2には、本発明の粘着シートを用いた有機EL素子の例を示す。この有機EL素子10では、ガラス基板12上に、透明電極、正孔輸送層、発光層及び背面電極等が積層された構造体14が形成されている。本発明の粘着シート1は、基材2上にガスバリア層3、及び粘着剤層4が積層している構成を有する。この本発明の粘着シート1の粘着剤層4が、構造体14とガラス基板12と密着し固着されることにより、構造体14が封止される。
有機EL素子10は、ガラス基板12上に構造体14を形成した後、本発明の粘着シート16を貼付して封止される。本発明の粘着シートによれば、簡便に素子を封止できる。
本発明の電子デバイスは、本発明の粘着シートを電子デバイス用部材として備える。本発明の粘着シートは、優れたガスバリア性、透明性、耐折れ曲げ性等を有するため、各種電子デバイスに用いることができる。本発明の電子デバイスとしては、液晶ディスプレイ、有機ELディスプレイ、無機ELディスプレイ、電子ペーパー、太陽電池等が挙げられる。
用いたプラズマイオン注入装置、XPS測定装置、X線反射率法による膜密度測定装置、折り曲げ試験の方法、水蒸気透過率測定装置と測定条件、粘着剤層の端部の水蒸気透過試験の方法、粘着力の測定方法、及び可視光透過率測定装置は以下のとおりである。
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」
なお、用いたプラズマイオン注入装置は外部電界を用いてイオンを注入する装置である。
プラズマイオン注入の条件を以下に示す。
・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):5分間
・搬送速度:0.2m/min
ガスバリア層の表層部(表面から5nm付近)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、X線光電子分光(XPS:X-ray Photoelectron Spectroscopy)による元素分析により、XPS測定装置を用いて行った。測定装置と測定条件は以下のとおりである。
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、その値から算出した。測定装置と測定条件は以下のとおりである。
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;ldeg./min.
サンプリング間隔;0.002°/step
なお、原子数比(上記式4中のxi)は、X線光電子分光測定により得られたガスパ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。
粘着シートのガスバリア層の表層部を外側にし、中央部分で半分に折り曲げて、ラミネーター(フジプラ社製、製品名「LAMIPACKER LPC1502」)の2本のロール間を、ラミネート速度5m/分、温度23℃の条件で通した後、折り曲げた部分を顕微鏡で観察(100倍)してガスバリア層のクラック発生の有無を観察した。クラックの発生が認められなかった場合を「なし」、クラックの発生が認められた場合を「あり」と評価した。
水蒸気透過率が0.01g/m2/day以上のときは、水蒸気透過度計(LYSSY社製、製品名「L89-500」)を用い、水蒸気透過率が0.01g/m2/day未満のときは、TECHNOLOX社製、「deltaperm」を用いて、40℃、相対湿度90%の条件で粘着シートの水蒸気透過率(表1における、「折り曲げ前の水蒸気透過率」)を測定した。また、上記の折り曲げ試験後の粘着シートの水蒸気透過率(表1における、「折り曲げ後の水蒸気透過率」)についても、同様に測定した。
ただし、粘着剤層の水蒸気透過率に関しては、「ポリエチレンテレフタレートフィルム(三菱樹脂社製、商品名「K200-6E」、厚さ6μm)(以下、「PET6μm」ともいう)」を粘着剤層50μmの両面に貼付し、PET6μm/粘着剤層50μm/PET6μmの構成で測定した。
粘着剤の端部の水蒸気透過試験用の粘着シートを、外形寸法60mm×60mmで幅が2mmの額縁状に裁断し、軽剥離シートを剥がし、70mm×70mm×2mm厚のガラス板に貼付した。次いで、重剥離シートを剥がし、前記粘着シートの額縁の内側に湿度インジケータシール(アセイ工業社製、製品名「RH-70」)を貼付後、もう一枚のガラス板に貼付し、額縁の内側の空間がガラス板2枚と粘着シートで封止されるようにした。作製した試験体を、60℃、相対湿度90%の雰囲気下に放置し、その後、額縁内の湿度を評価した。なお、用いた湿度インジケータは、相対湿度70%で白から青へと着色し、その精度は25℃で±5%RH(RH:相対湿度)である。評価基準は、以下に示すとおりである。
◎:湿度インジケータシールの色変化なし
○:湿度インジケータシールの色変化がわずかにあり
粘着シート作製後、ステンレス板に23℃、50%RH環境下にて接着させ、JIS Z 0237(2000年度改正版)の粘着力の測定法に準じて貼付して、24時間後、180°における引き剥がし粘着強度(N/25mm)を測定した。
可視光透過率測定装置(島津製作所社製、「UV-3101PC」)を用いて、測定波長550nmで、粘着シートの可視光透過率(%)を測定した。
ガスバリア層の材料として、下記A及びBのポリシラザン化合物を用いた
・ポリシラザン化合物A: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、商品名「アクアミカNL110-20」
・ポリシラザン化合物B:飽和炭化水素基を有するオルガノポリシラザン化合物の混合物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、商品名「tutoPromBright」)
基材として、ポリエチレンテレフタレートフィルム(三菱樹脂社製、「PET38 T-100」、厚さ38μm、以下、「PETフィルム」という。)に、ポリシラザン化合物Aをスピンコートにより塗布し、120℃で1分間加熱してPETフィルム上にペルヒドロポリシラザンを含む厚さ60nmの層のポリシラザン層を形成した。次に、プラズマイオン注入装置を用いてペルヒドロポリシラザンを含む層の表面に、アルゴン(Ar)をプラズマイオン注入して、「ガスバリア層1付きの基材」を作製した。
加熱時間を1分間から5分間に変更した以外は、製造例1と同様にして「ガスバリア層2付きの基材」を得た。
(製造例3)
PETフィルム上に形成するペルヒドロポリシラザンを含む層の厚さを60nmから100nmとした以外は、製造例2と同様にして「ガスバリア層3付きの基材」を得た。
(製造例4)
PETフィルム上に形成するペルヒドロポリシラザンを含む層の厚さを60nmから150nmとした以外は、製造例2と同様にして「ガスバリア層4付きの基材」を得た。
(製造例5)
加熟時間を1分間から20分間に変更した以外は、製造例1と同様にして「ガスバリア層5付きの基材」を得た。
(製造例6)
プラズマ生成ガスとしてアルゴンに変えて窒素(N2)を用いた以外は、製造例2と同様にして「ガスバリア層6付きの基材」を得た。
(製造例7)
イオン注入を行う際の印加電圧を-10kVに変えて-5kVとした以外は、製造例2と同様にして「ガスバリア層7付きの基材」を得た。
(製造例8)
イオン注入を行う際の印加電圧を-10kVに変えて-15kVとした以外は、製造例2と同様にして「ガスバリア層8付きの基材」を得た。
(製造例9)
ポリシラザン化合物Aの変わりに、ポリシラザン化合物Bを用いた以外は、製造例2と同様にして「ガスバリア層9付きの基材」を得た。
(製造例10)
プラズマ生成ガスとしてアルゴンに変えて水素(H2)を用いた以外は、製造例2と同様にして「ガスバリア層10付きの基材」を得た。
(製造例11)
プラズマ生成ガスとしてアルゴンに変えて酸素(O2)を用いた以外は、製造例2と同様にして「ガスバリア層11付きの基材」を得た。
(製造例12)
プラズマ生成ガスとしてアルゴンに変えてヘリウム(He)を用いた以外は、製造例2と同様にして「ガスバリア層12付きの基材」を得た。
(製造例13)
プラズマ生成ガスとしてアルゴンに変えてネオン(Ne)を用いた以外は、製造例2と同様にして「ガスバリア層13付きの基材」を得た。
(製造例14)
プラズマ生成ガスとしてアルゴンに変えてキセノン(Xe)を用いた以外は、製造例2と同様にして「ガスバリア層14付きの基材」を得た。
(製造例15)
プラズマ生成ガスとしてアルゴンに変えてクリプトン(Kr)を用いた以外は、製造例2と同様にして「ガスバリア層15付きの基材」を得た。
イオン注入を行わない以外は、製造例2と同様にしてガスバリア層16付きの基材を作製した。
(製造例17)
PETフィルムに、スパッタリング法により、厚さ60nmの窒化ケイ素(SiN)の膜を設け、「ガスバリア層17付きの基材」を得た。
(製造例A)
ポリイソブチレン樹脂として「オパノールB50(BASF製、Mw:340,000)」100質量部、ポリブテン樹脂として「日石ポリブテン グレードHV-1900(新日本石油社製、Mw:1900)」30質量部、環状オレフィン系重合体として「Eastotac H-100L Resin(イーストマンケミカル.Co.製、Mw:1000)50質量部をトルエンに溶解し、固形分濃度約18質量%の「粘着剤組成物A」を得た。
(製造例B)
製造例Aにおいて、ポリイソブチレン系樹脂を「オパノールB30SF(BASF製、Mw:200,000)」に変えた以外は製造例Aと同様にして、「粘着剤組成物B」を得た。
(製造例C)
製造例Aにおいて、ポリイソブチレン系樹脂を「オパノールB80SF(BASF製、Mw:750,000)」に変えて、ポリブテン樹脂を加えないこと以外は製造例Aと同様にして、「粘着剤組成物C」を得た。
(製造例D)
ポリイソブチレン樹脂として、「オパノールB50(BASF製、Mw:340,000)」100質量部、「オパノールB30SF(BASF製、Mw:200,000)」30質量部、水素化石油樹脂として「アルコンP-100(荒川化学工業社製)」30質量部をトルエンに溶解し、固形分濃度約18質量%の「粘着剤組成物D」を得た。
(製造例E)
製造例Dにおいて、「オパノールB30SF」を30質量部から10質量部に変えた以外は製造例Eと同様にして、「粘着剤組成物E」を得た。
(製造例F)
製造例Aにおいて、更にヒンダードアミン系光安定剤として「TINUVIN765(チバ・ジャパン製)」0.5質量部、ヒンダードフェノール系酸化防止剤として「IRGANOX1010(チバ・ジャパン製)」0.5質量部、を加えた以外は製造例Aと同様にして、「粘着剤組成物F」を得た。
(製造例G)
ゴム系粘着剤としてTN-560(MORESCO社製)をトルエンに溶解し、固形分濃度約20質量%の「粘着剤組成物G」を得た。
(製造例H)
アクリル系溶剤型粘着剤としてPK(商品名、リンテック社製)を「粘着剤組成物H」として用いた。
(実施例1~22、比較例1~3)
上記のようにして得られた粘着剤組成物と、製造例1~17で得られたガスバリア層付きの基材を用いて、実施例1~22、及び比較例1~3の粘着シートを以下のように作製した。
粘着剤組成物及びガスバリア層付きの基材の組み合わせは、表1に示すとおりである。
上記粘着剤組成物A~Hを、軽剥離シート(リンテック社製、商品名「SP-PET1031」)の剥離処理面に、ロールナイフコーターを用いて乾燥後の膜厚が20μmになるように塗布し、100℃で約1分間乾燥し、粘着剤層を形成した。次いで、上記ガスバリア層1~17付きの基材のガスバリア層面を粘着剤面にラミネートして貼り合わせて、粘着シートを得た。
粘着剤の端部の水蒸気透過試験用として、実施例及び比較例に対応する粘着剤組成物を、重剥離シート(リンテック社製、製品名「SP-PET3811」)の剥離処理面に、ロールナイフコーターを用いて乾燥後の膜厚が50μmになるように塗布し、100℃で約1分間乾燥後、厚さ50μmの粘着剤層を形成した。次いで、得られた粘着剤層と、実施例1~22、比較例1~3の粘着シートの基材面とをラミネートして貼り合わせて、粘着剤の端部の水蒸気透過試験用の粘着シート(重剥離シート/粘着剤層50μm/PETフィルム/粘着剤層20μm/軽剥離シート)を得た。
このようにして作製した実施例1~22及び比較例1~3の粘着シートについて、上述の各種物性値の測定結果や試験結果を表1に示す。
また、折り曲げ試験後におけて、実施例の粘着シートは、ガスバリア層のクラックの発生が見られなかったが、無機膜(窒化ケイ素膜)を形成した比較例3は、クラックの発生が見られた。また、実施例の粘着シートは、比較例3と比べても、水蒸気透過率の上昇が少なく、耐折れ曲げ性に優れており、さらに透明性にも優れていた。
2、2a、2b 基材
3、3a、3b ガスバリア層
4、4a、4b、4c 粘着剤層
10 有機EL素子
12 ガラス基板
14 構造体
Claims (8)
- 基材上に、少なくともガスバリア層と粘着剤層とを有する粘着シートであって、
前記ガスバリア層が、少なくとも、酸素原子及びケイ素原子を含む材料から構成されてなり、
前記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量全体に対する、酸素原子の存在割合が60~75%、窒素原子の存在割合が0~10%、ケイ素原子の存在割合が25~35%であり、かつ、
前記ガスバリア層の表層部における膜密度が、2.4~4.0g/cm3である、粘着シート。 - 前記ガスバリア層を構成する材料が、ポリシラザン化合物よりなる、請求項1に記載の粘着シート。
- 前記ポリシラザン化合物が、ペルヒドロポリシラザンである、請求項2に記載の粘着シート。
- 前記ガスバリア層が、イオンが注入されてなる、請求項1~3のいずれか1項に記載の粘着シート。
- 前記イオンが、水素、窒素、酸素、アルゴン、ヘリウム、ネオン、キセノン、及びクリプトンからなる群から選ばれる少なくとも一種のガスがイオン化されたものである、請求項4に記載の粘着シート。
- 前記粘着剤層の厚み50μmにおける水蒸気透過率が、40℃、相対湿度90%の雰囲気下で、25g/m2/day以下である、請求項1~5のいずれか1項に記載の粘着シート。
- 前記粘着剤層を形成する粘着剤が、ゴム系粘着剤又はアクリル系粘着剤である、請求項1~6のいずれか1項に記載の粘着シート。
- 請求項1~7のいずれか1項に記載の粘着シートを電子デバイス用部材として備えた、電子デバイス。
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Also Published As
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TWI504718B (zh) | 2015-10-21 |
US20130209800A1 (en) | 2013-08-15 |
KR101886455B1 (ko) | 2018-08-07 |
CN103154172A (zh) | 2013-06-12 |
EP2615144B1 (en) | 2018-10-17 |
TW201217485A (en) | 2012-05-01 |
EP2615144A4 (en) | 2014-10-29 |
EP2615144A1 (en) | 2013-07-17 |
CN103154172B (zh) | 2014-12-10 |
JP5422055B2 (ja) | 2014-02-19 |
KR20140018174A (ko) | 2014-02-12 |
JPWO2012032907A1 (ja) | 2014-01-20 |
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