WO2014084352A1 - 接着剤組成物、接着シート、電子デバイス及びその製造方法 - Google Patents
接着剤組成物、接着シート、電子デバイス及びその製造方法 Download PDFInfo
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- WO2014084352A1 WO2014084352A1 PCT/JP2013/082173 JP2013082173W WO2014084352A1 WO 2014084352 A1 WO2014084352 A1 WO 2014084352A1 JP 2013082173 W JP2013082173 W JP 2013082173W WO 2014084352 A1 WO2014084352 A1 WO 2014084352A1
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- adhesive
- adhesive layer
- gas barrier
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- electronic device
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- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 description 1
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- YACLQRRMGMJLJV-UHFFFAOYSA-N chloroprene Chemical compound ClC(=C)C=C YACLQRRMGMJLJV-UHFFFAOYSA-N 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000011086 glassine Substances 0.000 description 1
- 235000010985 glycerol esters of wood rosin Nutrition 0.000 description 1
- 229920005555 halobutyl Polymers 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052945 inorganic sulfide Inorganic materials 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002587 poly(1,3-butadiene) polymer Polymers 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- MSFGZHUJTJBYFA-UHFFFAOYSA-M sodium dichloroisocyanurate Chemical compound [Na+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O MSFGZHUJTJBYFA-UHFFFAOYSA-M 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229920006132 styrene block copolymer Polymers 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- SYRHIZPPCHMRIT-UHFFFAOYSA-N tin(4+) Chemical compound [Sn+4] SYRHIZPPCHMRIT-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/16—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
- B32B37/18—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only
- B32B37/182—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only one or more of the layers being plastic
-
- 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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
-
- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/383—Natural or synthetic rubber
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
-
- 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
- H10K50/842—Containers
- H10K50/8426—Peripheral sealing arrangements, e.g. adhesives, sealants
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/871—Self-supporting sealing arrangements
- H10K59/8722—Peripheral sealing arrangements, e.g. adhesives, sealants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/412—Transparent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/206—Organic displays, e.g. OLED
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/414—Additional features of adhesives in the form of films or foils characterized by the presence of essential components presence of a copolymer
-
- 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
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
-
- 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
- C09J2409/00—Presence of diene 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
- C09J2423/00—Presence of polyolefin
-
- 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
- C09J2467/00—Presence of polyester
- C09J2467/005—Presence of polyester in the release coating
-
- 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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
- H01L21/565—Moulds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
- H01L23/3107—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed
- H01L23/3121—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed a substrate forming part of the encapsulation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/564—Details not otherwise provided for, e.g. protection against moisture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
Definitions
- the present invention relates to an adhesive composition useful as a material for forming an adhesive layer having excellent moisture barrier properties and adhesive strength, an adhesive sheet having an adhesive layer formed using the adhesive composition, and a gas barrier.
- An adhesive sheet having an adhesive layer formed on the gas barrier film, a film, an electronic device including a sealing material formed using the adhesive composition, and a photoelectric conversion element by an adhesive layer of the adhesive sheet The present invention relates to a sealed electronic device and a method for manufacturing the electronic device.
- organic EL elements have attracted attention as light-emitting elements that can emit light with high luminance by low-voltage direct current drive.
- the organic EL element has a problem that light emission characteristics such as light emission luminance, light emission efficiency, and light emission uniformity are likely to deteriorate with time.
- Patent Document 1 discloses an organic EL element in which an organic EL layer sandwiched between a thin transparent electrode and a back electrode on a glass substrate is covered with a photocurable resin layer (sealing material) having moisture resistance. It is disclosed.
- Patent Document 2 discloses a method of sealing an organic EL element using a sealing film formed of a moisture-proof polymer film and an adhesive layer.
- acrylic adhesives and pressure-sensitive adhesives have been proposed from the viewpoint of optical properties such as transparency.
- Patent Document 3 discloses an acrylic adhesive having an ultraviolet curing function and a room temperature curing function as a sealant for an organic EL display.
- Patent Document 4 discloses an acrylic adhesive as an adhesive that can form an adhesive layer that can propagate light from an organic EL display element to the display surface with excellent propagation efficiency even after receiving a thermal history. System adhesives are disclosed.
- a sealing material formed using an acrylic adhesive or the like does not have sufficient moisture barrier properties, sealing that requires extremely high moisture barrier properties, such as a sealing material for organic EL elements.
- the material was not satisfactory in terms of performance.
- the sealing material formed using an acrylic adhesive or the like has a crosslinked structure, the sealing material is easily peeled off from the adherend due to impact, vibration, heat generation, etc. There was a risk that the blocking performance would be greatly reduced.
- Patent Document 5 discloses an adhesive composition containing a specific hydrogenated cyclic olefin polymer and a polyisobutylene resin, which is used as an encapsulant for an organic EL element.
- JP-A-5-182759 Japanese Patent Laid-Open No. 5-101884 JP 2004-87153 A Japanese Patent Application Laid-Open No. 2004-224991 JP 2009-524705 A (WO2007 / 08871 pamphlet)
- the sealing material obtained using the adhesive composition containing the polyisobutylene resin described in Patent Document 5 has better moisture barrier properties than the sealing material using an acrylic adhesive, As a sealing material for EL elements, it did not have sufficient moisture barrier properties. In particular, when an extremely high moisture barrier property is required, such as an organic EL device, it is important to prevent moisture from entering from the interface and side surfaces of the sealing material. The encapsulant obtained by use was not satisfactory. Further, this document does not particularly mention the characteristics of the film laminated on the sealing material.
- an adhesive composition useful as a material for forming an adhesive layer having excellent moisture barrier properties and excellent adhesive strength (Ii) an adhesive sheet (A) having an adhesive layer formed using the adhesive composition; (Iii) an adhesive sheet (B) having a gas barrier film excellent in gas barrier properties and transparency, and an adhesive layer formed on the gas barrier film and excellent in moisture barrier properties, transparency, and adhesive strength; (Iv) an electronic device comprising a sealing material formed using the adhesive composition, and (V)
- An object is to provide an electronic device in which an element such as an organic EL element is sealed by the adhesive layer of the adhesive sheet (B), and a method for manufacturing the electronic device.
- an adhesive composition containing an isobutylene / isoprene copolymer as a main component is formed on a transparent substrate because it has excellent moisture barrier properties and adhesive strength.
- a gas barrier film having a specific gas barrier property and transparency, and an adhesive containing an isobutylene / isoprene copolymer as a main component on the gas barrier film has been found that an adhesive sheet having an adhesive layer formed from a composition is excellent in moisture barrier properties, transparency, and adhesive strength, and thus is suitable as a sealing material for a photoelectric conversion element formed on a transparent substrate.
- the present invention has been completed.
- the following adhesive compositions (1) to (3), the following adhesive sheets (4) to (11), the following electronic devices (12) to (14), and the electronic devices (15) An invention of a device manufacturing method is provided.
- An adhesive composition for sealing an electronic device An adhesive composition comprising, as a main component, an isobutylene / isoprene copolymer whose content of repeating units derived from isoprene is 0.1 to 99 mol% based on all repeating units.
- An adhesive composition according to (1) wherein 5 to 100 parts by mass of a tackifier is contained with respect to 100 parts by mass of the isobutylene / isoprene copolymer.
- the tackifier is an aliphatic petroleum resin.
- An adhesive sheet having a release sheet and an adhesive layer formed on the release sheet, wherein the adhesive layer is the adhesive composition according to any one of (1) to (3) An adhesive sheet formed using a material.
- (5) comprising a gas barrier film and an adhesive layer formed on the gas barrier film;
- the gas barrier film has a water vapor transmission rate of 0.1 g / m 2 / day or less and a total light transmittance of 80% or more in an environment of a temperature of 40 ° C. and a relative humidity of 90%, and the adhesive.
- the layer is made of an adhesive composition containing an isobutylene / isoprene copolymer as a main component.
- the product of the water vapor transmission rate X (g / m 2 / day) in the environment of a temperature of 40 ° C. and a relative humidity of 90% of the adhesive layer and the thickness Y ( ⁇ m) of the adhesive layer is The adhesive sheet according to (4) or (5), wherein the adhesive sheet is less than 300.
- An electronic device comprising a transparent substrate, an element formed on the transparent substrate, and a sealing material for sealing the element, wherein the sealing material comprises (1) to (3 An electronic device comprising the adhesive composition according to any one of the above. (13) An electronic device comprising a transparent substrate, an element formed on the transparent substrate, and a sealing material for sealing the element, wherein the sealing material includes (4) to (11 An electronic device characterized by being formed using the adhesive sheet according to any one of the above.
- An electronic device including a transparent substrate, an element formed on the transparent substrate, and an adhesive sheet laminated so as to cover the element, the adhesive sheet including a gas barrier film and the gas barrier film
- the adhesive layer is made of a composition containing an isobutylene / isoprene copolymer as a main component, and the gas barrier film has a temperature of 40 ° C. and a relative humidity of 90%.
- the water vapor transmittance is 0.1 g / m 2 / day or less and the total light transmittance is 80% or more, and the element is sealed by the adhesive layer.
- a method for manufacturing an electronic device comprising a transparent substrate, an element formed on the transparent substrate, and an adhesive sheet laminated so as to cover the element, and covers the element formed on the transparent substrate
- a method for producing an electronic device comprising the step of laminating the adhesive sheet according to any one of (4) to (11).
- an adhesive composition useful in forming an adhesive layer excellent in moisture barrier properties and adhesive strength, an adhesive sheet having an adhesive layer formed using this adhesive composition, and An electronic device including a sealing material formed using the adhesive composition and a method for manufacturing the electronic device are provided.
- Adhesive composition (A) is an adhesive composition for sealing an electronic device, and isoprene. It is characterized in that it contains an isobutylene / isoprene copolymer whose main component is a content of repeating units derived from 0.1 to 99 mol% with respect to all repeating units.
- “having isobutylene / isoprene copolymer as the main component” means that the blending ratio of isobutylene / isoprene copolymer is 50% by mass or more in the adhesive composition as a solid content. .
- the adhesive composition (A) has an isoprene-derived repeating unit as a polymerization component, and the content of the repeating unit derived from isoprene is in the above range as a main component.
- An adhesive composition having both barrier properties and tackiness is obtained.
- the adhesive composition (A) is suitably used as a sealing material for electronic devices that can prevent oxygen, moisture, etc. from entering the electronic devices and deteriorating the electrodes and organic layers. It is what
- isobutylene / isoprene copolymer those similar to the isobutylene / isoprene copolymer used as a component of the above-mentioned adhesive composition (A) can be used.
- Synthetic rubber having a repeating unit [—CH 2 —CH (CH 3 ) 2 —] derived from isobutylene and a repeating unit [—CH 2 —C (CH 3 ) ⁇ CH—CH 2 —] derived from isoprene in the molecule It is.
- the content of repeating units derived from isoprene in the isobutylene / isoprene copolymer is usually from 0.1 to 99 mol%, preferably from 0.5 to 50 mol%, more preferably from all repeating units. 1 to 10 mol%.
- the isobutylene / isoprene copolymer can be obtained, for example, by cationically copolymerizing isobutylene and a small amount of isoprene at a low temperature using aluminum chloride as a catalyst.
- the isobutylene / isoprene copolymer may be copolymerized with other rubber components as long as the effects of the present invention are not impaired.
- the type of the isobutylene / isoprene copolymer is not particularly limited, and examples thereof include a regenerated isobutylene / isoprene copolymer and a synthetic isobutylene / isoprene copolymer. Among these, a synthetic isobutylene / isoprene copolymer is preferable.
- the isobutylene / isoprene copolymer can be used singly or in combination of two or more.
- the number average molecular weight of the isobutylene / isoprene copolymer to be used is usually 100,000 to 5,000,000, preferably 150,000 to 2,000,000, and more preferably 200,000 to 1,000,000.
- the number average molecular weight of the isobutylene / isoprene copolymer can be obtained as a standard polystyrene equivalent value by performing gel permeation chromatography.
- the Mooney viscosity of the isobutylene / isoprene copolymer to be used is preferably 30 to 60 (ML1 + 4, 100 ° C.), 35 to 55 (ML1 + 4, 100 ° C.). Since the Mooney viscosity of the isobutylene / isoprene copolymer used in the present invention is in such a range, the adhesive composition (A) can be efficiently prepared because it is easily dissolved in a general organic solvent.
- the blending ratio of the isobutylene / isoprene copolymer is preferably 50 to 90% by mass, more preferably 60 to 80% by mass in the adhesive composition as a solid content.
- an adhesive composition (A) useful for forming an adhesive layer having excellent moisture barrier properties and excellent adhesive strength is obtained. Can do.
- the adhesive composition (A) may be blended with other rubber-based polymer components as long as the effects of the present invention are not hindered.
- Other rubber-based polymer components include natural rubber (NR), isobutylene homopolymer (polyisobutylene, IM), a copolymer of isobutylene and n-butene, a butadiene homopolymer (butadiene rubber, BR), Chloroprene homopolymer (chloroprene rubber, CR), isoprene homopolymer (isoprene rubber, IR), isobutylene-butadiene copolymer, isobutylene-isoprene copolymer (butyl rubber, IIR), halogenated butyl rubber, styrene And 1,3-butadiene copolymer (styrene butadiene rubber, SBR), acrylonitrile and 1,3-butadiene copolymer (nitrile rubber),
- the adhesive composition (A) preferably contains a tackifier in addition to the isobutylene / isoprene copolymer.
- a tackifier By containing a tackifier, an adhesive composition (A) useful for forming an adhesive layer that is excellent in moisture barrier properties and excellent in adhesive strength can be obtained.
- the tackifier is not particularly limited as long as it improves the tackiness of the adhesive layer, and a known one can be used.
- aliphatic petroleum resins, terpene resins, rosin ester resins, rosin resins and the like are preferable.
- a hydrogenated resin is preferable because an adhesive layer that hardly changes color even under high-temperature and humid heat can be formed.
- the hydrogenated resin may be a partially hydrogenated product or a fully hydrogenated product.
- the weight average molecular weight of the tackifier is preferably 100 to 10,000, more preferably 500 to 5,000.
- the softening point of the tackifier is preferably 50 to 160 ° C, more preferably 60 to 140 ° C, still more preferably 70 to 130 ° C.
- a commercially available product can be used as it is as a tackifier.
- commercially available products include aliphatic petroleum resins such as Escorez 1000 series (Exxon Chemical Co., Ltd.), Quinton A, B, R, CX series (Nihon Zeon Co., Ltd.); Alcon P, M series (Arakawa Chemical Co., Ltd.) ), ESCOREZ series (manufactured by Exxon Chemical), EASTOTAC series (manufactured by Eastman Chemical), IVARV series (manufactured by Idemitsu Kosan), etc .; ), Clearon P series (manufactured by Yasuhara Chemical), picolite A, C series (manufactured by Hercules), etc .; Foal series (manufactured by Hercules), Pencel A series, ester gum, super ester, pine crystal Ester resins such as Arakawa Chemical Industries, etc .;
- the blending ratio is usually 5 to 100 parts by weight, preferably 10 to 70 parts by weight, with respect to 100 parts by weight of the isobutylene / isoprene copolymer.
- the amount of the tackifier is 5 parts by mass or more with respect to 100 parts by mass of the isobutylene / isoprene copolymer, whereby an adhesive layer that is superior in tackiness can be efficiently formed, and 70 parts by mass or less. Therefore, it is possible to avoid a decrease in cohesive force of the adhesive layer.
- the adhesive composition (A) other components can be blended within a range not impeding the effects of the present invention.
- other components include additives such as silane coupling agents, antistatic agents, light stabilizers, antioxidants, ultraviolet absorbers, resin stabilizers, fillers, pigments, extenders, and softeners. These can be used singly or in combination of two or more.
- the blending amount in the adhesive composition is preferably 0.01 to 5% by mass, and more preferably 0.01 to 2% by mass.
- the adhesive composition (A) can be prepared by appropriately mixing and stirring the above isobutylene / isoprene copolymer, and, if necessary, a tackifier, other components and a solvent according to a conventional method. it can.
- Solvents include aromatic hydrocarbon solvents such as benzene and toluene; ester solvents such as ethyl acetate and butyl acetate; ketone solvents such as acetone, methyl ethyl ketone, and methyl isobutyl ketone; n-pentane, n-hexane, n- And aliphatic hydrocarbon solvents such as heptane; alicyclic hydrocarbon solvents such as cyclopentane and cyclohexane; and the like. These solvents can be used alone or in combination of two or more.
- the solid content concentration of the adhesive composition (A) is preferably 10 to 60% by mass, more preferably 10 to 45% by mass, and further preferably 15 to 30% by mass.
- the adhesive composition (A) it is possible to form an adhesive layer having excellent water vapor barrier properties and tackiness.
- the adhesive layer formed using the adhesive composition (A) and having a thickness of 60 ⁇ m preferably has a water vapor permeability of 10 g / m 2 / day or less in an environment of a temperature of 40 ° C. and a relative humidity of 90%, More preferably, it is 8 g / m ⁇ 2 > / day or less, More preferably, it is 5 g / m ⁇ 2 > / day or less.
- the water vapor transmission rate of the adhesive layer can be measured by the method described in the examples.
- the moisture vapor transmission rate of the adhesive layer formed using the adhesive composition and having a thickness of 60 ⁇ m is in such a range, and as a sealing material for electronic devices, the entry of water vapor is more effectively suppressed. it can.
- the value of the water-vapor-permeation rate of an adhesive bond layer is dependent on the thickness of an adhesive bond layer, when the thickness of an adhesive bond layer is not 60 micrometers, it can calculate
- the storage elastic modulus at 20 to 60 ° C. of the adhesive layer formed using the adhesive composition of the present invention is preferably 10 5 to 10 6 Pa.
- the storage elastic modulus can be sufficiently adhered to an element or the like formed on the transparent substrate, and water vapor can be more effectively prevented from entering.
- a storage elastic modulus can be measured and calculated
- an adhesive layer having an excellent adhesive force can be formed.
- the adhesive layer formed using the adhesive composition (A) has a water vapor transmission rate X (g / m 2 / day) in an environment of a temperature of 40 ° C. and a relative humidity of 90%, and the adhesive layer
- the product of the thickness Y ( ⁇ m) is preferably less than 300, more preferably 10 to 300, and still more preferably 100 to 200.
- the product of the water vapor transmission rate X and the thickness Y of the adhesive layer By setting the product of the water vapor transmission rate X and the thickness Y of the adhesive layer to a specific range, for example, an element formed on the transparent substrate is sealed using an adhesive composition, and is described later in FIG.
- the intrusion of water vapor from the side surface of the adhesive layer can be effectively suppressed. If the product of the water vapor transmission rate X and the thickness Y of the adhesive layer exceeds 300, water vapor may enter from the thickness direction (side surface) of the adhesive layer and the photoelectric conversion element may be deteriorated. If the product of the water vapor transmission rate X and the thickness Y of the adhesive layer is too small, sufficient tackiness cannot be obtained, and the water vapor barrier property may be lowered.
- the adhesive strength of the adhesive layer formed using the adhesive composition (A) to the glass substrate is preferably 1 N / 25 mm or more, more preferably 2 N / 25 mm or more, still more preferably 3 N / 25 mm or more, and particularly preferably Is 5 N / 25 mm or more, most preferably 10 N / 25 mm or more.
- the adhesive strength of the adhesive layer can be measured by the method described in the examples.
- the adhesive composition (A) is also useful as a sealing material for elements formed on a transparent substrate and a raw material for producing the adhesive sheet of the present invention described later.
- Adhesive sheet The adhesive sheet of the present invention is used as a sealing material for electronic devices, and has a release sheet and an adhesive layer formed on the release sheet [adhesive sheet (A)]. Or a gas barrier film and an adhesive layer formed on the gas barrier film [adhesive sheet (B)].
- the adhesive layer of the adhesive sheet of the present invention is formed using the adhesive composition of the present invention.
- the adhesive sheet (A) of the present invention is not particularly limited to the layer configuration as long as it has at least a release sheet and an adhesive layer formed on the release sheet.
- a layer structure unit comprising an adhesive layer sandwiched between the release sheets so as to be in contact with the release surfaces of two release sheets, or a layer structural unit composed of the release sheet and an adhesive layer formed on the release sheet is provided. The thing etc. which have the layer structure laminated
- the adhesive sheet 10A shown in FIG. 1 has two release sheets 2a (first release sheet), 2b (second release sheet), and the release sheet so as to be in contact with the release surfaces of the two release sheets. And an adhesive layer 1a sandwiched between the two.
- the adhesive layer 1a is formed using the adhesive composition (A) of the present invention. Since the adhesive layer of the adhesive sheet (A) is formed using the adhesive composition (A), it has a sufficient cohesive force, is excellent in moisture barrier properties, and is excellent in adhesive strength.
- the release sheet constituting the adhesive sheet 10A is not particularly limited, and for example, a release sheet having a release layer that has been subjected to a release treatment with a release agent can be used.
- the adhesive sheet of the present invention has two or more release sheets, the two or more release sheets may be made of the same material or different materials.
- paper base materials such as glassine paper, coated paper, high-quality paper; laminated paper obtained by laminating a thermoplastic resin such as polyethylene on these paper base materials; polyethylene terephthalate resin, polybutylene terephthalate resin, Examples thereof include plastic films such as polyethylene naphthalate resin, polypropylene resin, and polyethylene resin.
- the release agent include rubber elastomers such as silicone resins, olefin resins, isoprene resins, and butadiene resins, long chain alkyl resins, alkyd resins, and fluorine resins.
- the release sheet may be a double-sided release sheet in which release layers are formed on both sides of the substrate, or a single-sided release sheet in which a release layer is formed on one side of the substrate.
- the thickness of the release sheet is not particularly limited, but is usually 20 to 200 ⁇ m, preferably 25 to 150 ⁇ m.
- the method for forming the adhesive layer is not particularly limited.
- the adhesive composition is formed by applying the adhesive composition (A) on the release-treated surface of the release sheet or the sealing substrate by a known method, and drying the obtained coating film. A method is mentioned.
- Examples of the method for applying the adhesive composition (A) include spin coating, spray coating, bar coating, knife coating, roll coating, blade coating, die coating, and gravure coating. It is done.
- the drying conditions for drying the coating film include, for example, 80 to 150 ° C. for 30 seconds to 5 minutes.
- the thickness of the adhesive layer is not particularly limited and can be appropriately determined according to the use.
- the thickness of the adhesive layer is preferably 0.5 to 200 ⁇ m, more preferably 1 to 100 ⁇ m, and still more preferably 5 to 80 ⁇ m.
- the thickness of the adhesive layer is 0.5 ⁇ m or more, more excellent tackiness is easily exhibited, and when the thickness of the adhesive layer is 100 ⁇ m or less, the adhesive layer can be formed with high productivity.
- the second release sheet is superimposed on the adhesive sheet so as to be opposed to the release layer of the second release sheet via the adhesive layer. A Can be obtained.
- the adhesive layer of the adhesive sheet (A) obtained as described above is excellent in moisture barrier properties and excellent in adhesive strength. Therefore, when this adhesive layer is used as a sealing material, it is possible to sufficiently prevent moisture from entering, and even when it generates heat or vibrates when driving a device, it is separated at the adhesive interface. Since it is difficult, it is possible to prevent intrusion of moisture and the like over a long period of time. Therefore, the adhesive sheet (A) can be preferably used for forming a sealing material for an electronic device described later.
- the adhesive sheet (A) is an element sealing material that can prevent oxygen or moisture from entering the element such as an organic EL formed on the transparent substrate and deteriorating the electrode and the organic layer. It is used.
- the adhesive sheet (B) of the present invention is used as a sealing material for an electronic device, and includes a gas barrier film and an adhesive layer formed on the gas barrier film.
- the gas barrier film used for the adhesive sheet (B) has a water vapor transmission rate of 0.1 g / m in an environment of a temperature of 40 ° C. and a relative humidity of 90% (hereinafter abbreviated as “90% RH”). 2 / day or less, preferably, 0.05 g / m 2 / day or less, and more preferably not more than 0.005 g / m 2 / day.
- the gas barrier film used has a water vapor transmission rate of 0.1 g / m 2 / day or less in an environment of 40 ° C. and 90% RH, so that oxygen or oxygen is contained inside the element such as an organic EL element formed on the transparent substrate. It is possible to effectively suppress the penetration of moisture and the like and the deterioration of the electrode and the organic layer.
- the transmittance of the gas barrier film such as water vapor can be measured using a known gas permeability measuring device.
- the gas barrier film used for the adhesive sheet (B) has a total light transmittance of 80% or more, preferably 85% or more. Since the total light transmittance of the gas barrier film to be used is 80% or more, incident light to the element and light emission from the element are less likely to be impaired. Therefore, the adhesive sheet of the present invention is required to be transparent. It can be used as a sealing material for an element formed on a substrate. The total light transmittance can be determined by measurement by the method described in the examples.
- the gas barrier film to be used is not particularly limited as long as it has a water vapor transmission rate of 0.1 g / m 2 / day or less and a total light transmittance of 80% or more in a temperature of 40 ° C. and 90% RH environment.
- a known film such as a laminated film in which a gas barrier layer is formed directly or via another layer on a base film can be used.
- the base film used includes polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cyclohexane Resin films such as olefin polymers, aromatic polymers, and polyurethane polymers can be used.
- the thickness of the base film is not particularly limited, but is preferably 0.5 to 500 ⁇ m, more preferably 1 to 200 ⁇ m, and further preferably 5 to 100 ⁇ m from the viewpoint of ease of handling.
- a material etc. will not be specifically limited if a gas barrier layer can provide desired gas barrier property.
- a gas barrier layer can provide desired gas barrier property.
- examples thereof include an inorganic film and a gas barrier layer obtained by implanting ions into a layer containing a polymer compound.
- the gas barrier layer is preferably a gas barrier layer made of an inorganic film and a gas barrier layer obtained by implanting ions into a layer containing a polymer compound because a layer having a small thickness and excellent gas barrier properties can be efficiently formed. .
- the inorganic film is not particularly limited, and examples thereof include an inorganic vapor deposition film.
- the inorganic vapor deposition film include vapor deposition films of inorganic compounds and metals.
- the raw material for the vapor-deposited film of the inorganic compound inorganic oxides such as silicon oxide, aluminum oxide, magnesium oxide, zinc oxide, indium oxide and tin oxide; inorganic nitrides such as silicon nitride, aluminum nitride and titanium nitride; inorganic carbides; Inorganic sulfides; inorganic oxynitrides such as silicon oxynitride; inorganic oxide carbides; inorganic nitride carbides; inorganic oxynitride carbides and the like.
- the raw material for the metal vapor deposition film include aluminum, magnesium, zinc, and tin.
- the polymer compound used is a silicon-containing polymer such as polyorganosiloxane or polysilazane compound.
- a silicon-containing polymer such as polyorganosiloxane or polysilazane compound.
- These polymer compounds can be used alone or in combination of two or more.
- silicon-containing polymer compounds are preferable, and polysilazane compounds are more preferable.
- the polysilazane compound a commercially available product as a glass coating material or the like can be used as it is.
- Polysilazane compounds can be used alone or in combination of two or more.
- the polymer layer may contain other components in addition to the above-described polymer compound as long as the object of the present invention is not impaired. Examples of other components include curing agents, other polymers, anti-aging agents, light stabilizers, and flame retardants.
- a method for forming a polymer layer for example, a known device such as a spin coater, a knife coater, a gravure coater, or the like is used to form a layer forming solution containing at least one kind of a polymer compound, and optionally other components and a solvent.
- a spin coater such as a spin coater, a knife coater, a gravure coater, or the like is used to form a layer forming solution containing at least one kind of a polymer compound, and optionally other components and a solvent.
- coating and forming the coating film obtained by drying moderately is mentioned.
- ions implanted into the polymer layer ions of rare gases such as argon, helium, neon, krypton, and xenon; ions such as fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, and sulfur; Ions of alkane gases such as methane and ethane; Ions of alkene gases such as ethylene and propylene; Ions of alkadiene gases such as pentadiene and butadiene; Ions of alkyne gases such as acetylene; Benzene, toluene, etc.
- rare gases such as argon, helium, neon, krypton, and xenon
- ions such as fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, and sulfur ions of alkane gases such as methane and ethane
- Ions of alkene gases such as ethylene and propylene
- Ions of alkadiene gases such
- Ions of aromatic hydrocarbon gases such as: ions of cycloalkane gases such as cyclopropane; ions of cycloalkene gases such as cyclopentene; ions of metals; ions of organosilicon compounds; These ions can be used alone or in combination of two or more.
- ions of rare gases such as argon, helium, neon, krypton, and xenon are preferable because ions can be more easily implanted and a gas barrier layer having particularly excellent gas barrier properties can be obtained.
- the method for implanting ions is not particularly limited.
- a method of irradiating ions accelerated by an electric field (ion beam), a method of injecting ions in plasma, and the like can be mentioned.
- a gas barrier film can be easily obtained, and the latter method of injecting plasma ions. Is preferred.
- the gas barrier film may further have other layers such as a protective layer, a conductor layer, and a primer layer.
- a protective layer such as a styrene, a styrene, a styrene, a styrene, a styrene, a styrene, a styrene, a styrene, a styrene, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium oxide, titanium
- the thickness of the gas barrier film is not particularly limited, but is usually in the range of 10 to 2000 nm, preferably 20 to 1000 nm, more preferably 30 to 500 nm, and still more preferably 40 to 200 nm from the viewpoints of gas barrier properties and handling properties.
- the gas barrier layer may be a single layer or a plurality of layers.
- Adhesive layer The adhesive sheet (B) may be referred to as an adhesive composition (hereinafter, referred to as “adhesive composition (B)”) having an isobutylene / isoprene copolymer as a main component on the gas barrier film. .) With an adhesive layer formed from.
- “having isobutylene / isoprene copolymer as the main component” means that the blending ratio of isobutylene / isoprene copolymer is 50% by mass or more in the adhesive composition as a solid content. .
- the isobutylene / isoprene copolymer in such a blending ratio, it is possible to obtain an adhesive composition useful for forming an adhesive layer that is excellent in all of moisture barrier properties, transparency, and adhesive strength. . That is, when this adhesive layer is used as a sealing material for an element formed on a transparent substrate, it is possible to sufficiently prevent moisture from entering, and further from incident light to the photoelectric conversion element and from the photoelectric conversion element. The light emission is less likely to be impaired, and it is difficult for the light emission to be separated at the adhesion interface, so that intrusion of moisture and the like can be prevented over a long period of time.
- Examples of the isobutylene / isoprene copolymer used here include the same as the isobutylene / isoprene copolymer used as the main component of the adhesive composition (A).
- the blending ratio of the isobutylene / isoprene copolymer is preferably 50 to 90% by mass, more preferably 60 to 80% by mass in the adhesive composition as a solid content.
- an adhesive composition (B) useful for forming an adhesive layer having excellent moisture barrier properties and excellent adhesive strength is obtained. Can do.
- the adhesive composition of the present invention may be blended with other rubber-based polymer components as long as the effects of the present invention are not hindered.
- examples of other rubber-based polymer components include the same rubber-based polymer components used as components of the above-described adhesive composition (A).
- the adhesive composition (B) preferably contains a tackifier in addition to the isobutylene / isoprene copolymer.
- a tackifier By containing a tackifier, an adhesive composition useful for forming an adhesive layer that is superior in moisture barrier properties, transparency, and adhesive strength can be obtained.
- the blending ratio is usually 5 to 100 parts by mass, preferably 10 to 70 parts by mass with respect to 100 parts by mass of the isobutylene / isoprene copolymer. is there.
- the amount of the tackifier is 5 parts by mass or more with respect to 100 parts by mass of the isobutylene / isoprene copolymer, whereby an adhesive layer that is superior in tackiness can be efficiently formed, and 70 parts by mass or less. Therefore, it is possible to avoid a decrease in cohesive force of the adhesive layer.
- other components can be mix
- the other components include the same components as the other components that can be contained in the above-described adhesive composition (A).
- the blending amount is preferably 0.01 to 5% by mass, more preferably 0.01 to 2% by mass in the adhesive composition (B).
- the adhesive composition (B) can be prepared by appropriately mixing and stirring the isobutylene / isoprene copolymer and, if necessary, a tackifier, other components and a solvent according to a conventional method. .
- Solvents include aromatic hydrocarbon solvents such as benzene and toluene; ester solvents such as ethyl acetate and butyl acetate; ketone solvents such as acetone, methyl ethyl ketone, and methyl isobutyl ketone; n-pentane, n-hexane, n- And aliphatic hydrocarbon solvents such as heptane; alicyclic hydrocarbon solvents such as cyclopentane and cyclohexane; and the like. These solvents can be used alone or in combination of two or more.
- the solid content concentration of the obtained adhesive composition is preferably 10 to 60% by mass, more preferably 10 to 45% by mass, and further preferably 15 to 30% by mass.
- the thickness of the adhesive layer is preferably 0.5 to 200 ⁇ m, more preferably 1 to 100 ⁇ m, and still more preferably 5 to 80 ⁇ m. If the thickness of the adhesive layer is 0.5 ⁇ m or more, more excellent tackiness is easily exhibited, and if the thickness of the adhesive layer is 200 ⁇ m or less, the adhesive layer can be formed with high productivity.
- the adhesive sheet (B) of the present invention only needs to have at least a gas barrier film and an adhesive layer formed on the gas barrier film, and each has two or more gas barrier films and / or adhesive layers. There may be.
- an adhesive sheet 10B comprising a gas barrier film 3a and an adhesive layer 1b formed on the gas barrier film 3a, or FIG. 2A, an adhesive sheet 10C having a configuration in which two adhesive sheets shown in FIG. 2A are laminated, and an adhesive sheet 10D in which a release sheet 2c is laminated on the adhesive layer of the adhesive sheet in FIG. 2A.
- the adhesive sheet (B) of the present invention is not limited to that shown in FIG. For example, you may have the structure which laminated
- the adhesive layer of the adhesive sheet (B) has a good adhesive strength.
- the adhesive strength to the glass substrate is preferably 3 N / 25 mm or more, More preferably, it is 5 N / 25mm or more, More preferably, it is 10 N / 25mm or more.
- Adhesive strength of the adhesive layer with respect to the glass substrate is in such a range, whereby sufficient adhesion to a transparent substrate such as a glass plate can be obtained, and the photoelectric conversion element can be effectively sealed.
- the adhesive strength of the adhesive layer to the polyethylene terephthalate film is preferably 0.5 N / 25 mm or more, more preferably 1 N / 25 mm or more, and further preferably 5 N / 25 mm or more.
- the adhesive force of the adhesive layer to the polyethylene terephthalate film is within such a range, for example, sufficient adhesion between the gas barrier film and the adhesive layer is obtained, and water vapor enters from the interface between the gas barrier film and the adhesive layer. This can be suppressed more effectively.
- the adhesive layer formed using the adhesive composition (B) has a water vapor transmission rate of 10 g / m 2 / day or less in an environment of a temperature of 40 ° C. and a relative humidity of 90% when the thickness is 60 ⁇ m. It is preferable. More preferably, it is 8 g / m ⁇ 2 > / day or less, More preferably, it is 5 g / m ⁇ 2 > / day or less.
- the water vapor transmission rate can be measured by the method described in the examples. When the water vapor transmission rate of the adhesive layer is in such a range, the penetration of water vapor can be more effectively suppressed as a sealing material for the photoelectric conversion element formed on the transparent substrate.
- the value of the water-vapor-permeation rate of an adhesive bond layer is dependent on the thickness of an adhesive bond layer, when the thickness of an adhesive bond layer is not 60 micrometers, it can calculate
- the adhesive layer of the adhesive sheet (B) has a water vapor transmission rate X (g / m 2 / day) in an environment of a temperature of 40 ° C. and a relative humidity of 90%, and a thickness Y ( ⁇ m) of the adhesive layer. Is preferably less than 300, more preferably 10 to 300, and still more preferably 100 to 200. When the product of X and Y is less than 300, when the photoelectric conversion element formed on the transparent substrate is sealed with an adhesive composition, it is effective in intruding water vapor from the side surface of the adhesive layer. Can be suppressed.
- the product of the water vapor transmission rate X and the thickness Y of the adhesive layer exceeds 300, water vapor may enter from the thickness direction (side surface) of the adhesive layer and the photoelectric conversion element may be deteriorated. If the product of the water vapor transmission rate X and the thickness Y of the adhesive layer is too small, sufficient tackiness cannot be obtained, and the water vapor barrier property may be lowered.
- the adhesive sheet (B) can be manufactured by a known method.
- the adhesive sheet 10B shown in FIG. 2A can be manufactured as follows.
- the gas barrier film 3a is prepared, and the adhesive composition (B) is coated on the gas barrier film 3a by a known method, and the obtained coating film is dried to form the adhesive layer 1b.
- the target adhesive sheet 10B can be obtained.
- the release sheet 2c is laminated on the adhesive layer, thereby providing the release sheet shown in FIG.
- the adhesive sheet 10D can be obtained.
- Examples of the method for applying the adhesive composition (B) include spin coating, spray coating, bar coating, knife coating, roll coating, blade coating, die coating, and gravure coating. It is done.
- the drying conditions for drying the coating film include, for example, 80 to 150 ° C. for 30 seconds to 5 minutes. After the drying treatment, the adhesive layer may be cured by leaving it still for about one week.
- examples of the release sheet to be used include the same release sheets that can be used for manufacturing the above-described adhesive sheet 10A.
- the adhesive sheet (B) can also be obtained by the following method. First, a release sheet having one surface peel-treated with a release agent is prepared, and the adhesive composition is formed on the release-treated surface of the release sheet in the same manner as in Production Method 1 by the above-described known method. The adhesive layer with a release sheet is obtained by coating and drying the resulting coating to form an adhesive layer. Next, the obtained adhesive sheet with release sheet and the gas barrier film can be laminated to obtain an adhesive sheet 10D with release sheet as shown in FIG.
- the adhesive sheet (B) obtained as described above has a gas barrier film excellent in gas barrier properties and transparency, and an adhesive layer excellent in moisture barrier properties, transparency, and adhesive strength. Therefore, the adhesive sheet of the present invention is an element of the element formed on the transparent substrate that can prevent oxygen and moisture from entering the element formed on the transparent substrate and deteriorating the electrode and element. It can be suitably used as a sealing material.
- the adhesive sheet of the present invention is preferably used for sealing electronic devices described later. be able to. Since the adhesive layer is excellent in adhesive strength and moisture barrier property, the performance of the gas barrier film can be fully exhibited, and the element formed on the transparent substrate can be sealed.
- the adhesive sheet (B) of the present invention is an element seal that can prevent oxygen, moisture, etc. from entering inside an element such as an organic EL formed on a transparent substrate and deteriorating an electrode or an organic layer. It is used as a stop material.
- the electronic device of the present invention is an electronic device comprising a transparent substrate, an element formed on the transparent substrate, and a sealing material for sealing the element, and the sealing material Comprising the adhesive composition (A) of the present invention [electronic device (A)], or a transparent substrate, an element formed on the transparent substrate, and covering the element
- Electronic devices include organic devices such as organic transistors, organic memories, and organic EL devices; liquid crystal displays; electronic paper; thin film transistors; electrochromic devices; electrochemiluminescence devices; touch panels; solar cells; Device; and the like.
- elements elements that convert electric energy into light (light emitting diodes, semiconductor lasers, etc.), and photoelectric conversion elements that are elements that convert light into electric energy (photodiodes, solar cells, etc.); organic EL elements, etc. And the like.
- the type, size, shape, number, etc. of the elements formed on the transparent substrate are not particularly limited as long as they are sealed with the adhesive composition of the present invention.
- the transparent substrate on which the element is formed is not particularly limited, and various substrate materials can be used.
- a substrate material having a high visible light transmittance it is preferable to use a substrate material having a high visible light transmittance.
- a material that has a high blocking performance for blocking moisture and gas that tends to enter from the outside of the element and is excellent in solvent resistance and weather resistance is preferable.
- transparent inorganic materials such as quartz and glass; polyethylene terephthalate, polyethylene naphthalate, polycarbonate, polystyrene, polyethylene, polypropylene, polyphenylene sulfide, polyvinylidene fluoride, acetyl cellulose, brominated phenoxy, aramids, polyimides, And transparent plastics such as polystyrenes, polyarylates, polysulfones, and polyolefins.
- the thickness of the transparent substrate is not particularly limited, and can be appropriately selected in consideration of light transmittance and performance for blocking the inside and outside of the element.
- a transparent conductive layer may be provided on the transparent substrate.
- the sheet resistance of the transparent electrode layer is preferably 500 ⁇ / ⁇ or less, and more preferably 100 ⁇ / ⁇ or less.
- known materials can be used. Specifically, indium-tin composite oxide (ITO), fluorine-doped tin oxide (IV) SnO 2 (FTO), Examples thereof include tin (IV) SnO 2 , zinc (II) ZnO, and indium-zinc composite oxide (IZO). These materials can be used alone or in combination of two or more.
- An electronic device (A) of the present invention is an electronic device comprising a transparent substrate, an element formed on the transparent substrate, and a sealing material for sealing the element, wherein the sealing material is The adhesive composition (A) of the present invention is used.
- FIG. 1 a structural cross-sectional view of an organic EL element is shown in FIG.
- the organic EL element 20 ⁇ / b> A has a structure in which the structure 12 is formed on the glass substrate 11.
- the structure 12 is formed by laminating a transparent electrode, a hole transport layer, a light emitting layer, a back electrode, and the like (not shown).
- the adhesive layer 10 ⁇ / b> A and the sealing substrate 4 are laminated on the structure 12 and the glass substrate 11. Since the structure 12 of the organic EL element is covered with the adhesive layer 10A, intrusion of moisture and the like is suppressed.
- the adhesive layer 10A is excellent in adhesive strength, the interface between the adhesive layer 10A and the sealing substrate 4 and the interface between the adhesive layer 10A and the structure 12 are difficult to peel off, so that moisture or the like enters from the interface. Is suppressed.
- the electronic device (A) can be manufactured as follows, for example. First, an adhesive sheet [adhesive sheet (A) of the present invention] having a release sheet and an adhesive layer formed on the release sheet is prepared. The adhesive layer of the adhesive sheet (A) is formed from the adhesive composition (A) of the present invention. Next, by adhering the adhesive layer of the adhesive sheet (A) so as to cover the adherend (optical element such as an organic EL element), it is excellent in adhesion and moisture blocking properties with the adherend. An adhesive layer that functions as a material can be disposed on the adherend surface.
- the release sheet is removed, and the sealing substrate 4 is laminated on the exposed adhesive layer, so that the adhesion with the adherend and the moisture blocking property are excellent, and the adhesive can function as a sealing material.
- the agent layer can be disposed on the adherend surface.
- the sealing substrate 4 a known material such as a glass plate or a plastic film can be used.
- Plastic films include polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin Resin films and sheets such as polymers, aromatic polymers, and polyurethane polymers can be used.
- the thickness of the sealing substrate 4 is not particularly limited, but is preferably 0.5 to 500 ⁇ m, more preferably 1 to 200 ⁇ m, and further preferably 5 to 100 ⁇ m from the viewpoint of ease of handling.
- the gas barrier layer may be formed in the said plastic film directly or through another layer.
- the thickness of the gas barrier layer is not particularly limited, but is usually in the range of 10 to 2000 nm, preferably 20 to 1000 nm, more preferably 30 to 500 nm, and still more preferably 40 to 200 nm from the viewpoints of gas barrier properties and handling properties.
- the gas barrier layer may be a single layer or a plurality of layers, but the gas barrier layer is preferably a plurality of layers from the viewpoint of obtaining higher gas barrier properties. A material etc. will not be specifically limited if a gas barrier layer can provide desired gas barrier property.
- the sealing substrate 4 may be laminated with a protective layer, a conductor layer, a primer layer, and the like. The position where these layers are laminated is not particularly limited.
- Water vapor permeability of the sealing substrate 4 the temperature 40 ° C., under a relative humidity of 90% environment, preferably 0.5g / (m 2 ⁇ day) or less, more preferably 0.05g / (m 2 ⁇ day) It is as follows.
- the electronic device (B) of the present invention is an electronic device comprising a transparent substrate, an element formed on the transparent substrate, and an adhesive sheet laminated so as to cover the element.
- the device has a water vapor transmission rate of 0.1 g / m 2 / day or less in an environment of 90 ° C. and a relative humidity of 90%, and a total light transmittance of 80% or more. Is sealed.
- the structure of an organic EL element which is a kind of photoelectric conversion element is shown in FIG.
- a structure 12 is formed on a glass substrate (transparent substrate) 11.
- the adhesive sheet 10B comprised from the adhesive bond layer 1 and the gas barrier film 3 is laminated
- the organic EL element 20B shown in FIG. 4 can be manufactured as follows, for example. First, the organic EL element 20B shown in FIG. 4 can be obtained by bonding the adhesive layer 1 of the adhesive sheet 10B of the present invention on the structure 12 and the glass substrate 11. In the organic EL element 20B, the structure 12 is covered with the adhesive layer 1 by the adhesive sheet (B) of the present invention, so that intrusion of moisture and the like is suppressed.
- the adhesive layer 1 formed from the gas barrier film 3 excellent in moisture barrier properties and transparency, and the adhesive layer 1 formed from an adhesive composition mainly composed of an isobutylene / isoprene copolymer excellent in moisture barrier properties and adhesive strength.
- the adhesive sheet 10B of the present invention Since the adhesive sheet 10B of the present invention is used, it is difficult for the interface between the adhesive layer 1 and the gas barrier film 3 to be peeled off, and oxygen, moisture and the like enter the element, and deterioration of the electrode and the organic layer is suppressed.
- Isobutylene / isoprene copolymer (1) (Nippon Butyl Co., Exxon Butyl 268, number average molecular weight 260,000, isoprene content 1.7 mol%)
- Isobutylene / isoprene copolymer (2) (Nippon Butyl Co., Exxon Butyl 288, number average molecular weight 260,000, isoprene content 2.3 mol%)
- Polyisobutylene resin (2) (manufactured by BASF, Opanol B50, number average molecular weight: 340,000, isoprene content 0 mol%)
- the number average molecular weight of the isobutylene / isoprene copolymer was determined as a standard polystyrene equivalent value by performing gel permeation chromatography under the following conditions.
- Developing solvent Tetrahydrofuran Flow rate: 1.0 mL / min
- Tackifier (1) Aliphatic petroleum resin (manufactured by Nippon Zeon Co., Ltd., Quinton A100, softening point 100 ° C.)
- Tackifier (2) Aliphatic petroleum resin (manufactured by Nippon Zeon, Quinton B170, softening point 70 ° C.)
- Tackifier (3) Aliphatic petroleum resin (manufactured by Nippon Zeon Co., Ltd., Quinton R100, softening point 96 ° C.)
- the softening points of the tackifiers (1) to (3) were measured according to JIS K2531.
- Release sheet (1) Polyethylene terephthalate film subjected to silicone release treatment (SP-PET381130, thickness 38 ⁇ m, manufactured by Lintec Corporation)
- Release sheet (2) Silicone release-treated polyethylene terephthalate film (Lintec Corp., SP-PET38T103-1, thickness 38 ⁇ m)
- Example 1 (Preparation of adhesive composition) 100 parts of isobutylene / isoprene copolymer (1) was dissolved in toluene to prepare an adhesive composition having a solid content of 20%.
- the adhesive composition was applied onto the release-treated surface of the release sheet (2) so that the thickness after drying was 60 ⁇ m, and the resulting coating film was dried at 120 ° C. for 2 minutes to form an adhesive layer. Formed. Next, the release sheet (1) was bonded to the adhesive layer on the release treatment surface to obtain an adhesive sheet.
- Examples 2 to 18, Comparative Examples 1 to 5 An adhesive composition was obtained in the same manner as in Example 1 except that each component and the blending amount thereof were changed to those shown in Table 1, and an adhesive sheet was produced using the adhesive composition.
- an ethyl acetate solution of trimethylolpropane-modified tolylene diisocyanate manufactured by Nippon Polyurethane Co., Ltd., Coronate L, solid content: 75% by mass
- an adhesive composition containing a 20% solid content acrylic copolymer as a main component was obtained by adding toluene and then adding toluene.
- An adhesive sheet was produced in the same manner as in Example 1 except that this adhesive composition was used. Table 1 summarizes the composition of the adhesive layer of the adhesive sheets obtained in Examples and Comparative Examples.
- ITO indium tin oxide
- N, N′-bis (naphthalen-1-yl) -N, N′-bis (phenyl) -benzidene) (manufactured by Luminescence Technology) was 60 nm
- (8-hydroxy-quinolinolate) lithium was sequentially deposited at a rate of 10 nm and 0.1 to 0.2 nm / s to form a light emitting layer.
- aluminum (Al) manufactured by Kojundo Chemical Laboratory Co., Ltd. was deposited at a rate of 0.1 nm / s to 100 nm to form a cathode. Note that the degree of vacuum during the deposition is 1 ⁇ 10 ⁇ 4 Pa or less.
- the release sheet (1) of the adhesive sheet obtained in Example 1 was peeled off, and the polyethylene terephthalate sheet sheet (12 ⁇ m) was formed on both sides of the exposed adhesive layer and an aluminum foil (7 ⁇ m) as a sealing substrate. And a laminated film (made by Aya Aluminum Co., Ltd.) bonded with a urethane adhesive layer to obtain a sealing substrate with an adhesive layer.
- the sealing substrate with the adhesive layer was dried by heating at 120 ° C. for 10 minutes using a hot plate in a nitrogen atmosphere, and then left to cool to room temperature.
- an organic EL device was produced in the same manner as in Example 1 using the adhesive sheets obtained in Examples 2 to 18 and Comparative Examples 1 to 5.
- Table 2 shows the measurement results and the evaluation results.
- the obtained sample was cut into a size of 25 mm ⁇ 300 mm, the release sheet (2) was peeled off, and the exposed adhesive layer was attached to the following adherend in an environment of 23 ° C. and 50% RH.
- a test piece was obtained by reciprocating a roller with a weight of 2 kg from above and pressing it. The test piece was left in an environment of 23 ° C. and 50% RH for 24 hours after pressure bonding, and then peeled at a peeling rate of 300 mm / min using a tensile tester (Orientec, Tensilon) in the same environment. A peel test was performed at an angle of 180 °, and the adhesive strength (N / 25 mm) was measured.
- the adherend used for the measurement of the adhesive strength is as follows.
- PET film manufactured by Toyobo Co., Ltd., Cosmo Shine A4100, thickness 50 ⁇ m ⁇ Glass plate (soda lime glass): manufactured by Nippon Sheet Glass
- the release sheet (1) of the adhesive sheet is peeled off, affixed to a laminated film (made by Aya Aluminum Co., Ltd.) in which a polyethylene terephthalate sheet sheet (12 ⁇ m) is bonded to both sides of an aluminum foil (7 ⁇ m) with a urethane adhesive layer, and a moisture penetration test A sample for was obtained.
- a non-alkali glass substrate Cornning Corp., 45 mm ⁇ 45 mm
- a calcium layer having a thickness of 32 mm and a width of 40 mm and a film thickness of 100 nm was formed by vacuum deposition.
- the release sheet (2) is peeled from the sample for moisture penetration test, and the exposed adhesive layer and the calcium layer on the glass substrate are bonded using a laminator under a nitrogen atmosphere, and the calcium layer A test piece for moisture penetration test was obtained.
- the obtained test piece was allowed to stand for 170 hours in an environment of 60 ° C. and 90% RH, and the rate of discoloration of the calcium layer (the rate of moisture ingress) was visually confirmed, and the moisture barrier property was evaluated according to the following criteria. .
- Table 2 shows the following.
- the adhesive layers formed using the adhesive compositions of Examples 1 to 18 have a low water vapor transmission rate, excellent moisture barrier properties, and excellent adhesive strength.
- the organic EL elements sealed with the sealing materials formed using the adhesive compositions of Examples 1 to 18 showed high performance in the moisture penetration test and had high durability.
- the adhesive layer formed using the adhesive composition containing as a main component a polyisobutylene-based resin not containing isoprene in Comparative Examples 1 to 4 has insufficient water penetration test performance, The durability of the device is not high.
- the adhesive layer formed using the adhesive composition containing the acrylic copolymer of Comparative Example 5 as a main component has a high water vapor transmission rate, low performance in a water penetration test, and durability of the organic EL device.
- the sex is inferior.
- gas barrier film (A) As a base material, a polyethylene terephthalate film (Toyobo Co., Ltd., Cosmo Shine A4100, thickness 50 ⁇ m, hereinafter referred to as “PET film”), a polysilazane compound (a coating material containing perhydropolysilazane as a main component (manufactured by Clariant Japan, Aquamica NL110-20) was applied by spin coating and heated at 120 ° C.
- PET film polyethylene terephthalate film
- a polysilazane compound a coating material containing perhydropolysilazane as a main component (manufactured by Clariant Japan, Aquamica NL110-20) was applied by spin coating and heated at 120 ° C.
- a gas barrier film (A) was produced by plasma-implanting argon (Ar) under the following conditions to form a gas barrier layer.
- the plasma ion implantation apparatus and ion implantation conditions used for forming the gas barrier layer are as follows.
- RF power source JEOL Ltd., model number “RF” 56000
- High voltage pulse power supply “PV-3-HSHV-0835” manufactured by Kurita Manufacturing Co., Ltd.
- Plasma generation gas Ar Gas flow rate: 100sccm Duty ratio: 0.5% Applied voltage: -15 kV RF power supply: frequency 13.56 MHz, applied power 1000 W Chamber internal pressure: 0.2 Pa
- Pulse width 5 ⁇ sec Processing time (ion implantation time): 200 seconds
- gas barrier film (B) As a base material, a polyethylene terephthalate film (Toyobo Co., Ltd., Cosmo Shine A4100, thickness 50 ⁇ m, hereinafter referred to as “PET film”), a polysilazane compound (a coating material containing perhydropolysilazane as a main component (manufactured by Clariant Japan, Aquamica NL110-20) was applied by spin coating and heated at 120 ° C.
- PET film polyethylene terephthalate film
- a polysilazane compound a coating material containing perhydropolysilazane as a main component (manufactured by Clariant Japan, Aquamica NL110-20) was applied by spin coating and heated at 120 ° C.
- a gas barrier film (B) was produced by plasma-implanting argon (Ar) under the following conditions to form a gas barrier layer.
- the plasma ion implantation apparatus and ion implantation conditions used for forming the gas barrier layer are as follows.
- RF power source JEOL Ltd., model number “RF” 56000
- High voltage pulse power supply “PV-3-HSHV-0835” manufactured by Kurita Manufacturing Co., Ltd.
- Plasma generation gas Ar Gas flow rate: 100sccm Duty ratio: 0.5%
- Applied voltage -6kV
- RF power supply frequency 13.56 MHz
- Chamber internal pressure 0.2 Pa
- Pulse width 5 ⁇ sec Processing time (ion implantation time): 200 seconds
- a gas barrier layer made of silicon oxide having a thickness of 100 nm is formed by sputtering on a polyethylene terephthalate film (Mitsubishi Plastics, PET38 T-100, thickness 38 ⁇ m, hereinafter referred to as “PET film”) as a base material, A gas barrier film (C) was produced.
- PET film polyethylene terephthalate film
- gas barrier film (D) As a base material, a gas barrier layer made of silicon nitride having a thickness of 100 nm is formed by sputtering on a polyethylene terephthalate film (Mitsubishi Resin, PET38 T-100, thickness 38 ⁇ m, hereinafter referred to as “PET film”), A gas barrier film (D) was produced.
- PET film polyethylene terephthalate film
- Example 19 (Preparation of adhesive composition) 100 parts of isobutylene / isoprene copolymer (1) was dissolved in toluene to prepare an adhesive composition 1 having a solid content of 20%.
- the adhesive composition 1 was applied on the gas barrier layer of the gas barrier film (A) so that the thickness after drying was 20 ⁇ m, and the obtained coating film was dried at 110 ° C. for 1 minute to form an adhesive layer. Formed.
- a release sheet a polyethylene terephthalate film subjected to silicone release treatment (SP-PET381130, thickness 38 ⁇ m, manufactured by Lintec Corporation) was bonded to the adhesive layer on the release treatment surface to obtain an adhesive sheet.
- Adhesive compositions 2 to 24 were obtained in the same manner as in Example 19 except that the adhesive composition was changed to that shown in Table 3. Next, the obtained adhesive composition and gas barrier film were changed to those shown in Table 4 to prepare an adhesive sheet.
- an ethyl acetate solution of trimethylolpropane-modified tolylene diisocyanate manufactured by Nippon Polyurethane Co., Ltd., Coronate L, solid content: 75% by mass
- an adhesive composition containing a 20% solid content acrylic copolymer as a main component was obtained by adding toluene and then adding toluene.
- An adhesive sheet was produced in the same manner as in Example 19 except that this adhesive composition was used.
- Table 3 shows the composition of the adhesive layer of the adhesive sheets obtained in Examples and Comparative Examples.
- Tris (8-hydroxy-quinolinate) aluminum manufactured by Luminescence Technology 40 nm
- N, N′-bis (naphthalen-1-yl) -N, N′-bis (phenyl) -benzidene) Luminescence
- Luminescence Technology manufactured by Technology
- an indium tin oxide (ITO) film was formed by a sputtering method to form an anode. Note that the degree of vacuum during the deposition is 1 ⁇ 10 ⁇ 4 Pa or less.
- the adhesive sheets obtained in Examples and Comparative Examples were dried by heating at 120 ° C. for 30 minutes using a hot plate in a nitrogen atmosphere, and then left to cool to room temperature. Next, the release sheet of the adhesive sheet was peeled off, and the exposed adhesive layer was opposed to the cathode, and was laminated so as to completely cover the cathode to obtain an organic EL element.
- the water vapor transmission rate of the gas barrier films (A) to (C) in an environment of 40 ° C. and 90% RH was measured using a water vapor transmission rate measuring device (manufactured by MOCON, AQUATRON).
- the adhesive compositions used in the examples and comparative examples were dried on the release treatment surface of a release sheet (polyethylene terephthalate film subjected to silicone release treatment, Lintec Corporation, SP-PET38T103-1, thickness 38 ⁇ m). Coating was performed to 60 ⁇ m, and the obtained coating film was dried at 120 ° C. for 2 minutes to form an adhesive layer.
- a polyethylene terephthalate film (manufactured by Mitsubishi Plastics, thickness 6 ⁇ m) was bonded to the adhesive layer.
- the release sheet is peeled off, and another polyethylene terephthalate film (Mitsubishi Resin, thickness 6 ⁇ m) is bonded to the exposed adhesive layer, and the adhesive layer sandwiched between the two polyethylene terephthalate films.
- a sample for measuring water vapor transmission rate was obtained. Using the water vapor transmission rate measuring device (L80-5000, manufactured by LYSSY) for the obtained sample, the water vapor transmission rate was measured at an adhesive layer temperature of 40 ° C. and a relative humidity of 90%. The water vapor transmission rate of the agent layer was used.
- the adherend used for the measurement of the adhesive strength is as follows.
- PET film manufactured by Toyobo Co., Ltd., Cosmo Shine A4100, thickness 50 ⁇ m ⁇ Glass plate (soda lime glass): manufactured by Nippon Sheet Glass
- the organic EL device was allowed to stand for 200 hours in an environment of 23 ° C. and 50% RH, and then the organic EL device was activated, and the presence or absence of dark spots (non-light emitting portions) was observed and evaluated according to the following criteria.
- D Dark spot is 90% or more of light emitting area
- Total light transmittance measurement Using a total light transmittance turbidity clock (manufactured by Nippon Denshoku Industries Co., Ltd., HAZE METER NDH5000), according to JIS K7631-1, the gas barrier films used in Examples and Comparative Examples and the adhesive sheets of Examples and Comparative Examples The total light transmittance was measured. The total light transmittance of the adhesive sheet was measured with the release sheet peeled off.
- Table 4 shows the following.
- the adhesive sheets of Examples 19 to 38 show high performance in the moisture penetration test, and the organic EL device provided with the adhesive sheet has high durability. In addition, despite the sealing with the gas barrier film, a decrease in the luminance of the emitted light was less than before the sealing, and a good organic EL device without any change in the color of the emitted color could be obtained.
- the adhesive sheet formed using the acrylic adhesive of Comparative Example 8 has a high water vapor permeability of the adhesive layer, poor moisture barrier properties, and poor durability of the organic EL element.
- the adhesive sheet of Comparative Example 6 has a low water vapor transmission rate of the adhesive layer, but since the gas barrier film has a high water vapor transmission rate, the performance of the adhesive layer cannot be fully utilized, and the durability of the organic EL device is not improved. The nature is not high.
- the gas barrier film has a low water vapor transmission rate, but the adhesive layer has a high water vapor transmission rate, so that the performance of the gas barrier film cannot be fully utilized, and the durability of the organic EL element is high. Absent.
- the pressure-sensitive adhesive sheet of Comparative Example 9 has a low water vapor transmission rate of the gas barrier film, but has a low total light transmittance of the gas barrier film, obstructs light emission from the organic EL, and the emission luminance is significantly higher than before sealing. is decreasing.
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Abstract
Description
しかし、有機EL素子には、時間の経過とともに発光輝度、発光効率、発光均一性等の発光特性が低下し易いという問題があった。
例えば、特許文献1には、ガラス基板上に薄膜状の透明電極及び背面電極によって挟持された有機物EL層を、耐湿性を有する光硬化性樹脂層(封止材)で被覆した有機EL素子が開示されている。また、特許文献2には、防湿性高分子フィルムと接着層により形成された封止フィルムを用いて、有機EL素子を封止する方法が開示されている。
例えば、特許文献3には、有機ELディスプレイ用の封止剤として、紫外線硬化機能と室温硬化機能を有するアクリル系接着剤が開示されている。
特許文献4には、熱履歴を受けた後であっても、有機EL表示素子による光を、優れた伝播効率でディスプレイ表面に伝播することができる粘着剤層を形成し得る粘着剤として、アクリル系粘着剤が開示されている。
さらに、アクリル系接着剤等を用いて形成された封止材が架橋構造を有するものである場合には、衝撃、振動、発熱等により、封止材が被着体から剥離し易くなり、水分遮断性が大きく低下するおそれがあった。
例えば、特許文献5には、有機EL素子の封入剤として用いられる、特定の水素添加環状オレフィン系ポリマーとポリイソブチレン樹脂を含有する接着性組成物が開示されている。
(i)水分遮断性に優れ、かつ、粘着力に優れる接着剤層の形成材料として有用な接着剤組成物、
(ii)前記接着剤組成物を用いて形成された接着剤層を有する接着シート(A)、
(iii)ガスバリア性と透明性に優れるガスバリアフィルムと、このガスバリアフィルム上に形成された、水分遮断性、透明性、および粘着力に優れる接着剤層を有する接着シート(B)、
(iv)前記接着剤組成物を用いて形成された封止材を備える電子デバイス、並びに、
(v)前記接着シート(B)の接着剤層により、有機EL素子等の素子が封止されている電子デバイス及びその製造方法、を提供することを目的とする。
イソプレン由来の繰り返し単位の含有率が、全繰り返し単位に対して0.1~99モル%であるイソブチレン・イソプレン共重合体を主成分として含有することを特徴とする、接着剤組成物。
(2)前記イソブチレン・イソプレン共重合体100質量部に対して、粘着付与剤を5~100質量部含有することを特徴とする(1)に記載の接着剤組成物。
(3)前記粘着付与剤が、脂肪族系石油樹脂であることを特徴とする(2)に記載の接着剤組成物。
(5)ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、
前記ガスバリアフィルムは、温度40℃、相対湿度90%の環境下における水蒸気透過率が0.1g/m2/day以下で、かつ、全光線透過率が80%以上のものであり、前記接着剤層は、イソブチレン・イソプレン共重合体を主成分として含む接着剤組成物からなることを特徴とする接着シート。
(6)前記イソブチレン・イソプレン共重合体は、イソプレン由来の繰り返し単位の含有率が、全繰り返し単位に対して0.1~99モル%であることを特徴とする(5)に記載の接着シート。
(7)前記接着剤層が厚み60μmの場合、温度40℃、相対湿度90%環境下における水蒸気透過率が、10g/m2/day以下であることを特徴とする(4)または(5)に記載の接着シート。
(8)前記接着剤層は、イソブチレン・イソプレン共重合体100部に対して、粘着付与剤を5~100質量部含有することを特徴とする(4)または(5)に記載の接着シート。
(9)前記接着剤層の、20~60℃の貯蔵弾性率が105~106Paであることを特徴とする(4)または(5)に記載の接着シート。
(10)前記接着剤層の、ガラス基板に対する粘着力が、3N/25mm以上であることを特徴とする(4)または(5)に記載の接着シート。
(11)前記接着剤層の、温度40℃、相対湿度90%の環境下における水蒸気透過率X(g/m2/day)と、前記前記接着剤層の厚みY(μm)の積が、300未満であることを特徴とする(4)または(5)に記載の接着シート。
(13)透明基板と、該透明基板上に形成された素子と、該素子を封止するための封止材とを備える電子デバイスであって、前記封止材が、(4)~(11)のいずれか1項に記載の接着シートを用いて形成されたものであること特徴とする電子デバイス。
(14)透明基板と、該透明基板上に形成された素子と、該素子を覆うように積層された接着シートを備える電子デバイスであって、該接着シートは、ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、該接着剤層が、イソブチレン・イソプレン共重合体を主成分として含む組成物からなるものであり、前記ガスバリアフィルムは、温度40℃、相対湿度90%環境下における水蒸気透過率が0.1g/m2/day以下であり、かつ、全光線透過率が80%以上であるものであって、前記接着剤層によって、前記素子が封止されていることを特徴とする電子デバイス。
本発明の接着剤組成物(以下、「接着剤組成物(A)」ということがある。)は、電子デバイスを封止するための接着剤組成物であって、イソプレン由来の繰り返し単位の含有率が、全繰り返し単位に対して0.1~99モル%である、イソブチレン・イソプレン共重合体を主成分として含有することを特徴とする。
ここで、「イソブチレン・イソプレン共重合体を主成分とする」とは、イソブチレン・イソプレン共重合体の配合割合が、固形分として、接着剤組成物中、50質量%以上であることを意味する。
分子内に、イソブチレン由来の繰り返し単位〔-CH2-CH(CH3)2-〕と、イソプレン由来の繰り返し単位〔-CH2-C(CH3)=CH-CH2-〕を有する合成ゴムである。イソブチレン・イソプレン共重合体中のイソプレン由来の繰り返し単位の含有率は、通常、全繰り返し単位に対して、0.1~99モル%であり、好ましくは0.5~50モル%、さらに好ましくは、1~10モル%である。
イソブチレン・イソプレン共重合体は、例えば、イソブチレンと少量のイソプレンを、塩化アルミニウムを触媒として、低温でカチオン共重合させて得ることが出来る。
イソブチレン・イソプレン共重合体は、本発明の効果を妨げない範囲で、その他のゴム成分が共重合されていてもよい。
イソブチレン・イソプレン共重合体は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
数平均分子量がこのような範囲にあるイソブチレン・イソプレン共重合体を用いることで、接着剤組成物(A)の流動性が低くなり過ぎず、十分な粘着性が得られ、かつ一般的な有機溶剤に溶解し易いため、接着剤組成物(A)を効率よく調製することができる。
なお、イソブチレン・イソプレン共重合体の数平均分子量は、ゲルパーミエーションクロマトグラフィーを行い、標準ポリスチレン換算値として求めることができる。
本発明に用いるイソブチレン・イソプレン共重合体のムーニー粘度がこのような範囲であることで、一般的な有機溶剤に溶解し易いため、接着剤組成物(A)を効率よく調製することができる。
イソブチレン・イソプレン共重合体をこのような配合割合で含有させることで、水分遮断性に優れ、かつ、粘着力に優れる接着剤層を形成する際に有用な接着剤組成物(A)を得ることができる。
その他のゴム系のポリマー成分としては、天然ゴム(NR)、イソブチレンの単独重合体(ポリイソブチレン、IM)、イソブチレンとn-ブテンの共重合体、ブタジエンの単独重合体(ブタジエンゴム、BR)、クロロプレンの単独重合体(クロロプレンゴム、CR)、イソプレンの単独重合体(イソプレンゴム、IR)、イソブチレンとブタジエンの共重合体、イソブチレンとイソプレンの共重合体(ブチルゴム、IIR)、ハロゲン化ブチルゴム、スチレンと1,3-ブタジエンの共重合体(スチレンブタジエンゴム、SBR)、アクリロニトリルと1,3-ブタジエンの共重合体(ニトリルゴム)、スチレン-1,3-ブタジエン-スチレンブロック共重合体(SBS)、スチレン-イソプレン-スチレンブロック共重合体(SIS)、エチレン-プロピレン-非共役ジエン三元共重合体等が挙げられる。
粘着付与剤を含有させることで、水分遮断性により優れ、かつ、粘着力により優れる接着剤層を形成する際に有用な接着剤組成物(A)を得ることができる。
これらの中でも、高温湿熱下であっても変色しにくい接着剤層を形成し得ることから、水素添加された樹脂が好ましい。水素添加された樹脂は、部分水添物であっても、完全水添物であっても良い。
粘着付与剤の軟化点は、好ましくは、50~160℃、より好ましくは60~140℃、さらに好ましくは70~130℃である。
粘着付与剤の配合量が、イソブチレン・イソプレン共重合体100質量部に対して、5質量部以上であることで、粘着性により優れる接着剤層を効率よく形成することができ、70質量部以下であることで、接着剤層の凝集力の低下を避けることができる。
その他の成分としては、シランカップリング剤、帯電防止剤、光安定剤、酸化防止剤、紫外線吸収剤、樹脂安定剤、充填剤、顔料、増量剤、軟化剤等の添加剤が挙げられる。
これらは、1種単独で、あるいは2種以上を組み合わせて用いることができる。
その他の成分を配合する場合、それぞれの配合量は、接着剤組成物中、好ましくは0.01~5質量%、より好ましくは0.01~2質量%である。
これらの溶媒は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
接着剤組成物(A)を用いて形成される、厚みが60μmの接着剤層の、温度40℃、相対湿度90%の環境下における水蒸気透過率は、好ましくは10g/m2/day以下、より好ましくは8g/m2/day以下、さらに好ましくは、5g/m2/day以下である。
接着剤層の水蒸気透過率は、実施例に記載された方法で測定することができる。
接着剤組成物を用いて形成される、厚みが60μmの接着剤層の水蒸気透過率がこのような範囲にあることで、電子デバイス用の封止材として、水蒸気の侵入をより効果的に抑制できる。
なお、接着剤層の水蒸気透過率の値は、接着剤層の厚みに依存するため、接着剤層の厚みが60μmでない場合には、厚みから換算して求めることができる。例えば、厚みがAμmで、水蒸気透過率がB(g/m2/day)の接着剤層の場合、厚みが60μmの時の水蒸気透過率は、A×B/60という式に当てはめて換算して求めることができる。
貯蔵弾性率がこのような範囲にあることで、透明基板上に形成された素子等に十分に密着し、水蒸気の侵入をより効果的に抑制できる。
貯蔵弾性率は、公知の動的粘弾性測定装置を使用して測定し求めることができる。
前記水蒸気透過率Xと接着剤層の厚みYの積が300を超えると、接着剤層の厚み方向(側面)から水蒸気の侵入し、光電変換素子が劣化する可能性がある。前記水蒸気透過率Xと接着剤層の厚みYの積が小さすぎると、十分な粘着性が得られず、水蒸気遮断性が低下するおそれがある。
接着剤組成物(A)を用いて形成される接着剤層の、ガラス基板に対する粘着力は、好ましくは1N/25mm以上、より好ましくは2N/25mm以上、さらに好ましくは3N/25mm以上、特に好ましくは5N/25mm以上、最も好ましくは10N/25mm以上である。
粘着力がこのような範囲にあることで、透明基板に十分に密着し、水蒸気の侵入をより効果的に抑制できる。
接着剤層の粘着力は、実施例に記載された方法で測定することができる。
接着剤組成物(A)は、透明基板上に形成された素子の封止材や、後述する本発明接着シートの製造原料としても有用である。
本発明の接着シートは、電子デバイスの封止材として用いられるものであって、剥離シートと、該剥離シート上に形成された接着剤層を有するもの〔接着シート(A)〕、又は、ガスバリアフィルムと、該ガスバリアフィルム上に形成された接着剤層を備えるもの〔接着シート(B)〕である。
本発明の接着シートの接着剤層は、本発明の接着剤組成物を用いて形成されたものである。
本発明の接着シート(A)は、少なくとも、剥離シートと、該剥離シート上に形成された接着剤層を有するものであれば、その層構成に特に制限されない。例えば、2枚の剥離シートの剥離面と接するように、前記剥離シートに挟持された接着剤層を備えるものや、剥離シートと該剥離シート上に形成された接着剤層からなる層構造単位が複数積層された層構成を有するものなどが挙げられる。
接着シート(A)の接着剤層は、接着剤組成物(A)を用いて形成されたものであるため、十分な凝集力を有し、水分遮断性により優れ、かつ、粘着力により優れる。
剥離剤としては、シリコーン系樹脂、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、フッ素系樹脂等が挙げられる。
剥離シートの厚みは、特に制限されないが、通常20~200μm、好ましくは25~150μmである。
塗膜を乾燥するときの乾燥条件としては、例えば80~150℃で30秒~5分間が挙げられる。
を得ることができる。
したがって、接着シート(A)は、後述する電子デバイスの封止材の形成に好ましく用いることができる。
接着シート(A)は、透明基板上に形成された有機EL等の素子内部に酸素や水分等が浸入し、電極や有機層を劣化させることを防止することができる、素子の封止材として用いられるものである。
本発明の接着シート(B)は、電子デバイスの封止材として用いられるものであって、ガスバリアフィルムと、該ガスバリアフィルム上に形成された接着剤層を備えるものである。
接着シート(B)に用いるガスバリアフィルムは、温度40℃、相対湿度90%(以下、「90%RH」と略記する。)の環境下における水蒸気透過率が0.1g/m2/day以下、好ましくは、0.05g/m2/day以下、より好ましくは、0.005g/m2/day以下である。
用いるガスバリアフィルムの温度40℃、90%RHの環境下における水蒸気透過率が0.1g/m2/day以下であることで、透明基板上に形成された有機EL素子等の素子内部に酸素や水分等が浸入し、電極や有機層が劣化することを効果的に抑制することができる。
ガスバリアフィルムの水蒸気等の透過率は、公知のガス透過率測定装置を使用して測定することができる。
用いるガスバリアフィルムの全光線透過率が80%以上であることで、素子への入射光や素子からの発光が損なわれることが少ないため、本発明の接着シートを、透明性が要求される、透明基板上に形成された素子の封止材として用いることができる。
全光線透過率は、実施例に記載した方法により測定して求めることが出来る。
基材フィルムの厚みは、特に制限はないが、取り扱い易さの観点から、好ましくは0.5~500μm、より好ましくは1~200μm、さらに好ましくは5~100μmである。
これらの中でも、厚みが薄く、ガスバリア性に優れる層を効率よく形成できることから、ガスバリア層は、無機膜からなるガスバリア層、及び高分子化合物を含む層にイオンを注入して得られるガスバリア層が好ましい。
無機蒸着膜としては、無機化合物や金属の蒸着膜が挙げられる。
無機化合物の蒸着膜の原料としては、酸化珪素、酸化アルミニウム、酸化マグネシウム、酸化亜鉛、酸化インジウム、酸化スズ等の無機酸化物;窒化ケイ素、窒化アルミニウム、窒化チタン等の無機窒化物;無機炭化物;無機硫化物;酸化窒化ケイ素等の無機酸化窒化物;無機酸化炭化物;無機窒化炭化物;無機酸化窒化炭化物等が挙げられる。
金属の蒸着膜の原料としては、アルミニウム、マグネシウム、亜鉛、及びスズ等が挙げられる。
これらの中でも、優れたガスバリア性を有するガスバリア層を形成できる観点から、ケイ素含有高分子化合物が好ましく、ポリシラザン系化合物がより好ましい。
ポリシラザン系化合物は、ガラスコーティング材等として市販されている市販品をそのまま使用することもできる。
ポリシラザン系化合物は1種単独で、あるいは2種以上を組み合わせて用いることができる。
前記高分子層は、上述した高分子化合物の他に、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。
メタン、エタン等のアルカン系ガス類のイオン;エチレン、プロピレン等のアルケン系ガス類のイオン;ペンタジエン、ブタジエン等のアルカジエン系ガス類のイオン;アセチレン等のアルキン系ガス類のイオン;ベンゼン、トルエン等の芳香族炭化水素系ガス類のイオン;シクロプロパン等のシクロアルカン系ガス類のイオン;シクロペンテン等のシクロアルケン系ガス類のイオン;金属のイオン;有機ケイ素化合物のイオン;等が挙げられる。
これらのイオンは1種単独で、あるいは2種以上を組み合わせて用いることができる。
これらの中でも、より簡便にイオンを注入することができ、特に優れたガスバリア性を有するガスバリア層が得られることから、アルゴン、ヘリウム、ネオン、クリプトン、キセノン等の希ガスのイオンが好ましい。
ガスバリア層は、単層であっても、複数層であってもよい。
接着シート(B)は、前記ガスバリアフィルム上に、イソブチレン・イソプレン共重合体を主成分とする接着剤組成物(以下、「接着剤組成物(B)」ということがある。)から形成された接着剤層を有する。
イソブチレン・イソプレン共重合体をこのような配合割合で含有させることで、水分遮断性、透明性及び粘着力のすべてに優れる接着剤層を形成する際に有用な接着剤組成物を得ることができる。すなわち、この接着剤層を、透明基板上に形成された素子の封止材として用いた場合、水分の浸入を十分に防ぐことができ、さらに、光電変換素子への入射光や光電変換素子からの発光が損なわれることが少なく、接着界面で乖離しにくいため、長期間にわたり水分等の浸入を防ぐことができる。
イソブチレン・イソプレン共重合体の配合割合は、固形分として、接着剤組成物中、好ましくは50~90質量%、より好ましくは60~80質量%である。
イソブチレン・イソプレン共重合体をこのような配合割合で含有させることで、水分遮断性に優れ、かつ、粘着力に優れる接着剤層を形成する際に有用な接着剤組成物(B)を得ることができる。
その他のゴム系のポリマー成分としては、上述の接着剤組成物(A)の成分として用いるゴム系のポリマー成分と同様のものが挙げられる。
粘着付与剤を含有させることで、水分遮断性、透明性、および粘着力により優れる接着剤層を形成する際に有用な接着剤組成物を得ることができる。
接着剤組成物(B)が粘着付与剤を含有する場合、その配合割合は、イソブチレン・イソプレン共重合体100質量部に対して、通常5~100質量部、好ましくは、10~70質量部である。
粘着付与剤の配合量が、イソブチレン・イソプレン共重合体100質量部に対して、5質量部以上であることで、粘着性により優れる接着剤層を効率よく形成することができ、70質量部以下であることで、接着剤層の凝集力の低下を避けることができる。
その他の成分としては、上述の接着剤組成物(A)に含有させることができるその他の成分と同様のものが挙げられる。
その他の成分を配合する場合、それぞれの配合量は、接着剤組成物(B)中、好ましくは0.01~5質量%、より好ましくは0.01~2質量%である。
これらの溶媒は、1種単独で、あるいは2種以上を組み合わせて用いることができる。
粘着力は、例えば、23℃、50%RHの環境下でガラス基板に接着シートを貼付後、そのまま24時間放置してから測定した場合、ガラス基板に対する粘着力は、好ましくは3N/25mm以上、より好ましくは5N/25mm以上、さらに好ましくは10N/25mm以上である。
接着剤層のガラス基板に対する粘着力がこのような範囲にあることで、ガラス板等の透明基板上と十分な密着性が得られ、効果的に光電変換素子を封止することができる。
また、接着剤層のポリエチレンテレフタレートフィルムに対する粘着力は、好ましくは0.5N/25mm以上、より好ましくは1N/25mm以上、さらに好ましくは5N/25mm以上である。接着剤層のポリエチレンテレフタレートフィルムに対する粘着力がこのような範囲にあることで、例えば、ガスバリアフィルムと接着剤層の十分な密着性が得られ、ガスバリアフィルムと接着剤層の界面から水蒸気の侵入することをより効果的に抑制できる。
水蒸気透過率は、実施例に記載のされた方法で測定することができる。
接着剤層の水蒸気透過率がこのような範囲にあることで、透明基板上に形成された光電変換素子の封止材として、水蒸気の侵入をより効果的に抑制できる。
なお、接着剤層の水蒸気透過率の値は、接着剤層の厚みに依存するため、接着剤層の厚みが60μmでない場合には、厚みから換算して求めることができる。例えば、厚みがAμmで、水蒸気透過率がB(g/m2/day)の接着剤層の場合、厚みが60μmの時の水蒸気透過率は、A×B/60という式に当てはめて換算して求めることができる。
前記XとYの積が300未満であることで、透明基板上に形成された光電変換素子を、接着剤組成物を用いて封止した時に、接着剤層の側面からの水蒸気の侵入を効果的に抑制することができる。前記水蒸気透過率Xと接着剤層の厚みYの積が300を超えると、接着剤層の厚み方向(側面)から水蒸気の侵入し、光電変換素子が劣化する可能性がある。前記水蒸気透過率Xと接着剤層の厚みYの積が小さすぎると、十分な粘着性が得られず、水蒸気遮断性が低下するおそれがある。
接着シート(B)は、公知の方法で製造することができる。例えば、図2(a)に示す接着シート10Bは、次のようにして製造することができる。
先ず、ガスバリアフィルム3aを用意し、このガスバリアフィルム3a上に、接着剤組成物(B)を公知の方法により塗工し、得られた塗膜を乾燥して、接着剤層1bを形成することで、目的とする接着シート10Bを得ることができる。
また、接着剤層を形成した後、得られた接着シートの接着剤層を保護するために、該接着剤層上に剥離シート2cを積層することにより、図2(c)に示す剥離シート付の接着シート10Dを得ることができる。
塗膜を乾燥するときの乾燥条件としては、例えば80~150℃で30秒~5分間が挙げられる。
乾燥処理を行った後、そのまま1週間程度静置し、接着剤層を養生させてもよい。
また、接着シート(B)は次の方法によっても得ることができる。
先ず、一方の面が剥離剤により剥離処理された剥離シートを用意し、該剥離シートの剥離処理面上に、製造方法1と同様にして、上述した公知の方法により、前記接着剤組成物を塗工し、得られた塗膜を乾燥して、接着剤層を形成することで、剥離シート付接着剤層を得る。次いで、得られた剥離シート付接着剤層とガスバリアフィルムとを積層して、図2(c)に示す剥離シート付の接着シート10Dを得ることもできる。
したがって、本発明の接着シートは、透明基板上に形成された素子内部に酸素や水分等が浸入し、電極や素子を劣化させることを防止することができる、透明基板上に形成された素子の封止材として好適に用いることができる。
接着剤層の粘着力と水分遮断性に優れるため、ガスバリアフィルムの性能を十分に発揮させ、透明基板上に形成された素子を封止することができる。
本発明の接着シート(B)は、透明基板上に形成された有機EL等の素子内部に酸素や水分等が浸入し、電極や有機層を劣化させることを防止することができる、素子の封止材として用いられるものである。
本発明の電子デバイスは、透明基板と、該透明基板上に形成された素子と、該素子を封止するための封止材とを備える電子デバイスであって、前記封止材が、本発明の接着剤組成物(A)からなることを特徴とするもの〔電子デバイス(A)〕、又は、透明基板と、該透明基板上に形成された素子と、該素子を覆うように積層された接着シートとを備える電子デバイスであって、前記接着シートは、ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、該接着剤層が、イソブチレン・イソプレン共重合体を主成分として含む組成物からなるものであり、前記ガスバリアフィルムは、温度40℃、相対湿度90%環境下における水蒸気透過率が0.1g/m2/day以下であり、かつ、全光線透過率が80%以上であるものであって、前記接着剤層によって、前記素子が封止されていることを特徴とするもの〔電子デバイス(B)〕である。
透明基板上に形成される素子の、種類や大きさ、形状、個数等は、本発明の接着剤組成物により封止されるものであれば、特に制限されない。
透明基板の厚さは特に制限されず、光の透過率や、素子内外を遮断する性能を勘案して、適宜選択することができる。
透明導電層を形成する材料としては、公知の材料を用いることができる、具体的には、インジウム-スズ複合酸化物(ITO)、フッ素がドープされた酸化スズ(IV)SnO2 (FTO)、酸化スズ(IV)SnO2 、酸化亜鉛(II)ZnO、インジウム-亜鉛複合酸化物(IZO)などが挙げられる。
これらの材料は、一種単独で、あるいは二種以上を組み合わせて用いることができる。
本発明の電子デバイス(A)は、透明基板と、該透明基板上に形成された素子と、該素子を封止するための封止材とを備える電子デバイスであって、前記封止材が、本発明の接着剤組成物(A)からなることを特徴とする。
有機EL素子20Aは、ガラス基板11上に構造体12が形成された構造を有する。構造体12は、透明電極、正孔輸送層、発光層及び背面電極等(図示を省略する。)が積層されたものである。そして、この構造体12及びガラス基板11上に、接着剤層10A及び封止用基板4が積層されている。
有機EL素子の構造体12は接着剤層10Aで覆われているため、水分等の浸入が抑制される。また、接着剤層10Aは粘着力に優れるため、接着剤層10Aと封止用基板4の界面や、接着剤層10Aと構造体12の界面が剥離しにくいため、界面からの水分等の浸入が抑制される。
プラスチックフィルムとしては、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、ポリウレタン系ポリマー等の樹脂製のフィルムやシートを用いることができる。
封止用基板4の厚みは、特に制限はないが、取り扱い易さの観点から、好ましくは0.5~500μm、より好ましくは1~200μm、さらに好ましくは5~100μmである。
ガスバリア層は、単層であってもよく、複数層であってもよいが、より高いガスバリア性が得られるという観点から、ガスバリア層は複数層であることが好ましい。
ガスバリア層は、所望のガスバリア性を付与することができれば、材質等は特に限定されない。
また、封止用基板4には、保護層、導電体層、プライマー層等が積層されていてもよい。これらの層が積層される位置は、特に限定されない。
本発明の電子デバイス(B)は、透明基板と、該透明基板上に形成された素子と、該素子を覆うように積層された接着シートとを備える電子デバイスであって、前記接着シートは、ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、該接着剤層が、イソブチレン・イソプレン共重合体を主成分として含む組成物からなるものであり、前記ガスバリアフィルムは、温度40℃、相対湿度90%環境下における水蒸気透過率が0.1g/m2/day以下であり、かつ、全光線透過率が80%以上であるものであって、前記接着剤層によって、前記素子が封止されていることを特徴とする。
先ず、本発明の接着シート10Bの接着剤層1を、構造体12及びガラス基板11上に貼り合わせることにより、図4に示す有機EL素子20Bを得ることができる。
有機EL素子20Bは、本発明の接着シート(B)によって、構造体12が接着剤層1で覆われているため、水分等の浸入が抑制される。本発明においては、水分遮断性と透明性に優れるガスバリアフィルム3と、水分遮断性と粘着力に優れるイソブチレン・イソプレン共重合体を主成分とする接着剤組成物から形成された接着剤層1からなる本発明の接着シート10Bを用いているので、接着剤層1とガスバリアフィルム3の界面が剥離しにくく、素子内部に酸素や水分等が浸入し、電極や有機層が劣化することが抑制される。
また、透明性に優れるガスバリアフィルム3および接着剤層1によって、構造体12が封止されているため、構造体12への入射光や構造体12からの発光が損なわれることが少なく、構造体12の性能を高レベルで維持することができる。
各例中の部及び%は、特に断りのない限り、質量基準である。
各例で用いた化合物や材料を以下に示す。
イソブチレン・イソプレン共重合体(1):(日本ブチル社製、Exxon Butyl 268、数平均分子量260,000、イソプレンの含有率1.7モル%)
イソブチレン・イソプレン共重合体(2):(日本ブチル社製、Exxon Butyl 288、数平均分子量260,000、イソプレンの含有率2.3モル%)
ポリイソブチレン系樹脂(1):(BASF社製、オパノールB30、数平均分子量:200,000、イソプレンの含有率0モル%)
ポリイソブチレン系樹脂(2):(BASF社製、オパノールB50、数平均分子量:340,000、イソプレンの含有率0モル%)
装置:東ソー社製、HLC-8020
カラム:東ソー社製、TSK guard column HXL-H、TSK gel GMHXL(×2)、TSK gel G2000HXL
カラム温度:40℃
展開溶媒:テトラヒドロフラン
流速:1.0mL/min
粘着付与剤(2):脂肪族系石油樹脂(日本ゼオン社製、クイントンB170、軟化点70℃)
粘着付与剤(3):脂肪族系石油樹脂(日本ゼオン社製、クイントンR100、軟化点96℃)
剥離シート(2):シリコーン剥離処理したポリエチレンテレフタレートフィルム(リンテック社製、SP-PET38T103-1、厚み38μm)
(接着剤組成物の調製)
イソブチレン・イソプレン共重合体(1)100部をトルエンに溶解し、固形分濃度20%の接着剤組成物を調製した。
接着剤組成物を、剥離シート(2)の剥離処理面上に、乾燥後の厚みが60μmになるように塗工し、得られた塗膜を120℃で2分間乾燥して接着剤層を形成した。次いで、剥離シート(1)を、その剥離処理面で接着剤層と貼り合せて、接着シートを得た。
各成分とその配合量を第1表に記載のものに変更したことを除き、実施例1と同様にして、接着剤組成物を得、これを用いて接着シートを作製した。
アクリル酸ブチル90部、及びアクリル酸10部、重合開始剤としてアゾビスイソブチロニトリル0.2部を反応器に入れ混合した。次いで、得られた混合物内に窒素ガスを4時間吹き込んで脱気した後、攪拌しながら60℃まで昇温した。そのまま、撹拌を60℃で24時間続けることで重合反応を行った。次いで、反応混合物を酢酸エチルで希釈することで、固形分濃度が33%のアクリル系共重合体(重量平均分子量:650,000)の酢酸エチル溶液を得た。
架橋剤として、トリメチロールプロパン変性トリレンジイソシアネートの酢酸エチル溶液(日本ポリウレタン社製、コロネートL、固形分75質量%)を、その固形分が、前記酢酸エチル溶液の固形分100部に対して1.5部になるように添加し、次いで、トルエンを加えることで、固形分濃度20%のアクリル系共重合体を主成分とする接着剤組成物を得た。
この接着剤組成物を用いたこと以外は、実施例1と同様の方法により、接着シートを作製した。
実施例及び比較例で得た接着シートの接着剤層の組成を表1にまとめて示す。
ガラス基板の表面に、酸化インジウムスズ(ITO)膜(厚さ:150nm、シート抵抗:30Ω/□)をスパッタリング法により形成し、次いで、溶媒洗浄とUV/オゾン処理を行うことで陽極を作製した。
得られた陽極(ITO膜)上に、N,N’-ビス(ナフタレン-1-イル)-N,N’-ビス(フェニル)-ベンジデン)(Luminescence Technology社製)を60nm、トリス(8-ヒドロキシ-キノリネート)アルミニウム(Luminescence Technology社製)を40nm、2,9-ジメチル-4,7-ジフェニル-1,10-フェナントロリン(Luminescence Technology社製)を10nm、(8-ヒドロキシ-キノリノレート)リチウム(Luminescence Technology社製)を、10nm、0.1~0.2nm/sの速度で順次蒸着させ、発光層を形成した。
得られた発光層上に、アルミニウム(Al)(高純度化学研究所社製)を0.1nm/sの速度で100nm蒸着させて陰極を形成した。
なお、蒸着時の真空度は、全て1×10-4Pa以下である。
また、実施例2~18及び比較例1~5で得た接着シートを用いて、実施例1と同様にして有機EL素子を作製した。
接着シートの剥離シート(1)及び(2)を剥離し、ポリエチレンテレフタレートフィルム(三菱樹脂社製、厚さ6μm)に貼付し、2枚のポリエチレンテレフタレートフィルムで挟まれた接着剤層からなる水蒸気透過率測定用のサンプルを得た。水蒸気透過率測定装置(LYSSY社製、L80-5000)を用いて、40℃、90%RHの環境下における、接着剤層の水蒸気透過率を測定した。
実施例1~18及び比較例1~5で用いた接着剤組成物を、剥離シート(2)の剥離処理面上に、乾燥後の厚みが20μmになるように塗工し、得られた塗膜を120℃で2分間乾燥して接着剤層を形成した。次いで、アルミニウム箔(7μm)の両面にポリエチレンテレフタレートシートシート(12μm)をウレタン系接着剤層で接着した積層フィルム(アジアアルミ社製)を接着剤層と貼り合せて、粘着力測定用のサンプルを得た。
得られたサンプルを25mm×300mmの大きさに裁断し、剥離シート(2)を剥離し、露出した接着剤層を、23℃、50%RHの環境下で下記被着体に貼付し、その上から重さ2kgのローラーを1往復させて圧着して試験片を得た。
試験片を、圧着後24時間、23℃、50%RHの環境下で放置した後、同環境下で、引張試験機(オリエンテック社製、テンシロン)を用いて、剥離速度300mm/分、剥離角度180°の条件で剥離試験を行い、粘着力(N/25mm)を測定した。
・PETフィルム:東洋紡績社製、コスモシャインA4100、厚み50μm
・ガラス板(ソーダライムガラス):日本板硝子社製
接着シートの剥離シート(1)を剥離し、アルミニウム箔(7μm)の両面にポリエチレンテレフタレートシートシート(12μm)をウレタン系接着剤層で接着した積層フィルム(アジヤアルミ社製)に貼付し、水分浸入試験用のサンプルを得た。
一方、無アルカリガラス基板(コーニング社製、45mm×45mm)上に、真空蒸着法にて、縦32mm、横40mmで膜厚100nmのカルシウム層を形成した。
次いで、水分浸入試験用のサンプルから剥離シート(2)を剥離し、露出した接着剤層と、ガラス基板上のカルシウム層とを、窒素雰囲気下にて、ラミネータを用いて貼合し、カルシウム層が封止された水分浸入試験用試験片を得た。
得られた試験片を、60℃、90%RHの環境下で170時間放置し、カルシウム層の変色の割合(水分浸入の割合)を目視で確認し、下記の基準により水分遮断性を評価した。
A:変色しているカルシウム層の面積が全体の20%未満
B:変色しているカルシウム層の面積が全体の20%以上40%未満
C:変色しているカルシウム層の面積が全体の40%以上
上記で作製した有機EL素子を、23℃、50%RHの環境下で200時間放置した後、有機EL素子を起動させ、ダークスポット(非発光箇所)の有無を観察し、以下の基準で評価した。
○:ダークスポットが発光面積の5%未満
△:ダークスポットが発光面積の5%以上10%未満
×:ダークスポットが発光面積の10%以上
実施例1~18の接着剤組成物を用いて形成された接着剤層は、水蒸気透過率が低く、水分遮断性に優れ、また粘着力に優れる。また、実施例1~18の接着剤組成物を用いて形成された封止材により封止された有機EL素子は、水分浸入試験で高い性能を示し、高い耐久性を有することが分かった。一方、比較例1~4のイソプレンを含有しないポリイソブチレン系樹脂を主成分とする接着剤組成物を用いて形成された接着剤層は、水分浸入試験の性能が不十分であるため、有機EL素子の耐久性が高くない。また、比較例5のアクリル系共重合体を主成分とする接着剤組成物を用いて形成された接着剤層は、水蒸気透過率が高く、水分浸入試験で性能が低く、有機EL素子の耐久性が劣っている。
基材として、ポリエチレンテレフタレートフィルム(東洋紡績社製、コスモシャインA4100、厚さ50μm、以下、「PETフィルム」という。)、ポリシラザン化合物(ペルヒドロポリシラザンを主成分とするコーティング材(クラリアントジャパン社製、アクアミカNL110-20)をスピンコート法により塗布し、120℃で1分間加熱して、厚さ150nmの、ペルヒドロポリシラザンを含むポリシラザン層を形成した。次に、プラズマイオン注入装置を用いてポリシラザン層の表面に、下記の条件にて、アルゴン(Ar)をプラズマイオン注入して、ガスバリア層を形成して、ガスバリアフィルム(A)を作製した。
(プラズマイオン注入装置)
RF電源:日本電子社製、型番号「RF」56000
高電圧パルス電源:栗田製作所社製、「PV-3-HSHV-0835」
(プラズマイオン注入条件)
プラズマ生成ガス:Ar
ガス流量:100sccm
Duty比:0.5%
印加電圧:-15kV
RF電源:周波数 13.56MHz、印加電力 1000W
チャンバー内圧:0.2Pa
パルス幅:5μsec
処理時間(イオン注入時間):200秒
基材として、ポリエチレンテレフタレートフィルム(東洋紡績社製、コスモシャインA4100、厚さ50μm、以下、「PETフィルム」という。)、ポリシラザン化合物(ペルヒドロポリシラザンを主成分とするコーティング材(クラリアントジャパン社製、アクアミカNL110-20)をスピンコート法により塗布し、120℃で1分間加熱して、厚さ150nmの、ペルヒドロポリシラザンを含むポリシラザン層を形成した。次に、プラズマイオン注入装置を用いてポリシラザン層の表面に、下記の条件にて、アルゴン(Ar)をプラズマイオン注入して、ガスバリア層を形成して、ガスバリアフィルム(B)を作製した。
(プラズマイオン注入装置)
RF電源:日本電子社製、型番号「RF」56000
高電圧パルス電源:栗田製作所社製、「PV-3-HSHV-0835」
(プラズマイオン注入条件)
プラズマ生成ガス:Ar
ガス流量:100sccm
Duty比:0.5%
印加電圧:-6kV
RF電源:周波数 13.56MHz、印加電力 1000W
チャンバー内圧:0.2Pa
パルス幅:5μsec
処理時間(イオン注入時間):200秒
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、スパッタリング法により、厚み100nmの酸化ケイ素からなるガスバリア層を形成し、ガスバリアフィルム(C)を作製した。
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、スパッタリング法により、厚み100nmの窒化ケイ素からなるガスバリア層を形成し、ガスバリアフィルム(D)を作製した。
(接着剤組成物の調製)
イソブチレン・イソプレン共重合体(1)100部をトルエンに溶解し、固形分濃度20%の接着剤組成物1を調製した。
接着剤組成物1を、ガスバリアフィルム(A)のガスバリア層上に、乾燥後の厚みが20μmになるように塗工し、得られた塗膜を110℃で1分間乾燥して接着剤層を形成した。次いで、剥離シートとして、シリコーン剥離処理したポリエチレンテレフタレートフィルム〕(リンテック社製、SP-PET381130、厚み38μm)を、その剥離処理面で接着剤層と貼り合わせて、接着シートを得た。
接着剤組成物を表3に記載のものに変更したことを除き、実施例19と同様にして、接着剤組成物2~24を得た。次いで、得られた接着剤組成物およびガスバリアフィルムを表4に記載のものに変更してこれを用いて接着シートを作製した。
アクリル酸ブチル90部、及びアクリル酸10部、重合開始剤としてアゾビスイソブチロニトリル0.2部を反応器に入れ混合した。次いで、得られた混合物内に窒素ガスを4時間吹き込んで脱気した後、攪拌しながら60℃まで昇温した。そのまま、撹拌を60℃で24時間続けることで重合反応を行った。次いで、反応混合物を酢酸エチルで希釈することで、固形分濃度が33%のアクリル系共重合体(重量平均分子量:650,000)の酢酸エチル溶液を得た。
架橋剤として、トリメチロールプロパン変性トリレンジイソシアネートの酢酸エチル溶液(日本ポリウレタン社製、コロネートL、固形分75質量%)を、その固形分が、前記酢酸エチル溶液の固形分100部に対して1.5部になるように添加し、次いで、トルエンを加えることで、固形分濃度20%のアクリル系共重合体を主成分とする接着剤組成物を得た。
この接着剤組成物を用いたこと以外は、実施例19と同様の方法により、接着シートを作製した。
実施例及び比較例で得た接着シートの接着剤層の組成を表3に示す。
ガラス基板を溶媒洗浄とUV/オゾン処理で洗浄した後、アルミニウム(Al)(高純度化学研究所社製)を0.1nm/sの速度で100nm蒸着させて陰極を形成した。得られた陰極(Al膜)上に、(8-ヒドロキシ-キノリノレート)リチウム(Luminescence Technology社製)を10nm、2,9-ジメチル-4,7-ジフェニル-1,10-フェナントロリン(Luminescence Technology社製)を10nm、トリス(8-ヒドロキシ-キノリネート)アルミニウム(Luminescence Technology社製)を40nm、N,N’-ビス(ナフタレン-1-イル)-N,N’-ビス(フェニル)-ベンジデン)(Luminescence Technology社製)を60nm、0.1~0.2nm/sの速度で順次蒸着させ、発光層を形成した。得られた発光層上に、酸化インジウムスズ(ITO)膜(厚さ:100nm、シート抵抗:50Ω/□)をスパッタリング法により形成し、陽極を形成した。
なお、蒸着時の真空度は、全て1×10-4Pa以下である。
ガスバリアフィルム(A)~(C)の40℃、90%RHの環境下における水蒸気透過率は、水蒸気透過率測定装置(MOCON社製、AQUATRON)を用いて、の水蒸気透過率を測定した。
実施例および比較例で使用した接着剤組成物を、剥離シート(シリコーン剥離処理したポリエチレンテレフタレートフィルム、リンテック社製、SP-PET38T103-1、厚み38μm)の剥離処理面上に、乾燥後の厚みが60μmになるように塗工し、得られた塗膜を120℃で2分間乾燥して接着剤層を形成した。次いで、ポリエチレンテレフタレートフィルム(三菱樹脂社製、厚さ6μm)を、接着剤層と貼り合せた。次いで、剥離シートを剥離し、露出した接着剤層に、もう1枚のポリエチレンテレフタレートフィルム(三菱樹脂社製、厚さ6μm)を貼り合わせ、2枚のポリエチレンテレフタレートフィルムで挟まれた接着剤層からなる、水蒸気透過率測定用のサンプルを得た。
得られたサンプルについて、水蒸気透過率測定装置(LYSSY社製、L80-5000)を用いて、接着剤層の温度40℃、相対湿度90%環境下における水蒸気透過率を測定し、この値を接着剤層の水蒸気透過率とした。
実施例および比較例で得られたを25mm×300mmの大きさに裁断し、剥離シートを剥離し、露出した接着剤層を、23℃、50%RHの環境下で下記被着体に貼付し、その上から重さ2kgのローラーを1往復させて圧着して試験片を得た。
試験片を、圧着後24時間、23℃、50%RHの環境下で放置した後、同環境下で、引張試験機(オリエンテック社製、テンシロン)を用いて、剥離速度300mm/分、剥離角度180°の条件で剥離試験を行い、粘着力(N/25mm)を測定した。
・PETフィルム:東洋紡績社製、コスモシャインA4100、厚み50μm
・ガラス板(ソーダライムガラス):日本板硝子社製
無アルカリガラス基板(コーニング社製、45mm×45mm)上に、真空蒸着法にて、縦32mm、横40mmで膜厚100nmのカルシウム層を形成した。
次いで、接着シートから剥離シートを剥離し、露出した接着剤層と、ガラス基板上のカルシウム層とを、窒素雰囲気下にて、ラミネータを用いて貼合し、カルシウム層が封止された水分浸入試験用試験片を得た。
得られた試験片を、60℃、90%RHの環境下で170時間放置し、カルシウム層の変色の割合(水分浸入の割合)を目視で確認し、下記の基準により水分遮断性を評価した。
A:変色しているカルシウム層の面積が全体の20%未満
B:変色しているカルシウム層の面積が全体の20%以上40%未満
C:変色しているカルシウム層の面積が全体の40%以上
有機EL素子を、23℃、50%RHの環境下で200時間放置した後、有機EL素子を起動させ、ダークスポット(非発光箇所)の有無を観察し、以下の基準で評価した。
A:ダークスポットが発光面積の5%未満
B:ダークスポットが発光面積の5%以上10%未満
C:ダークスポットが発光面積の10%以上90%未満
D:ダークスポットが発光面積の90%以上
有機EL素子の封止前後の発光輝度測定を行い、発光印加電圧(5V)での封止前後の発光輝度を測定した。下記式により、有機EL素子の封止前の発光輝度を100%とし、封止前の発光輝度に対する封止後の発光輝度の割合を求めた。
式:(封止後発光輝度)/(封止前発光輝度)×100
全光線透過率濁時計(日本電色工業社製、HAZE METER NDH5000)を用いて、JIS K7631-1に準じて、実施例および比較例で使用したガスバリアフィルムおよび実施例および比較例の接着シートの全光線透過率を測定した。なお、接着シートの全光線透過率は、剥離シートを剥離した状態で測定を行った。
実施例19~38の接着シートは、水分浸入試験で高い性能を示し、接着シートを備える有機EL素子は高い耐久性を有する。さらに、ガスバリアフィルムにより封止しているにも関わらず、封止前に比べて発光輝度の低下が少なく、発光色の色味変化のない良好な有機EL素子を得ることができた。
一方、比較例8のアクリル系接着剤を用いて形成された接着シートは、接着剤層の水蒸気透過率が高く、水分遮断性が劣り、有機EL素子の耐久性が劣っている。
また、比較例6の接着シートは、接着剤層の水蒸気透過率は低いが、ガスバリアフィルムの水蒸気透過率が高いため、接着剤層の性能を十分に生かすことができず、有機EL素子の耐久性は高くない。
比較例7の接着シートは、ガスバリアフィルムの水蒸気透過率は低いが、接着剤層の水蒸気透過率が高いため、ガスバリアフィルムの性能を十分に生かすことができず、有機EL素子の耐久性は高くない。
また、比較例9の粘着シートはガスバリアフィルムの水蒸気透過率は低いが、ガスバリアフィルムの全光線透過率が低く、有機ELからの発光を阻害し、封止前に比べて、発光輝度が大幅に減少している。
1、1a、1b、1c、1d・・・接着剤層
2a、2b、2c・・・剥離シート
3、3a、3b、3c、3d・・・ガスバリア層(ガスバリアフィルム)
4・・・封止用基板
11・・・ガラス基板
12・・・構造体
20A、20B・・・有機EL素子
Claims (15)
- 電子デバイスを封止するための接着剤組成物であって、
イソプレン由来の繰り返し単位の含有率が、全繰り返し単位に対して0.1~99モル%であるイソブチレン・イソプレン共重合体を主成分として含有することを特徴とする、接着剤組成物。 - 前記イソブチレン・イソプレン共重合体100質量部に対して、粘着付与剤を5~100質量部含有することを特徴とする、請求項1に記載の接着剤組成物。
- 前記粘着付与剤が、脂肪族系石油樹脂であることを特徴とする請求項2に記載の接着剤組成物。
- 剥離シートと、該剥離シート上に形成された接着剤層を有する接着シートであって、
前記接着剤層は、請求項1~3のいずれか1項に記載の接着剤組成物を用いて形成されたものであることを特徴とする接着シート。 - ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、
前記ガスバリアフィルムは、温度40℃、相対湿度90%の環境下における水蒸気透過率が0.1g/m2/day以下で、かつ、全光線透過率が80%以上のものであり、
前記接着剤層は、イソブチレン・イソプレン共重合体を主成分として含む接着剤組成物からなることを特徴とする接着シート。 - 前記イソブチレン・イソプレン共重合体は、イソプレン由来の繰り返し単位の含有率が、全繰り返し単位に対して0.1~99モル%であることを特徴とする、請求項5に記載の接着シート。
- 前記接着剤層が厚み60μmの場合、温度40℃、相対湿度90%環境下における水蒸気透過率が、10g/m2/day以下であることを特徴とする請求項4または5に記載の接着シート。
- 前記接着剤層は、イソブチレン・イソプレン共重合体100部に対して、粘着付与剤を5~100質量部含有することを特徴とする、請求項4または5に記載の接着シート。
- 前記接着剤層の、20~60℃の貯蔵弾性率が105~106Paであることを特徴とする請求項4または5に記載の接着シート。
- 前記接着剤層の、ガラス基板に対する粘着力が、3N/25mm以上であることを特徴とする、請求項4または5に記載の接着シート。
- 前記接着剤層の、温度40℃、相対湿度90%の環境下における水蒸気透過率X(g/m2/day)と、前記前記接着剤層の厚みY(μm)の積が、300未満であることを特徴とする、請求項4または5に記載の接着シート。
- 透明基板と、該透明基板上に形成された素子と、該素子を封止するための封止材とを備える電子デバイスであって、
前記封止材が、請求項1~3のいずれか1項に記載の接着剤組成物からなること特徴とする電子デバイス。 - 透明基板と、該透明基板上に形成された素子と、該素子を封止するための封止材とを備える電子デバイスであって、
前記封止材が、請求項4~11のいずれか1項に記載の接着シートを用いて形成されたものであること特徴とする電子デバイス。 - 透明基板と、該透明基板上に形成された素子と、該素子を覆うように積層された接着シートを備える電子デバイスであって、
該接着シートは、ガスバリアフィルムと、前記ガスバリアフィルム上に形成された接着剤層を備え、
該接着剤層が、イソブチレン・イソプレン共重合体を主成分として含む組成物からなるものであり、
前記ガスバリアフィルムは、温度40℃、相対湿度90%環境下における水蒸気透過率が0.1g/m2/day以下であり、かつ、全光線透過率が80%以上であるものであって、
前記接着剤層によって、前記素子が封止されている
ことを特徴とする電子デバイス。 - 透明基板と、該透明基板上に形成された素子と、該素子を覆うように積層された接着シートを備える電子デバイスの製造方法であって、
透明基板上に形成された素子を覆うように請求項4~11のいずれかに記載の接着シートを積層する工程を有する、電子デバイスの製造方法。
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Also Published As
Publication number | Publication date |
---|---|
CN104797670B (zh) | 2017-12-29 |
TWI639667B (zh) | 2018-11-01 |
US20150299519A1 (en) | 2015-10-22 |
KR20150092093A (ko) | 2015-08-12 |
US9809728B2 (en) | 2017-11-07 |
JPWO2014084352A1 (ja) | 2017-01-05 |
JP2018141166A (ja) | 2018-09-13 |
KR102189387B1 (ko) | 2020-12-11 |
JP6482704B2 (ja) | 2019-03-13 |
EP2927297A1 (en) | 2015-10-07 |
JP6734955B2 (ja) | 2020-08-05 |
CN104797670A (zh) | 2015-07-22 |
TW201435026A (zh) | 2014-09-16 |
EP2927297A4 (en) | 2016-08-03 |
JP2019116098A (ja) | 2019-07-18 |
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