WO2015098647A1 - シート状封止材、封止シート、電子デバイス封止体および有機el素子 - Google Patents
シート状封止材、封止シート、電子デバイス封止体および有機el素子 Download PDFInfo
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- WO2015098647A1 WO2015098647A1 PCT/JP2014/083391 JP2014083391W WO2015098647A1 WO 2015098647 A1 WO2015098647 A1 WO 2015098647A1 JP 2014083391 W JP2014083391 W JP 2014083391W WO 2015098647 A1 WO2015098647 A1 WO 2015098647A1
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- 125000005641 methacryl group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- JAYXSROKFZAHRQ-UHFFFAOYSA-N n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound C1OC1CN(C=1C=CC=CC=1)CC1CO1 JAYXSROKFZAHRQ-UHFFFAOYSA-N 0.000 description 1
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- SJPFBRJHYRBAGV-UHFFFAOYSA-N n-[[3-[[bis(oxiran-2-ylmethyl)amino]methyl]phenyl]methyl]-1-(oxiran-2-yl)-n-(oxiran-2-ylmethyl)methanamine Chemical compound C1OC1CN(CC=1C=C(CN(CC2OC2)CC2OC2)C=CC=1)CC1CO1 SJPFBRJHYRBAGV-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 description 1
- BMOMBHKAYGMGCR-UHFFFAOYSA-N octadecyl 3-oxobutanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CC(C)=O BMOMBHKAYGMGCR-UHFFFAOYSA-N 0.000 description 1
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
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- JTBKFHQUYVNHSR-UHFFFAOYSA-N propan-2-yloxyalumane Chemical compound CC(C)O[AlH2] JTBKFHQUYVNHSR-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- 150000003870 salicylic acids Chemical class 0.000 description 1
- 239000012945 sealing adhesive Substances 0.000 description 1
- 239000005394 sealing glass Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 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
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- 239000011593 sulfur Substances 0.000 description 1
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- 229920003051 synthetic elastomer Polymers 0.000 description 1
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- 238000010345 tape casting Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- XBFJAVXCNXDMBH-UHFFFAOYSA-N tetracyclo[6.2.1.1(3,6).0(2,7)]dodec-4-ene Chemical compound C1C(C23)C=CC1C3C1CC2CC1 XBFJAVXCNXDMBH-UHFFFAOYSA-N 0.000 description 1
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- SYRHIZPPCHMRIT-UHFFFAOYSA-N tin(4+) Chemical compound [Sn+4] SYRHIZPPCHMRIT-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- IUCJMVBFZDHPDX-UHFFFAOYSA-N tretamine Chemical compound C1CN1C1=NC(N2CC2)=NC(N2CC2)=N1 IUCJMVBFZDHPDX-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H10K50/86—Arrangements for improving contrast, e.g. preventing reflection of ambient light
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- B32B2581/00—Seals; Sealing equipment; Gaskets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2203/16—Applications used for films
- C08L2203/162—Applications used for films sealable films
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2003/1034—Materials or components characterised by specific properties
- C09K2003/1081—Water-proofed materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0617—Polyalkenes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0625—Polyacrylic esters or derivatives thereof
-
- 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
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Definitions
- the present invention relates to a sheet-like sealing material excellent in moisture barrier properties, light resistance and colorless transparency, a sealing sheet having this sheet-like sealing material and a gas barrier layer, and these sheet-like sealing materials or sealing sheets. It is related with the organic EL element which has an electronic device sealing body obtained by using as a sealing material, and the said sheet-like sealing material.
- 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.
- As a cause of the deterioration of the light emission characteristics of the organic EL element it is conceivable that oxygen, moisture, or the like permeates into the organic EL element and degrades the electrode or the organic layer.
- several methods using a sealing material have been proposed.
- 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 that are sealing materials for organic EL elements
- acrylic adhesives and pressure-sensitive adhesives are known from the viewpoint of optical properties such as transparency. It has been.
- Patent Document 3 discloses an acrylic adhesive having an ultraviolet curing function and a room temperature curing function as a sealing material for an organic EL display.
- Patent Document 4 discloses a pressure-sensitive adhesive that can form a pressure-sensitive 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.
- An acrylic pressure-sensitive adhesive is disclosed.
- 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.
- Patent Document 6 proposes an organic EL element in which an organic EL layer is covered with a resin layer containing an ultraviolet absorber.
- JP-A-5-182759 Japanese Patent Laid-Open No. 5-101884 JP 2004-87153 A Japanese Patent Application Laid-Open No. 2004-224991 Special table 2009-524705 gazette (WO2007 / 08871 pamphlet) JP 2009-37809 A (US2010 / 0244073A1)
- the present invention has been made in view of the actual situation of the prior art, and has a sheet-shaped sealing material excellent in all of moisture barrier properties, light resistance and colorless transparency, and includes the sheet-shaped sealing material and a gas barrier layer.
- An object of the present invention is to provide a sealing sheet, an electronic device sealing body obtained by using these sheet-shaped sealing materials or sealing sheets as a sealing material, and an organic EL element having the sheet-shaped sealing material. To do.
- the inventors of the present invention have a low water vapor transmission rate and a specific b * value in the CIE L * a * b * color system defined in JIS Z 8729-1994.
- the sheet-like encapsulant that is in the range has a low light transmittance at a wavelength of 370 nm, and a high light transmittance at a wavelength of 420 nm is excellent in all of moisture blocking properties, light resistance, and colorless transparency.
- the headline and the present invention were completed.
- the following sheet-shaped sealing materials (1) to (7), the sealing sheets (8) to (10), the electronic device sealing body (11), and the organic EL (12) An element is provided.
- a sheet-shaped encapsulant comprising one or more encapsulating resin layers, the water vapor permeation when the sheet-form encapsulant is converted to a thickness of 50 ⁇ m at a temperature of 40 ° C. and a relative humidity of 90%.
- the rate is 20 g / (m 2 ⁇ day) or less, and the b * value in the CIE L * a * b * color system defined by JIS Z 8729-1994 is ⁇ 2 2 to 2%, and the sheet-like encapsulant has a light transmittance at a wavelength of 370 nm of 1% or less and a light transmittance at a wavelength of 420 nm of 85% or more. .
- the sealing resin layer contains at least one selected from the group consisting of a rubber-based polymer, a (meth) acrylic polymer, a polyolefin-based polymer, a polyester-based polymer, a styrene-based thermoplastic elastomer, and a silicone-based polymer.
- the sheet-like sealing material according to (1) which is a layer containing a stop resin.
- the sheet-like sealing material according to (1), wherein at least one layer of the sealing resin layer contains an ultraviolet absorber.
- the sheet-like sealing material according to (1) which is used for sealing an electronic device.
- the sealing sheet according to (8) which is used for sealing an electronic device.
- Organic EL having a first electrode, an organic EL layer, a second electrode, a sheet-like encapsulant composed of one or more encapsulating resin layers, and an encapsulating substrate in this order on a transparent substrate It is an element,
- the said sheet-like sealing material is a sheet-like sealing material as described in (1),
- the organic EL element characterized by the above-mentioned.
- a sheet-like encapsulant excellent in moisture barrier properties, light resistance and colorless transparency, an encapsulating sheet having this sheet-like encapsulant and a gas barrier layer, these sheet-like encapsulants or encapsulating An electronic device sealing body obtained by using a sheet as a sealing material, and an organic EL element having the sheet-shaped sealing material are provided.
- Sheet-like encapsulant of the present invention is a sheet-like encapsulant comprising one or more encapsulating resin layers, and the temperature of the sheet-like encapsulant is 40 ° C., relative
- the water vapor permeability when converted to a thickness of 50 ⁇ m at a humidity of 90% is 20 g / (m 2 ⁇ day) or less, and CIE L * a defined in JIS Z 8729-1994 of the sheet-shaped sealing material.
- the b * value in the color system is -2 to 2%, and the sheet-form sealing material has a light transmittance of 1% or less at a wavelength of 370 nm and a light transmittance of 420% at a wavelength of 420 nm. It is the above, It is characterized by the above.
- the water vapor permeability of the sheet-shaped sealing material of the present invention when converted to a thickness of 50 ⁇ m at a temperature of 40 ° C. and a relative humidity of 90% is 20 g / (m 2 ⁇ day) or less, preferably 10 g / (M 2 ⁇ day) or less, more preferably 8 g / (m 2 ⁇ day) or less, and further preferably 5 g / (m 2 ⁇ day) or less.
- Such a sheet-like sealing material is suitably used as a sealing material for electronic devices.
- the value of the water vapor transmission rate of the sheet-like sealing material depends on the thickness of the sheet-like sealing material. Therefore, when the thickness of the sheet-like sealing material is not 50 ⁇ m, the water vapor transmission rate at a thickness of 50 ⁇ m can be obtained by converting from the thickness. For example, in the case of a sheet-like sealing material having a thickness of A ⁇ m and a water vapor transmission rate of B ⁇ g / (m 2 ⁇ day) ⁇ , the water vapor transmission rate when the thickness is 50 ⁇ m is expressed by the formula A ⁇ B / 50. It can be calculated by fitting.
- the water vapor transmission rate can be controlled by appropriately selecting a sealing resin to be used.
- a sheet-shaped sealing material having a low water vapor transmission rate can be obtained by containing a large amount of a rubber-based polymer in the sealing resin layer.
- the water vapor transmission rate can be measured by the method described in the examples.
- the b * value in the CIE L * a * b * color system defined by JIS Z 8729-1994 of the sheet-like sealing material of the present invention is ⁇ 2 to 2%, preferably ⁇ 1.5. It is ⁇ 1.5%, more preferably ⁇ 1.0 to 1.0%, particularly preferably ⁇ 0.5 to 0.5%.
- the b * value represents the degree of yellow and blue when the color is digitized. If the b * value is positive, it is yellowish, and if it is negative, it is bluish. When the b * value is in the above range, the sheet-like sealing material becomes more colorless.
- Such a sheet-like sealing material is suitably used as a sealing material for a light emitting device.
- the b * value can be controlled by appropriately selecting the sealing resin to be used and other components.
- the b * value may be increased depending on the type and content thereof, so that selection and determination of the content are important.
- b * is determined by selecting an ultraviolet absorber to be used with the light transmittance at a wavelength of 420 nm as an index, and further appropriately determining the content, the thickness of the sheet-like sealing material, and the like . The value can be controlled.
- the a * value in the CIE L * a * b * color system defined by JIS Z 8729-1994 of the sheet-like sealing material of the present invention is preferably ⁇ 2 to 2%, more preferably -1.5 to 1.5%, more preferably -1.0 to 1.0%, particularly preferably -0.5 to 0.5%.
- the a * value represents the degree of redness and greenness when the color is digitized. If the a * value is positive, it is reddish, if it is negative, This means that it is greenish. When the a * value is in the above range, the sheet-like sealing material becomes more colorless.
- Such a sheet-like sealing material is suitably used as a sealing material for a light emitting device.
- the a * value can be controlled by appropriately selecting the sealing resin to be used and other components.
- the b * value and a * value in the CIE L * a * b * color system defined in JIS Z 8729-1994 can be measured by the method described in the examples.
- the light transmittance at a wavelength of 370 nm of the sheet-shaped sealing material of the present invention is 1% or less, preferably 0.5% or less.
- the light transmittance at a wavelength of 420 nm is 85% or more, preferably 90% or more.
- the light transmittance can be measured by the method described in Examples.
- a sheet-like encapsulant having a light transmittance of 1% or less at a wavelength of 370 nm can sufficiently absorb ultraviolet rays and has excellent light resistance.
- Such a sheet-like sealing material is suitably used for sealing an organic EL layer or the like that is easily deteriorated by ultraviolet rays.
- the light transmittance at a wavelength of 370 nm can be lowered, for example, by containing an ultraviolet absorber in at least one sealing resin layer.
- the light transmittance at a wavelength of 370 nm is controlled to 1% or less by appropriately determining the content and the thickness of the sheet-like sealing material in consideration of the maximum absorption wavelength and absorption coefficient of the ultraviolet absorber to be used. be able to.
- a sheet-like encapsulant having a light transmittance of 85% or more at a wavelength of 420 nm tends to have a b * value within the above range and is excellent in colorless transparency.
- the light transmittance at a wavelength of 420 nm is, for example, 85% or more by appropriately determining the content and thickness of the sheet-like sealing material when using an additive that may absorb visible light such as an ultraviolet absorber. Can be controlled.
- the thickness of the sheet-like sealing material of the present invention is not particularly limited, but is preferably 0.1 to 100 ⁇ m, more preferably 5 to 90 ⁇ m, and still more preferably 10 to 80 ⁇ m.
- the thickness of the sheet-like encapsulant is within the above range, it becomes easy to obtain an encapsulant that balances moisture barrier properties, light resistance, and colorless transparency.
- the adhesiveness of the sheet-like sealing material of the present invention can be evaluated by performing a 180 ° peel test. Specifically, a sheet-like sealing material having a width of 25 mm is pasted on glass in an environment of a temperature of 23 ° C. and a relative humidity of 50%, and then left as it is for 24 hours. Then, using a tensile tester, 300 mm / When the tensile test is performed under the condition of the separation angle of 180 °, the adhesive strength is preferably 3N / 25 mm or more. Such a sheet-like sealing material can sufficiently prevent moisture and the like from entering from the interface with the object to be sealed when sealed.
- the adhesiveness of the sheet-like sealing material can be controlled by selecting the type of sealing resin or additive to be used, forming a crosslinked structure in the sealing resin layer, or the like.
- the sealing resin layer of the sheet-like sealing material of the present invention is a layer containing a sealing resin.
- the sealing resin is not particularly limited as long as the effects of the present invention can be obtained.
- the sealing resin include rubber polymers, (meth) acrylic polymers, polyolefin polymers, polyester polymers, silicone polymers, styrene thermoplastic elastomers, and the like.
- the rubber-based polymer has rubber elasticity such as natural rubber or synthetic rubber.
- natural rubber NR
- butadiene homopolymer butadiene rubber, BR
- chloroprene homopolymer chloroprene rubber, CR
- isoprene homopolymer acrylonitrile-butadiene copolymer (nitrile rubber)
- NR natural rubber
- butadiene homopolymer butadiene rubber, BR
- chloroprene homopolymer chloroprene rubber, CR
- isoprene homopolymer acrylonitrile-butadiene copolymer
- nitrile rubber acrylonitrile-butadiene copolymer
- examples thereof include an ethylene-propylene-nonconjugated diene terpolymer, an isobutylene polymer, or a modified product thereof.
- isobutylene polymers are more preferable.
- the isobutylene polymer refers to a polymer having repeating units derived from isobutylene in the main chain and / or side chain.
- the amount of the isobutylene-derived repeating unit is preferably 50% by mass or more, more preferably 60% by mass or more, and further preferably 70 to 99% by mass.
- isobutylene polymer examples include a homopolymer of isobutylene (polyisobutylene), a copolymer of isobutylene and isoprene (butyl rubber), a copolymer of isobutylene and n-butene, a copolymer of isobutylene and butadiene, and these polymers And an isobutylene polymer such as a halogenated polymer obtained by brominating or chlorinating a benzene. Among these, a copolymer of isobutylene and isoprene (butyl rubber) is preferable.
- the (meth) acrylic polymer is a polymer having a repeating unit derived from a (meth) acrylic monomer in the main chain and / or side chain.
- a (meth) acrylic monomer in the main chain and / or side chain For example, homopolymers or copolymers of (meth) acrylic monomers, or modified ones thereof may be mentioned.
- (meth) acryl means acryl or methacryl (the same applies hereinafter).
- the amount of the repeating unit derived from the (meth) acrylic monomer in the (meth) acrylic polymer is preferably 50% by mass or more, more preferably 60% by mass or more, and further preferably 70 to 99% by mass.
- (meth) acrylic monomers the carbon number of alkyl groups such as (meth) acrylic acid, methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, etc.
- alkyl groups such as (meth) acrylic acid, methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, etc.
- examples thereof include (meth) acrylic acid esters having a reactive functional group such as 1 to 20 (meth) acrylic acid esters, 2-ethylhexyl (meth) acrylate, and hydroxymethyl (meth) acrylate.
- the polyolefin-based polymer is a polymer having a repeating unit derived from an olefin-based monomer in the main chain and / or side chain.
- olefin monomers include ethylene; ⁇ -olefins having 3 to 20 carbon atoms such as propylene, 1-butene, 4-methyl-1-pentene, 3-methyl-1-butene, 1-hexene, 1-octene; cyclobutene And cyclic olefins having 4 to 20 carbon atoms such as tetracyclododecene and norbornene; or modified ones thereof.
- the polyester polymer is a polymer obtained by polycondensation of a polyvalent carboxylic acid and a polyol, or a modification thereof.
- the polyvalent carboxylic acid include terephthalic acid, isophthalic acid, orthophthalic acid, succinic acid, adipic acid, sebacic acid, cyclohexanedicarboxylic acid, trimellitic acid and the like.
- the polyol include aliphatic alcohols such as ethylene glycol and propylene glycol, and polyether polyols such as polyethylene glycol and polypropylene glycol.
- the silicone-based polymer is a polymer having a (poly) siloxane structure in the main chain and / or side chain, or a modification thereof.
- examples of the silicone polymer include dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, and the like.
- the styrene-based thermoplastic elastomer is a polymer having a repeating unit derived from styrene or a modified one thereof.
- SBS styrene-butadiene-styrene block copolymer
- SEBS SBS hydrogenated styrene-ethylene-butene-styrene block copolymer
- SEBS styrene-isoprene-styrene block copolymer
- SIS SIS hydrogenated styrene-ethylene-propylene-styrene block copolymer
- SEPS styrene-butadiene copolymer
- SBR styrene-isoprene copolymer
- SBR styrene-isobutylene diblock
- IB styrene-isobutylene-stylene diblock
- sealing resins can be used alone or in combination of two or more.
- a rubber-based polymer or a polyolefin-based polymer is preferable as the sealing resin because a sheet-shaped sealing material having a low water vapor transmission rate is easily obtained.
- the number average molecular weight (Mn) of the sealing resin is preferably 100,000 to 2,000,000, more preferably 100,000 to 1,500,000, and still more preferably 100,000 to 1,000,000. When the number average molecular weight (Mn) of the sealing resin is within the above range, a sheet-shaped sealing material having a low water vapor transmission rate is easily obtained.
- the number average molecular weight (Mn) of the sealing resin can be obtained as a standard polystyrene equivalent value by performing gel permeation chromatography using tetrahydrofuran as a solvent.
- the sealing resin layer may be formed with a crosslinked structure.
- the sealing resin layer has a sufficient cohesive force, is superior in adhesiveness, and has a lower water vapor transmission rate.
- a crosslinked structure is formed in the sealing resin layer, a known crosslinked structure forming method using an adhesive or the like can be used.
- a crosslinked structure is formed by using a crosslinking agent such as an isocyanate crosslinking agent, an epoxy crosslinking agent, an aziridine crosslinking agent, or a metal chelate crosslinking agent.
- a crosslinking agent such as an isocyanate crosslinking agent, an epoxy crosslinking agent, an aziridine crosslinking agent, or a metal chelate crosslinking agent.
- the isocyanate-based crosslinking agent is a compound having an isocyanate group as a crosslinkable group.
- Isocyanate-based crosslinking agents include trimethylolpropane-modified tolylene diisocyanate, tolylene diisocyanate, diphenylmethane diisocyanate, xylylene diisocyanate, etc .; aliphatic polyisocyanates such as hexamethylene diisocyanate; isophorone diisocyanate, hydrogenated diphenylmethane diisocyanate, etc.
- Alicyclic polyisocyanates of these compounds biurets, isocyanurates of these compounds, and also reactants with low molecular active hydrogen-containing compounds such as ethylene glycol, propylene glycol, neopentyl glycol, trimethylolpropane, castor oil Adduct body; and the like.
- the epoxy-based crosslinking agent is a compound having an epoxy group as a crosslinkable group.
- Epoxy crosslinking agents include 1,3-bis (N, N'-diglycidylaminomethyl) cyclohexane, N, N, N ', N'-tetraglycidyl-m-xylylenediamine, ethylene glycol diglycidyl ether 1,6-hexanediol diglycidyl ether, trimethylolpropane diglycidyl ether, diglycidylaniline, diglycidylamine and the like.
- An aziridine-based crosslinking agent is a compound having an aziridine group as a crosslinkable group.
- the aziridine-based crosslinking agent include diphenylmethane-4,4′-bis (1-aziridinecarboxamide), trimethylolpropane tri- ⁇ -aziridinylpropionate, tetramethylolmethanetri- ⁇ -aziridinylpro Pionate, toluene-2,4-bis (1-aziridinecarboxamide), triethylenemelamine, bisisophthaloyl-1- (2-methylaziridine), tris-1- (2-methylaziridine) phosphine, tri And methylolpropane tri- ⁇ - (2-methylaziridine) propionate.
- metal chelate-based crosslinking agent examples include chelate compounds in which the metal atom is aluminum, zirconium, titanium, zinc, iron, tin, etc. Among them, aluminum chelate compounds are preferable.
- Aluminum chelate compounds include diisopropoxy aluminum monooleyl acetoacetate, monoisopropoxy aluminum bis oleyl acetoacetate, monoisopropoxy aluminum monooleate monoethyl acetoacetate, diisopropoxy aluminum monolauryl acetoacetate, diisopropoxy aluminum mono Examples include stearyl acetoacetate and diisopropoxyaluminum monoisostearyl acetoacetate.
- crosslinking agents can be used alone or in combination of two or more.
- the amount used is that the crosslinking group of the crosslinking agent (in the case of a metal chelate crosslinking agent, the metal chelate crosslinking agent) is the hydroxyl group and carboxyl of the sealing resin.
- the amount is preferably 0.1 to 5 equivalents, more preferably 0.2 to 3 equivalents, based on the group.
- a crosslinked structure can be formed by using a photopolymerization initiator or a thermal polymerization initiator.
- photopolymerization initiator examples include benzophenone, acetophenone, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, benzoin benzoic acid, benzoin benzoic acid methyl, benzoin dimethyl ketal, 2,4-diethylthioxanthone, 1 -Hydroxycyclohexyl phenyl ketone, benzyldiphenyl sulfide, tetramethylthiuram monosulfide, azobisisobutyronitrile, 2-chloroanthraquinone, diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide, bis (2,4,6 -Trimethylbenzoyl) -phenyl-phosphine oxide.
- thermal polymerization initiator examples include hydrogen peroxide; peroxodisulfates such as ammonium peroxodisulfate, sodium peroxodisulfate, and potassium peroxodisulfate; 2,2′-azobis (2-amidinopropane) dihydrochloride, 4,4 Azo compounds such as' -azobis (4-cyanovaleric acid), 2,2'-azobisisobutyronitrile, 2,2'-azobis (4-methoxy-2,4-dimethylvaleronitrile); benzoyl peroxide Organic peroxides such as lauroyl peroxide, peracetic acid, persuccinic acid, di-t-butyl peroxide, t-butyl hydroperoxide, cumene hydroperoxide, and the like.
- peroxodisulfates such as ammonium peroxodisulfate, sodium peroxodisulfate, and potassium peroxodisulfate
- polymerization initiators can be used singly or in combination of two or more.
- the amount used is preferably 0.1 to 100 parts by mass and more preferably 1 to 100 parts by mass with respect to 100 parts by mass of the sealing resin.
- the content of the sealing resin in the sealing resin layer is preferably 50 to 100% by mass with respect to the entire sealing resin layer, and 55 to 99% by mass is more preferable, and 60 to 99% by mass is more preferable.
- the sealing resin layer further contains an ultraviolet absorber.
- the light transmittance at a wavelength of 370 nm of the sheet-shaped sealing material is 1% or less by appropriately determining the content and the thickness of the sheet-shaped sealing material in consideration of the maximum absorption wavelength and the absorption coefficient of the ultraviolet absorber. It becomes easy to control.
- the ultraviolet absorber preferably has a maximum absorption wavelength ( ⁇ max ) in the range of 330 to 370 nm, more preferably has a maximum absorption wavelength ( ⁇ max ) in the range of 335 to 365 nm, and 340 to 360 nm. Those having a maximum absorption wavelength ( ⁇ max ) within the range are further preferred.
- the UV absorber preferably has a maximum absorbance of 1.0 to 5.0 when the UV absorber is added to the resin at 2% and the film thickness is 20 ⁇ m, and 1.5 to 5.0. Are more preferable, and those of 2.0 to 5.0 are more preferable.
- the maximum absorption wavelength ( ⁇ max ) of the ultraviolet absorber is less than 330 nm, it may be difficult to control the light transmittance at a wavelength of 370 nm to 1% or less. On the other hand, if the maximum absorption wavelength ( ⁇ max ) of the ultraviolet absorber exceeds 370 nm, it may be difficult to obtain a sheet-shaped sealing material having a light transmittance of 85% or more at a wavelength of 420 nm.
- ultraviolet absorbers include salicylic acids such as phenyl salicylate, pt-butylphenyl salicylate, p-octylphenyl salicylate; 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy- 4-octoxybenzophenone, 2-hydroxy-4-dodecyloxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2-hydroxy-4-methoxy Benzophenones such as -5-sulfobenzophenone; 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, 2- (2'-hydroxy-5'-tert-butylphenyl) benzotriazole, 2- (2 '-Hydroxy-3', 5'- Di-tert-butylphenyl) benzotriazole, 2- (2′-hydroxy-3′-tert-tert
- the content of the ultraviolet absorber in the sealing resin layer can be appropriately determined according to the ultraviolet absorber to be used.
- the content of the ultraviolet absorber in the sealing resin layer is preferably 0.1 to 50% by mass, more preferably 0.3 to 30% by mass, and more preferably 0.5 to 20% by mass with respect to the entire sealing resin layer. % Is more preferable, and 1.0 to 10% by mass is particularly preferable.
- the sealing resin layer may further contain a tackifier.
- a tackifier By including a tackifier in the sealing resin layer, it becomes easy to obtain a sheet-like sealing material that is excellent in moisture barrier properties and excellent in adhesive strength.
- a tackifier will not be specifically limited if it improves the adhesiveness of a sheet-like sealing material, A well-known thing can be used.
- aliphatic petroleum resins, terpene resins, rosin ester resins, rosin resins and the like are preferable.
- a tackifier can be used individually by 1 type or in combination of 2 or more types.
- 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 Escolets 1000 Series (Exxon Chemical Co., Ltd.), Quinton A, B, R, CX Series (Zeon Japan Co., Ltd.); Alcon P, M Series (Arakawa Chemical Co., Ltd.) ), ESCOREZ series (manufactured by Exxon Chemical), EASTOTAC series (manufactured by Eastman Chemical), ILARV series (manufactured by Idemitsu Kosan Co., Ltd.); ), Clearon P series (manufactured by Yashara 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 content of the encapsulating resin in the encapsulating resin layer is preferably 0.1 to 40% by mass with respect to the entire encapsulating resin layer, and 1 to 30% by mass. % Is more preferable.
- the sealing resin layer may contain other components as long as the effects of the present invention are not hindered.
- other components include additives such as a silane coupling agent, an antistatic agent, a light stabilizer, an antioxidant, a resin stabilizer, a filler, a pigment, a bulking agent, and a softening agent. These can be used singly or in combination of two or more.
- the sealing resin layer contains other components, the content thereof is preferably 0.01 to 5% by mass and more preferably 0.01 to 2% by mass with respect to the entire sealing resin layer.
- the thickness of the sealing resin layer is not particularly limited, and can be appropriately determined according to the thickness of the target sheet-like sealing material.
- the thickness of the sealing resin layer is usually 0.1 to 100 ⁇ m, preferably 1.0 to 80 ⁇ m, more preferably 5.0 to 50 ⁇ m.
- the sheet-like sealing material of the present invention comprises one or two or more sealing resin layers.
- the upper limit of the number of sealing resin layers is not particularly limited, but is usually 10 layers or less.
- the sheet-like sealing material of the present invention is composed of two or more sealing resin layers, such a sheet-like sealing material is a laminate of two or more of the same sealing resin layers.
- two or more different sealing resin layers may be laminated. Examples of the different sealing resin layers include layers having different sealing resins, components other than the sealing resin, layers having different contents, and the like.
- an ultraviolet absorber is contained excessively in the sealing resin layer, the adhesive force may be reduced.
- the adhesive deterioration can be suppressed by making the sheet-shaped sealing material into a laminate composed of two or more sealing resin layers.
- a sheet-shaped sealing material having a three-layer structure composed of both outermost layers and an intermediate layer it is possible to prevent a decrease in adhesiveness due to the addition of the ultraviolet absorber by including the ultraviolet absorber only in the intermediate layer.
- by laminating two or more sealing resin layers it is possible to efficiently obtain a sheet-like sealing material that is excellent in all of moisture barrier properties, light resistance, and colorless transparency without deteriorating adhesiveness. Can do.
- the sheet-like sealing material of the present invention is composed of one or two or more sealing resin layers, and this represents a state functioning as a sealing material. That is, the sheet-like sealing material of the present invention may have a layer that is peeled off before use, such as a peeling sheet.
- the sheet-like sealing material of the present invention has a release sheet
- the water vapor transmission rate and the thickness of the sheet-like sealing material described below are the values excluding the release sheet (sealing resin layer).
- a conventionally well-known thing can be utilized as a peeling sheet.
- the base material for the release sheet 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 manufacturing method of the sheet-like sealing material of the present invention is not particularly limited.
- the sheet-like sealing material of the present invention can be produced using a casting method or an extrusion method.
- a resin composition containing a predetermined component such as a sealing resin is prepared, and this resin composition is prepared by a known method using a release sheet. It is possible to form a sealing resin layer with a release sheet (the sheet-like sealing material of the present invention with a release sheet) by applying to the release-treated surface and drying the obtained coating film.
- the resin composition can be prepared by appropriately mixing and stirring predetermined components, a solvent and the like 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 resin composition is preferably 10 to 60% by mass, more preferably 10 to 45% by mass, and further preferably 15 to 30% by mass.
- Examples of the method for applying the resin composition include spin coating, spray coating, bar coating, knife coating, roll coating, blade coating, die coating, and gravure coating.
- the drying conditions for drying the coating film include, for example, 80 to 150 ° C. for 30 seconds to 5 minutes.
- the sealing resin layer may be cured by leaving it still for about one week. By curing the sealing resin layer, a crosslinked structure can be sufficiently formed.
- the sealing resin layer After the sealing resin layer is formed, another sheet of release sheet is laminated on the sealing resin layer, whereby a sheet-like sealing material having release sheets as both outermost layers can be obtained.
- the sheet-like sealing material consisting of two or more sealing resin layers can be obtained by forming a plurality of sealing resin layers and laminating them so that the sealing resin layers face each other. it can.
- a sheet-like sealing composed of two or more sealing resin layers can be obtained by applying a resin composition on the sealing resin layer and drying the obtained coating film. A material can be obtained.
- a film is formed by an extrusion film forming method.
- a sheet-like sealing material can be obtained.
- a sheet-like sealing material made of two or more sealing resin layers can be obtained by forming a film by a multilayer extrusion film forming method.
- the well-known method used when manufacturing a co-extrusion multilayer film can be utilized.
- the sheet-like sealing material of the present invention is excellent in all of moisture barrier properties, light resistance and colorless transparency. Therefore, as will be described later, the sheet-like encapsulant of the present invention is suitably used when encapsulating an electronic device, and particularly suitable as an encapsulant for encapsulating an organic EL element that is easily deteriorated by ultraviolet rays. Used.
- the sealing sheet of this invention is a sealing sheet which has the sheet-like sealing material which consists of 1 or 2 or more sealing resin layers, and a gas barrier layer, Comprising:
- the said sheet-like sealing material is, It is a sheet-like sealing material of the present invention.
- the gas barrier layer of the sealing sheet of the present invention is not particularly limited. Examples thereof include a gas barrier layer obtained by implanting ions into a layer containing an inorganic film or a polymer compound, plasma treatment, ultraviolet irradiation treatment, and the like.
- the “gas barrier layer” is a layer having a property that it is difficult for gas such as air, oxygen, and water vapor to pass therethrough.
- 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.
- 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 nitride carbides inorganic oxynitride carbides and the like.
- Examples of the raw material for the metal vapor deposition film include aluminum, magnesium, zinc, and tin. These can be used alone or in combination of two or more. Among these, an inorganic vapor-deposited film using an inorganic oxide, inorganic nitride or metal as a raw material is preferable from the viewpoint of gas barrier properties, and further, an inorganic material using an inorganic oxide or inorganic nitride as a raw material from the viewpoint of transparency. A vapor deposition film is preferred.
- a PVD (physical vapor deposition) method such as a vacuum vapor deposition method, a sputtering method, or an ion plating method, a thermal CVD (chemical vapor deposition) method, a plasma CVD method, a photo CVD method, etc.
- the CVD method is mentioned.
- polymer layer examples include polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, Examples include polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin polymer, aromatic polymer, and silicon-containing polymer compound. These polymer compounds can be used alone or in combination of two or more. Among these, a silicon-containing polymer compound is preferable from the viewpoint of forming a gas barrier layer having excellent gas barrier properties.
- a well-known thing can be used as a silicon-containing high molecular compound.
- examples thereof include polysilazane compounds, polycarbosilane compounds, polysilane compounds, and polyorganosiloxane compounds.
- a polysilazane compound is preferable.
- the polysilazane compound is a polymer compound having a repeating unit represented by (—Si—N—) in the molecule, and examples thereof include organic polysilazane, inorganic polysilazane, and modified polysilazane.
- 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.
- 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 inorganic film or 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 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. For example, there are a method of irradiating ions accelerated by an electric field (ion beam), a method of implanting ions in plasma (plasma ion implantation method), etc., and a gas barrier film can be easily obtained.
- Plasma ion implantation is preferred. Specifically, the plasma ion implantation method generates plasma in an atmosphere containing a plasma generating gas and applies a negative high-voltage pulse to an inorganic film or a polymer layer, thereby generating ions (positive ions) in the plasma. Ion) is injected into the surface of the inorganic film or polymer layer.
- the thickness of the gas barrier layer is not particularly limited. From the viewpoint of gas barrier properties and handleability, it 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. Further, the arrangement position of the gas barrier layer is not particularly limited, and may be formed directly on the sealing resin layer or may be formed through another layer.
- the sealing sheet of the present invention is a sealing sheet having a sheet-shaped sealing material composed of one or more sealing resin layers and a gas barrier film, wherein the sheet-shaped sealing material is the sheet of the present invention. What is a shape sealing material is mentioned.
- the gas barrier film is formed by forming a gas barrier layer on a base film directly or via another layer.
- the sheet-shaped sealing material is preferably laminated on the gas barrier layer side surface of the gas barrier film. .
- Base film includes polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin
- a resin film such as a polymer, an aromatic polymer, or a polyurethane polymer 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.
- the gas barrier layer may be a single layer or a plurality of layers.
- 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 temperature 40 ° C., water vapor permeability at 90% relative humidity preferably 0.1g / (m 2 ⁇ day) or less, 0.05g / (m 2 ⁇ day ) , more preferably less, 0.005 g / (M 2 ⁇ day) or less is more preferable.
- the water vapor transmission rate is 0.1 g / (m 2 ⁇ day) or less, the amount of water passing through the upper and lower surfaces of the sheet-shaped sealing material can be sufficiently reduced.
- the water vapor permeability of the gas barrier film can be measured using a known gas permeability measuring device.
- the total light transmittance of the gas barrier film is preferably 80% or more, and more preferably 85% or more.
- the sealing sheet of the present invention can be suitably used as a sealing material for an element formed on a transparent substrate that requires transparency. .
- the thickness of the gas barrier layer of the gas barrier film is not particularly limited. From the viewpoint of gas barrier properties and handleability, it 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.
- Examples of the method for producing the sealing sheet of the present invention using a gas barrier film include the following production method 1 and production method 2.
- a release sheet is prepared, and a resin composition for forming a sealing resin layer is applied onto the release-treated surface of the release sheet, and the resulting coating film is dried to form a sheet-like sealing material
- the sheet-like sealing material with a release sheet (the sheet-like sealing material of this invention with a release sheet) is obtained.
- the sealing sheet with a peeling sheet can be obtained by laminating
- the method for laminating the sheet-shaped sealing material with release sheet and the gas barrier film is not particularly limited.
- a sheet-like sealing material with a release sheet and a gas barrier film can be laminated and pressed by using a roller or the like.
- pressing it may be performed at room temperature or while heating.
- the temperature is not particularly limited, but is usually 150 ° C. or lower.
- a gas barrier film is prepared, and a resin composition for forming a sealing resin layer is applied onto the gas barrier layer of the gas barrier film by a known method, and the obtained coating film is dried to form a sheet-like sealing
- a target sealing sheet can be obtained.
- a sealing sheet in order to protect the sheet-like sealing material of the obtained sealing sheet, by laminating
- the encapsulating sheet of the present invention has a sheet-like encapsulant that is excellent in moisture barrier properties, light resistance, and colorless transparency. Therefore, as will be described later, the sheet-like encapsulant of the present invention is suitably used when encapsulating an electronic device, and particularly suitable as an encapsulant for encapsulating an organic EL element that is easily deteriorated by ultraviolet rays. Used.
- the electronic device sealing body of the present invention is obtained by sealing an electronic device with the sheet-shaped sealing material of the present invention or the sealing sheet of the present invention.
- the electronic device sealing body of the present invention is, for example, an electronic device sealing body comprising a transparent substrate, an element formed on the transparent substrate, and a sealing material for sealing the element.
- the sealing material is the sheet-like sealing material of the present invention, or a transparent substrate, an element formed on the transparent substrate, and a sealing sheet laminated so as to cover the element. What is an electronic device sealing body with which the said sealing sheet is the sealing sheet of this invention is mentioned.
- 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. There are no particular restrictions on the type, size, shape, number, etc. of the elements formed on the transparent substrate.
- 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 having a high blocking performance for blocking moisture and gas to enter from the outside of the element and having excellent 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) SnO2 (FTO), oxidation 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.
- the sheet-shaped sealing material or the sealing sheet of the present invention is placed on the electronic device, and then on the electronic device. If necessary, a method of placing a gas barrier film or the like and bonding them by thermocompression bonding can be mentioned.
- the electronic device encapsulant of the present invention is obtained by encapsulating an electronic device using the sheet-like encapsulant or the encapsulating sheet of the present invention. Therefore, the electronic device encapsulant of the present invention is less susceptible to moisture penetration and performance degradation due to ultraviolet rays. Moreover, in the electronic device sealing body which emits light, the light emitted in a state before sealing and the light whose hue is hardly changed can be emitted.
- Organic EL element of the present invention comprises a first electrode, an organic EL layer, a second electrode, a sheet-like sealing material comprising one or two or more sealing resin layers on a transparent substrate, a sealing material. It is an organic EL element which has a stop base material in this order, Comprising:
- the said sheet-like sealing material is a sheet-like sealing material of this invention, It is characterized by the above-mentioned.
- the transparent substrate As the transparent substrate, the first electrode, the organic EL layer, the second electrode, and the sealing substrate constituting the organic EL element of the present invention, conventionally known ones can be appropriately used.
- the above-described transparent substrate or gas barrier film is preferably used as the sealing substrate.
- the organic EL element of this invention can be formed using the sheet-like sealing material or sealing sheet of this invention mentioned above.
- the method for producing the organic EL element of the present invention is not particularly limited. For example, after preparing the first electrode, the organic EL layer, and the second electrode on a transparent substrate by a known method, the sheet-shaped sealing material of the present invention is placed, and a sealing substrate is formed thereon.
- the organic EL element of the present invention can be obtained by placing materials and bonding them by thermocompression bonding. Also, the organic EL element of the present invention can be obtained by laminating the sealing sheet of the present invention after preparing the first electrode, the organic EL layer, and the second electrode on the transparent substrate by a known method. Can be obtained.
- the organic EL element of the present invention uses the sheet-shaped encapsulant of the present invention, the performance of the organic EL layer is hardly deteriorated due to moisture intrusion or ultraviolet rays. In addition, light emission characteristics such as light emission luminance, light emission efficiency, and light emission uniformity are unlikely to deteriorate.
- Sealing resin (1) copolymer of isobutylene and isoprene (manufactured by Nippon Butyl Co., Exxon Butyl 268, number average molecular weight 260,000, isoprene content 1.7 mol%)
- Sealing resin (2) Maleic anhydride-modified polyolefin resin (manufactured by Mitsui Chemicals, AdmerSE731)
- Sealing resin (3) copolymer of butyl acrylate and acrylic acid (butyl acrylate 90 mol%: acrylic acid 10 mol%, weight average molecular weight 650,000)
- the number average molecular weight of sealing resin (1) and the weight average molecular weight of sealing resin (3) performed the gel permeation chromatography on the following conditions, and calculated
- Isocyanate compound (1) trimethylolpropane-modified tolylene diisocyanate (manufactured by Nippon Polyurethane Co., Ltd., Coronate L, ethyl acetate solution, solid content 75% by mass)
- Ultraviolet absorber (1) Benzotriazole ultraviolet absorber (manufactured by BASF, Tinuvin 900, maximum absorption wavelength 348 nm, absorbance 1.7)
- Gas barrier film As a base film, a polyethylene terephthalate film (manufactured by Toyobo Co., Ltd., Cosmo Shine A4100, thickness 50 ⁇ m) is used. A coating material (Clariant Japan, Aquamica NL110-20) is applied by spin coating, and the resulting coating is heated at 120 ° C. for 1 minute to form a polysilazane layer having a thickness of 150 nm and containing perhydropolysilazane. Next, argon (Ar) was ion-implanted into the surface of the polysilazane layer using a plasma ion implantation apparatus under the following conditions to form a gas barrier layer, thereby producing a gas barrier film.
- argon (Ar) was ion-implanted into the surface of the polysilazane layer using a plasma ion implantation apparatus under the following conditions to form a gas barrier layer, thereby producing a gas barrier film.
- 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
- Example 1 100 parts of the sealing resin (1) and 6 parts of the ultraviolet absorber (1) were dissolved in toluene to obtain a resin composition A having a solid content concentration of 20%.
- the resin composition A was applied onto the release-treated surface of the release sheet (1) so that the thickness after drying was 20 ⁇ m, and the obtained coating film was dried at 120 ° C. for 2 minutes to obtain a sealing resin layer Formed.
- the release sheet (2) was bonded on the release treatment surface to obtain a sheet-like sealing material with a release sheet.
- Examples 2 to 6, Comparative Examples 1 to 4 Except having changed each component, its compounding quantity, and the thickness after drying to the thing of Table 1, it carried out similarly to Example 1, and obtained the sheet-like sealing material with a peeling sheet.
- Example 7 100 parts of the sealing resin (2) and 3 parts of the ultraviolet absorber (1) were dry blended to obtain a sheet-shaped sealing material having a thickness of 40 ⁇ m by an extrusion film forming method.
- Example 8 Resin composition B was obtained in the same manner as in Example 1 except that the resin composition prepared without blending the ultraviolet absorber (1) was used. The resin composition B was applied onto the release-treated surface of the release sheet (1) so that the thickness after drying was 5 ⁇ m, and the resulting coating film was dried at 120 ° C. for 2 minutes to obtain a sealing resin layer Formed. In the following laminating process, since two sealing resin layers are used, they are represented as a sealing resin layer 1 and a sealing resin layer 3.
- a peeling sheet (1) by the method similar to Example 1 except having changed each component, its compounding quantity, and the thickness after drying to the thing of Table 3 Coating was performed so that the thickness after drying was 40 ⁇ m, and the obtained coating film was dried at 120 ° C. for 2 minutes to form a sealing resin layer 2.
- the release sheet (2) was bonded to the release treatment surface to obtain a sealing resin layer 2 with a release sheet.
- One release sheet (1) of the sealing resin layer 2 with a release sheet was peeled off to expose the sealing resin layer 2, and the exposed surface and the sealing resin layer 1 were laminated and bonded.
- the other release sheet (2) is peeled off, the sealing resin layer 2 is exposed, and the exposed surface and the sealing resin layer 3 are laminated and bonded together, whereby the sealing resin layer 1 ( A sheet-like sealing material having a three-layer structure of 5 ⁇ m thickness / sealing resin layer 2 (thickness 40 ⁇ m) / sealing resin layer 3 (thickness 5 ⁇ m) was obtained.
- Example 9 100 parts of the sealing resin (2) and 3 parts of the ultraviolet absorber (1) were dry blended. On the other hand, only sealing resin (2) is prepared, and sealing resin layer 1 (thickness 5 ⁇ m, layer consisting only of sealing resin (2)) / sealing resin layer 2 (by a multilayer extrusion film forming method) A sheet-like seal having a three-layer structure of 40 ⁇ m in thickness, a layer made of a sealing resin (2) and an ultraviolet absorber (1)) / a sealing resin layer 3 (a layer made only of a sealing resin (2) having a thickness of 5 ⁇ m) A stop was obtained.
- the sheet-like sealing material from which the release sheet was peeled was a glass plate (manufactured by NS Precision Corporation, Corning Glass Eagle XG, 150 mm ⁇ 70 mm). ⁇ 2 mm) was applied while heating to obtain a measurement sample comprising a sheet-like sealing material and a glass plate.
- the light transmittance of this sample was measured using a visible light transmittance measuring device (manufactured by Shimadzu Corporation, UV-3101PC).
- the light transmittances at 370 nm and 420 nm are shown in Tables 1 to 3.
- the sheet-like sealing material from which the release sheet was peeled (in Examples 7 and 10, the obtained sheet-like sealing material) was attached to a polyethylene terephthalate sheet, and then cut into a size of 25 mm ⁇ 300 mm. This was affixed to a glass plate (soda lime glass, manufactured by Nippon Sheet Glass Co., Ltd.) in an environment of a temperature of 23 ° C. and a relative humidity of 50%, and was subjected to pressure bonding to obtain a measurement sample. After crimping, the measurement sample was allowed to stand for 24 hours in an environment at a temperature of 23 ° C.
- the sheet-like sealing material from which the release sheet was peeled (in Examples 7 and 10, the obtained sheet-like sealing material) was sandwiched between two glass plates to obtain a measurement sample. This was placed on a polyethylene terephthalate film to obtain a laminate having a layer structure in the order of polyethylene terephthalate film / glass plate / sheet-like sealing material / glass plate. Next, using an accelerated weathering tester (Iwasaki Electric Co., Ltd., I Super UV Tester SUV-13), ultraviolet rays (illuminance: 900 W / m 2 ) from the glass plate side at a temperature of 63 ° C. and a relative humidity of 70%. For 100 hours.
- an accelerated weathering tester Iwasaki Electric Co., Ltd., I Super UV Tester SUV-13
- ultraviolet rays (illuminance: 900 W / m 2 ) from the glass plate side at a temperature of 63 ° C. and a relative humidity of 70%. For 100 hours.
- 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
- ITO indium tin oxide
- the sheet-like sealing material from which the release sheet was peeled was heated at 120 ° C. for 10 minutes using a hot plate in a nitrogen atmosphere. After drying, it was allowed to cool to room temperature.
- a sheet-like sealing material is placed so as to cover the organic EL element formed on the glass substrate, and a gas barrier film is placed thereon, and at room temperature (Examples 1 to 6, Comparative Examples 1 to 5). ) Or 100 ° C. (Examples 7 and 9) to seal the organic EL element to obtain a top emission type electronic device.
- the organic EL element is activated, and the presence or absence of dark spots (non-light emitting portions) is observed and evaluated according to the following criteria: did.
- the evaluation results are shown in Tables 1 to 3.
- the sheet-like encapsulants of Examples 1 to 9 of the present application have a water vapor transmission rate of 20 g / (m 2 ⁇ day) or less, b * is a value in the range of ⁇ 2 to 2%, and a wavelength of 370 nm.
- the light transmittance at is 1% or less, and the light transmittance at a wavelength of 420 nm is 85% or more. Therefore, it is excellent in all of moisture barrier properties, light resistance, and colorless transparency. Moreover, it has sufficient adhesive force and is excellent in light resistance and durability of an organic EL element.
- the sheet-like sealing materials of Comparative Examples 1 and 2 are inferior in light resistance.
- the amount of the ultraviolet absorber was too large to disperse, and a film could not be formed.
- the sheet-like sealing material of Comparative Example 4 has a large b * and is strongly yellowish.
- the sheet-like sealing material of Comparative Example 5 is inferior in durability of the organic EL element.
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。
有機EL素子の発光特性が低下する原因としては、酸素や水分等が有機EL素子の内部に浸入し、電極や有機層を劣化させることが考えられる。そして、この問題を解決すべく、封止材を用いる方法がいくつか提案されている。
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材料として、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。
また、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。
(1)1又は2以上の封止樹脂層からなるシート状封止材であって、前記シート状封止材の、温度40℃、相対湿度90%における、50μm厚に換算したときの水蒸気透過率が、20g/(m2・day)以下であり、前記シート状封止材の、JIS Z 8729-1994に規定されるCIE L*a*b*表色系におけるb*値が、-2~2%であり、かつ、前記シート状封止材の、波長370nmにおける光線透過率が1%以下、波長420nmにおける光線透過率が85%以上であることを特徴とする、シート状封止材。
(2)前記シート状封止材の厚みが、0.1~100μmである、(1)に記載のシート状封止材。
(3)前記シート状封止材の、温度23℃、相対湿度50%の環境下での、ガラスに対する接着力が、3N/25mm以上である、(1)に記載のシート状封止材。
(4)前記封止樹脂層は、ゴム系ポリマー、(メタ)アクリル系ポリマー、ポリオレフィン系ポリマー、ポリエステル系ポリマー、スチレン系熱可塑性エラストマー及びシリコーン系ポリマーからなる群から選ばれる少なくとも1種を含む封止樹脂を含有する層である、(1)に記載のシート状封止材。
(5)前記封止樹脂層の少なくとも1層が、紫外線吸収剤を含有するものである、(1)に記載のシート状封止材。
(6)前記紫外線吸収剤が、330~370nmの範囲内に最大吸収波長を有するものである、(5)に記載のシート状封止材。
(7)電子デバイスの封止に用いられる、(1)に記載のシート状封止材。
(8)1又は2以上の封止樹脂層からなるシート状封止材とガスバリア層とを有する封止シートであって、前記シート状封止材が、(1)に記載のシート状封止材であることを特徴とする封止シート。
(9)前記シート状封止材と、基材フィルム上に、直接又はその他の層を介して、前記ガスバリア層が形成されてなるガスバリアフィルムとを有するものである、前記(8)に記載の封止シート。
(10)電子デバイスの封止に用いられる、(8)に記載の封止シート。
(11)前記(1)に記載のシート状封止材、又は前記(8)に記載の封止シートによって、電子デバイスが封止されてなる電子デバイス封止体。
(12)透明基板上に、第1の電極、有機EL層、第2の電極、1又は2以上の封止樹脂層からなるシート状封止材、封止基材をこの順で有する有機EL素子であって、前記シート状封止材が、(1)に記載のシート状封止材であることを特徴とする有機EL素子。
本発明のシート状封止材は、1又は2以上の封止樹脂層からなるシート状封止材であって、前記シート状封止材の、温度40℃、相対湿度90%における、50μm厚に換算したときの水蒸気透過率が、20g/(m2・day)以下であり、前記シート状封止材の、JIS Z 8729-1994に規定されるCIE L*a*b*表色系におけるb*値が、-2~2%であり、かつ、前記シート状封止材の、波長370nmにおける光線透過率が1%以下、波長420nmにおける光線透過率が85%以上であることを特徴とするものである。
この水蒸気透過率が、このような範囲にあることで、水分の浸入を十分に抑制することができる。このようなシート状封止材は、電子デバイス用の封止材として好適に用いられる。
水蒸気透過率は、実施例に記載の方法により測定することができる。
b*値は、色を数値化したときの、黄みと青みの程度を表すものである。b*値が正の値であれば、黄みを帯びていることを、負の値であれば、青みを帯びていることを表す。
b*値が上記範囲にあることで、そのシート状封止材はより無色に近いものとなる。このようなシート状封止材は、発光デバイスの封止材として好適に用いられる。
具体的には、後述するように、波長420nmにおける光線透過率を指標として、用いる紫外線吸収剤を選択し、さらに、含有量、シート状封止材の厚み等を適宜決定することで、b*値を制御することができる。
a*値は、色を数値化したときの、赤みと緑みの程度を表すものであり、a*値が正の値であれば、赤みを帯びていることを、負の値であれば、緑みを帯びていることを表す。
a*値が上記範囲にあることで、そのシート状封止材はより無色に近いものとなる。このようなシート状封止材は、発光デバイスの封止材として好適に用いられる。
a*値は、用いる封止樹脂やその他の成分を適宜選択することで、制御することができる。
JIS Z 8729-1994に規定されるCIE L*a*b*表色系におけるb*値やa*値は、実施例に記載の方法により測定することができる。
波長420nmにおける光線透過率は、例えば、紫外線吸収剤等の可視光を吸収する恐れのある添加剤を用いる場合、その含有量やシート状封止材の厚みを適宜決定することで、85%以上に制御することができる。
シート状封止材の厚みが上記範囲内であることで、水分遮断性、耐光性及び無色透明性のバランスが取れた封止材が得られ易くなる。
このようなシート状封止材であれば、封止したときに、被封止体との界面から水分等が浸入することを十分に防ぐことができる。
封止樹脂は、本発明の効果が得られるものである限り、特に限定されない。
封止樹脂としては、ゴム系ポリマー、(メタ)アクリル系ポリマー、ポリオレフィン系ポリマー、ポリエステル系ポリマー、シリコーン系ポリマー、スチレン系熱可塑性エラストマー、等が挙げられる。
イソブチレン系重合体は、主鎖及び/又は側鎖に、イソブチレン由来の繰り返し単位を有する重合体をいう。イソブチレン由来の繰り返し単位の量は、50質量%以上が好ましく、60質量%以上がより好ましく、70~99質量%がさらに好ましい。
イソブチレン系重合体としては、イソブチレンの単独重合体(ポリイソブチレン)、イソブチレンとイソプレンの共重合体(ブチルゴム)、イソブチレンとn-ブテンの共重合体、イソブチレンとブタジエンの共重合体、及びこれら重合体を臭素化又は塩素化して得られるハロゲン化重合体等のイソブチレン系重合体、等が挙げられる。これらの中でも、イソブチレンとイソプレンの共重合体(ブチルゴム)が好ましい。
(メタ)アクリル系ポリマーにおける(メタ)アクリル系モノマー由来の繰り返し単位の量は、50質量%以上が好ましく、60質量%以上がより好ましく、70~99質量%がさらに好ましい。
(メタ)アクリル系モノマーとしては、(メタ)アクリル酸、(メタ)アクリル酸メチル、(メタ)アクリル酸エチル、(メタ)アクリル酸プロピル、(メタ)アクリル酸ブチル等のアルキル基の炭素数が1から20の(メタ)アクリル酸エステル、(メタ)アクリル酸2-エチルヘキシル、(メタ)アクリル酸ヒドロキシメチル等の反応性官能基を有する(メタ)アクリル酸エステルが挙げられる。
オレフィン系モノマーとしては、エチレン;プロピレン、1-ブテン、4-メチル-1-ペンテン、3-メチル-1-ブテン、1-ヘキセン、1-オクテン等の炭素数3~20のα-オレフィン;シクロブテン、テトラシクロドデセン、ノルボルネン等の炭素数4~20の環状オレフィン;又はこれらを変性したもの等が挙げられる。
多価カルボン酸としては、テレフタル酸、イソフタル酸、オルソフタル酸、コハク酸、アジピン酸、セバシン酸、シクロヘキサンジカルボン酸、トリメリット酸等が挙げられる。ポリオールとしては、エチレングリコール、プロピレングリコール等の脂肪族アルコールや、ポリエチレングリコール、ポリプロピレングリコール等のポリエーテルポリオールが挙げられる。
シリコーン系ポリマーとしては、ジメチルポリシロキサン、メチルフェニルポリシロキサン、メチルハイドロジェンポリシロキサン等が挙げられる。
これらの中でも、水蒸気透過率が低いシート状封止材が得られ易いことから、封止樹脂としては、ゴム系ポリマー又はポリオレフィン系ポリマーが好ましい。
封止樹脂の数平均分子量(Mn)が上記範囲内であることで、水蒸気透過率が低いシート状封止材が得られ易くなる。
封止樹脂の数平均分子量(Mn)は、テトラヒドロフランを溶媒として用いて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。
封止樹脂層中に架橋構造を形成する際は、接着剤等における公知の架橋構造形成方法を利用することができる。
イソシアネート系架橋剤としては、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、トリレンジイソシアネート、ジフェニルメタンジイソシアネート、キシリレンジイソシアネート等の芳香族ポリイソシアネート;ヘキサメチレンジイソシアネート等の脂肪族ポリイソシアネート;イソホロンジイソシアネート、水素添加ジフェニルメタンジイソシアネート等の脂環式ポリイソシアネート;これらの化合物のビウレット体、イソシアヌレート体、さらにはエチレングリコール、プロピレングリコール、ネオペンチルグリコール、トリメチロールプロパン、ヒマシ油等の低分子活性水素含有化合物との反応物であるアダクト体;等が挙げられる。
エポキシ系架橋剤としては、1,3-ビス(N,N’-ジグリシジジルアミノメチル)シクロヘキサン、N,N,N’,N’-テトラグリシジル-m-キシリレンジアミン、エチレングリコールジグリシジルエーテル、1,6-ヘキサンジオールジグリシジルエーテル、トリメチロールプロパンジグリシジルエーテル、ジグリシジルアニリン、ジグリシジルアミン等が挙げられる。
アジリジン系架橋剤はとしては、ジフェニルメタン-4,4’-ビス(1-アジリジンカーボキサミド)、トリメチロールプロパントリ-β-アジリジニルプロピオネート、テトラメチロールメタントリ-β-アジリジニルプロピオネート、トルエン-2,4-ビス(1-アジリジンカーボキサミド)、トリエチレンメラミン、ビスイソフタロイル-1-(2-メチルアジリジン)、トリス-1-(2-メチルアジリジン)フォスフィン、トリメチロールプロパントリ-β-(2-メチルアジリジン)プロピオネート等が挙げられる。
アルミニウムキレート化合物としては、ジイソプロポキシアルミニウムモノオレイルアセトアセテート、モノイソプロポキシアルミニウムビスオレイルアセトアセテート、モノイソプロポキシアルミニウムモノオレエートモノエチルアセトアセテート、ジイソプロポキシアルミニウムモノラウリルアセトアセテート、ジイソプロポキシアルミニウムモノステアリルアセトアセテート、ジイソプロポキシアルミニウムモノイソステアリルアセトアセテート等が挙げられる。
これらの架橋剤を用いて架橋構造を形成する場合、その使用量は、架橋剤の架橋性基(金属キレート系架橋剤の場合は、金属キレート系架橋剤)が、封止樹脂の水酸基及びカルボキシル基に対して、0.1~5当量となる量が好ましく、0.2~3当量となる量がより好ましい。
これらの重合開始剤を用いて架橋構造を形成する場合、その使用量は、封止樹脂100質量部に対して、0.1~100質量部が好ましく、1~100質量部がより好ましい。
紫外線吸収剤の最大吸収波長や、吸光係数を考慮して、その含有量やシート状封止材の厚みを適宜決定することで、シート状封止材の波長370nmにおける光線透過率を1%以下に制御し易くなる。
紫外線吸収剤の最大吸収波長(λmax)が330nm未満の場合は、波長370nmにおける光線透過率が1%以下に制御することが困難となるおそれがある。一方、紫外線吸収剤の最大吸収波長(λmax)が370nmを超えると、波長420nmにおける光線透過率が85%以上であるシート状封止材が得られ難くなるおそれがある。
紫外線吸収剤は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。
封止樹脂層に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シート状封止材が得られ易くなる。
粘着付与剤は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。
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、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。
封止樹脂層がその他の成分を含有する場合、その含有量は、それぞれ、封止樹脂層全体に対して、0.01~5質量%が好ましく、0.01~2質量%がより好ましい。
本発明のシート状封止材が、2以上の封止樹脂層からなるものである場合、そのようなシート状封止材としては、同じ封止樹脂層を2層以上積層させたものであってもよく、異なる封止樹脂層を2層以上積層させたものであってもよい。
異なる封止樹脂層としては、封止樹脂が異なる層、封止樹脂以外の成分や、その含有量が異なる層等が挙げられる。
また、封止樹脂層中に紫外線吸収剤を過剰に含有させると、接着力が低下することがある。このような場合、シート状封止材を、2以上の封止樹脂層からなる積層体にすることで、接着性の低下を抑制することができる。例えば、両最外層と中間層からなる3層構造のシート状封止材において、中間層のみに紫外線吸収剤を含有させることで、紫外線吸収剤の添加による接着性の低下を防ぐことができる。
上記のように、封止樹脂層を2層以上積層することで、接着性を低下させることなく、水分遮断性、耐光性及び無色透明性のすべてに優れるシート状封止材を効率よく得ることができる。
剥離シート用の基材としては、グラシン紙、コート紙、上質紙等の紙基材;これらの紙基材にポリエチレン等の熱可塑性樹脂をラミネートしたラミネート紙;ポリエチレンテレフタレート樹脂、ポリブチレンテレフタレート樹脂、ポリエチレンナフタレート樹脂、ポリプロピレン樹脂、ポリエチレン樹脂等のプラスチックフィルム;等が挙げられる。
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。
本発明のシート状封止材を、キャスト法により製造する場合、例えば、封止樹脂等の所定の成分を含有する樹脂組成物を調製し、この樹脂組成物を、公知の方法により、剥離シートの剥離処理面に塗工し、得られた塗膜を乾燥することで、剥離シート付封止樹脂層(剥離シート付の本発明のシート状封止材)を形成することができる。
溶媒としては、ベンゼン、トルエン等の芳香族炭化水素系溶媒;酢酸エチル、酢酸ブチル等のエステル系溶媒;アセトン、メチルエチルケトン、メチルイソブチルケトン等のケトン系溶媒;n-ペンタン、n-ヘキサン、n-ヘプタン等の脂肪族炭化水素系溶媒;シクロペンタン、シクロヘキサン等の脂環式炭化水素系溶媒;等が挙げられる。
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。
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、封止樹脂層を養生させてもよい。封止樹脂層を養生させることで、架橋構造を十分に形成することができる。
また、2以上の封止樹脂層からなるシート状封止材は、複数の封止樹脂層を形成し、これを、その封止樹脂層同士が対向するように積層させることで、得ることができる。
また、封止樹脂層の形成後に、その封止樹脂層上に樹脂組成物を塗工し、得られた塗膜を乾燥する方法によっても、2以上の封止樹脂層からなるシート状封止材を得ることができる。
このとき、多層押出製膜法により製膜することで、2以上の封止樹脂層からなシート状封止材を得ることができる。
本発明のシート状封止材を、多層押出製膜法により製造する場合は、共押出多層フィルムを製造する際に用いられる公知の方法を利用することができる。
本発明の封止シートは、1又は2以上の封止樹脂層からなるシート状封止材とガスバリア層とを有する封止シートであって、前記シート状封止材が、本発明のシート状封止材であるものである。
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。
これらは1種単独で、あるいは2種以上を組み合わせて用いることができる。
これらの中では、ガスバリア性の観点から、無機酸化物、無機窒化物又は金属を原料とする無機蒸着膜が好ましく、さらに、透明性の観点から、無機酸化物又は無機窒化物を原料とする無機蒸着膜が好ましい。
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い。ケイ素含有高分子化合物としては、公知のものを用いることができる。例えば、ポリシラザン化合物、ポリカルボシラン化合物、ポリシラン化合物、及びポリオルガノシロキサン化合物等が挙げられる。これらの中でも、ポリシラザン化合物が好ましい。
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。
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。
また、ガスバリア層の配置位置は特に限定されず、封止樹脂層上に直接形成されていてもよいし、その他の層を介して形成されていてもよい。
ガスバリアフィルムは、基材フィルム上に、直接又はその他の層を介して、ガスバリア層が形成されてなるものである。
1又は2以上の封止樹脂層からなるシート状封止材とガスバリアフィルムとを有する封止シートにおいては、ガスバリアフィルムのガスバリア層側の面にシート状封止材が積層されていることが好ましい。
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。
ガスバリア層は、単層であっても、複数層であってもよい。
水蒸気透過率が0.1g/(m2・day)以下であることで、シート状封止材の上下面を通過する水分量を十分に低下させることができる。
ガスバリアフィルムの水蒸気の透過率は、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。
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、本発明の封止シートを、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好適に用いることができる。
先ず、剥離シートを用意し、該剥離シートの剥離処理面上に、封止樹脂層形成用の樹脂組成物を塗工し、得られた塗膜を乾燥して、シート状封止材を形成することで、剥離シート付シート状封止材(剥離シート付の、本発明のシート状封止材)を得る。次いで、得られた剥離シート付シート状封止材とガスバリアフィルムを積層することで、剥離シート付の封止シートを得ることができる。
剥離シート付シート状封止材とガスバリアフィルムの積層方法は特に限定されない。例えば、剥離シート付シート状封止材とガスバリアフィルムとを重ね合わせ、ローラー等を用いて押圧することでこれらを積層することができる。押圧する際は、室温で行ってもよいし、加熱しながら行ってもよい。加熱しながら押圧する場合、温度は特に限定されないが、通常、150℃以下である。
先ず、ガスバリアフィルムを用意し、このガスバリアフィルムのガスバリア層上に、封止樹脂層形成用の樹脂組成物を公知の方法により塗工し、得られた塗膜を乾燥して、シート状封止材を形成することで、目的とする封止シートを得ることができる。また、封止シートを形成した後、得られた封止シートのシート状封止材を保護するために、該シート状封止材上に剥離シートを積層することにより、剥離シート付の封止シートを得ることができる。
また、本発明のシート状封止材の製造方法で示したものと同様の方法により、複数の封止樹脂層を有するシート状封止材を形成してもよい。
本発明の電子デバイス封止体は、本発明のシート状封止材、又は、本発明の封止シートによって、電子デバイスが封止されてなるものである。
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、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)等が挙げられる。
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。
本発明の有機EL素子は、透明基板上に、第1の電極、有機EL層、第2の電極、1又は2以上の封止樹脂層からなるシート状封止材、封止基材をこの順で有する有機EL素子であって、前記シート状封止材が本発明のシート状封止材であることを特徴とするものである。
本発明の有機EL素子は、前述した本発明のシート状封止材又は封止シートを用いて形成することができる。
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。
封止樹脂(1):イソブチレンとイソプレンの共重合体(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%)
封止樹脂(2):無水マレイン酸変性ポリオレフィン樹脂(三井化学社製、AdmerSE731)
封止樹脂(3):アクリル酸ブチルとアクリル酸の共重合体(アクリル酸ブチル90モル%:アクリル酸10モル%、重量平均分子量650,000)
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
紫外線吸収剤(1):ベンゾトリアゾール系紫外線吸収剤(BASF社製、Tinuvin900、最大吸収波長348nm、吸光度1.7)
紫外線吸収剤(2):ベンゾトリアゾール系紫外線吸収剤(BASF社製、Tinuvin326、最大吸収波長355nm、吸光度2.1)
紫外線吸収剤(3):ベンゾトリアゾール系紫外線吸収剤(BASF社製、Tinuvin460、最大吸収波長349nm、吸光度4.1)
紫外線吸収剤(4):ベンゾトリアゾール系紫外線吸収剤(BASF社製、Tinuvin CarboProtect、最大吸収波長378nm、吸光度1.2)
剥離シート(1):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)
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)
なお、上記の吸光度は、紫外線吸収剤を封止樹脂に対して2%添加し、膜厚20μmとした際の最大吸光度である。このとき、ブランクとして、紫外線吸収剤未添加の樹脂を使用した。
基材フィルムとして、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)を用い、この基材フィルム上に、ポリシラザン化合物(ペルヒドロポリシラザンを主成分とするコーティング材(クラリアントジャパン社製、アクアミカNL110-20)をスピンコート法により塗布し、得られた塗膜を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
封止樹脂(1)100部、紫外線吸収剤(1)6部をトルエンに溶解し、固形分濃度20%の樹脂組成物Aを得た。
樹脂組成物Aを、剥離シート(1)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、封止樹脂層を形成した。次いで、剥離シート(2)を、その剥離処理面で貼り合せて、剥離シート付シート状封止材を得た。
各成分とその配合量及び乾燥後の厚みを、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、剥離シート付シート状封止材を得た。
封止樹脂(2)100部、紫外線吸収剤(1)3部をドライブレンドし、押出製膜法にて厚み40μmのシート状封止材を得た。
封止樹脂(3)100部に、イソシアネート化合物(1)1.5部、及び紫外線吸収材(1)3部を添加し、トルエンを加えることで、固形分濃度20%の樹脂組成物を得た。この樹脂組成物を用いたことを除き、実施例1と同様にして、剥離シート付シート状封止材を得た。
紫外線吸収剤(1)を配合しないで調製した樹脂組成物を用いたことを除き、実施例1と同様にして、樹脂組成物Bを得た。
樹脂組成物Bを、剥離シート(1)の剥離処理面上に、乾燥後の厚みが5μmになるように塗工し、得られた塗膜を120℃で2分間乾燥し、封止樹脂層を形成した。なお、以下の積層工程においては、この封止樹脂層を2枚用いるため、これらを封止樹脂層1、封止樹脂層3と表す。
また、各成分とその配合量及び乾燥後の厚みを、第3表に記載のものに変更したことを除き、実施例1と同様の方法により、剥離シート(1)の剥離処理面上に、乾燥後の厚みが40μmになるように塗工し、得られた塗膜を120℃で2分間乾燥し、封止樹脂層2を形成した。次いで、剥離シート(2)を、その剥離処理面で貼り合せて、剥離シート付封止樹脂層2を得た。
剥離シート付封止樹脂層2の一方の剥離シート(1)を剥離し、封止樹脂層2を露出させ、この露出面と、封止樹脂層1を重ねて貼合した。次いで、もう一枚の剥離シート(2)を剥離し、封止樹脂層2を露出させ、この露出面と、封止樹脂層3とを重ねて貼合することで、封止樹脂層1(厚み5μm)/封止樹脂層2(厚み40μm)/封止樹脂層3(厚み5μm)、の3層構造のシート状封止材を得た。
封止樹脂(2)100部、紫外線吸収剤(1)3部をドライブレンドした。その一方で、封止樹脂(2)のみを用意し、多層押出製膜法にて、封止樹脂層1(厚み5μm、封止樹脂(2)のみからなる層)/封止樹脂層2(厚み40μm、封止樹脂(2)及び紫外線吸収剤(1)からなる層)/封止樹脂層3(厚み5μm、封止樹脂(2)のみからなる層)、の3層構造のシート状封止材を得た。
(水蒸気透過率測定)
剥離シートを剥離したシート状封止材(実施例7、9においては、得られたシート状封止材)を2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)で挟むことで、水蒸気透過率測定用のサンプルを得た。次いで、水蒸気透過率測定装置(LYSSY社製、L80-5000)を用いて、温度40℃、相対湿度90%における、封止材の水蒸気透過率を測定した。
測定結果に対して、下記の計算を行い、厚みが50μmのときの水蒸気透過率を算出した。得られた、厚みが50μmのときの水蒸気透過率を第1表~第3表に示す。
剥離シートを剥離したシート状封止材(実施例7、9においては、得られたシート状封止材)をガラス板(エヌ・エス・ジー・プレシジョン社製、コーニングガラスイーグルXG、150mm×70mm×2mm)に加熱しながら貼付し、シート状封止材とガラス板からなる測定用サンプルを得た。
このサンプルの光線透過率を、可視光透過率測定装置(島津製作所社製、UV-3101PC)を用いて測定した。
370nm及び420nmにおける光線透過率を第1表~第3表に示す。
可視光透過率の測定用サンプルの作製法と同様の方法により、測定用サンプルを得た。
このサンプルの、CIE1976L*a*b*表色系により規定される色彩値b*を、JIS Z 8729-1994に準拠し、分光光度計(島津製作所社製、MPC3100)を用いて測定した。
測定結果を第1表~第3表に示す。
剥離シートを剥離したシート状封止材(実施例7、10においては、得られたシート状封止材)をポリエチレンテレフタレートシートに貼付し、次いで、これを25mm×300mmの大きさに裁断した。このものを、温度23℃、相対湿度50%の環境下で、ガラス板(ソーダライムガラス、日本板硝子社製)に加熱しながら貼付し、圧着して測定用サンプルを得た。
圧着後、測定用サンプルを、温度23℃、相対湿度50%の環境下に24時間静置した後、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、接着力(N/25mm)を測定した。
測定結果を第1表~第3表に示す。
剥離シートを剥離したシート状封止材(実施例7、10においては、得られたシート状封止材)を、2枚のガラス板で挟み、測定用サンプルを得た。このものを、ポリエチレンテレフタレートフィルム上に載置し、ポリエチレンテレフタレートフィルム/ガラス板/シート状封止材/ガラス板、の順の層構造を有する積層体とした。
次いで、促進耐候性試験機(岩崎電気社製、アイ スーパーUVテスター SUV-13)を用いて、温度63℃、相対湿度70%の条件で、ガラス板側から、紫外線(照度900W/m2)を100時間照射した。
紫外線照射後に、上記の色相評価における測定と同様の測定により、ポリエチレンテレフタレートの色彩値b*を測定し、以下の基準により耐候性を評価した。評価結果を第1表~第3表に示す。
○:b*が2未満
×:b*が2以上
ガラス基板を溶媒で洗浄し、次いでUV/オゾン処理を行った後、その表面に、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。
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て陽極を作製し、有機EL素子を得た。なお、蒸着時の真空度は、全て1×10-4Pa以下である。
次いで、ガラス基板上に形成された有機EL素子を覆うように、シート状封止材を載置し、その上にガスバリアフィルムを載置し、常温(実施例1~6、比較例1~5)、又は100℃(実施例7,9)で圧着して、有機EL素子を封止し、トップエミッション型の電子デバイスを得た。
次いで、有機EL素子を、温度23℃、相対湿度50%の環境下で50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。評価結果を第1表~第3表に示す。
○:ダークスポットが発光面積の10%未満
×:ダークスポットが発光面積の10%以上
本願実施例1~9のシート状封止材は、水蒸気透過率が、20g/(m2・day)以下であり、b*が-2~2%の範囲の値であり、かつ、波長370nmにおける光線透過率が1%以下、波長420nmにおける光線透過率が85%以上の値である。したがって、水分遮断性、耐光性及び無色透明性のすべてに優れる。また、十分な接着力を有し、耐光性、有機EL素子の耐久性にも優れている。
一方、比較例1,2のシート状封止材は、耐光性に劣っている。
比較例3のシート状封止材は、紫外線吸収剤の量が多すぎて分散ができず、膜を形成することができなかった。
比較例4のシート状封止材は、b*が大きな値であり、黄色味を強く帯びている。
比較例5のシート状封止材は、有機EL素子の耐久性に劣っている。
Claims (12)
- 1又は2以上の封止樹脂層からなるシート状封止材であって、
前記シート状封止材の、温度40℃、相対湿度90%における、50μm厚に換算したときの水蒸気透過率が、20g/(m2・day)以下であり、
前記シート状封止材の、JIS Z 8729-1994に規定されるCIE L*a*b*表色系におけるb*値が、-2~2%であり、かつ、
前記シート状封止材の、波長370nmにおける光線透過率が1%以下、波長420nmにおける光線透過率が85%以上であることを特徴とする、シート状封止材。 - 前記シート状封止材の厚みが、0.1~100μmである、請求項1に記載のシート状封止材。
- 前記シート状封止材の、温度23℃、相対湿度50%の環境下での、ガラスに対する接着力が、3N/25mm以上である、請求項1に記載のシート状封止材。
- 前記封止樹脂層は、ゴム系ポリマー、(メタ)アクリル系ポリマー、ポリオレフィン系ポリマー、ポリエステル系ポリマー、スチレン系熱可塑性エラストマー及びシリコーン系ポリマーからなる群から選ばれる少なくとも1種を含む封止樹脂を含有する層である、請求項1に記載のシート状封止材。
- 前記封止樹脂層の少なくとも1層が、紫外線吸収剤を含有するものである、請求項1に記載のシート状封止材。
- 前記紫外線吸収剤が、330~370nmの範囲内に最大吸収波長を有するものである、請求項5に記載のシート状封止材。
- 電子デバイスの封止に用いられる、請求項1に記載のシート状封止材。
- 1又は2以上の封止樹脂層からなるシート状封止材とガスバリア層とを有する封止シートであって、
前記シート状封止材が、請求項1に記載のシート状封止材であることを特徴とする封止シート。 - 前記シート状封止材と、基材フィルム上に、直接又はその他の層を介して、前記ガスバリア層が形成されてなるガスバリアフィルムとを有するものである、請求項8に記載の封止シート。
- 電子デバイスの封止に用いられる、請求項8に記載の封止シート。
- 請求項1に記載のシート状封止材、又は請求項8に記載の封止シートによって、電子デバイスが封止されてなる電子デバイス封止体。
- 透明基板上に、第1の電極、有機EL層、第2の電極、1又は2以上の封止樹脂層からなるシート状封止材、封止基材をこの順で有する有機EL素子であって、
前記シート状封止材が、請求項1に記載のシート状封止材であることを特徴とする有機EL素子。
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JP2015554779A JP6480346B2 (ja) | 2013-12-26 | 2014-12-17 | シート状封止材、封止シート、電子デバイス封止体および有機el素子 |
CN201480070950.XA CN105849220B (zh) | 2013-12-26 | 2014-12-17 | 片状密封材料、密封片材、电子器件密封体和有机el元件 |
EP14873776.0A EP3088485B1 (en) | 2013-12-26 | 2014-12-17 | Sheet-like sealing material, sealing sheet, electronic-device sealing body, and organic electroluminescent element |
US15/108,035 US20160329522A1 (en) | 2013-12-26 | 2014-12-17 | Sheet-like sealing material, sealing sheet, electronic-device sealing body, and organic electroluminescent element |
KR1020167016991A KR20160102437A (ko) | 2013-12-26 | 2014-12-17 | 시트상 봉지재, 봉지 시트, 전자 디바이스 봉지체 및 유기 el 소자 |
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US (1) | US20160329522A1 (ja) |
EP (1) | EP3088485B1 (ja) |
JP (1) | JP6480346B2 (ja) |
KR (1) | KR20160102437A (ja) |
CN (1) | CN105849220B (ja) |
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JP2019029355A (ja) * | 2017-08-02 | 2019-02-21 | 積水化学工業株式会社 | 有機el表示素子用封止剤 |
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KR20200047521A (ko) | 2017-09-01 | 2020-05-07 | 가부시끼가이샤 쓰리본드 | 광경화성 조성물 |
US11739168B2 (en) | 2017-09-01 | 2023-08-29 | Threebond Co., Ltd. | Photocurable composition |
JP7161864B2 (ja) | 2018-04-23 | 2022-10-27 | 信越ポリマー株式会社 | 表面保護基材付き封止材 |
JP2019190078A (ja) * | 2018-04-23 | 2019-10-31 | 信越ポリマー株式会社 | 表面保護基材付き封止材 |
JP2022103204A (ja) * | 2018-05-24 | 2022-07-07 | 大日本印刷株式会社 | 自発光型表示体 |
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US11851509B2 (en) | 2018-05-30 | 2023-12-26 | Threebond Co., Ltd. | Photocurable composition and cured material thereof |
JP2020035743A (ja) * | 2018-08-30 | 2020-03-05 | 三星エスディアイ株式会社Samsung SDI Co., Ltd. | 有機発光素子封止用組成物及びこれから製造された有機層を含む有機発光素子表示装置 |
JP7475119B2 (ja) | 2018-08-30 | 2024-04-26 | 三星エスディアイ株式会社 | 有機発光素子封止用組成物及びこれから製造された有機層を含む有機発光素子表示装置 |
JP2020049706A (ja) * | 2018-09-25 | 2020-04-02 | 大日本印刷株式会社 | 自発光型表示体用の離型フィルム一体型封止材 |
JP7139833B2 (ja) | 2018-09-25 | 2022-09-21 | 大日本印刷株式会社 | 自発光型表示体用の離型フィルム一体型封止材 |
JP7139833B6 (ja) | 2018-09-25 | 2024-02-02 | 大日本印刷株式会社 | 自発光型表示体用の離型フィルム一体型封止材 |
JP2020064889A (ja) * | 2018-10-15 | 2020-04-23 | 東洋インキScホールディングス株式会社 | 配線シート |
Also Published As
Publication number | Publication date |
---|---|
CN105849220B (zh) | 2018-04-10 |
JPWO2015098647A1 (ja) | 2017-03-23 |
EP3088485A4 (en) | 2017-09-06 |
US20160329522A1 (en) | 2016-11-10 |
JP6480346B2 (ja) | 2019-03-06 |
TW201526335A (zh) | 2015-07-01 |
KR20160102437A (ko) | 2016-08-30 |
CN105849220A (zh) | 2016-08-10 |
EP3088485B1 (en) | 2020-08-12 |
TWI648892B (zh) | 2019-01-21 |
EP3088485A1 (en) | 2016-11-02 |
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