WO2016152756A1 - 封止体の製造方法 - Google Patents
封止体の製造方法 Download PDFInfo
- Publication number
- WO2016152756A1 WO2016152756A1 PCT/JP2016/058641 JP2016058641W WO2016152756A1 WO 2016152756 A1 WO2016152756 A1 WO 2016152756A1 JP 2016058641 W JP2016058641 W JP 2016058641W WO 2016152756 A1 WO2016152756 A1 WO 2016152756A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sealing
- sealing sheet
- resin composition
- infrared
- composition layer
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007789 sealing Methods 0.000 claims abstract description 237
- 239000011342 resin composition Substances 0.000 claims abstract description 102
- 239000013039 cover film Substances 0.000 claims abstract description 70
- 238000001035 drying Methods 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 238000010030 laminating Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 4
- 239000010408 film Substances 0.000 description 50
- 239000011575 calcium Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 20
- 230000004888 barrier function Effects 0.000 description 19
- 239000011521 glass Substances 0.000 description 19
- 229920000139 polyethylene terephthalate Polymers 0.000 description 19
- 239000005020 polyethylene terephthalate Substances 0.000 description 19
- -1 polyethylene terephthalate Polymers 0.000 description 18
- 239000002985 plastic film Substances 0.000 description 17
- 229920006255 plastic film Polymers 0.000 description 17
- 229920001187 thermosetting polymer Polymers 0.000 description 17
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 15
- 239000011261 inert gas Substances 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 13
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 238000003475 lamination Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 229920002799 BoPET Polymers 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000004711 α-olefin Substances 0.000 description 8
- 230000002411 adverse Effects 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 7
- 239000011888 foil Substances 0.000 description 7
- 238000002161 passivation Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 239000011112 polyethylene naphthalate Substances 0.000 description 6
- 229920001155 polypropylene Polymers 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 6
- 229910052721 tungsten Inorganic materials 0.000 description 6
- 239000010937 tungsten Substances 0.000 description 6
- 239000002966 varnish Substances 0.000 description 6
- 239000004642 Polyimide Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000006866 deterioration Effects 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 229920001721 polyimide Polymers 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 4
- 229920005672 polyolefin resin Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 229920002367 Polyisobutene Polymers 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 235000010724 Wisteria floribunda Nutrition 0.000 description 3
- 229920000180 alkyd Polymers 0.000 description 3
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 229960001545 hydrotalcite Drugs 0.000 description 3
- 229910001701 hydrotalcite Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920001083 polybutene Polymers 0.000 description 3
- 229920000515 polycarbonate Polymers 0.000 description 3
- 239000004417 polycarbonate Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- XUZIWKKCMYHORT-UHFFFAOYSA-N 2,4,6-tris(diaminomethyl)phenol Chemical compound NC(N)C1=CC(C(N)N)=C(O)C(C(N)N)=C1 XUZIWKKCMYHORT-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000010539 anionic addition polymerization reaction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 238000003851 corona treatment Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 229910000953 kanthal Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920006287 phenoxy resin Polymers 0.000 description 2
- 239000013034 phenoxy resin Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920006290 polyethylene naphthalate film Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 229920005604 random copolymer Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- AKSROGHADDORBX-UHFFFAOYSA-M 2-acetamidoacetate;tetrabutylphosphanium Chemical compound CC(=O)NCC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC AKSROGHADDORBX-UHFFFAOYSA-M 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000013032 Hydrocarbon resin Substances 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- 229920002402 Oppanol® B 100 Polymers 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910004541 SiN Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000705989 Tetrax Species 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000005443 coulometric titration Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229920006270 hydrocarbon resin Polymers 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
-
- 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
- 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
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
Definitions
- the present invention relates to a method for producing a sealed body (in particular, an organic EL device) in which an organic EL (electroluminescence) element on a substrate is sealed with a resin composition layer.
- the present invention also relates to a method for sealing an organic EL element on a substrate.
- An organic EL element is a light emitting element using an organic substance as a light emitting material, and has recently attracted attention because it can emit light with high luminance at a low voltage.
- the organic EL element is very weak against moisture, and there are problems that the luminance is lowered, the light is not emitted, the interface between the electrode and the light emitting layer is peeled off, the metal is oxidized and the resistance is increased. For this reason, in order to shield the inside of the device from moisture in the outside air, for example, a resin composition layer is formed so as to cover the entire surface of the light emitting layer formed on the substrate, and the organic EL device is sealed. (For example, Patent Documents 1 to 3).
- the device may be adversely affected. Therefore, it is desirable to transport and store the sealing sheet in a dry state. However, even in that case, it is difficult to completely prevent the entry of moisture, and the entry of a minute amount of moisture still becomes a problem.
- the resin composition layer of the sealing sheet before being used for sealing is generally protected by a cover film.
- moisture is mainly contained in the resin composition layer, and it is efficient to dry the resin composition layer of the sealing sheet after peeling the cover film.
- cover film is peeled off and dried, dust or the like adheres to the surface of the resin composition layer during drying, which may adversely affect the organic EL element.
- the present invention has been made in view of the circumstances as described above, and its purpose is to peel off the cover film of the sealing sheet in which the support, the resin composition layer, and the cover film are laminated in this order. It is providing the manufacturing method of the sealing body of an organic EL element including the process of drying the sheet
- a method for producing a sealed body in which an organic EL element on a substrate is sealed with a resin composition layer (1) a step of drying a sealing sheet in which a support, a resin composition layer and a cover film are laminated in this order with a near-infrared to mid-infrared dryer without peeling the cover film, and (2) drying The manufacturing method including the process of sealing an organic EL element with the resin composition layer of the sheet
- the peak wavelength of the near infrared ray to the mid infrared ray irradiated from the near infrared ray to mid infrared ray dryer is in the range of 1.0 to 4.0 ⁇ m.
- the peak wavelength of the near infrared ray to mid infrared ray irradiated from the near infrared ray to mid infrared ray dryer is in the range of 1.0 to 3.5 ⁇ m. The manufacturing method as described.
- the peak wavelength of the near infrared ray to the mid infrared ray irradiated from the near infrared ray to mid infrared ray dryer is in the range of 1.25 to 3.5 ⁇ m.
- the peak wavelength of the near infrared ray to the mid infrared ray irradiated from the near infrared ray to mid infrared ray dryer is in the range of 1.5 to 3.5 ⁇ m. The manufacturing method as described.
- cover film is a polyethylene terephthalate film, a polyethylene naphthalate film, a polypropylene film, or a cycloolefin polymer film.
- cover film is a polyethylene terephthalate film, a polyethylene naphthalate film, or a cycloolefin polymer film.
- cover film is a polyethylene terephthalate film.
- the sealing of the organic EL element in the step (2) is performed by laminating a sealing sheet and a substrate so that the resin composition layer is in contact with the organic EL element, [1] to [51] ]
- the sealing sheet can be efficiently dried without peeling off the cover film of the sealing sheet in which the support, the resin composition layer, and the cover film are laminated in this order. it can. Moreover, according to the method of the present invention, the sealing sheet can be efficiently dried even at a relatively low temperature.
- the method of the present invention includes a step (1) of drying the sealing sheet using a near-infrared to mid-infrared dryer without peeling off the cover film.
- the near-infrared to mid-infrared dryer means a dryer that irradiates near-infrared to mid-infrared.
- the filament (heat source) used in the light source (heater) of the near-infrared to mid-infrared dryer include tungsten, nichrome, carbon, Kantal (registered trademark), and tungsten and Kanthal are preferable, and tungsten is particularly preferable.
- the near-infrared to mid-infrared region means a wavelength range of 0.78 to 4.0 ⁇ m
- the near-infrared region means a range of 0.78 ⁇ m to less than 2.0 ⁇ m
- the mid-infrared region Means a range of 2.0 ⁇ m to 4.0 ⁇ m.
- near-infrared to mid-infrared may be abbreviated as infrared
- near-infrared to mid-infrared dryer may be abbreviated as infrared dryer.
- Drying by a near infrared or mid infrared dryer is preferably performed in a dry air or dry inert gas atmosphere.
- the inert gas include nitrogen, argon, helium, neon, and the like.
- the amount of water vapor contained in the air or inert gas is preferably 0 to 500 ppm (that is, 0 to 500 ⁇ mol / mol), more preferably 0 to 250 ppm, still more preferably 0 to 100 ppm, still more preferably 0 to 50 ppm, particularly Preferably, it is 0 to 30 ppm.
- the drying temperature is preferably 60 to 160 ° C., more preferably 60 to 140 ° C., even more preferably 60 to 130 ° C., and still more preferably. Is 80 to 130 ° C., particularly preferably 90 to 130 ° C., and the drying time is preferably 0.5 to 60 minutes, more preferably 1 to 30 minutes, even more preferably 5 to 30 minutes, still more preferably 5 ⁇ 15 minutes.
- the drying temperature means the surface temperature of the cover film on the resin composition, and can be measured by attaching a surface contact type K thermocouple on the cover film.
- the drying time means a time during which the surface temperature of the cover film is a predetermined drying temperature.
- Infrared rays are preferably applied to the sealing sheet from the cover film side.
- the distance between the light source (heater) of the near-infrared to mid-infrared dryer and the sealing sheet is preferably 5 to 100 cm, more preferably 10 to 50 cm, and still more preferably. Is 10 to 30 cm, and the infrared irradiation angle is preferably 0 to 80 degrees, more preferably 0 to 70 degrees, and still more preferably 0 to 60 degrees.
- the sealing sheet When transporting to an infrared dryer, the sealing sheet can be transported to an infrared dryer and dried in a state where the sealing sheet is fixed to a glass substrate or the like in order to prevent the sealing sheet from being bent.
- a commercially available near-infrared to mid-infrared dryer can be used.
- Examples of the commercially available near infrared to mid infrared dryer include a near infrared wavelength control system manufactured by NGK.
- step (1) the sealing sheet in which the support, the resin composition layer, and the cover film are laminated in this order is dried without peeling off the cover film.
- a conventionally known sealing sheet can be used as the sealing sheet.
- Support examples of the support for the sealing sheet include polyolefins such as polyethylene and polypropylene (PP), polyesters such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), and polycarbonate (PC ), Polyimide (PI), cycloolefin polymer (COP), polyvinyl chloride and other plastic films. Only one type of plastic film may be used, or two or more types may be used in combination.
- the support is preferably a PET film, a PEN film or a COP film, and more preferably a PET film.
- a plastic film having a barrier layer may be used as a support.
- the barrier layer and the resin composition layer may be in contact with each other, and the barrier layer and the resin composition layer may not be in contact (that is, a support in contact with the resin composition layer).
- a barrier layer may be formed on the surface of the support opposite to the surface of the substrate). Examples of the barrier layer include nitrides such as silicon nitride, oxides such as aluminum oxide, metal foils such as stainless steel foil and aluminum foil, and the like.
- the barrier layer may have a multilayer structure of two or more layers.
- plastic film having a barrier layer examples include films of polyethylene terephthalate, polyethylene naphthalate, polycarbonate, cycloolefin polymer, and the like.
- the plastic film may have a multilayer structure of two or more layers.
- a commercial product may be used as the plastic film having the barrier layer.
- commercially available polyethylene terephthalate films with aluminum foil include “Al with PET (1N30)” manufactured by Tokai Toyo Aluminum Sales Co., “PET Tsuki AL3025” manufactured by Fukuda Metals.
- a polarizing plate or the like may be used as a support.
- the support may be composed of a plurality of layers having different functions such as a plastic film having a barrier layer and a polarizing plate.
- a plastic film having a barrier layer and a polarizing plate bonded together with an adhesive such as an optical pressure-sensitive adhesive sheet (OCA) may be used as the support.
- OCA optical pressure-sensitive adhesive sheet
- the sealing sheet is configured such that the plastic film having the barrier layer is in contact with the resin composition layer.
- the support may be subjected to a release treatment using a silicone resin release agent, an alkyd resin release agent, a fluororesin release agent, a mat treatment, a corona treatment, or the like.
- the thickness of the support is not particularly limited. From the viewpoint of handleability and the like, the lower limit of the thickness of the support is preferably 10 ⁇ m, more preferably 20 ⁇ m, and the upper limit is preferably 200 ⁇ m, more preferably 125 ⁇ m.
- the preferred range of the thickness of the support is (i) 10-200 ⁇ m, (ii) 20-200 ⁇ m, (iii) 10-125 ⁇ m, and (iv) 20-125 ⁇ m.
- the cover film of the sealing sheet is preferably a PET film, PEN film, PP film or COP film, more preferably a PET film, PEN film or COP film, and further preferably a PET film.
- the cover film may be subjected to a release treatment with a silicone resin release agent, an alkyd resin release agent, a fluororesin release agent, a mat treatment, a corona treatment, or the like.
- the cover film may have a multilayer structure of two or more layers. The thickness of the cover film is not particularly limited.
- the lower limit of the thickness of the cover film is preferably 10 ⁇ m, more preferably 20 ⁇ m, and the upper limit thereof is preferably 200 ⁇ m, more preferably 125 ⁇ m.
- Preferred ranges of cover film thickness are (i) 10-200 ⁇ m, (ii) 20-200 ⁇ m, (iii) 10-125 ⁇ m, and (iv) 20-125 ⁇ m.
- the sealing sheet used in the present invention may be a thermosetting sealing sheet or a pressure-sensitive adhesive sealing sheet.
- the thermosetting sealing sheet is a sealing sheet having a thermosetting resin composition layer, and after the sealing sheet and the substrate are laminated, they are heated and cured.
- seat which forms the formed resin composition layer (sealing layer) is meant.
- the pressure-sensitive adhesive sealing sheet means a sealing sheet on which a sealing layer has already been formed, and does not necessarily require heating after the sealing sheet and the substrate are laminated.
- thermosetting resin composition for forming the resin composition layer of the thermosetting sealing sheet there is no particular limitation on the thermosetting resin composition for forming the resin composition layer of the thermosetting sealing sheet, and conventionally known ones such as those described in WO 2010/084938 can be used. .
- the resin composition for forming the resin composition layer of the pressure-sensitive adhesive type sealing sheet (hereinafter also referred to as “pressure-sensitive adhesive composition”), and WO 2013 / Conventionally known ones such as those described in 108731, WO 2011/062167 can be used.
- the resin composition layer may have a multilayer structure in which two or more resin composition layers are formed, such as those described in WO 2011/016408.
- the thermosetting resin composition preferably contains an epoxy resin and a curing agent. There is no limitation in particular in an epoxy resin and a hardening
- the thermosetting resin composition may contain a thermoplastic resin.
- the pressure-sensitive adhesive composition preferably contains an ⁇ -olefin resin and a tackifier.
- the ⁇ -olefin resin and the tackifier are not particularly limited, and conventionally known ones can be used.
- the ⁇ -olefin resin include ⁇ -olefin polymers such as polyethylene and polyisobutylene.
- the ⁇ -olefin resin may be a copolymer.
- the copolymer include copolymers of different ⁇ -olefins, and copolymers of ⁇ -olefins and monomers other than ⁇ -olefins (eg, styrene, non-conjugated dienes, etc.).
- Both the thermosetting resin composition and the pressure-sensitive adhesive composition may contain an additive.
- the additive include hygroscopic metal oxides (for example, calcium oxide and calcined hydrotalcite) and inorganic fillers other than the hygroscopic metal oxide (for example, silica, mica, talc, and the like).
- the method of this invention includes the process (2) of sealing an organic EL element with the resin composition layer of the sheet
- the step (2) is preferably performed in the same production line as the step (1). Moreover, for the same reason, it is preferable that the period from step (1) to step (2) is within 60 minutes. For the same reason, the step (2) is performed following the step (1) (specifically, the step (2) is performed without performing other steps after the step (1)). preferable.
- Substrate there is no particular limitation on the substrate used in the present invention, and a known substrate can be used.
- the substrate is preferably selected from the group consisting of glass, glass with indium tin oxide (ITO), polyimide (PI), polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate (PC) and cycloolefin polymer (COP). Is at least one.
- the thickness of the substrate is preferably 0.1 to 1.0 mm, more preferably 0.1 to 0.7 mm.
- the thickness of the organic EL element is preferably 0.01 to 1 ⁇ m, more preferably 0.05 to 0.5 ⁇ m.
- the organic EL element may have another structure for suppressing deterioration due to moisture.
- a passivation film may be formed on the organic EL element.
- the sealing sheet is laminated on the passivation film.
- the passivation film is not particularly limited, and for example, an inorganic film such as SiN, SiON, SiO 2 , Al 2 O 3 , or TiO 2 formed by sputtering, CVD, or the like; a polymer film such as acrylic resin or polyimide-based parylene
- a known passivation film such as a laminated film having a multilayer structure in which an inorganic film is laminated can be used.
- the thickness of the passivation film is not particularly limited, but is preferably 1 to 3 ⁇ m.
- either one of the substrate and the support for the sealing sheet is transparent.
- an opaque support for example, a plastic film having an opaque barrier layer
- the organic EL element includes an organic EL element having another structure for suppressing deterioration as described above.
- the resin composition layer is in contact with the organic EL element means “the resin composition layer is in contact with the passivation film of the organic EL element”.
- the substrate having the organic EL element is immediately sealed with the resin composition layer of the sealing sheet after drying in the step (1).
- the time from the drying in the step (1) to the start of the sealing in the step (2) is preferably 1 to 60 minutes, more preferably 1 to 30 minutes, and even more preferably 1 to 15 minutes in an air atmosphere. Particularly preferred is 1 to 10 minutes.
- “sealing start in step (2)” refers to a point in time when the resin composition layer of the sealing sheet is in contact with the organic EL element after peeling the cover film from the sealing sheet.
- the sealing is preferably performed under an inert gas atmosphere or under vacuum in order to prevent moisture from adsorbing on the resin composition layer of the dried sealing sheet.
- the inert gas include nitrogen, argon, helium, neon, and the like.
- the ambient pressure (pressure of inert gas) when sealing is performed in an inert gas atmosphere is preferably about 1 ⁇ 10 5 Pa.
- the ambient pressure (degree of reduced pressure) when sealing under vacuum is preferably 1 to 1 ⁇ 10 3 Pa, more preferably 1 to 1 ⁇ 10 2 Pa.
- the apparatus used for the lamination there is no particular limitation on the apparatus used for the lamination, and a known apparatus such as a roll laminator or a press machine can be used. A plurality of devices, for example, a roll laminator and a press machine may be used in combination.
- the roll speed is preferably 10 to 1500 mm / min, more preferably, in order to achieve good adhesion of the resin composition layer to the support. 100 to 500 mm / min.
- the roll pressure of the roll laminator is preferably 0 to 0.5 MPa, more preferably 0 to 0.3 MPa in order to avoid damage to the organic EL element.
- the roll pressure means an applied pressure by an air syringe and is displayed as a gauge pressure (original pressure).
- the roll pressure being 0 means that the applied pressure is 0.
- the roll pressure it is preferable to press the laminate with a press machine described later after the lamination by the roll laminator.
- the roll temperature of the roll laminator is preferably 30 to 120 ° C., more preferably 40 to 110 ° C., and further preferably 50 to 100 ° C. in order to soften the resin composition layer and improve the followability to the substrate.
- the roll temperature means a roll surface temperature that is digitally controlled by incorporating a heater in the roll, and can be measured by a surface contact type K thermocouple.
- a commercially available roll laminator can be used for lamination.
- Examples of commercially available roll laminators include “LPD2325” manufactured by Fuji Plastics, “roll laminator VA770H” manufactured by Taisei Laminator, “roll laminator VA700”, “roll laminator VAII-700”, “Mach630up” manufactured by Hakuto Co., Ltd. .
- Examples of the material of the roll of the roll laminator include stainless steel and rubber, and silicone rubber is preferable.
- the press pressure is preferably 0.01 to 0.5 MPa, more preferably 0.01 to 0, in order to prevent cracking of the EL element due to the pressure. .3 MPa.
- the press pressure of the press means a pressure applied to the pressed body controlled by a vacuum hydraulic cylinder or a load (that is, a pressure applied to the surface of the sealing sheet).
- the pressing temperature of the press machine is preferably 30 to 120 ° C., more preferably 40 to 120 ° C., further preferably 50 to 110 ° C., and still more preferably 60 to 100 ° C.
- the pressing time is preferably 20 to 120 ° C. 450 seconds, more preferably 60 to 300 seconds.
- the press temperature of the press means the temperature of the press part surface that is digitally controlled by incorporating a cartridge heater on the surface of the press part (for example, a flat plate such as a metal plate) of the press machine. Can be measured.
- a commercially available press can be used for lamination.
- Examples of commercially available presses include flat plate presses such as “Batch type vacuum pressure laminator CVP-300” manufactured by Morton, and Kitakawa Seiki Co., Ltd., vacuum pressure press “VHI-2051”.
- Examples of the material for the flat plate for pressing include alloys such as stainless steel and iron, and stainless steel is preferable.
- the laminate of the sealing sheet and the substrate is heated to cure the cured resin composition layer (ie, sealing Layer).
- Curing can be performed using, for example, a hot-air circulating oven, an infrared heater, a heat gun, a high-frequency induction heating device, a hot plate, or the like.
- hot pressing is performed using a press machine for lamination, the lamination and the resin composition layer may be simultaneously cured.
- the curing temperature varies depending on the resin composition layer and support used, but is preferably 80 to 120 ° C., more preferably 80 to 110 ° C., and the curing time is preferably 10 to 120 minutes, more preferably 10 to 60 minutes.
- the thickness of the cured resin composition layer to be formed is preferably 3 to 200 ⁇ m, more preferably 5 to 150 ⁇ m, and still more preferably 10 to 100 ⁇ m.
- the resin composition layer is already cured by heating the sealing sheet before laminating the sealing sheet and the substrate. However, after laminating the sealing sheet and the substrate, these may be further heated.
- the heating temperature is preferably 50 to 150 ° C., more preferably 60 to 100 ° C., and still more preferably, in order to avoid thermal deterioration of the organic EL element. 60-90 ° C.
- the moisture of the sealing sheet can be measured using a Karl Fischer moisture measuring device under the conditions described in Test Example 1 described later.
- the moisture content of the sealing sheet can be calculated based on the following formula from the measured moisture (weight) and the weight of the sealing sheet.
- Moisture content (weight ppm) of sealing sheet (measured moisture) / (weight of sealing sheet) ⁇ 10 6
- the water content of the sealing sheet after step (1) is preferably 500 ppm by weight or less, more preferably 400 ppm by weight or less, further preferably 300 ppm by weight or less, particularly preferably 250 ppm by weight or less, and most preferably 200 ppm. Weight ppm or less.
- moisture contained in the sealing sheet is considered to be exclusively contained in the resin composition layer
- the evaluation of the moisture content assumes that moisture is contained only in the resin composition layer and is contained in the resin composition layer. It is preferable to carry out based on the value converted to the moisture content.
- the moisture content contained in the resin composition layer is calculated based on the following formula from the moisture content (weight) of the sealing sheet measured as described above, the weight of the sealing sheet, and the weight ratio of the resin composition layer. can do.
- Moisture content of resin composition layer (weight ppm) (measured moisture) / (weight of sealing sheet ⁇ weight ratio of resin composition layer) ⁇ 10 6
- the weight ratio of the resin composition layer used in the above formula can be calculated based on the following formula, for example, by previously measuring the weight of other layers such as the support and the cover film in the sealing sheet. .
- Weight ratio of resin composition layer (weight of sealing sheet ⁇ weight of other layer) / weight of sealing sheet
- the water content of the resin composition layer after the step (1) is preferably 2000 ppm by weight or less, more preferably 1800 ppm by weight or less, still more preferably 1600 ppm by weight or less, still more preferably 1400 ppm by weight or less, even more preferably.
- thermosetting sealing sheet 1 56 parts by weight of liquid bisphenol A type epoxy resin (Mitsubishi Chemical "jER828EL", epoxy equivalent: about 185 g / eq), silane coupling agent (Shin-Etsu Chemical Co., Ltd.) After mixing 1.2 parts by weight of “KBM403”, 2 parts by weight of talc powder (“FG-15” manufactured by Nippon Talc Co., Ltd.), and 15 parts by weight of calcined hydrotalcite (“KW2200” manufactured by Kyowa Chemical Co., Ltd.) Dispersion was performed with a three-roll mill to obtain a mixture.
- liquid bisphenol A type epoxy resin Mitsubishi Chemical "jER828EL", epoxy equivalent: about 185 g / eq
- silane coupling agent Shin-Etsu Chemical Co., Ltd.
- a plastic film having a barrier layer as a support (“Al (1N30) with PET” manufactured by Tokai Toyo Aluminum Sales Co., Ltd., plastic film: polyethylene terephthalate (PET) film having a thickness of 25 ⁇ m, barrier layer: aluminum foil having a thickness of 30 ⁇ m)
- PET polyethylene terephthalate
- barrier layer aluminum foil having a thickness of 30 ⁇ m
- the obtained resin composition varnish was uniformly coated on the barrier layer of the support with a die coater so that the thickness of the resin composition layer after drying was 20 ⁇ m, and was 80 to 100 ° C. (average 90 ° C.) for 5 minutes (residual solvent amount in the resin composition layer: 2% by weight).
- a 38 ⁇ m-thick PET film treated with an alkyd mold release agent was used as a cover film, and the film was wound into a roll while being bonded to the surface of the resin composition layer.
- the roll-shaped sealing sheet was slit to a width of 507 mm to obtain a sealing sheet 1 (width: 507 mm, length: 336 mm).
- a plastic film having a barrier layer as a support (“Al (1N30) with PET” manufactured by Tokai Toyo Aluminum Sales Co., Ltd., plastic film: polyethylene terephthalate (PET) film having a thickness of 25 ⁇ m, barrier layer: aluminum foil having a thickness of 30 ⁇ m)
- PET polyethylene terephthalate
- barrier layer aluminum foil having a thickness of 30 ⁇ m
- a resin composition sheet was obtained.
- a PET film having a thickness of 30 ⁇ m treated with a silicone release agent was used as the cover film, and the film was wound up in a roll while being bonded to the surface of the resin composition layer.
- the roll-shaped sealing sheet was slit to a width of 507 mm to obtain a sealing sheet 2 (width: 507 mm, length: 336 mm).
- a plastic film having a barrier layer as a support (“Al (1N30) with PET” manufactured by Tokai Toyo Aluminum Sales Co., Ltd., plastic film: polyethylene terephthalate (PET) film having a thickness of 25 ⁇ m, barrier layer: aluminum foil having a thickness of 30 ⁇ m)
- PET polyethylene terephthalate
- barrier layer aluminum foil having a thickness of 30 ⁇ m
- a resin composition sheet was obtained.
- a 38 ⁇ m-thick PET film treated with a silicone-based release agent was used as the cover film, and the film was wound into a roll while being bonded to the surface of the resin composition layer.
- the roll-shaped sealing sheet was slit to a width of 507 mm to obtain a sealing sheet 3 (width: 507 mm, length: 336 mm).
- Test Example 1 Calculation of moisture content of dried sealing sheet and resin composition layer Infrared dryer (“Near Infrared Wavelength Control System” manufactured by NGK, Filament: Kanthal or Tungsten), hot air dryer (Yamato Science) Using the “Precision Incubator”) or vacuum dryer (Yamato Kagaku “Square Vacuum Dryer”, degree of vacuum: 100 Pa) at the temperatures and times shown in Tables 1 to 3 below.
- the sealing sheets 1 to 3 obtained in this manner were dried with the cover film peeled off or without peeling off the cover film.
- Drying using an infrared dryer was performed by irradiating the sealing sheet from the cover film side with infrared rays under a nitrogen atmosphere (water vapor amount: 20 ppm or less).
- the peak wavelength of infrared rays irradiated from the infrared dryer was around 3 ⁇ m when the filament was cantal and around 1.5 ⁇ m when the filament was tungsten.
- the filament of the infrared dryer used for drying the sealing sheets 1 and 3 was cantal, and the filament of the infrared dryer used for drying the sealing sheet 2 was tungsten. Further, the distance between the light source (heater) of the infrared dryer and the sealing sheet was adjusted to 15 cm, and the infrared irradiation angle was adjusted to 0 to 60 degrees.
- a sample (width: about 100 mm, length: about 100 mm, weight: 100-300 mg) is cut out from the dried sealing sheets 1 to 3, the cover film is peeled off, and the moisture of the sealing sheet is measured using a coulometric titration method.
- Karl Fischer moisture measuring device (“Mitsubishi Chemical Analyzer CA-200” manufactured by Mitsubishi Chemical Analytech Co., Ltd.).
- the apparatus is composed of a glass container in which a heatable sample is placed and a titration apparatus containing a reaction liquid for titrating water vaporized when the sample is heated.
- the vaporized water moves from the glass container to the reaction liquid side of the titration apparatus by flowing nitrogen at a flow rate of 250 ⁇ 25 ml / min.
- the measurement is carried out by putting a sample into a glass container substituted under a nitrogen atmosphere (water vapor amount ⁇ 0.1 ppm), measuring moisture vaporized at 130 ° C., and determining the moisture content and resin composition of the sealing sheet. The moisture content of the physical layer was calculated. The results are shown in Tables 1 to 3 below.
- Test Example 2 Sealing property evaluation test with Ca film of dried sealing sheet Using a glass substrate on which a Ca film was formed instead of an organic EL element, an organic EL element sealing simulation experiment was performed and dried. The sealing property by the sealing sheet was evaluated.
- Ca was vapor-deposited on a glass substrate (thickness: 700 ⁇ m, width: 50 mm, length: 50 mm) to form a Ca film (thickness: about 300 nm, width: 40 mm, length: 40 mm).
- the obtained glass substrate had a sealing width of 5 mm around the Ca film (that is, a width where the glass substrate on which the Ca film was not formed and the sealing sheet were in contact).
- the sealing sheets 1 to 3 were dried as described in Test Example 1 at the temperatures and times shown in Tables 1 to 3 below, and after 180 seconds from the drying, the resin
- the sealing sheet and the glass substrate were laminated so that the composition layer was in contact with the Ca film, and the Ca film was sealed.
- a roll laminator (“LPD2325" manufactured by Fuji Plastics, roll material: rubber) is used under the conditions of a roll temperature: 90 ° C, a roll speed: 360 mm / min, a roll pressure: 0.2 MPa, under a nitrogen atmosphere. went.
- a laminate of the sealing sheet and the glass substrate is heated to 110 ° C. in an atmosphere using a hot plate (“HP-2SA” manufactured by ASONE).
- the resin composition layer was thermoset by heating for 30 minutes.
- thermosetting type sealing sheet 1 when the thermosetting type sealing sheet 1 was used, the Ca film surface was visually observed after the thermosetting of the resin composition layer, and evaluated according to the following criteria. Moreover, the Ca film surface at the time of using the pressure sensitive adhesive type sealing sheet 3 was visually observed and evaluated according to the following criteria. The results are shown in Tables 1 and 3 below. ⁇ : There is no change in the Ca film surface before and after sealing, and a mirror-like silvery luster is seen. ⁇ : Silver gloss on the surface of the Ca film becomes dull and turns gray. X: Ca film
- the sealing sheet 1 that was not dried (No. 1-5, moisture content of the sealing sheet: 1290 ppm by weight) or a vacuum dryer was used to dry without peeling off the cover film.
- the sealing property evaluation test using the sealing sheet 1 (No. 1-4, moisture content of the sealing sheet: 768 ppm by weight)
- the surface of the Ca film on the glass substrate was cured after the resin composition layer was cured. Deteriorated.
- a sealing sheet 1 No. 1-3, moisture content of the sealing sheet: 511 weight ppm
- a hot air dryer 100 ° C., 5 minutes
- the sealing sheet 1 (No. 1-2), which was dried by removing the cover film using a hot air dryer (100 ° C., 5 minutes), had a moisture content of 153 wt. It was ppm and the reduced disclosure time exceeded 600 hours, and both the water content and the sealing property were good. However, when the cover film is peeled off and dried, the resin composition layer is contaminated during drying, and as a result, the organic EL element may be adversely affected.
- the water content of the sealing sheet 1 (No. 1-1) can be obtained without removing the cover film.
- the rate can be reduced to 75 ppm by weight. This is presumably because the moisture in the cover film and the resin composition layer was excited by near infrared irradiation and evaporated through the cover film.
- the moisture content of the sealing sheet 2 (No. 2-5) which was not dried is as high as 2900 ppm by weight, which suggests that it is inappropriate for sealing.
- the moisture content (No. 2-4) of the sealing sheet 2 dried without peeling off the cover film using a hot air dryer (100 ° C., 5 minutes) is as high as 1131 ppm by weight, and the shrinkage thereof is started. The time was as short as less than 300 hours.
- the water content of the sealing sheet 2 (No. 2-1) can be obtained without removing the cover film.
- the rate can be reduced to 31 ppm by weight. From this result, it can be seen that drying using a near-infrared to mid-infrared dryer is useful not only for thermosetting sealing sheets but also for pressure-sensitive adhesive sealing sheets.
- the sealing sheet 3 that was not dried (No. 3-6, the moisture content of the sealing sheet: 3890 wtppm, the moisture content of the resin composition layer: 18507 wtppm) or the cover film
- the sealing sheet 3 (No. 3-3, moisture content of the sealing sheet: 1114 ppm by weight, water content of the resin composition layer) dried using a hot air dryer (130 ° C., 30 minutes) without peeling off
- the Ca film surface on the glass substrate was deteriorated. From these results, it is suggested that a sealing sheet having a water content of the resin composition layer exceeding 2000 ppm by weight is inappropriate for sealing.
- the sealing sheet can be sealed to some extent without peeling off the cover film. Although the water content can be reduced, it is suggested that the drying efficiency is poor and the sealing performance tends to be difficult to improve.
- the sealing sheet 3 (No. 3-) can be obtained in a short time (10 to 30 minutes) without peeling off the cover film. 1 and No. 3-2) can be reduced to 57 to 64 ppm by weight, and the moisture content of the resin composition layer can be reduced to 272 to 307 ppm by weight, thereby improving the sealing performance.
- Test Example 3 Sealing Performance Evaluation Test of Dry Sealing Sheet with Organic EL Using an organic EL element, sealing performance with a dry sealing sheet was evaluated. Specifically, first, an organic EL element (the thickness of the organic film: 110 nm, the thickness of the Al cathode: 100 nm) is formed on the glass substrate with indium tin oxide (ITO) (manufactured by Geomatek Co., Ltd.) so that the emitting area is 4 mm 2. did.
- ITO indium tin oxide
- the sealing sheet 1 or 3 (width: 15 mm, height: 25 mm) was dried as described in Test Example 1 at the temperatures and times shown in Tables 4 and 5 below, and after 180 seconds from the drying, the resin A sealing sheet and a glass substrate with ITO were laminated so that the composition was in contact with the organic EL element, and the organic EL element was sealed.
- a roll laminator (“LPD2325" manufactured by Fuji Plastics, roll material: rubber) is used under the conditions of a roll temperature: 90 ° C, a roll speed: 360 mm / min, a roll pressure: 0.2 MPa, under a nitrogen atmosphere. went.
- thermosetting sealing sheet 1 when used, a hot plate (“HP-2SA” manufactured by ASONE Co., Ltd.) is used, and the resin sheet and the glass substrate are at 110 ° C. for 30 minutes in a nitrogen atmosphere.
- the resin composition was thermally cured by heating.
- the light emitting surface of the organic EL element sealed with the sealing sheet 1 obtained as described above is observed at a magnification of 100 times with a CCD camera (manufactured by Keyence Corporation), and sealing in the entire area of the light emitting surface.
- the ratio of the dark spot immediately after was measured and evaluated.
- the dark spot means a non-light-emitting portion generated when the element comes into contact with moisture.
- the results are shown in Table 4.
- ⁇ Dark spot ratio is 1.0% or more and less than 5.0%
- Dark spot ratio is 5.0% or more
- the pressure-sensitive adhesive sealing sheet 3 When the pressure-sensitive adhesive sealing sheet 3 is used, first, before the acceleration test described later, the light emitting surface of the organic EL element sealed with the sealing sheet obtained as described above is used as the CCD. Observation was performed at a magnification of 100 times with a camera, and the light emission area (initial light emission area) was measured. Next, the sealing sheet was heated at 85 ° C. for 100 hours in a nitrogen atmosphere, and an accelerated deterioration test was performed. The light emitting surface of the organic EL element after this acceleration test was observed with a CCD camera at a magnification of 100 times, and the area of the light emitting surface that emitted light even after the acceleration test (light emission remaining area) was measured.
- ⁇ Ratio of remaining light emission area is 70% or more
- ⁇ Ratio of remaining light emission area is 50% or more and less than 70%
- ⁇ Ratio of remaining light emission area is less than 50%
- the sealing sheet 1 that was not dried (No. 1-10, the moisture content of the sealing sheet: 1290 weight ppm) or the cover film was dried without peeling using a hot air dryer.
- the sealing performance evaluation test using the sealing sheet 1 (No. 1-9, moisture content of the sealing sheet: 511 ppm by weight)
- many dark spots were formed on the light emitting surface of the organic EL element immediately after sealing. Existed.
- the sealing sheet having a moisture content exceeding 500 ppm by weight is inappropriate for sealing, even in this Test Example using the organic EL element. It is suggested.
- the sealing sheet 1 (No. 1-8), which was dried by peeling off the cover film using a hot air dryer (100 ° C., 10 minutes), was water content of the sealing sheet.
- the rate was 107 ppm by weight, and there were few dark spots present on the light emitting surface of the organic EL device immediately after sealing.
- the cover film is peeled off and dried, the resin composition is contaminated during drying, and as a result, the organic EL element may be adversely affected.
- the sealing sheet 1 (No. 1-6) can be obtained without peeling the cover film. And the water content of No. 1-7) can be reduced to 150 ppm by weight. When these were used to seal the organic EL element, the ratio of dark spots was small and sealing was possible.
- the sealing sheet 3 that was not dried (No. 3-12, moisture content of the sealing sheet: 2900 ppm by weight) or a hot air dryer was used to remove the cover film without peeling.
- the sealing performance evaluation test using the time-dried sealing sheet 3 (No. 3-10, moisture content of the sealing sheet: 710 ppm by weight)
- the ratio of the remaining light emission area was significantly reduced. This result is considered to be because the moisture was left in the sealing sheet 3 due to insufficient drying, leading to deterioration of the organic EL element.
- the sealing sheet 3 (No. 3-7 and No. 3-7 and The water content of No. 3-8) can be reduced to about 100 ppm by weight. From this result, it can be seen that drying using a near-infrared to mid-infrared dryer is useful not only for thermosetting sealing sheets but also for pressure-sensitive adhesive sealing sheets.
- the sealing sheet can be efficiently dried without peeling off the cover film of the sealing sheet in which the support, the resin composition layer, and the cover film are laminated in this order. it can. Therefore, the method of this invention is useful for manufacture of the sealing body (especially organic EL device) by which the organic EL element on a board
- the sealing body especially organic EL device
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Abstract
Description
(1)支持体、樹脂組成物層およびカバーフィルムがこの順序で積層された封止用シートを、カバーフィルムを剥離せずに近赤外線乃至中赤外線乾燥機で乾燥する工程、および
(2)乾燥した封止用シートからカバーフィルムを剥離した後、封止用シートの樹脂組成物層で有機EL素子を封止する工程
を含む製造方法。
[2] 工程(2)が、工程(1)と同一製造ライン内で行われる前記[1]に記載の製造方法。
[3] 工程(1)に続いて、工程(2)が行われる前記[1]または[2]に記載の製造方法。
[5] 工程(1)の乾燥後から工程(2)の封止開始までの時間が1~30分である前記[1]~[3]のいずれか一つに記載の製造方法。
[6] 工程(1)の乾燥後から工程(2)の封止開始までの時間が1~15分である前記[1]~[3]のいずれか一つに記載の製造方法。
[7] 工程(1)の乾燥後から工程(2)の封止開始までの時間が1~10分である前記[1]~[3]のいずれか一つに記載の製造方法。
[9] 近赤外線乃至中赤外線乾燥機から照射される近赤外線乃至中赤外線のピーク波長が、1.0~3.5μmの範囲内にある前記[1]~[7]のいずれか一つに記載の製造方法。
[10] 近赤外線乃至中赤外線乾燥機から照射される近赤外線乃至中赤外線のピーク波長が、1.25~3.5μmの範囲内にある前記[1]~[7]のいずれか一つに記載の製造方法。
[11] 近赤外線乃至中赤外線乾燥機から照射される近赤外線乃至中赤外線のピーク波長が、1.5~3.5μmの範囲内にある前記[1]~[7]のいずれか一つに記載の製造方法。
[14] 近赤外線乃至中赤外線乾燥機における乾燥温度が60~130℃である前記[12]に記載の製造方法。
[15] 近赤外線乃至中赤外線乾燥機における乾燥温度が80~130℃である前記[12]に記載の製造方法。
[16] 近赤外線乃至中赤外線乾燥機における乾燥温度が90~130℃である前記[12]に記載の製造方法。
[18] 近赤外線乃至中赤外線乾燥機における乾燥時間が5~30分である前記[12]~[16]のいずれか一つに記載の製造方法。
[19] 近赤外線乃至中赤外線乾燥機における乾燥時間が5~15分である前記[12]~[16]のいずれか一つに記載の製造方法。
[21] 工程(1)後の封止用シートの含水率が、400重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[22] 工程(1)後の封止用シートの含水率が、300重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[23] 工程(1)後の封止用シートの含水率が、250重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[24] 工程(1)後の封止用シートの含水率が、200重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[26] 工程(1)後の樹脂組成物層の含水率が、1800重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[27] 工程(1)後の樹脂組成物層の含水率が、1600重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[28] 工程(1)後の樹脂組成物層の含水率が、1400重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[29] 工程(1)後の樹脂組成物層の含水率が、1200重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[30] 工程(1)後の樹脂組成物層の含水率が、1000重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[31] 工程(1)後の樹脂組成物層の含水率が、850重量ppm以下である前記[1]~[19]のいずれか一つに記載の製造方法。
[34] 乾燥した空気または乾燥した不活性ガス中に含まれる水蒸気量が0~250ppmである前記[32]に記載の製造方法。
[35] 乾燥した空気または乾燥した不活性ガス中に含まれる水蒸気量が0~100ppmである前記[32]に記載の製造方法。
[36] 乾燥した空気または乾燥した不活性ガス中に含まれる水蒸気量が0~50ppmである前記[32]に記載の製造方法。
[37] 乾燥した空気または乾燥した不活性ガス中に含まれる水蒸気量が0~30ppmである前記[32]に記載の製造方法。
[40] 近赤外線乃至中赤外線乾燥機の光源と封止用シートとの距離が、10~50cmである前記[1]~[38]のいずれか一つに記載の製造方法。
[41] 近赤外線乃至中赤外線乾燥機の光源と封止用シートとの距離が、10~30cmである前記[1]~[38]のいずれか一つに記載の製造方法。
[43] 封止用シートに対する赤外線の照射角度が、0~70度である前記[1]~[41]のいずれか一つに記載の製造方法。
[44] 封止用シートに対する赤外線の照射角度が、0~60度である前記[1]~[41]のいずれか一つに記載の製造方法。
[46] カバーフィルムが、ポリエチレンテレフタレートフィルム、ポリエチレンナフタレートフィルム、またはシクロオレフィンポリマーフィルムである前記[1]~[44]のいずれか一つに記載の製造方法。
[47] カバーフィルムが、ポリエチレンテレフタレートフィルムである前記[1]~[44]のいずれか一つに記載の製造方法。
[49] カバーフィルムの厚さが、20~200μmである前記[1]~[47]のいずれか一つに記載の製造方法。
[50] カバーフィルムの厚さが、10~125μmである前記[1]~[47]のいずれか一つに記載の製造方法。
[51] カバーフィルムの厚さが、20~125μmである前記[1]~[47]のいずれか一つに記載の製造方法。
本発明の方法は、近赤外線乃至中赤外線乾燥機を用いて、カバーフィルムを剥離せずに封止用シートを乾燥する工程(1)を含む。
本明細書において近赤外線乃至中赤外線乾燥機とは、近赤外線乃至中赤外線を照射する乾燥機を意味する。近赤外線乃至中赤外線乾燥機の光源(ヒーター)に用いられるフィラメント(熱源)としては、例えばタングステン、ニクロム、カーボン、カンタル(登録商標)等が挙げられ、タングステン、カンタルが好ましく、特にタングステンが好ましい。効率的に樹脂組成物層を乾燥させるために、ピーク波長が1.0~4.0μmの範囲内にある近赤外線乃至中赤外線を照射する乾燥機を用いることが好ましい。ピーク波長は、より好ましくは1.0~3.5μm、さらに好ましくは1.25~3.5μm、さらに好ましくは1.5~3.5μmの範囲内にある。なお、本明細書において近赤外線乃至中赤外線領域は、波長が0.78~4.0μmの範囲を意味し、近赤外線領域は0.78μm以上2.0μm未満の範囲を意味し、中赤外線領域は2.0μm以上4.0μm以下の範囲を意味する。本明細書においては、近赤外線乃至中赤外線を赤外線、近赤外線乃至中赤外線乾燥機を赤外線乾燥機と略称することがある。
工程(1)では、支持体、樹脂組成物層およびカバーフィルムがこの順序で積層された封止用シートを、カバーフィルムを剥離せずに乾燥させる。封止用シートとしては、従来公知の封止用シートを使用することができる。
封止用シートの支持体としては、例えば、ポリエチレン、ポリプロピレン(PP)等のポリオレフィン、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)等のポリエステル、ポリカーボネート(PC)、ポリイミド(PI)、シクロオレフィンポリマー(COP)、ポリ塩化ビニル等のプラスチックフィルムが挙げられる。プラスチックフィルムは1種のみを使用してもよく、2種以上を併用してもよい。支持体は、好ましくは、PETフィルム、PENフィルムまたはCOPフィルムであり、より好ましくはPETフィルムである。
封止用シートのカバーフィルムとしては、支持体のプラスチックフィルムと同様のものが挙げられる。カバーフィルムは、好ましくはPETフィルム、PENフィルム、PPフィルムまたはCOPフィルムであり、より好ましくはPETフィルム、PENフィルムまたはCOPフィルムであり、さらに好ましくはPETフィルムである。カバーフィルムには、シリコーン樹脂系離型剤、アルキッド樹脂系離型剤、フッ素樹脂系離型剤等による離型処理、マット処理、コロナ処理等が施されていてもよい。カバーフィルムは2層以上の複層構造であってもよい。カバーフィルムの厚さは、特に限定されない。取り扱い性および封止用シートの乾燥等の観点から、カバーフィルムの厚さの下限は、好ましくは10μm、より好ましくは20μmであり、その上限は、好ましくは200μm、より好ましくは125μmである。カバーフィルムの厚さの好ましい範囲(即ち、好ましい上下限の組合せ)は、(i)10~200μm、(ii)20~200μm、(iii)10~125μm、および(iv)20~125μmである。
本発明で用いる封止用シートは、熱硬化型の封止用シートでもよく、感圧接着型の封止用シートでもよい。ここで、熱硬化型の封止用シートとは、熱硬化性樹脂組成物層を有する封止用シートであって、該封止用シートと基板との積層後に、それらを加熱して、硬化した樹脂組成物層(封止層)を形成するシートを意味する。感圧接着型の封止用シートとは、既に封止層が形成されている封止用シートであって、該封止用シートと基板との積層後に加熱が必ずしも必要ではないシートを意味する。熱硬化型の封止用シートの樹脂組成物層を形成するための熱硬化性樹脂組成物に特に限定は無く、WO 2010/084938 に記載のもの等、従来公知のものを使用することができる。感圧接着型の封止用シートの樹脂組成物層を形成するための樹脂組成物(以下「感圧接着型の組成物」と略称することがある。)も特に限定は無く、WO 2013/108731、WO 2011/062167に記載のもの等の、従来公知のものを使用することができる。樹脂組成物層はWO 2011/016408に記載のもの等の、樹脂組成物層が2層以上された複層構造であってもよい。
本発明の方法は、乾燥した封止用シートからカバーフィルムを剥離した後、封止用シートの樹脂組成物層で有機EL素子を封止する工程(2)を含む。工程(1)の効果を活かすため、工程(2)が、工程(1)と同一製造ライン内で行われることが好ましい。また同理由により、工程(1)の後から工程(2)までの間が60分以内であることが好ましい。また同理由により、工程(1)に続いて、工程(2)が行われること(詳しくは、工程(1)の後に、他の工程が行われずに、工程(2)が行われること)が好ましい。
本発明で使用する基板に特に限定はなく、公知のものを使用することができる。基板は、好ましくはガラス、酸化インジウムスズ(ITO)付きガラス、ポリイミド(PI)、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)、ポリカーボネート(PC)およびシクロオレフィンポリマー(COP)からなる群から選ばれる少なくとも一つである。基板の厚さは、好ましくは0.1~1.0mm、より好ましくは0.1~0.7mmである。有機EL素子の厚さは、好ましくは0.01~1μm、より好ましくは0.05~0.5μmである。
封止は、樹脂組成物層が有機EL素子と接するように、封止用シートと基板とを積層することにより行うことができる。なお、前記有機EL素子には、上述したような、劣化を抑制するための他の構造を有する有機EL素子も含まれる。例えば、前記有機EL素子がパッシベーション膜を有する場合、「樹脂組成物層が有機EL素子と接する」とは、「樹脂組成物層が有機EL素子のパッシベーション膜と接する」ことを意味する。
ロールラミネーターを使用する場合、そのロール速度は、支持体に対する樹脂組成物層の良好な密着性を達成するために、好ましくは10~1500mm/分、より好ましくは100~500mm/分である。
プレス機を使用する場合、そのプレス圧は、圧力によるEL素子へのクラックを防ぐために、好ましくは0.01~0.5MPa、より好ましくは0.01~0.3MPaである。ここでプレス機のプレス圧とは、真空油圧シリンダーや荷重によって制御された被プレス体にかかる圧力(即ち、封止用シート表面にかかる圧力)を意味する。
熱硬化型の封止用シートを使用する場合、封止用シートと基板との積層体を加熱して、硬化した樹脂組成物層(即ち、封止層)を形成する。硬化は、例えば、熱風循環式オーブン、赤外線ヒーター、ヒートガン、高周波誘導加熱装置、ホットプレートなどを用いて行うことができる。積層のためにプレス機を用いて熱プレスを行う場合、積層および樹脂組成物層の硬化を同時に行ってもよい。硬化温度は、使用する樹脂組成物層および支持体により異なるが、好ましくは80~120℃、より好ましくは80~110℃であり、硬化時間は、好ましくは10~120分、より好ましくは10~60分である。形成される硬化した樹脂組成物層の厚さは、好ましくは3~200μm、より好ましくは5~150μm、さらに好ましくは10~100μmである。
封止用シートの含水率(重量ppm)=(測定された水分)/(封止用シートの重量)×106
樹脂組成物層の含水率(重量ppm)=(測定された水分)/(封止用シートの重量×樹脂組成物層の重量比)×106
樹脂組成物層の重量比=(封止用シートの重量-他の層の重量)/封止用シートの重量
液状ビスフェノールA型エポキシ樹脂(三菱化学社製「jER828EL」、エポキシ当量:約185g/eq)56重量部、シランカップリング剤(信越化学工業社製「KBM403」)1.2重量部、タルク粉末(日本タルク社製「FG-15」)2重量部、および焼成ハイドロタルサイト(協和化学社製「KW2200」)15重量部を混練後、3本ロールミルにて分散を行い、混合物を得た。
ポリイソブチレン(BASF社製「Oppanol B100」、33重量%イプゾール150溶液)41重量部に、水添脂環式石油樹脂(エクソンモービル社製「Escorez5340」)20重量部と、液状ポリイソブチレン(新日本石油社製「Tetrax3T」)5重量部と、無水マレイン酸変性イソブチレン(新日本石油社製「HV-300M」)9重量部とを混合し、高速回転ミキサーで均一に分散して混合溶液を得た。この混合溶液に、エポキシ樹脂(DIC社製「HP7200H」、50重量%イプゾール溶液)5.3重量部と、アニオン重合型硬化剤(2,4,6-トリス(ジアミノメチル)フェノール)0.6重量部とを混合し、高速回転ミキサーで均一に分散して、ワニスを得た。
無水マレイン酸変性ポリプロピレン/ポリブテン共重合体(星光PMC社製「T-YP279」、プロピレン単位/ブテン単位=64重量%/36重量%、無水マレイン酸基濃度0.464mmol/g、数平均分子量35000、ランダム共重合体、40重量%スワゾール溶液)20重量部と、焼成ハイドロタルサイト(協和化学工業社製「DHT-4C」)14重量部とを混合し3本ロールで混練した後、シクロヘキシル環含有飽和炭化水素樹脂精製物(荒川化学社製「TFS13-030」、60重量%トルエン溶液)50重量部を高速回転ミキサーで混合して均一の混合溶液を得た。得られた混合溶液と、グリシジルメタクリレート変性プロピレン/ポリブテン共重合体(星光PMC社製「T-YP276」、グリシジルメタクリレート変性ポリプロピレン/ポリブテン共重合体、プロピレン単位/ブテン単位=64重量%/36重量%、グリシジル基濃度0.638mmol/g、数平均分子量57000、ランダム共重合体、40重量%スワゾール溶液)14重量部と、アニオン重合型硬化剤(2,4,6-トリス(ジアミノメチル)フェノール)0.5重量部とを高速回転ミキサーで均一に混合し、ワニスを得た。
赤外線乾燥機(日本ガイシ社製「近赤外波長制御システム」、フィラメント:カンタルまたはタングステン)、熱風乾燥機(ヤマト科学社製「精密恒温器」)または真空乾燥機(ヤマト科学社製「角型真空乾燥機」、減圧度:100Pa)を用いて、下記表1~3に示す温度および時間で、上述のようにして得られた封止用シート1~3を、カバーフィルムを剥離して、またはカバーフィルムを剥離せずに乾燥した。
有機EL素子の代わりにCa膜を形成したガラス基板を用いて、有機EL素子封止の模擬実験を行い、乾燥した封止用シートによる封止性を評価した。
○:縮小開始時間が600時間以上
△:縮小開始時間が300時間以上600時間未満
×:縮小開始時間が300時間未満
○:封止前後でCa膜表面に変化がなく、鏡面状の銀色の光沢が見られる。
△:Ca膜表面の銀色の光沢が鈍くなり、灰色に変色する。
×:Ca膜が消失し、基材側から見た際に多数の凹凸が見られる。
有機EL素子を用いて、乾燥した封止用シートによる封止性を評価した。
詳しくは、まず酸化インジウムスズ(ITO)付ガラス基板(ジオマテック社製)に発面積が4mm2となるように有機EL素子(有機膜の厚さ:110nm、Al陰極の厚さ:100nm)を形成した。
○:ダークスポットの割合が1.0%未満
△:ダークスポットの割合が1.0%以上5.0%未満
×:ダークスポットの割合が5.0%以上
発光残存面積の割合(%)=初期発光面積/発光残存面積×100
に基づき算出した。結果を下記表5に示す。
○:発光残存面積の割合が70%以上
△:発光残存面積の割合が50%以上70%未満
×:発光残存面積の割合が50%未満
Claims (10)
- 基板上の有機EL素子が樹脂組成物層で封止されている封止体の製造方法であって、
(1)支持体、樹脂組成物層およびカバーフィルムがこの順序で積層された封止用シートを、カバーフィルムを剥離せずに近赤外線乃至中赤外線乾燥機で乾燥する工程、および
(2)乾燥した封止用シートからカバーフィルムを剥離した後、封止用シートの樹脂組成物層で有機EL素子を封止する工程
を含む製造方法。 - 工程(2)が、工程(1)と同一製造ライン内で行われる請求項1に記載の製造方法。
- 工程(1)に続いて、工程(2)が行われる請求項1または2に記載の製造方法。
- 工程(1)の乾燥後から工程(2)の封止開始までの時間が1~60分である請求項1~3のいずれか一項に記載の製造方法。
- 近赤外線乃至中赤外線乾燥機から照射される近赤外線乃至中赤外線のピーク波長が、1.0~3.5μmの範囲内にある請求項1~4のいずれか一項に記載の製造方法。
- 近赤外線乃至中赤外線乾燥機における乾燥温度が60~160℃であり、乾燥時間が0.5~60分である請求項1~5のいずれか一項に記載の製造方法。
- 近赤外線乃至中赤外線乾燥機における乾燥温度が60~130℃である請求項6に記載の製造方法。
- 工程(1)後の封止用シートの含水率が、500重量ppm以下である請求項1~6のいずれか一項に記載の製造方法。
- 工程(1)後の樹脂組成物層の含水率が、2000重量ppm以下である請求項1~6のいずれか一項に記載の製造方法。
- 工程(2)における有機EL素子の封止が、樹脂組成物層が有機EL素子と接するように封止用シートと基板とを積層することにより行われる、請求項1~9のいずれか一項に記載の製造方法。
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JPWO2016158770A1 (ja) * | 2015-03-27 | 2018-01-18 | 味の素株式会社 | 封止用樹脂組成物 |
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JP7318462B2 (ja) * | 2019-09-30 | 2023-08-01 | 味の素株式会社 | 封止用樹脂組成物 |
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JP2021075009A (ja) * | 2019-11-12 | 2021-05-20 | 味の素株式会社 | 封止用シートの製造方法 |
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JP2021154627A (ja) * | 2020-03-27 | 2021-10-07 | 味の素株式会社 | 封止用シート |
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JPWO2016152756A1 (ja) | 2017-12-28 |
KR20170128578A (ko) | 2017-11-22 |
TWI738641B (zh) | 2021-09-11 |
JP6724900B2 (ja) | 2020-07-15 |
KR102578975B1 (ko) | 2023-09-18 |
TW201705580A (zh) | 2017-02-01 |
CN107409447A (zh) | 2017-11-28 |
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