JP6353991B1 - Adhesive composition, sealing sheet, and sealing body - Google Patents
Adhesive composition, sealing sheet, and sealing body Download PDFInfo
- Publication number
- JP6353991B1 JP6353991B1 JP2017561979A JP2017561979A JP6353991B1 JP 6353991 B1 JP6353991 B1 JP 6353991B1 JP 2017561979 A JP2017561979 A JP 2017561979A JP 2017561979 A JP2017561979 A JP 2017561979A JP 6353991 B1 JP6353991 B1 JP 6353991B1
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- Prior art keywords
- component
- sealing sheet
- adhesive composition
- sealing
- mass
- Prior art date
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- 238000007789 sealing Methods 0.000 title claims abstract description 109
- 239000000853 adhesive Substances 0.000 title claims abstract description 96
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 96
- 239000000203 mixture Substances 0.000 title claims abstract description 85
- 150000001875 compounds Chemical class 0.000 claims abstract description 60
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 49
- 239000004593 Epoxy Substances 0.000 claims abstract description 45
- 239000012790 adhesive layer Substances 0.000 claims abstract description 44
- 239000007787 solid Substances 0.000 claims abstract description 15
- 239000010408 film Substances 0.000 claims description 85
- 239000010410 layer Substances 0.000 claims description 51
- 230000004888 barrier function Effects 0.000 claims description 39
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 33
- 229920005989 resin Polymers 0.000 claims description 30
- 239000011347 resin Substances 0.000 claims description 30
- 239000011521 glass Substances 0.000 claims description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000010409 thin film Substances 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004973 liquid crystal related substance Substances 0.000 claims description 4
- 229940126062 Compound A Drugs 0.000 claims 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 47
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- 238000000034 method Methods 0.000 description 28
- -1 azole compound Chemical class 0.000 description 24
- 150000002500 ions Chemical class 0.000 description 24
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- 239000000178 monomer Substances 0.000 description 16
- 238000010943 off-gassing Methods 0.000 description 16
- 239000000126 substance Substances 0.000 description 14
- 239000002904 solvent Substances 0.000 description 13
- 239000000758 substrate Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- 239000003566 sealing material Substances 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 229920001709 polysilazane Polymers 0.000 description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
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- 238000012986 modification Methods 0.000 description 9
- 230000004048 modification Effects 0.000 description 9
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
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- 125000000524 functional group Chemical group 0.000 description 7
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
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- 230000000052 comparative effect Effects 0.000 description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
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- 125000001931 aliphatic group Chemical group 0.000 description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000004734 Polyphenylene sulfide Substances 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
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- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
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- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 229920001684 low density polyethylene Polymers 0.000 description 4
- 239000004702 low-density polyethylene Substances 0.000 description 4
- 229920003986 novolac Polymers 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
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- 229920002223 polystyrene Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 4
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 3
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 3
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical class CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- XUCHXOAWJMEFLF-UHFFFAOYSA-N bisphenol F diglycidyl ether Chemical compound C1OC1COC(C=C1)=CC=C1CC(C=C1)=CC=C1OCC1CO1 XUCHXOAWJMEFLF-UHFFFAOYSA-N 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 229920000092 linear low density polyethylene Polymers 0.000 description 3
- 239000004707 linear low-density polyethylene Substances 0.000 description 3
- 150000001247 metal acetylides Chemical class 0.000 description 3
- 150000003961 organosilicon compounds Chemical group 0.000 description 3
- 238000009832 plasma treatment Methods 0.000 description 3
- 229920002492 poly(sulfone) Polymers 0.000 description 3
- 229920000515 polycarbonate Polymers 0.000 description 3
- 239000004417 polycarbonate Substances 0.000 description 3
- 229920013716 polyethylene resin Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 150000003505 terpenes Chemical class 0.000 description 3
- 235000007586 terpenes Nutrition 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
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- 125000005370 alkoxysilyl group Chemical group 0.000 description 2
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
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- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
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- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
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- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
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- SYIUWAVTBADRJG-UHFFFAOYSA-N 2H-pyran-2,6(3H)-dione Chemical compound O=C1CC=CC(=O)O1 SYIUWAVTBADRJG-UHFFFAOYSA-N 0.000 description 1
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/26—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09J7/00—Adhesives in the form of films or foils
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1339—Gaskets; Spacers; Sealing of cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/724—Permeability to gases, adsorption
- B32B2307/7242—Non-permeable
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
本発明は、(A)成分:変性ポリオレフィン系樹脂、及び(B)成分:多官能エポキシ化合物を含有する接着剤組成物であって、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm3あたりのアウトガス量が20mg以下であることを特徴とする接着剤組成物、この接着剤組成物を用いて形成された接着剤層を有する封止シート、及び被封止物が前記封止シートで封止されてなる封止体である。本発明によれば、シート状に成形し易く、かつ、低アウトガス性の接着剤組成物、この接着剤組成物を用いて形成された、低アウトガス性の接着剤層を有する封止シート、及び被封止物が前記封止シートで封止されてなる封止体が提供される。The present invention is an adhesive composition containing (A) component: modified polyolefin resin, and (B) component: polyfunctional epoxy compound, and the amount of outgas is 20 ° C. for 20 minutes with respect to the solid content. When measured, the amount of outgas per 1 cm 3 of solid content is 20 mg or less, a sealing sheet having an adhesive layer formed using this adhesive composition, and encapsulation It is a sealing body formed by sealing a stationary object with the sealing sheet. According to the present invention, it is easy to form into a sheet and has a low outgas adhesive composition, a sealing sheet having a low outgas adhesive layer formed using this adhesive composition, and A sealing body is provided in which an object to be sealed is sealed with the sealing sheet.
Description
本発明は、シート状に成形し易く、かつ、低アウトガス性の接着剤組成物、この接着剤組成物を用いて形成された、低アウトガス性の接着剤層を有する封止シート、及び被封止物が前記封止シートで封止されてなる封止体に関する。 The present invention relates to an adhesive composition that is easy to be molded into a sheet and has a low outgassing property, a sealing sheet having a low outgassing adhesive layer formed by using this adhesive composition, and an encapsulant It is related with the sealing body by which a stationary thing is sealed with the said sealing sheet.
近年、有機EL素子は、低電圧直流駆動による高輝度発光が可能な発光素子として注目されている。
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。
この発光特性の低下の問題の原因として、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た。そのため、封止材を用いて有機EL素子を封止し、酸素や水分の浸入を防ぐことが行われてきた。
また、封止材を用いて有機EL素子を封止する場合、封止材からアウトガスが発生すると有機EL素子を劣化させることから、低アウトガス性の封止材の開発が行われてきた。In recent years, organic EL elements have attracted attention as light-emitting elements that can emit light with high luminance by low-voltage direct current drive.
However, 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 problem of the deterioration of the light emission characteristics, it has been considered that oxygen, moisture and the like enter the inside of the organic EL element to deteriorate the electrode and the organic layer. For this reason, it has been practiced to seal the organic EL element using a sealing material to prevent the entry of oxygen and moisture.
Moreover, when sealing an organic EL element using a sealing material, when an outgas generate | occur | produces from a sealing material, since an organic EL element will be deteriorated, the development of the low outgassing sealing material has been performed.
例えば、特許文献1には、特定のカチオン硬化性化合物、光カチオン重合開始剤、及びアゾール系化合物を含有する封止用組成物が記載されている。
特許文献1には、その封止用組成物の硬化物は、低アウトガス性及び防湿性を有することも記載されている。For example, Patent Document 1 describes a sealing composition containing a specific cationic curable compound, a photocationic polymerization initiator, and an azole compound.
Patent Document 1 also describes that the cured product of the sealing composition has low outgassing and moisture resistance.
特許文献1には、硬化遅延剤としてアゾール系化合物を用いることで、低アウトガス性の封止用組成物が得られると記載されている。
しかしながら、本発明者らの検討によれば、封止材におけるアウトガスの発生原因は硬化遅延剤だけではないため、より低アウトガス性の封止材を得るためには、さらなる検討が必要であることが分かった。Patent Document 1 describes that a low outgassing sealing composition can be obtained by using an azole compound as a curing retarder.
However, according to the study by the present inventors, the cause of outgas generation in the sealing material is not only the curing retarder, and therefore further investigation is necessary to obtain a lower outgassing sealing material. I understood.
本発明は、上記実情に鑑みてなされたものであり、シート状に成形し易く、かつ、低アウトガス性の接着剤組成物、この接着剤組成物を用いて形成された、低アウトガス性の接着剤層を有する封止シート、及び被封止物が前記封止シートで封止されてなる封止体を提供することを目的とする。 The present invention has been made in view of the above circumstances, and is easily formed into a sheet shape and has a low outgassing adhesive composition, and a low outgassing adhesive formed using this adhesive composition. It aims at providing the sealing sheet which has a sealing sheet which has an agent layer, and a to-be-sealed material is sealed with the said sealing sheet.
本発明者らは、上記課題を解決すべく鋭意検討した結果、変性ポリオレフィン系樹脂及び多官能エポキシ化合物を含有する接着剤組成物は、低アウトガス性の封止材の形成材料として適していることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the present inventors have found that an adhesive composition containing a modified polyolefin resin and a polyfunctional epoxy compound is suitable as a material for forming a low-outgas sealing material. As a result, the present invention has been completed.
かくして本発明によれば、下記(1)〜(9)の接着剤組成物、(10)〜(13)の封止シート、及び(14)、(15)の封止体、が提供される。
(1)下記の(A)成分、及び(B)成分を含有する接着剤組成物であって、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm3あたりのアウトガス量が20mg以下であることを特徴とする接着剤組成物。
(A)成分:変性ポリオレフィン系樹脂
(B)成分:多官能エポキシ化合物
(2)前記(A)成分が、酸変性ポリオレフィン系樹脂である、(1)に記載の接着剤組成物。
(3)前記(B)成分の含有量が、前記(A)成分100質量部に対して25〜200質量部である、(1)又は(2)に記載の接着剤組成物。
(4)さらに、下記の(C)成分を含有する、(1)〜(3)のいずれかに記載の接着剤組成物。
(C)成分:軟化点が80℃以上の粘着付与剤
(5)前記(C)成分の含有量が、前記(A)成分100質量部に対して1〜200質量部である、(4)に記載の接着剤組成物。
(6)さらに、下記の(D)成分を含有する、(1)〜(5)のいずれかに記載の接着剤組成物。
(D)成分:イミダゾール系硬化触媒
(7)前記(D)成分の含有量が、前記(A)成分100質量部に対して0.1〜10質量部である、(6)に記載の接着剤組成物。
(8)さらに、下記の(E)成分を含有する、(1)〜(7)のいずれかに記載の接着剤組成物。
(E)成分:シランカップリング剤
(9)前記(E)成分の含有量が、前記(A)成分100質量部に対して0.01〜10質量部である、(8)に記載の接着剤組成物。
(10)2枚の剥離フィルムと、これらの剥離フィルムに挟持された接着剤層とからなる封止シートであって、前記接着剤層が、(1)〜(9)のいずれかに記載の接着剤組成物を用いて形成されたものである封止シート。
(11)剥離フィルム、ガスバリア性フィルム、及び、前記剥離フィルムとガスバリア性フィルムに挟持された接着剤層からなる封止シートであって、前記接着剤層が、(1)〜(9)のいずれかに記載の接着剤組成物を用いて形成されたものである封止シート。
(12)前記ガスバリア性フィルムが、金属箔、樹脂製フィルム、又は薄膜ガラスである(11)に記載の封止シート。
(13)接着剤層の厚みが5〜25μmである、(10)〜(12)のいずれかに記載の封止シート。
(14)被封止物が、(10)〜(13)のいずれかに記載の封止シートで封止されてなる封止体。
(15)前記被封止物が、有機EL素子、有機ELディスプレイ素子、液晶ディスプレイ素子、又は太陽電池素子である、(14)に記載の封止体。Thus, according to the present invention, the following adhesive compositions (1) to (9), the sealing sheets (10) to (13), and the sealing bodies (14) and (15) are provided. .
(1) An adhesive composition containing the following component (A) and component (B), the solid content of which is 1 cm 3 when the outgas amount is measured at 120 ° C. for 20 minutes. An adhesive composition, wherein the amount of pergassing is 20 mg or less.
(A) component: modified polyolefin resin (B) component: polyfunctional epoxy compound (2) The adhesive composition according to (1), wherein the component (A) is an acid-modified polyolefin resin.
(3) The adhesive composition according to (1) or (2), wherein the content of the component (B) is 25 to 200 parts by mass with respect to 100 parts by mass of the component (A).
(4) The adhesive composition according to any one of (1) to (3), further comprising the following component (C).
Component (C): Tackifier having a softening point of 80 ° C. or higher (5) The content of the component (C) is 1 to 200 parts by mass with respect to 100 parts by mass of the component (A), (4) The adhesive composition described in 1.
(6) The adhesive composition according to any one of (1) to (5), further comprising the following component (D).
Component (D): Imidazole-based curing catalyst (7) Adhesion according to (6), wherein the content of component (D) is 0.1 to 10 parts by mass with respect to 100 parts by mass of component (A). Agent composition.
(8) The adhesive composition according to any one of (1) to (7), further comprising the following component (E):
(E) Component: Silane coupling agent (9) Adhesion according to (8), wherein the content of component (E) is 0.01 to 10 parts by mass with respect to 100 parts by mass of component (A). Agent composition.
(10) A sealing sheet comprising two release films and an adhesive layer sandwiched between these release films, wherein the adhesive layer is any one of (1) to (9) A sealing sheet that is formed using an adhesive composition.
(11) A sealing sheet comprising a release film, a gas barrier film, and an adhesive layer sandwiched between the release film and the gas barrier film, wherein the adhesive layer is any one of (1) to (9) A sealing sheet formed using the adhesive composition according to claim 1.
(12) The sealing sheet according to (11), wherein the gas barrier film is a metal foil, a resin film, or thin film glass.
(13) The sealing sheet according to any one of (10) to (12), wherein the adhesive layer has a thickness of 5 to 25 μm.
(14) A sealed body in which an object to be sealed is sealed with the sealing sheet according to any one of (10) to (13).
(15) The sealed body according to (14), wherein the object to be sealed is an organic EL element, an organic EL display element, a liquid crystal display element, or a solar cell element.
本発明によれば、シート状に成形し易く、かつ、低アウトガス性の接着剤組成物、この接着剤組成物を用いて形成された、低アウトガス性の接着剤層を有する封止シート、及び被封止物が前記封止シートで封止されてなる封止体が提供される。 According to the present invention, it is easy to form into a sheet and has a low outgas adhesive composition, a sealing sheet having a low outgas adhesive layer formed using this adhesive composition, and A sealing body is provided in which an object to be sealed is sealed with the sealing sheet.
以下、本発明を、1)接着剤組成物、2)封止シート、及び、3)封止体、に項分けして詳細に説明する。
本明細書において、「低アウトガス性」とは、接着剤組成物の固形分(又は、接着剤組成物から形成された接着剤層)が高温環境下に置かれた場合であっても、放出されるアウトガス量が少ないという、接着剤組成物又は接着剤層の特性をいう。Hereinafter, the present invention will be described in detail by dividing it into 1) an adhesive composition, 2) a sealing sheet, and 3) a sealing body.
As used herein, “low outgassing” refers to release even when the solid content of the adhesive composition (or the adhesive layer formed from the adhesive composition) is placed in a high temperature environment. The characteristic of the adhesive composition or adhesive layer that the amount of outgas produced is small.
1)接着剤組成物
本発明の接着剤組成物は、下記の(A)成分、及び(B)成分を含有する接着剤組成物であって、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm3あたりのアウトガス量が20mg以下であることを特徴とする。
(A)成分:変性ポリオレフィン系樹脂
(B)成分:多官能エポキシ化合物1) Adhesive composition The adhesive composition of this invention is an adhesive composition containing the following (A) component and (B) component, Comprising: On the conditions for 120 degreeC and 20 minutes about the solid content When the outgas amount is measured, the outgas amount per 1 cm 3 of the solid content is 20 mg or less.
(A) component: modified polyolefin resin (B) component: polyfunctional epoxy compound
変性ポリオレフィン系樹脂は、官能基が導入されたポリオレフィン樹脂である。
ポリオレフィン樹脂は、オレフィン系単量体由来の繰り返し単位を含む重合体である。ポリオレフィン樹脂は、オレフィン系単量体由来の繰り返し単位の一種のみからなる単独重合体であっても、オレフィン系単量体由来の繰り返し単位の二種以上からなる共重合体であっても、オレフィン系単量体由来の繰り返し単位と、オレフィン系単量体と共重合可能な他の単量体(オレフィン系単量体以外の他の単量体)由来の繰り返し単位とからなる共重合体であってもよい。The modified polyolefin resin is a polyolefin resin having a functional group introduced therein.
The polyolefin resin is a polymer containing a repeating unit derived from an olefin monomer. The polyolefin resin may be a homopolymer consisting of only one type of repeating unit derived from an olefinic monomer or a copolymer consisting of two or more types of repeating units derived from an olefinic monomer. A copolymer comprising a repeating unit derived from a monomer and a repeating unit derived from another monomer copolymerizable with the olefin monomer (other monomers other than the olefin monomer) There may be.
オレフィン系単量体としては、炭素数2〜8のα−オレフィンが好ましく、エチレン、プロピレン、1−ブテン、イソブチレン、又は1−ヘキセンがより好ましく、エチレン又はプロピレンがさらに好ましい。
オレフィン系単量体と共重合可能な他の単量体としては、酢酸ビニル、(メタ)アクリル酸エステル、スチレン等が挙げられる。ここで、(メタ)アクリル酸とは、アクリル酸又はメタクリル酸の意味を表す(以下にて同じ)。The olefin monomer is preferably an α-olefin having 2 to 8 carbon atoms, more preferably ethylene, propylene, 1-butene, isobutylene, or 1-hexene, and further preferably ethylene or propylene.
Examples of other monomers copolymerizable with the olefin monomer include vinyl acetate, (meth) acrylic acid ester, and styrene. Here, (meth) acrylic acid represents the meaning of acrylic acid or methacrylic acid (the same applies hereinafter).
ポリオレフィン樹脂としては、超低密度ポリエチレン(VLDPE)、低密度ポリエチレン(LDPE)、中密度ポリエチレン(MDPE)、高密度ポリエチレン(HDPE)、直鎖状低密度ポリエチレン、ポリプロピレン(PP)、エチレン−プロピレン共重合体、オレフィン系エラストマー(TPO)、エチレン−酢酸ビニル共重合体(EVA)、エチレン−(メタ)アクリル酸共重合体、エチレン−(メタ)アクリル酸エステル共重合体などが挙げられるが、これらに限定されるものではない。 Examples of polyolefin resins include very low density polyethylene (VLDPE), low density polyethylene (LDPE), medium density polyethylene (MDPE), high density polyethylene (HDPE), linear low density polyethylene, polypropylene (PP), and ethylene-propylene. Polymer, olefin elastomer (TPO), ethylene-vinyl acetate copolymer (EVA), ethylene- (meth) acrylic acid copolymer, ethylene- (meth) acrylic acid ester copolymer, etc. It is not limited to.
変性ポリオレフィン樹脂は、前駆体としてのポリオレフィン樹脂に、変性剤を用いて変性処理を施して得ることができる。
ポリオレフィン樹脂の変性処理に用いる変性剤は、分子内に、官能基、すなわち、後述する架橋反応に寄与し得る基を有する化合物である。
官能基としては、カルボキシル基、カルボン酸無水物基、カルボン酸エステル基、水酸基、エポキシ基、アミド基、アンモニウム基、ニトリル基、アミノ基、イミド基、イソシアネート基、アセチル基、チオール基、エーテル基、チオエーテル基、スルホン基、リン酸基、ニトロ基、ウレタン基、ハロゲン原子等が挙げられる。これらの中でも、カルボキシル基、カルボン酸無水物基、カルボン酸エステル基、水酸基、アンモニウム基、アミノ基、イミド基、イソシアネート基が好ましく、カルボン酸無水物基、アルコキシシリル基がより好ましく、カルボン酸無水物基が特に好ましい。
官能基を有する化合物は、分子内に2種以上の官能基を有していてもよい。The modified polyolefin resin can be obtained by subjecting a polyolefin resin as a precursor to a modification treatment using a modifier.
The modifier used for the modification treatment of the polyolefin resin is a compound having a functional group in the molecule, that is, a group that can contribute to a crosslinking reaction described later.
Functional groups include carboxyl groups, carboxylic anhydride groups, carboxylic ester groups, hydroxyl groups, epoxy groups, amide groups, ammonium groups, nitrile groups, amino groups, imide groups, isocyanate groups, acetyl groups, thiol groups, ether groups. Thioether group, sulfone group, phosphoric acid group, nitro group, urethane group, halogen atom and the like. Among these, a carboxyl group, a carboxylic anhydride group, a carboxylic ester group, a hydroxyl group, an ammonium group, an amino group, an imide group, and an isocyanate group are preferable, a carboxylic anhydride group and an alkoxysilyl group are more preferable, and a carboxylic anhydride Physical groups are particularly preferred.
The compound having a functional group may have two or more kinds of functional groups in the molecule.
変性ポリオレフィン系樹脂としては、酸変性ポリオレフィン系樹脂、シラン変性ポリオレフィン系樹脂が挙げられる。なかでも、本発明のより優れた効果が得られる観点から、酸変性ポリオレフィン系樹脂が好ましい。 Examples of modified polyolefin resins include acid-modified polyolefin resins and silane-modified polyolefin resins. Among these, an acid-modified polyolefin resin is preferable from the viewpoint of obtaining the superior effect of the present invention.
酸変性ポリオレフィン系樹脂とは、ポリオレフィン樹脂に対して酸でグラフト変性したものをいう。例えば、ポリオレフィン樹脂に不飽和カルボン酸を反応させて、カルボキシル基を導入(グラフト変性)したものが挙げられる。なお、本明細書において、不飽和カルボン酸とは、カルボン酸無水物の概念を含み、カルボキシル基とは、カルボン酸無水物基の概念を含むものである。 The acid-modified polyolefin resin refers to a resin obtained by graft modification with an acid to a polyolefin resin. For example, a polyolefin resin may be reacted with an unsaturated carboxylic acid to introduce a carboxyl group (graft modification). In the present specification, the unsaturated carboxylic acid includes the concept of carboxylic anhydride, and the carboxyl group includes the concept of carboxylic anhydride group.
ポリオレフィン樹脂に反応させる不飽和カルボン酸としては、マレイン酸、フマル酸、イタコン酸、シトラコン酸、グルタコン酸、テトラヒドロフタル酸、アコニット酸、無水マレイン酸、無水イタコン酸、無水グルタコン酸、無水シトラコン酸、無水アコニット酸、ノルボルネンジカルボン酸無水物、テトラヒドロフタル酸無水物等が挙げられる。
これらは、1種を単独で、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、接着強度により優れる接着剤組成物が得られ易いことから、無水マレイン酸が好ましい。Examples of the unsaturated carboxylic acid to be reacted with the polyolefin resin include maleic acid, fumaric acid, itaconic acid, citraconic acid, glutaconic acid, tetrahydrophthalic acid, aconitic acid, maleic anhydride, itaconic anhydride, glutaconic anhydride, citraconic anhydride, Examples thereof include aconitic anhydride, norbornene dicarboxylic acid anhydride, and tetrahydrophthalic acid anhydride.
These can be used alone or in combination of two or more. Among these, maleic anhydride is preferable because an adhesive composition having better adhesive strength can be easily obtained.
ポリオレフィン樹脂に反応させる不飽和カルボン酸の量は、ポリオレフィン樹脂100質量部に対して、好ましくは0.1〜5質量部、より好ましくは0.2〜3質量部、さらに好ましくは0.2〜1.0質量部である。このようにして得られた酸変性ポリオレフィン系樹脂を含有する接着剤組成物は、接着強度により優れる。 The amount of the unsaturated carboxylic acid to be reacted with the polyolefin resin is preferably 0.1 to 5 parts by mass, more preferably 0.2 to 3 parts by mass, and still more preferably 0.2 to 100 parts by mass with respect to 100 parts by mass of the polyolefin resin. 1.0 part by mass. The adhesive composition containing the acid-modified polyolefin resin thus obtained is more excellent in adhesive strength.
本発明においては、酸変性ポリオレフィン系樹脂として、市販品を用いることもできる。市販品としては、例えば、アドマー(登録商標)(三井化学社製)、ユニストール(登録商標)(三井化学社製)、BondyRam(Polyram社製)、orevac(登録商標)(ARKEMA社製)、モディック(登録商標)(三菱化学社製)等が挙げられる。 In the present invention, a commercially available product may be used as the acid-modified polyolefin resin. Examples of commercially available products include Admer (registered trademark) (manufactured by Mitsui Chemicals), Unistor (registered trademark) (manufactured by Mitsui Chemicals), BondyRam (manufactured by Polyram), orevac (registered trademark) (manufactured by ARKEMA), Modic (registered trademark) (manufactured by Mitsubishi Chemical Corporation) and the like.
シラン変性ポリオレフィン系樹脂とは、ポリオレフィン樹脂に対して不飽和シラン化合物でグラフト変性したものをいう。シラン変性ポリオレフィン系樹脂は、主鎖であるポリオレフィン樹脂に不飽和シラン化合物がグラフト共重合した構造を有する。シラン変性ポリオレフィン系樹脂としては、特限定されないが、シラン変性ポリエチレン樹脂やシラン変性エチレン−酢酸ビニル共重合体が挙げられる。なかでも、シラン変性低密度ポリエチレン、シラン変性超低密度ポリエチレン、シラン変性直鎖状低密度ポリエチレン等のシラン変性ポリエチレン樹脂が好ましい。 A silane-modified polyolefin resin refers to a resin obtained by graft modification with an unsaturated silane compound to a polyolefin resin. The silane-modified polyolefin resin has a structure in which an unsaturated silane compound is graft copolymerized with a polyolefin resin as a main chain. Although it does not specifically limit as a silane modified polyolefin resin, A silane modified polyethylene resin and a silane modified ethylene-vinyl acetate copolymer are mentioned. Of these, silane-modified polyethylene resins such as silane-modified low-density polyethylene, silane-modified ultra-low-density polyethylene, and silane-modified linear low-density polyethylene are preferable.
上記ポリオレフィン樹脂に反応させる不飽和シラン化合物としては、ビニルシラン化合物が好ましい。ビニルシラン化合物としては、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリプロポキシシラン、ビニルトリイソプロポキシシラン、ビニルトリブトキシシラン、ビニルトリペンチロキシシラン、ビニルトリフェノキシシラン、ビニルトリベンジルオキシシラン、ビニルトリメチレンジオキシシラン、ビニルトリエチレンジオキシシラン、ビニルプロピオニルオキシシラン、ビニルトリアセトキシシラン、ビニルトリカルボキシシラン等が挙げられる。これらは、1種単独で、または2種以上を組み合わせて用いることができる。
不飽和シラン化合物を主鎖であるポリオレフィン樹脂にグラフト重合させるときの条件は、公知のグラフト重合の常法を採用すればよい。As the unsaturated silane compound to be reacted with the polyolefin resin, a vinyl silane compound is preferable. Vinyl silane compounds include vinyl trimethoxy silane, vinyl triethoxy silane, vinyl tripropoxy silane, vinyl triisopropoxy silane, vinyl tributoxy silane, vinyl tripentyloxy silane, vinyl triphenoxy silane, vinyl tribenzyloxy silane, vinyl tri Examples include methylenedioxysilane, vinyltriethylenedioxysilane, vinylpropionyloxysilane, vinyltriacetoxysilane, and vinyltricarboxysilane. These can be used individually by 1 type or in combination of 2 or more types.
As a condition for graft polymerization of the unsaturated silane compound to the polyolefin resin as the main chain, a known conventional method of graft polymerization may be employed.
ポリオレフィン樹脂に反応させる不飽和シラン化合物の量は、ポリオレフィン樹脂100質量部に対して、0.1〜10質量部であることが好ましく、特に0.3〜7質量部であることが好ましく、さらには0.5〜5質量部であることが好ましい。反応させる不飽和シラン化合物の量が上記の範囲にあると、得られるシラン変性ポリオレフィン系樹脂を含有する接着剤組成物は、接着強度により優れるものとなる。 The amount of the unsaturated silane compound to be reacted with the polyolefin resin is preferably 0.1 to 10 parts by mass, particularly preferably 0.3 to 7 parts by mass, with respect to 100 parts by mass of the polyolefin resin. Is preferably 0.5 to 5 parts by mass. When the amount of the unsaturated silane compound to be reacted is in the above range, the adhesive composition containing the resulting silane-modified polyolefin resin is more excellent in adhesive strength.
本発明においては、シラン変性ポリオレフィン系樹脂として、市販品を用いることもできる。市販品としては、例えば、リンクロン(登録商標)(三菱化学社製)等が挙げられ、中でも、低密度ポリエチレン系のリンクロン、直鎖状低密度ポリエチレン系のリンクロン、超低密度ポリエチレン系のリンクロン、およびエチレン−酢酸ビニル共重合体系のリンクロンを好ましく使用することができる。 In the present invention, a commercially available product can also be used as the silane-modified polyolefin resin. Commercially available products include, for example, Linklon (registered trademark) (manufactured by Mitsubishi Chemical Corporation), among others, low density polyethylene-based linklon, linear low-density polyethylene-based linkron, and ultra-low-density polyethylene-based. Of these, Rincron of ethylene-vinyl acetate copolymer system can be preferably used.
変性ポリオレフィン系樹脂は、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。 Modified polyolefin-type resin can be used individually by 1 type or in combination of 2 or more types.
変性ポリオレフィン系樹脂の数平均分子量(Mn)は特に限定されないが、本発明のより優れた効果が得られる観点から、10,000〜2,000,000が好ましく、20,000〜1,500,000であることがより好ましい。
変性ポリオレフィン系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。The number average molecular weight (Mn) of the modified polyolefin resin is not particularly limited, but is preferably 10,000 to 2,000,000, more preferably 20,000 to 1,500, from the viewpoint of obtaining the better effect of the present invention. More preferably, it is 000.
The number average molecular weight (Mn) of the modified polyolefin resin can be obtained as a standard polystyrene equivalent value by performing gel permeation chromatography using tetrahydrofuran as a solvent.
変性ポリオレフィン系樹脂の含有量は特に限定されないが、本発明のより優れた効果が得られる観点から、変性ポリオレフィン系樹脂と下記の(B)成分の合計量が、接着剤組成物の固形分を基準として、30質量%以上が好ましく、50質量%以上であることがより好ましい。 The content of the modified polyolefin resin is not particularly limited, but from the viewpoint of obtaining the better effect of the present invention, the total amount of the modified polyolefin resin and the following component (B) determines the solid content of the adhesive composition. As a reference, 30% by mass or more is preferable, and 50% by mass or more is more preferable.
(B)成分:多官能エポキシ化合物
本発明の接着剤組成物は、(B)成分として、多官能エポキシ化合物を含有する。
本発明の接着剤組成物は、多官能エポキシ化合物を含有するため、その硬化物は水蒸気遮断性に優れるものとなる。(B) component: Multifunctional epoxy compound The adhesive composition of this invention contains a polyfunctional epoxy compound as (B) component.
Since the adhesive composition of the present invention contains a polyfunctional epoxy compound, the cured product has excellent water vapor barrier properties.
多官能エポキシ化合物とは、分子内に少なくともエポキシ基を2つ以上有する化合物のことをいう。 The polyfunctional epoxy compound refers to a compound having at least two epoxy groups in the molecule.
エポキシ基を2つ以上有するエポキシ化合物としては、ビスフェノールAジグリシジルエーテル、ビスフェノールFジグリシジルエーテル、ビスフェノールSジグリシジルエーテル、臭素化ビスフェノールAジグリシジルエーテル、臭素化ビスフェノールFジグリシジルエーテル、臭素化ビスフェノールSジグリシジルエーテル、ノボラック型エポキシ樹脂(例えばフェノール・ノボラック型エポキシ樹脂、クレゾール・ノボラック型エポキシ樹脂、臭素化フェノール・ノボラック型エポキシ樹脂)、水添ビスフェノールAジグリシジルエーテル、水添ビスフェノールFジグリシジルエーテル、水添ビスフェノールSジグリシジルエーテル、ペンタエリスリトールポリ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、ヘキサヒドロフタル酸ジグリシジルエステル、ネオペンチルグリコールジグリシジルエーテル、トリメチロールプロパンポリグリシジルエーテル、2,2−ビス(3−グリシジル−4−グリシジルオキシフェニル)プロパン、ジメチロールトリシクロデカンジグリシジルエーテル等が挙げられる。
これらの多官能エポキシ化合物は、1種を単独で、あるいは2種以上を組み合わせて用いることができる。Examples of epoxy compounds having two or more epoxy groups include bisphenol A diglycidyl ether, bisphenol F diglycidyl ether, bisphenol S diglycidyl ether, brominated bisphenol A diglycidyl ether, brominated bisphenol F diglycidyl ether, and brominated bisphenol S. Diglycidyl ether, novolac type epoxy resin (for example, phenol novolac type epoxy resin, cresol novolac type epoxy resin, brominated phenol novolac type epoxy resin), hydrogenated bisphenol A diglycidyl ether, hydrogenated bisphenol F diglycidyl ether, Hydrogenated bisphenol S diglycidyl ether, pentaerythritol polyglycidyl ether, 1,6-hexanediol diglycidyl ether, Oxahydrophthalic acid diglycidyl ester, neopentyl glycol diglycidyl ether, trimethylolpropane polyglycidyl ether, 2,2-bis (3-glycidyl-4-glycidyloxyphenyl) propane, dimethyloltricyclodecane diglycidyl ether, etc. Can be mentioned.
These polyfunctional epoxy compounds can be used individually by 1 type or in combination of 2 or more types.
多官能エポキシ化合物の重量平均分子量の下限は、好ましくは1,000、より好ましくは1,200である。多官能エポキシ化合物の重量平均分子量の上限は、好ましくは5,000、より好ましくは4,500である。多官能エポキシ化合物の重量平均分子量が1,000以上の接着剤組成物を用いることで、より低アウトガス性の封止材を形成することができる。多官能エポキシ化合物の重量平均分子量が5,000以下の接着剤組成物は流動性により優れ、被封止物の表面の凹凸や被封止物の厚みにより生じる凹凸を十分に埋めることができる(凹凸追従性に優れる)。 The lower limit of the weight average molecular weight of the polyfunctional epoxy compound is preferably 1,000, more preferably 1,200. The upper limit of the weight average molecular weight of the polyfunctional epoxy compound is preferably 5,000, more preferably 4,500. By using an adhesive composition having a polyfunctional epoxy compound having a weight average molecular weight of 1,000 or more, a lower outgassing sealing material can be formed. The adhesive composition having a polyfunctional epoxy compound having a weight average molecular weight of 5,000 or less is excellent in fluidity, and can sufficiently fill the unevenness caused by the unevenness of the surface of the object to be sealed and the thickness of the object to be sealed ( Excellent ruggedness followability).
多官能エポキシ化合物のエポキシ当量は、好ましくは100g/eq以上500g/eq以下、より好ましくは150g/eq以上300g/eq以下である。多官能エポキシ化合物のエポキシ当量が100g/eq以上500g/eq以下の接着剤組成物を用いることで、より低アウトガス性の封止材を形成することができる。 The epoxy equivalent of the polyfunctional epoxy compound is preferably 100 g / eq or more and 500 g / eq or less, more preferably 150 g / eq or more and 300 g / eq or less. By using an adhesive composition having an epoxy equivalent of 100 g / eq or more and 500 g / eq or less of the polyfunctional epoxy compound, it is possible to form a lower outgassing sealing material.
本発明の接着剤組成物中における多官能エポキシ化合物の含有量は、前記(A)成分100質量部に対して、好ましくは25〜200質量部、より好ましくは50〜150質量部である。多官能エポキシ化合物の含有量がこの範囲内にある接着剤組成物の硬化物は水蒸気遮断性により優れる。 The content of the polyfunctional epoxy compound in the adhesive composition of the present invention is preferably 25 to 200 parts by mass, more preferably 50 to 150 parts by mass with respect to 100 parts by mass of the component (A). Hardened | cured material of the adhesive composition in which content of a polyfunctional epoxy compound exists in this range is excellent by water vapor | steam barrier property.
本発明の接着剤組成物は、前記(A)成分、(B)成分以外の成分を含有してもよい。
(A)成分、(B)成分以外の成分としては、下記(C)成分、(D)成分、及び(E)成分が挙げられる。
(C)成分:軟化点が80℃以上の粘着付与剤
(D)成分:イミダゾール系硬化触媒
(E)成分:シランカップリング剤The adhesive composition of this invention may contain components other than the said (A) component and (B) component.
As components other than (A) component and (B) component, the following (C) component, (D) component, and (E) component are mentioned.
Component (C): Tackifier having a softening point of 80 ° C. or higher (D) Component: Imidazole-based curing catalyst (E) component: Silane coupling agent
(C)成分:軟化点が80℃以上の粘着付与剤
(B)成分を含有する接着剤組成物は硬化前の貯蔵弾性率が低く、凹凸追従性に優れる。しかしながら、そのような接着剤組成物は、一定の形状を保ちにくく、シート状に成形するのが困難な場合がある。このようなときは、(C)成分を含有することで、成形性を改善することができる。Component (C): Tackifier having a softening point of 80 ° C. or higher The adhesive composition containing the component (B) has a low storage elastic modulus before curing and is excellent in unevenness followability. However, such an adhesive composition may be difficult to maintain a certain shape and difficult to be formed into a sheet shape. In such a case, the moldability can be improved by containing the component (C).
粘着付与剤としては、重合ロジン、重合ロジンエステル、ロジン誘導体等のロジン系樹脂;ポリテルペン樹脂、芳香族変性テルペン樹脂及びその水素化物、テルペンフェノール樹脂等のテルペン系樹脂;クマロン・インデン樹脂;脂肪族石油系樹脂、芳香族系石油樹脂及びその水素化物、脂肪族/芳香族共重合体石油樹脂等の石油樹脂;スチレン又は置換スチレンの低分子量重合体;α−メチルスチレン単一重合系樹脂、α−メチルスチレン/スチレン共重合系樹脂、スチレン系モノマー/脂肪族系モノマー共重合系樹脂、スチレン系モノマー/α−メチルスチレン/脂肪族系モノマー共重合系樹脂、スチレン系モノマー単一重合系樹脂、スチレン系モノマー/芳香族系モノマー共重合系樹脂等のスチレン系樹脂;等が挙げられる。これらの中でも、スチレン系樹脂が好ましく、スチレン系モノマー/脂肪族系モノマー共重合系樹脂がより好ましい。
これらの粘着付与剤は、1種を単独で、あるいは2種以上を組み合わせて用いることができる。Examples of tackifiers include rosin resins such as polymerized rosin, polymerized rosin ester, and rosin derivatives; terpene resins such as polyterpene resins, aromatic modified terpene resins and hydrides thereof, and terpene phenol resins; coumarone and indene resins; aliphatic Petroleum resins such as petroleum resins, aromatic petroleum resins and their hydrides, aliphatic / aromatic copolymer petroleum resins; low molecular weight polymers of styrene or substituted styrene; α-methylstyrene monopolymer resins, α -Methylstyrene / styrene copolymer resin, styrene monomer / aliphatic monomer copolymer resin, styrene monomer / α-methylstyrene / aliphatic monomer copolymer resin, styrene monomer monopolymer resin, Styrene resin such as styrene monomer / aromatic monomer copolymer resin; and the like. Among these, a styrene resin is preferable, and a styrene monomer / aliphatic monomer copolymer resin is more preferable.
These tackifiers can be used singly or in combination of two or more.
粘着付与剤の軟化点は80℃以上である。粘着付与剤の軟化点が80℃以上であることで、高温時における粘着性に優れる接着剤組成物が得られる。また、接着剤組成物をシート状に成形する際の作業性が向上する。 The softening point of the tackifier is 80 ° C. or higher. The adhesive composition which is excellent in the adhesiveness at the time of high temperature is obtained because the softening point of a tackifier is 80 degreeC or more. Moreover, the workability | operativity at the time of shape | molding an adhesive composition in a sheet form improves.
本発明の接着剤組成物が、軟化点が80℃以上の粘着付与剤を含有する場合、その含有量は、前記(A)成分100質量部に対して、好ましくは1〜200質量部、より好ましくは10〜150質量部である。軟化点が80℃以上の粘着付与剤が少な過ぎると、接着剤組成物をシート状に成形することが困難になるおそれがある。一方、軟化点が80℃以上の粘着付与剤が多過ぎると、接着剤層が脆くなるおそれがある。 When the adhesive composition of the present invention contains a tackifier having a softening point of 80 ° C. or higher, the content is preferably 1 to 200 parts by mass with respect to 100 parts by mass of the component (A). Preferably it is 10-150 mass parts. If there are too few tackifiers having a softening point of 80 ° C. or higher, it may be difficult to form the adhesive composition into a sheet. On the other hand, when there are too many tackifiers whose softening point is 80 degreeC or more, there exists a possibility that an adhesive bond layer may become weak.
(D)成分:イミダゾール系硬化触媒
イミダゾール系硬化触媒は、イミダゾール骨格を有する化合物であって、接着剤組成物の硬化反応を触媒する作用を有するものである。
イミダゾール系硬化触媒としては、2−メチルイミダゾール、2−フェニルイミダゾール、2−ウンデシルイミダゾール、2−ヘプタデシルイミダゾール、2−エチル−4−メチルイミダゾール、2−フェニル−4−メチルイミダゾール、2−フェニル−4−メチル−5−ヒドロキシメチルイミダゾール、2−フェニル−4,5−ジヒドロキシメチルイミダゾール等が挙げられる。これらの中でも、2−エチル−4−メチルイミダゾールが好ましい。
これらのイミダゾール系硬化触媒は、1種を単独で、あるいは2種以上を組み合わせて用いることができる。Component (D): Imidazole-based curing catalyst The imidazole-based curing catalyst is a compound having an imidazole skeleton, and has an action of catalyzing the curing reaction of the adhesive composition.
Examples of imidazole curing catalysts include 2-methylimidazole, 2-phenylimidazole, 2-undecylimidazole, 2-heptadecylimidazole, 2-ethyl-4-methylimidazole, 2-phenyl-4-methylimidazole, and 2-phenyl. Examples include -4-methyl-5-hydroxymethylimidazole, 2-phenyl-4,5-dihydroxymethylimidazole and the like. Among these, 2-ethyl-4-methylimidazole is preferable.
These imidazole-based curing catalysts can be used singly or in combination of two or more.
イミダゾール系硬化触媒を含有する接着剤組成物を用いることで、高温時においても優れた接着性を有する硬化物が得られ易くなる。 By using an adhesive composition containing an imidazole-based curing catalyst, a cured product having excellent adhesiveness can be easily obtained even at high temperatures.
本発明の接着剤組成物がイミダゾール系硬化触媒を含有する場合、その含有量は、前記(A)成分100質量部に対して、好ましくは0.1〜10質量部、より好ましくは0.2〜5質量部である。イミダゾール系硬化触媒の含有量がこの範囲内にある接着剤組成物の硬化物は高温時においても優れた接着性を有する。 When the adhesive composition of the present invention contains an imidazole-based curing catalyst, the content thereof is preferably 0.1 to 10 parts by mass, more preferably 0.2 to 100 parts by mass of the component (A). -5 parts by mass. The cured product of the adhesive composition having an imidazole-based curing catalyst content within this range has excellent adhesiveness even at high temperatures.
(E)成分:シランカップリング剤
シランカップリング剤は、分子内に有機材料と反応結合する官能基、および無機材料と反応結合する官能基(加水分解性基)を同時に有する有機ケイ素化合物である。
シランカップリング剤としては、公知のシランカップリング剤を用いることができ、なかでも、分子内にアルコキシシリル基を少なくとも1個有する有機ケイ素化合物が好ましい。
シランカップリング剤としては、ビニルトリメトキシシラン、ビニルトリエトキシシラン、メタクリロキシプロピルトリメトキシシラン等の重合性不飽和基含有ケイ素化合物;3−グリシドキシプロピルトリメトキシシラン、2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン等のエポキシ構造を有するケイ素化合物;3−アミノプロピルトリメトキシシラン、N−(2−アミノエチル)−3−アミノプロピルトリメトキシシラン、N−(2−アミノエチル)−3−アミノプロピルメチルジメトキシシラン等のアミノ基含有ケイ素化合物;3−クロロプロピルトリメトキシシラン;3−イソシアネートプロピルトリエトキシシラン;等が挙げられる。
これらのシランカップリング剤は、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。(E) Component: Silane Coupling Agent A silane coupling agent is an organosilicon compound having simultaneously a functional group reactively bonded to an organic material and a functional group reactively bonded to an inorganic material (hydrolyzable group) in the molecule. .
As the silane coupling agent, a known silane coupling agent can be used, and among them, an organosilicon compound having at least one alkoxysilyl group in the molecule is preferable.
Examples of the silane coupling agent include polymerizable unsaturated group-containing silicon compounds such as vinyltrimethoxysilane, vinyltriethoxysilane, and methacryloxypropyltrimethoxysilane; 3-glycidoxypropyltrimethoxysilane, 2- (3,4 -Epoxycyclohexyl) silicon compound having an epoxy structure such as ethyltrimethoxysilane; 3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, N- (2-aminoethyl) An amino group-containing silicon compound such as -3-aminopropylmethyldimethoxysilane; 3-chloropropyltrimethoxysilane; 3-isocyanatopropyltriethoxysilane;
These silane coupling agents can be used alone or in combination of two or more.
シランカップリング剤を含有する接着剤組成物を用いることで、常温(15℃〜30℃)及び高温(40℃〜100℃)環境下における接着強度により優れた硬化物が得られ易くなる。 By using an adhesive composition containing a silane coupling agent, it becomes easy to obtain a cured product having better adhesive strength in a normal temperature (15 ° C. to 30 ° C.) and high temperature (40 ° C. to 100 ° C.) environment.
本発明の接着剤組成物がシランカップリング剤を含有する場合、接着強度にさらに優れた硬化物が得られる観点から、その含有量は、前記(A)成分100質量部に対して、好ましくは0.01〜10質量部、より好ましくは0.02〜5質量部である。 In the case where the adhesive composition of the present invention contains a silane coupling agent, the content is preferably based on 100 parts by mass of the component (A) from the viewpoint of obtaining a cured product having further excellent adhesive strength. It is 0.01-10 mass parts, More preferably, it is 0.02-5 mass parts.
本発明の接着剤組成物は、溶媒を含有してもよい。
溶媒としては、ベンゼン、トルエンなどの芳香族炭化水素系溶媒;酢酸エチル、酢酸ブチルなどのエステル系溶媒;アセトン、メチルエチルケトン、メチルイソブチルケトンなどのケトン系溶媒;n−ペンタン、n−ヘキサン、n−ヘプタンなど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、メチルシクロヘキサンなど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。
溶媒の含有量は、塗工性等を考慮して適宜決定することができる。The adhesive composition of the present invention may contain a solvent.
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, and n- And aliphatic hydrocarbon solvents such as heptane; alicyclic hydrocarbon solvents such as cyclopentane, cyclohexane, and methylcyclohexane;
These solvents can be used alone or in combination of two or more.
The content of the solvent can be appropriately determined in consideration of coating properties and the like.
本発明の接着剤組成物は、本発明の効果を妨げない範囲で、その他の成分を含有してもよい。
その他の成分としては、紫外線吸収剤、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。
本発明の接着剤組成物がこれらの添加剤を含有する場合、その含有量は、目的に合わせて適宜決定することができる。The adhesive composition of the present invention may contain other components as long as the effects of the present invention are not hindered.
Examples of other components include additives such as ultraviolet absorbers, antistatic agents, light stabilizers, antioxidants, resin stabilizers, fillers, pigments, extenders and softeners.
These can be used alone or in combination of two or more.
When the adhesive composition of this invention contains these additives, the content can be suitably determined according to the objective.
本発明の接着剤組成物は、所定の成分を、常法に従って適宜混合・攪拌することにより調製することができる。 The adhesive composition of the present invention can be prepared by appropriately mixing and stirring predetermined components according to a conventional method.
本発明の接着剤組成物は、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm2あたりのアウトガス量が20mg以下であり、18mg以下が好ましく、15mg以下がより好ましく、10mg以下が特に好ましく、8mg以下が最も好ましい。下限値は特にないが、通常、0.1mg以上である。本明細書において、固形分とは、接着剤組成物から溶剤などの揮発する物質を除いた固形部分をいう。
また、重量平均分子量が1,000〜5,000である多官能性エポキシ化合物を用いることで、低アウトガス性の接着剤層をより容易に形成することができる。The adhesive composition of the present invention, the on solids 120 ° C., as measured outgas amount in for 20 minutes, and the outgas amount of the total solid content 1 cm 2 is 20mg or less, preferably 18 mg, 15 mg or less Is more preferably 10 mg or less, and most preferably 8 mg or less. Although there is no lower limit in particular, it is usually 0.1 mg or more. In this specification, solid content means the solid part remove | excluding volatile substances, such as a solvent, from an adhesive composition.
Moreover, a low outgassing adhesive layer can be more easily formed by using a polyfunctional epoxy compound having a weight average molecular weight of 1,000 to 5,000.
接着剤組成物の固形分についてのアウトガス量は、例えば、本発明の接着剤組成物を基材フィルム(又は剥離フィルム)上に塗工し、乾燥させることにより得られるシート状接着剤付フィルムを試験片として用いて、実施例に記載の方法に従って測定することができる。 The amount of outgas for the solid content of the adhesive composition is, for example, a film with a sheet-like adhesive obtained by coating the adhesive composition of the present invention on a base film (or a release film) and drying it. Using as a test piece, it can be measured according to the method described in Examples.
アウトガス量が少ない接着剤組成物は、比較的高分子量の多官能エポキシ化合物を用いることで、効率よく得ることができる。 An adhesive composition with a small outgas amount can be efficiently obtained by using a relatively high molecular weight polyfunctional epoxy compound.
本発明の接着剤組成物は、シート状に成形し易く、かつ、低アウトガス性を有する。このため、本発明の接着剤組成物は、封止材を形成する際に好適に用いられる。 The adhesive composition of the present invention is easy to be formed into a sheet and has low outgassing properties. For this reason, the adhesive composition of this invention is used suitably when forming a sealing material.
2)封止シート
本発明の封止シートは、下記の封止シート(α)又は封止シート(β)である。
封止シート(α):2枚の剥離フィルムと、これらの剥離フィルムに挟持された接着剤層とからなる封止シートであって、前記接着剤層が、本発明の接着剤組成物を用いて形成されたものであることを特徴とするもの
封止シート(β):剥離フィルムと、ガスバリア性フィルムと、前記剥離フィルムと前記ガスバリア性フィルムに挟持された接着剤層とからなる封止シートであって、前記接着剤層が、本発明の接着剤組成物を用いて形成されたものであることを特徴とするもの
なお、これらの封止シートは使用前の状態を表したものであり、本発明の封止シートを使用する際は、通常、剥離フィルムは剥離除去される。2) Sealing sheet The sealing sheet of this invention is the following sealing sheet ((alpha)) or sealing sheet ((beta)).
Sealing sheet (α): a sealing sheet comprising two release films and an adhesive layer sandwiched between these release films, wherein the adhesive layer uses the adhesive composition of the present invention. A sealing sheet (β): a sealing sheet comprising a release film, a gas barrier film, and an adhesive layer sandwiched between the release film and the gas barrier film The adhesive layer is formed by using the adhesive composition of the present invention. These sealing sheets represent a state before use. When using the sealing sheet of the present invention, the release film is usually peeled off.
〔封止シート(α)〕
封止シート(α)を構成する剥離フィルムは、封止シート(α)の製造工程においては支持体として機能するとともに、封止シート(α)を使用するまでの間は、接着剤層の保護シートとして機能する。[Sealing sheet (α)]
The release film constituting the sealing sheet (α) functions as a support in the manufacturing process of the sealing sheet (α) and protects the adhesive layer until the sealing sheet (α) is used. Functions as a sheet.
剥離フィルムとしては、従来公知のものを利用することができる。例えば、剥離フィルム用の基材上に、剥離剤により剥離処理された剥離層を有するものが挙げられる。
剥離フィルム用の基材としては、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。A conventionally well-known thing can be utilized as a peeling film. For example, what has the peeling layer by which the peeling process was carried out with the release agent on the base material for peeling films is mentioned.
As the substrate for the release film, paper substrates such as glassine paper, coated paper, and high-quality paper; laminated paper obtained by laminating a thermoplastic resin such as polyethylene on these paper substrates; polyethylene terephthalate resin, polybutylene terephthalate resin, Examples thereof include plastic films such as polyethylene naphthalate resin, polypropylene resin, and polyethylene resin.
Examples of 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.
封止シート(α)における2枚の剥離フィルム同士は同一であっても、異なっていてもよいが、2枚の剥離フィルムは異なる剥離力を有するものが好ましい。2枚の剥離フィルムの剥離力を異なるようにすることで、最初に剥離フィルムを剥離する工程をより効率よく行うことができる。 The two release films in the sealing sheet (α) may be the same or different, but the two release films preferably have different release forces. By making the peeling force of two peeling films different, the process of peeling a peeling film initially can be performed more efficiently.
封止シート(α)の接着剤層の厚みは特に限定されないが、5〜25μmであることが好ましく、10〜20μmであることがより好ましい。
このように接着剤層は非常に薄いものであるが、この接着剤層は本発明の接着剤組成物により形成されるものであるため、凹凸追従性に優れ、被着体の凹凸を十分に埋めることができる。Although the thickness of the adhesive bond layer of a sealing sheet ((alpha)) is not specifically limited, It is preferable that it is 5-25 micrometers, and it is more preferable that it is 10-20 micrometers.
Thus, although the adhesive layer is very thin, since this adhesive layer is formed by the adhesive composition of the present invention, it is excellent in uneven follow-up and sufficiently adheres to the unevenness of the adherend. Can be filled.
封止シート(α)の接着剤層は熱硬化性を有するものが好ましい。熱硬化性を有する接着剤層は、硬化後において、接着強度に極めて優れる。
接着剤層を熱硬化させる際の条件は特に限定されない。
加熱温度は、通常、80〜200℃、好ましくは90〜150℃である。
加熱時間は、通常、30分から12時間、好ましくは1〜6時間である。The adhesive layer of the sealing sheet (α) preferably has thermosetting properties. The adhesive layer having thermosetting property is extremely excellent in adhesive strength after curing.
The conditions for thermosetting the adhesive layer are not particularly limited.
The heating temperature is usually 80 to 200 ° C, preferably 90 to 150 ° C.
The heating time is usually 30 minutes to 12 hours, preferably 1 to 6 hours.
硬化処理後の接着剤層の23℃における引き剥がし接着強度は、通常、1〜100N/25mm、好ましくは、10〜50N/25mmであり、85℃における引き剥がし接着強度は、通常、1〜100N/25mm、好ましくは、5〜50N/25mmである。
上記の引き剥がし接着強度は、実施例に記載の方法に従って測定したものである。
硬化処理後の接着剤層の水蒸気透過率は、通常、0.1〜200g/m2/day、好ましくは1〜150g/m2/dayである。The peel adhesive strength at 23 ° C. of the adhesive layer after the curing treatment is usually 1 to 100 N / 25 mm, preferably 10 to 50 N / 25 mm, and the peel adhesive strength at 85 ° C. is usually 1 to 100 N. / 25 mm, preferably 5 to 50 N / 25 mm.
The peel adhesive strength is measured according to the method described in the examples.
The water vapor permeability of the adhesive layer after the curing treatment is usually 0.1 to 200 g / m 2 / day, preferably 1 to 150 g / m 2 / day.
封止シート(α)の製造方法は特に限定されない。例えば、公知のキャスト法を用いて、封止シート(α)を製造することができる。より具体的には、公知の方法を用いて、本発明の接着剤組成物を剥離フィルムの剥離処理面に塗工し、得られた塗膜を乾燥することで、剥離フィルム付接着剤層を製造し、次いで、もう1枚の剥離フィルムを接着剤層上に重ねることで、封止シート(α)を得ることができる。 The manufacturing method of a sealing sheet ((alpha)) is not specifically limited. For example, a sealing sheet ((alpha)) can be manufactured using a well-known casting method. More specifically, by using a known method, the adhesive composition of the present invention is applied to the release-treated surface of the release film, and the resulting coating film is dried to form an adhesive layer with a release film. The sealing sheet ((alpha)) can be obtained by manufacturing and then stacking another release film on the adhesive layer.
接着剤組成物を塗工する方法としては、例えば、スピンコート法、スプレーコート法、バーコート法、ナイフコート法、ロールコート法、ブレードコート法、ダイコート法、グラビアコート法等が挙げられる。
塗膜を乾燥するときの乾燥条件は特に限定されない。例えば、乾燥温度が80〜150℃、乾燥時間が30秒から5分間である。Examples of the method for applying the adhesive 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 are not particularly limited. For example, the drying temperature is 80 to 150 ° C., and the drying time is 30 seconds to 5 minutes.
〔封止シート(β)〕
封止シート(β)を構成する剥離フィルムと接着剤層は、それぞれ、封止シート(α)を構成する剥離フィルムと接着剤層として示したものと同様のものが挙げられる。
封止シート(β)を構成するガスバリア性フィルムは、水分遮断性を有するフィルムであれば特に限定されない。[Sealing sheet (β)]
Examples of the release film and the adhesive layer constituting the sealing sheet (β) are the same as those shown as the release film and the adhesive layer constituting the sealing sheet (α).
The gas barrier film which comprises a sealing sheet ((beta)) will not be specifically limited if it is a film which has a moisture barrier property.
ガスバリア性フィルムは、温度40℃、相対湿度90%(以下、「90%RH」と略記する。)の環境下における水蒸気透過率が0.1g/m2/day以下であることが好ましく、0.05g/m2/day以下であることがより好ましく、0.005g/m2/day以下であることがさらに好ましい。
ガスバリア性フィルムの温度40℃、90%RHの環境下における水蒸気透過率が0.1g/m2/day以下であることで、透明基板上に形成された有機EL素子等の素子内部に酸素や水分等が浸入し、電極や有機層が劣化することを効果的に抑制することができる。
ガスバリア性フィルムの水蒸気等の透過率は、公知のガス透過率測定装置を使用して測定することができる。The gas barrier film preferably has a water vapor transmission rate of 0.1 g / m 2 / day or less in an environment of a temperature of 40 ° C. and a relative humidity of 90% (hereinafter abbreviated as “90% RH”). It is more preferable that it is 0.05 g / m 2 / day or less, and it is more preferable that it is 0.005 g / m 2 / day or less.
The gas barrier film has a water vapor transmission rate of 0.1 g / m 2 / day or less in an environment of 40 ° C. and 90% RH, so that oxygen or oxygen can be contained inside the organic EL element formed on the transparent substrate. It is possible to effectively suppress the penetration of moisture and the like and the deterioration of the electrode and the organic layer.
The transmittance of water vapor and the like of the gas barrier film can be measured using a known gas permeability measuring device.
ガスバリア性フィルムとしては、金属箔、樹脂製フィルム、薄膜ガラス等が挙げられる。これらの中でも、樹脂製フィルムが好ましく、基材とガスバリア層とを有するガスバリア性フィルムがより好ましい。 Examples of the gas barrier film include metal foil, resin film, and thin film glass. Among these, a resin film is preferable, and a gas barrier film having a base material and a gas barrier layer is more preferable.
金属箔の金属としては、例えば、銅、ニッケル、アルミニウム等の金属材料;ステンレス又はアルミニウム合金等の合金材料;等が挙げられる。 Examples of the metal of the metal foil include metal materials such as copper, nickel, and aluminum; alloy materials such as stainless steel and aluminum alloys; and the like.
薄膜ガラスの成分・組成は特に限定されないが、より安定なフレキシブル性が得られる点で、無アルカリのホウケイ酸ガラスが好ましい。
薄膜ガラスは、薄膜ガラスを単体として用いてもよいが、アルミ箔等の金属箔や樹脂フィルムを、薄膜ガラスに積層あるいはラミネートしたものを用いてもよい。
また、薄膜ガラスとしては、厚みが10〜200μm程度のフレキシブル性を有するものが好ましい。The components and composition of the thin film glass are not particularly limited, but alkali-free borosilicate glass is preferable in terms of obtaining more stable flexibility.
As the thin film glass, the thin film glass may be used as a simple substance, or a metal foil such as an aluminum foil or a resin film laminated or laminated on the thin film glass may be used.
Moreover, as thin film glass, what has the flexibility which thickness is about 10-200 micrometers is preferable.
ガスバリア性フィルムの基材を構成する樹脂成分としては、ポリイミド、ポリアミド、ポリアミドイミド、ポリフェニレンエーテル、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリオレフィン、ポリエステル、ポリカーボネート、ポリスルフォン、ポリエーテルスルフォン、ポリフェニレンスルフィド、ポリアリレート、アクリル系樹脂、シクロオレフィン系ポリマー、芳香族系重合体、ポリウレタン系ポリマー等が挙げられる。
基材の厚みは、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。Examples of the resin component constituting the base material of the gas barrier film include polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyether sulfone, polyphenylene sulfide, and polyphenylene sulfide. Examples include arylate, acrylic resin, cycloolefin polymer, aromatic polymer, polyurethane polymer, and the like.
Although there is no restriction | limiting in particular in the thickness of a base material, From a viewpoint of the ease of handling, Preferably it is 0.5-500 micrometers, More preferably, it is 1-200 micrometers, More preferably, it is 5-100 micrometers.
ガスバリア層は、所望のガスバリア性を付与することができれば、材質等は特に限定されない。ガスバリア層としては、無機膜や、高分子化合物を含む層に改質処理を施して得られる層等が挙げられる。これらの中でも、厚みが薄く、ガスバリア性に優れる層を効率よく形成できることから、ガスバリア層は、無機膜からなるガスバリア層、及び高分子化合物を含む層に改質処理を施して得られるガスバリア層が好ましい。 A material etc. will not be specifically limited if a gas barrier layer can provide desired gas barrier property. Examples of the gas barrier layer include an inorganic film and a layer obtained by subjecting a layer containing a polymer compound to a modification treatment. Among these, since a layer having a small thickness and excellent gas barrier properties can be efficiently formed, the gas barrier layer includes a gas barrier layer made of an inorganic film and a gas barrier layer obtained by subjecting a layer containing a polymer compound to a modification treatment. preferable.
無機膜としては、特に制限されず、例えば、無機蒸着膜が挙げられる。
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。
られる。The inorganic film is not particularly limited, and examples thereof include an inorganic vapor deposition film.
Examples of the inorganic vapor deposition film include vapor deposition films of inorganic compounds and metals.
As the raw material for the vapor-deposited film of the inorganic compound, inorganic oxides such as silicon oxide, aluminum oxide, magnesium oxide, zinc oxide, indium oxide and tin oxide; inorganic nitrides such as silicon nitride, aluminum nitride and titanium nitride; inorganic carbides; Inorganic sulfides; inorganic oxynitrides such as silicon oxynitride; inorganic oxide carbides; inorganic nitride carbides; inorganic oxynitride carbides and the like.
Examples of the raw material for the metal vapor deposition film include aluminum, magnesium, zinc, and tin.
It is done.
無機膜の形成方法としては、真空蒸着法、EB蒸着法、スパッタリング法、イオンプレーティング法、ラミネート法、プラズマ気相成長法(CVD法)などが挙げられる。
無機膜の厚みは、無機材料の種類や構成により適宜選択されるが、通常、1〜500であり、好ましくは、2〜300nmである。Examples of the method for forming the inorganic film include a vacuum deposition method, an EB deposition method, a sputtering method, an ion plating method, a lamination method, a plasma vapor deposition method (CVD method), and the like.
Although the thickness of an inorganic film is suitably selected by the kind and structure of an inorganic material, it is 1-500 normally, Preferably, it is 2-300 nm.
高分子化合物を含む層(以下、「高分子層」ということがある)にイオン注入して得られるガスバリア層において、用いる高分子化合物としては、ポリオルガノシロキサン、ポリシラザン系化合物等のケイ素含有高分子化合物、ポリイミド、ポリアミド、ポリアミドイミド、ポリフェニレンエーテル、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリオレフィン、ポリエステル、ポリカーボネート、ポリスルホン、ポリエーテルスルホン、ポリフェニレンスルフィド、ポリアリレート、アクリル系樹脂、シクロオレフィン系ポリマー、芳香族系重合体等が挙げられる。これらの高分子化合物は1種単独で、あるいは2種以上を組合せて用いることができる。
これらの中でも、優れたガスバリア性を有するガスバリア層を形成できる観点から、ケイ素含有高分子化合物が好ましく、ポリシラザン系化合物がより好ましい。In a gas barrier layer obtained by ion implantation into a layer containing a polymer compound (hereinafter sometimes referred to as “polymer layer”), the polymer compound used is a silicon-containing polymer such as polyorganosiloxane or polysilazane compound. Compound, polyimide, polyamide, polyamideimide, polyphenylene ether, polyether ketone, polyether ether ketone, polyolefin, polyester, polycarbonate, polysulfone, polyethersulfone, polyphenylene sulfide, polyarylate, acrylic resin, cycloolefin polymer, aromatic System polymers and the like. These polymer compounds can be used alone or in combination of two or more.
Among these, from the viewpoint of forming a gas barrier layer having excellent gas barrier properties, silicon-containing polymer compounds are preferable, and polysilazane compounds are more preferable.
ポリシラザン系化合物は、分子内に−Si−N−結合(シラザン結合)を含む繰り返し単位を有する高分子化合物である。具体的には、式(1) A polysilazane compound is a polymer compound having a repeating unit containing a —Si—N— bond (silazane bond) in the molecule. Specifically, the formula (1)
で表される繰り返し単位を有する化合物が好ましい。また、用いるポリシラザン系化合物の数平均分子量は、特に限定されないが、100〜50,000であるのが好ましい。 The compound which has a repeating unit represented by these is preferable. The number average molecular weight of the polysilazane compound to be used is not particularly limited, but is preferably 100 to 50,000.
前記式(1)中、nは任意の自然数を表す。
Rx、Ry、Rzは、それぞれ独立して、水素原子、無置換若しくは置換基を有するアルキル基、無置換若しくは置換基を有するシクロアルキル基、無置換若しくは置換基を有するアルケニル基、無置換若しくは置換基を有するアリール基又はアルキルシリル基等の非加水分解性基を表す。これらの中でも、Rx、Ry、Rzとしては、水素原子、炭素数1〜6のアルキル基、又はフェニル基が好ましく、水素原子が特に好ましい。前記式(1)で表される繰り返し単位を有するポリシラザン系化合物としては、Rx、Ry、Rzが全て水素原子である無機ポリシラザン、Rx、Ry、Rzの少なくとも1つが水素原子ではない有機ポリシラザンのいずれであってもよい。In said formula (1), n represents arbitrary natural numbers.
Rx, Ry, and Rz each independently represent a hydrogen atom, an unsubstituted or substituted alkyl group, an unsubstituted or substituted cycloalkyl group, an unsubstituted or substituted alkenyl group, unsubstituted or substituted Represents a non-hydrolyzable group such as an aryl group having a group or an alkylsilyl group; Among these, as Rx, Ry, and Rz, a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, or a phenyl group is preferable, and a hydrogen atom is particularly preferable. Examples of the polysilazane compound having a repeating unit represented by the formula (1) include inorganic polysilazanes in which Rx, Ry, and Rz are all hydrogen atoms, and organic polysilazanes in which at least one of Rx, Ry, and Rz is not a hydrogen atom. It may be.
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。本発明においては、ポリシラザン系化合物として、ポリシラザン変性物を用いることもできる。また、本発明においては、ポリシラザン系化合物としては、ガラスコーティング材等として市販されている市販品をそのまま使用することもできる。 The polysilazane compounds can be used alone or in combination of two or more. In the present invention, a modified polysilazane compound can also be used as the polysilazane compound. In the present invention, as the polysilazane compound, a commercially available product as a glass coating material or the like can be used as it is.
前記高分子層は、上述した高分子化合物の他に、本発明の目的を阻害しない範囲で他の成分を含んでいてもよい。他の成分としては、硬化剤、他の高分子、老化防止剤、光安定剤、難燃剤等が挙げられる。
高分子層中の高分子化合物の含有量は、より優れたガスバリア性を有するガスバリア層が得られることから、50質量%以上が好ましく、70質量%以上がより好ましい。The polymer layer may contain other components in addition to the above-described polymer compound as long as the object of the present invention is not impaired. Examples of other components include curing agents, other polymers, anti-aging agents, light stabilizers, and flame retardants.
The content of the polymer compound in the polymer layer is preferably 50% by mass or more and more preferably 70% by mass or more because a gas barrier layer having better gas barrier properties can be obtained.
高分子層の厚みは特に制限されないが、好ましくは50〜300nm、より好ましくは50〜200nmの範囲である。
本発明においては、高分子層の厚みがナノオーダーであっても、充分なガスバリア性を有する封止シートを得ることができる。The thickness of the polymer layer is not particularly limited, but is preferably in the range of 50 to 300 nm, more preferably 50 to 200 nm.
In the present invention, a sealing sheet having a sufficient gas barrier property can be obtained even if the thickness of the polymer layer is nano-order.
高分子層を形成する方法としては、例えば、高分子化合物の少なくとも1種、所望により他の成分、及び溶剤等を含有する層形成用溶液を、スピンコーター、ナイフコーター、グラビアコーター等の公知の装置を使用し、塗布し、得られた塗膜を適度に乾燥して形成する方法が挙げられる。 As a method for forming a polymer layer, for example, a layer forming solution containing at least one polymer compound, optionally other components, a solvent, and the like is used as a known method such as a spin coater, a knife coater, a gravure coater, or the like. There is a method in which an apparatus is used for coating and the resulting coating film is appropriately dried to form.
高分子層の改質処理としては、イオン注入処理、プラズマ処理、放射線照射処理、熱処理等が挙げられ、高分子層の結合構造を変化させる処理が好ましい。これらの処理は、1種類を単独で行うこともできるが、2種類以上を組み合わせて行うこともできる。
イオン注入処理は、後述するように、高分子層にイオンを注入して、高分子層を改質する方法である。
プラズマ処理は、高分子層をプラズマ中に晒して、高分子層を改質する方法である。例えば、特開2012−106421号公報に記載の方法に従って、プラズマ処理を行うことができる。
放射線照射処理は、高分子層に放射線を照射して高分子層を改質する方法である。放射線は、高分子層の結合構造を変化させる効果の高い短波長のものが好ましく、紫外線、特に真空紫外光を用いることが好ましい。例えば、特開2013−226757号公報に記載の方法に従って、真空紫外光改質処理を行うことができる。
これらの中でも、高分子層の表面を荒らすことなく、その内部まで効率よく改質し、よりガスバリア性に優れるガスバリア層を形成できることから、イオン注入処理が好ましい。Examples of the polymer layer modification treatment include ion implantation treatment, plasma treatment, radiation irradiation treatment, heat treatment and the like, and treatment for changing the bonding structure of the polymer layer is preferable. These processes can be performed alone or in combination of two or more.
The ion implantation process is a method of modifying the polymer layer by implanting ions into the polymer layer, as will be described later.
The plasma treatment is a method for modifying the polymer layer by exposing the polymer layer to plasma. For example, plasma treatment can be performed according to a method described in Japanese Patent Application Laid-Open No. 2012-106421.
The radiation irradiation treatment is a method for modifying the polymer layer by irradiating the polymer layer with radiation. The radiation preferably has a short wavelength with a high effect of changing the bonding structure of the polymer layer, and it is preferable to use ultraviolet rays, particularly vacuum ultraviolet rays. For example, vacuum ultraviolet light modification treatment can be performed according to the method described in JP2013-226757A.
Among these, the ion implantation treatment is preferable because the gas barrier layer can be efficiently modified to the inside without roughening the surface of the polymer layer and more excellent in gas barrier properties.
高分子層に注入されるイオンとしては、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;フルオロカーボン、水素、窒素、酸素、二酸化炭素、塩素、フッ素、硫黄等のイオン;
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。As ions implanted into the polymer layer, ions of rare gases such as argon, helium, neon, krypton, and xenon; ions such as fluorocarbon, hydrogen, nitrogen, oxygen, carbon dioxide, chlorine, fluorine, and sulfur;
Ions of alkane gases such as methane and ethane; Ions of alkene gases such as ethylene and propylene; Ions of alkadiene gases such as pentadiene and butadiene; Ions of alkyne gases such as acetylene; Benzene, toluene, etc. 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.
Among these, 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.
イオンを注入する方法としては、特に限定されない。例えば、電界により加速されたイオン(イオンビーム)を照射する方法、プラズマ中のイオン(プラズマ生成ガスのイオン)を注入する方法等が挙げられ、簡便にガスバリア層が得られることから、後者のプラズマイオンを注入する方法が好ましい。プラズマイオン注入法は、例えば、プラズマ生成ガスを含む雰囲気下でプラズマを発生させ、イオンを注入する層に負の高電圧パルスを印加することにより、該プラズマ中のイオン(陽イオン)を、イオンを注入する層の表面部に注入して行うことができる。 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 injecting ions in plasma (ion of plasma generation gas), etc., and a gas barrier layer can be easily obtained. A method of implanting ions is preferred. In the plasma ion implantation method, for example, plasma is generated in an atmosphere containing a plasma generation gas, and a negative high voltage pulse is applied to a layer into which ions are implanted, whereby ions (positive ions) in the plasma are ionized. Can be performed by injecting into the surface portion of the layer to be injected.
封止シート(β)の製造方法は特に限定されない。例えば、先に説明した封止シート(α)の製造方法において、剥離フィルムの1枚をガスバリア性フィルムに置き換えることで封止シート(β)を製造することができる。
また、封止シート(α)を製造した後、その1枚の剥離フィルムを剥離し、露出した接着剤層とガスバリア性フィルムとを貼着することにより、封止シート(β)を製造することもできる。この場合、封止シート(α)が、異なる剥離力を有する2枚の剥離フィルムを有する場合には、取扱い性の観点から、剥離力の小さい方の剥離フィルムを剥離するのが好ましい。The manufacturing method of a sealing sheet ((beta)) is not specifically limited. For example, in the manufacturing method of the sealing sheet (α) described above, the sealing sheet (β) can be manufactured by replacing one of the release films with a gas barrier film.
Moreover, after manufacturing a sealing sheet ((alpha)), the sealing sheet ((beta)) is manufactured by peeling the one peeling film and sticking the exposed adhesive bond layer and a gas-barrier film. You can also. In this case, when the sealing sheet (α) has two release films having different release forces, it is preferable to release the release film having the smaller release force from the viewpoint of handleability.
上記のように、本発明の封止シートの接着剤層は、低アウトガス性を有する。このため、有機EL素子を封止したときに、その劣化を抑えることができる。 As described above, the adhesive layer of the sealing sheet of the present invention has low outgassing properties. For this reason, when an organic EL element is sealed, the deterioration can be suppressed.
3)封止体
本発明の封止体は、被封止物が、本発明の封止シートで封止されてなるものである。
本発明の封止体としては、例えば、透明基板と、該透明基板上に形成された素子(被封止物)と、該素子を封止するための封止材とを備えるものであって、前記封止材が、本発明の封止シートの接着剤層であるものが挙げられる。3) Sealing body The sealing body of the present invention is formed by sealing an object to be sealed with the sealing sheet of the present invention.
The sealing body of the present invention includes, for example, a transparent substrate, an element (an object to be sealed) formed on the transparent substrate, and a sealing material for sealing the element. The sealing material is an adhesive layer of the sealing sheet of the present invention.
透明基板は、特に限定されるものではなく、種々の基板材料を用いることができる。特に可視光の透過率が高い基板材料を用いることが好ましい。また、素子外部から浸入しようとする水分やガスを阻止する遮断性能が高く、耐溶剤性や耐候性に優れている材料が好ましい。具体的には、石英やガラスなどの透明無機材料;ポリエチレンテレフタラート、ポリエチレンナフタラート、ポリカーボネート、ポリスチレン、ポリエチレン、ポリプロピレン、ポリフェニレンスルフィド、ポリフッ化ビニリデン、アセチルセルロース、ブロム化フェノキシ、アラミド類、ポリイミド類、ポリスチレン類、ポリアリレート類、ポリスルホン類、ポリオレフィン類などの透明プラスチック、前述したガスバリア性フィルム;が挙げられる。
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。The transparent substrate is not particularly limited, and various substrate materials can be used. In particular, it is preferable to use a substrate material having a high visible light transmittance. In addition, 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. Specifically, 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, Examples thereof include transparent plastics such as polystyrenes, polyarylates, polysulfones, and polyolefins, and the gas barrier film described above.
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.
被封止物としては、有機EL素子、有機ELディスプレイ素子、液晶ディスプレイ素子、太陽電池素子等が挙げられる。 Examples of the object to be sealed include an organic EL element, an organic EL display element, a liquid crystal display element, and a solar cell element.
本発明の封止体の製造方法は特に限定されない。例えば、本発明の封止シートの接着剤層を被封止物上に重ねた後、加熱することにより、封止シートの接着剤層と被封止物を接着させる。
次いで、この接着剤層を硬化させることにより、本発明の封止体を製造することができる。The manufacturing method of the sealing body of this invention is not specifically limited. For example, after the adhesive layer of the sealing sheet of the present invention is stacked on the object to be sealed, the adhesive layer of the sealing sheet and the object to be sealed are bonded by heating.
Subsequently, the sealing body of this invention can be manufactured by hardening this adhesive bond layer.
封止シートの接着剤層と被封止物を接着させる際の接着条件は特に限定されない。接着温度は、例えば、23〜100℃、好ましくは40〜80℃である。この接着処理は、加圧しながら行ってもよい。
接着剤層を硬化させる際の硬化条件としては、先に説明した条件を利用することができる。There are no particular restrictions on the bonding conditions for bonding the adhesive layer of the sealing sheet and the object to be sealed. Adhesion temperature is 23-100 degreeC, for example, Preferably it is 40-80 degreeC. This adhesion treatment may be performed while applying pressure.
As the curing conditions for curing the adhesive layer, the conditions described above can be used.
本発明の封止体は、被封止物が、本発明の封止シートで封止されてなるものである。
したがって、本発明の封止体においては、長期にわたって被封止物の性能が維持される。The sealing body of the present invention is formed by sealing an object to be sealed with the sealing sheet of the present invention.
Therefore, in the sealed body of the present invention, the performance of the object to be sealed is maintained for a long time.
以下、実施例を挙げて本発明を更に詳細に説明する。但し、本発明は、以下の実施例になんら限定されるものではない。
各例中の部及び%は、特に断りのない限り、質量基準である。また、変性ポリオレフィン系樹脂及び多官能エポキシ化合物の重量平均分子量(Mw)は、以下の方法により測定した値である。
<変性ポリオレフィン系樹脂の重量平均分子量(Mw)>
変性ポリオレフィン系樹脂の重量平均分子量(Mw)は、ゲル浸透クロマトグラフ(GPC)装置(東ソー株式会社製、製品名「HLC−8320」)を用いて、下記の条件下で測定し、標準ポリスチレンの重量平均分子量に換算した値を用いた。
(測定条件)
・測定試料:変性ポリオレフィン系樹脂濃度1質量%のテトラヒドロフラン溶液
・カラム:「TSK gel Super HM−H」を2本、「TSK gel Super H2000」を1本(いずれも東ソー株式会社製)、順次連結したもの
・カラム温度:40℃
・展開溶媒:テトラヒドロフラン
・流速:0.60mL/min
<多官能エポキシ化合物の重量平均分子量(Mw)>
多官能エポキシ化合物の重量平均分子量(Mw)は、ゲル浸透クロマトグラフ(GPC)装置(東ソー株式会社製、製品名「HLC−8320」)を用いて、下記の条件下で測定し、複数観察されるピークのうち、面積が最大であるもののピークトップの保持時間に対応する標準ポリスチレンの重量平均分子量に換算したものである。
(測定条件)
・測定試料:多官能エポキシ化合物濃度1質量%のテトラヒドロフラン溶液
・カラム:「TSK gel Super HM−H」を2本、「TSK gel Super H2000」を1本(いずれも東ソー株式会社製)、順次連結したもの
・カラム温度:40℃
・展開溶媒:テトラヒドロフラン
・流速:0.60mL/minHereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to the following examples.
Unless otherwise indicated, the part and% in each example are based on mass. Moreover, the weight average molecular weight (Mw) of the modified polyolefin resin and the polyfunctional epoxy compound is a value measured by the following method.
<Weight average molecular weight of modified polyolefin resin (Mw)>
The weight average molecular weight (Mw) of the modified polyolefin resin was measured using a gel permeation chromatograph (GPC) apparatus (product name “HLC-8320” manufactured by Tosoh Corporation) under the following conditions. The value converted into the weight average molecular weight was used.
(Measurement condition)
・ Measurement sample: Tetrahydrofuran solution with a modified polyolefin resin concentration of 1 mass% ・ Column: Two “TSK gel Super HM-H” and one “TSK gel Super H2000” (both manufactured by Tosoh Corporation), sequentially connected -Column temperature: 40 ° C
・ Developing solvent: Tetrahydrofuran ・ Flow rate: 0.60 mL / min
<Weight average molecular weight of polyfunctional epoxy compound (Mw)>
The weight average molecular weight (Mw) of the polyfunctional epoxy compound was measured under the following conditions using a gel permeation chromatograph (GPC) apparatus (product name “HLC-8320” manufactured by Tosoh Corporation), and a plurality of weight average molecular weights were observed. Among the peaks having the largest area, the weight average molecular weight of the standard polystyrene corresponding to the retention time of the peak top is converted.
(Measurement condition)
・ Measurement sample: Tetrahydrofuran solution with a polyfunctional epoxy compound concentration of 1 mass% ・ Column: Two “TSK gel Super HM-H” and one “TSK gel Super H2000” (both manufactured by Tosoh Corporation), sequentially connected -Column temperature: 40 ° C
・ Developing solvent: Tetrahydrofuran ・ Flow rate: 0.60 mL / min
〔実施例1〕
酸変性ポリオレフィン系樹脂(α−オレフィン重合体、三井化学社製、商品名:ユニストールH−200、重量平均分子量:52,000)100部、多官能エポキシ化合物(1)(ビスフェノールAジグリシジルエーテル、三菱化学社製、商品名:YL980、エポキシ当量180〜190g/eq、分子量:2,400)100部、粘着付与剤(スチレン系モノマー脂肪族系モノマー共重合体、軟化点95℃、三井化学社製、商品名:FTR6100)50部、及び、イミダゾール系硬化触媒(四国化成社製、商品名:キュアゾール2E4MZ、2−エチル−4−メチルイミダゾール)1部をメチルエチルケトンに溶解し、固形分濃度30%の接着剤組成物1を調製した。
この接着剤組成物1を剥離フィルム(リンテック社製、商品名:SP−PET382150)の剥離処理面上に塗工し、得られた塗膜を100℃で2分間乾燥し、厚みが12μmの接着剤層を形成し、その上に、もう1枚の剥離フィルム(リンテック社製、商品名:SP−PET381031)の剥離処理面を貼り合わせて封止シート1を得た。[Example 1]
100 parts of acid-modified polyolefin resin (α-olefin polymer, manufactured by Mitsui Chemicals, trade name: Unistor H-200, weight average molecular weight: 52,000), polyfunctional epoxy compound (1) (bisphenol A diglycidyl ether) , Manufactured by Mitsubishi Chemical Corporation, trade name: YL980, epoxy equivalent 180-190 g / eq, molecular weight: 2,400, 100 parts, tackifier (styrene monomer aliphatic monomer copolymer, softening point 95 ° C., Mitsui Chemicals) 50 parts by company, product name: FTR6100), and 1 part by imidazole-based curing catalyst (manufactured by Shikoku Kasei Co., Ltd., trade name: Curesol 2E4MZ, 2-ethyl-4-methylimidazole) are dissolved in methyl ethyl ketone, and the solid content concentration is 30 % Adhesive composition 1 was prepared.
The adhesive composition 1 was applied onto a release-treated surface of a release film (product name: SP-PET382150, manufactured by Lintec Corporation), and the resulting coating film was dried at 100 ° C. for 2 minutes to bond with a thickness of 12 μm. An agent layer was formed, and the release treatment surface of another release film (manufactured by Lintec Corporation, trade name: SP-PET 381031) was bonded thereon to obtain a sealing sheet 1.
〔実施例2〕
実施例1において、多官能エポキシ化合物として、多官能エポキシ化合物(2)(水添ビスフェノールAジグリシジルエーテル、三菱化学社製、商品名:YX8000、エポキシ当量205g/eq、重量平均分子量:1,400)を使用したことを除き、実施例1と同様にして封止シート2を得た。[Example 2]
In Example 1, as a polyfunctional epoxy compound, polyfunctional epoxy compound (2) (hydrogenated bisphenol A diglycidyl ether, manufactured by Mitsubishi Chemical Corporation, trade name: YX8000, epoxy equivalent 205 g / eq, weight average molecular weight: 1,400 ) Was used in the same manner as in Example 1 except that a sealing sheet 2 was obtained.
〔実施例3〕
実施例1において、多官能エポキシ化合物として、多官能エポキシ化合物(3)(水添ビスフェノールAジグリシジルエーテル、三菱化学社製、商品名:YX8034、エポキシ当量270g/eq、重量平均分子量:3,200)を使用したことを除き、実施例1と同様にして封止シート3を得た。
Example 3
In Example 1, the polyfunctional epoxy compound (3) (hydrogenated bisphenol A diglycidyl ether, manufactured by Mitsubishi Chemical Corporation, trade name: YX8034, epoxy equivalent 270 g / eq, weight average molecular weight: 3,200) ) Was used in the same manner as in Example 1 except that a sealing sheet 3 was obtained.
〔実施例4〕
実施例1において、多官能エポキシ化合物として、多官能エポキシ化合物(4)(水添ビスフェノールAジグリシジルエーテル、三菱化学社製、商品名:YX8040、エポキシ当量1100g/eq、重量平均分子量:4,200)を使用したことを除き、実施例1と同様にして封止シート4を得た。Example 4
In Example 1, as the polyfunctional epoxy compound, polyfunctional epoxy compound (4) (hydrogenated bisphenol A diglycidyl ether, manufactured by Mitsubishi Chemical Corporation, trade name: YX8040, epoxy equivalent 1100 g / eq, weight average molecular weight: 4,200 ) Was used in the same manner as in Example 1 except that a sealing sheet 4 was obtained.
〔比較例1〕
実施例1において、多官能エポキシ化合物として、多官能エポキシ化合物(5)(水添ビスフェノールAジグリシジルエーテル、共栄社化学社製、商品名:エポライト4000、エポキシ当量215〜245g/eq、重量平均分子量:800)を使用したことを除き、実施例1と同様にして封止シート5を得た。[Comparative Example 1]
In Example 1, as a polyfunctional epoxy compound, polyfunctional epoxy compound (5) (hydrogenated bisphenol A diglycidyl ether, manufactured by Kyoeisha Chemical Co., Ltd., trade name: Epolite 4000, epoxy equivalent of 215 to 245 g / eq, weight average molecular weight: 800) was used in the same manner as in Example 1 to obtain a sealing sheet 5.
〔比較例2〕
実施例1において、多官能エポキシ化合物として、多官能エポキシ化合物(6)(水添ビスフェノールAジグリシジルエーテル、ADEKA社製、商品名:アデカレジン、EP−4080E、エポキシ当量215g/eq、分子量:800)を使用したことを除き、実施例1と同様にして封止シート6を得た。[Comparative Example 2]
In Example 1, as the polyfunctional epoxy compound, polyfunctional epoxy compound (6) (hydrogenated bisphenol A diglycidyl ether, manufactured by ADEKA, trade name: Adeka Resin, EP-4080E, epoxy equivalent 215 g / eq, molecular weight: 800) A sealing sheet 6 was obtained in the same manner as in Example 1 except that was used.
実施例1〜4、比較例1〜2で得た封止シート1〜6について、以下の試験を行った。
〔低アウトガス性評価試験〕
実施例又は比較例で得た封止シートの剥離フィルム1枚を剥がし、露出した接着剤層がガラス板に対向するように、この封止シートをガラス板上に置き、ヒートラミネーターを用いて60℃で接着した。
次いで、残りの剥離フィルムを剥がしたものを測定試料として使用し、120℃、20分の条件でアウトガスを発生させ、その発生量を定量した。
アウトガスの発生量の定量は、ガスクロマトグラフ質量分析計(島津社製、GCMS−QP2010)を使用し、カラムは5%−Diphenyl−95%Dimethyl polysiloxane(HP−5ms)を使用して行った。このとき、トルエンを用いて検量線を作成した。The following tests were done about the sealing sheets 1-6 obtained in Examples 1-4 and Comparative Examples 1-2.
[Low outgassing evaluation test]
One release film of the sealing sheet obtained in Examples or Comparative Examples is peeled off, and this sealing sheet is placed on the glass plate so that the exposed adhesive layer faces the glass plate. Bonded at ℃.
Subsequently, what peeled off the remaining peeling film was used as a measurement sample, outgas was generated on 120 degreeC and the conditions for 20 minutes, and the generation amount was quantified.
The amount of outgas generated was quantified using a gas chromatograph mass spectrometer (GCMS-QP2010, manufactured by Shimadzu Corporation), and a column using 5% -Diphenyl-95% Dimethylpolysiloxane (HP-5 ms). At this time, a calibration curve was prepared using toluene.
〔有機EL素子の評価試験〕
陽極として酸化インジウムスズ(ITO)膜(厚さ:100nm、シート抵抗:50Ω/□)が成膜されたガラス基板を用いて、以下の方法により有機EL素子を作製した。
前記ガラス基板のITO膜上に、N,N’−ビス(ナフタレン−1−イル)−N,N’−ビス(フェニル)−ベンジジン)(Luminescence Technology社製)を0.1〜0.2nm/分の速度で蒸着させ、厚みが50nmの正孔輸送層を形成し、次いで、正孔輸送層上に、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0.1〜0.2nm/分の速度で蒸着させ、厚みが50nmの発光層を形成した。前記発光層上に、フッ化リチウム(LiF)(高純度化学研究所社製)を0.1nm/分の速度で蒸着させ、厚みが4nmの電子注入層を形成し、次いで、電子注入層上に、アルミニウム(Al)(高純度化学研究所社製)を0.1nm/分の速度で蒸着させ、厚みが100nmの陰極を形成し、有機EL素子を得た。なお、蒸着時の真空度は、全て1×10−4Pa以下であった。[Evaluation test of organic EL elements]
Using a glass substrate on which an indium tin oxide (ITO) film (thickness: 100 nm, sheet resistance: 50Ω / □) was formed as an anode, an organic EL device was produced by the following method.
On the ITO film of the glass substrate, N, N′-bis (naphthalen-1-yl) -N, N′-bis (phenyl) -benzidine) (manufactured by Luminescence Technology) was 0.1 to 0.2 nm / A hole transport layer having a thickness of 50 nm is formed by vapor deposition at a rate of 30 minutes, and then, tris (8-hydroxy-quinolinate) aluminum (manufactured by Luminesence Technology) is 0.1 to 0. Evaporation was performed at a rate of 2 nm / min to form a light emitting layer having a thickness of 50 nm. On the light emitting layer, lithium fluoride (LiF) (manufactured by High Purity Chemical Laboratory) was deposited at a rate of 0.1 nm / min to form an electron injection layer having a thickness of 4 nm, and then on the electron injection layer Then, aluminum (Al) (manufactured by High Purity Chemical Research Laboratories) was vapor-deposited at a rate of 0.1 nm / min to form a cathode having a thickness of 100 nm to obtain an organic EL device. In addition, all the vacuum degrees at the time of vapor deposition were 1 * 10 <-4> Pa or less.
実施例及び比較例で得た封止シート1〜6の剥離フィルムをそれぞれ1枚剥がし、露出した接着剤層を金属箔フィルム上に重ね、ヒートラミネーターを用いてこれらを40℃で接着した。次いで、もう1枚の剥離フィルムを剥離し、露出した接着剤層を、ガラス基板上に形成された有機EL素子を覆うように重ね、ヒートラミネーターを用いてこれらを40℃で接着した。次いで、100℃で2時間加熱して接着剤層を硬化させ、有機EL素子が封止されたボトムエミッション型の電子デバイスを得た。
この電子デバイスを、85℃、相対湿度85%の環境下で240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)の面積を測定した。
85℃、相対湿度85%の環境下で放置する前の電子デバイスのダークスポットの面積を基準としたダークスポットの拡大率を算出し、以下の基準で評価した。
<基準>
○:ダークスポットの拡大率が150%未満
×:ダークスポットの拡大率が150%以上
評価結果を第1表に示す。One release film of each of the sealing sheets 1 to 6 obtained in Examples and Comparative Examples was peeled off, and the exposed adhesive layer was stacked on the metal foil film, and these were adhered at 40 ° C. using a heat laminator. Next, the other release film was peeled off, and the exposed adhesive layer was stacked so as to cover the organic EL element formed on the glass substrate, and these were adhered at 40 ° C. using a heat laminator. Subsequently, it heated at 100 degreeC for 2 hours, the adhesive bond layer was hardened, and the bottom emission type electronic device with which the organic EL element was sealed was obtained.
The electronic device was allowed to stand for 240 hours in an environment of 85 ° C. and a relative humidity of 85%, and then the organic EL element was activated to measure the area of the dark spot (non-light emitting portion).
The expansion ratio of the dark spot based on the area of the dark spot of the electronic device before being left in an environment of 85 ° C. and 85% relative humidity was calculated and evaluated according to the following criteria.
<Standard>
○: Dark spot enlargement ratio is less than 150% ×: Dark spot enlargement ratio is 150% or more The evaluation results are shown in Table 1.
第1表から以下のことがわかる。
実施例1〜4の封止シートは、低アウトガス性を有し、有機EL素子の評価試験において優れている。
一方、比較例1、2の封止シートは、アウトガスが大量に発生するものであり、有機EL素子の評価試験において劣っている。Table 1 shows the following.
The sealing sheets of Examples 1 to 4 have low outgassing properties and are excellent in evaluation tests of organic EL elements.
On the other hand, the sealing sheets of Comparative Examples 1 and 2 generate a large amount of outgas and are inferior in the evaluation test of the organic EL element.
Claims (18)
前記接着剤層が、下記の(A)成分、及び(B)成分を含有する接着剤組成物であって、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm 3 あたりのアウトガス量が20mg以下であることを特徴とする接着剤組成物を用いて形成されたものである封止シート。
(A)成分:変性ポリオレフィン系樹脂
(B)成分:多官能エポキシ化合物 A sealing sheet comprising two release films and an adhesive layer sandwiched between these release films,
The adhesive layer is an adhesive composition containing the following component (A) and component (B), and the solid content is measured when the outgas amount is measured at 120 ° C. for 20 minutes. An encapsulating sheet formed using an adhesive composition, wherein the amount of outgas per 1 cm 3 per minute is 20 mg or less .
Component (A): Modified polyolefin resin
(B) component: polyfunctional epoxy compound
前記接着剤層が、下記の(A)成分、及び(B)成分を含有する接着剤組成物であって、その固形分について120℃、20分の条件でアウトガス量を測定したときに、固形分1cm 3 あたりのアウトガス量が20mg以下であることを特徴とする接着剤組成物を用いて形成されたものである封止シート。
(A)成分:変性ポリオレフィン系樹脂
(B)成分:多官能エポキシ化合物 A release film, a gas barrier film, and an adhesive layer sandwiched between the release film and the gas barrier film,
The adhesive layer is an adhesive composition containing the following component (A) and component (B), and the solid content is measured when the outgas amount is measured at 120 ° C. for 20 minutes. An encapsulating sheet formed using an adhesive composition, wherein the amount of outgas per 1 cm 3 per minute is 20 mg or less.
Component (A): Modified polyolefin resin
(B) component: polyfunctional epoxy compound
(C)成分:軟化点が80℃以上の粘着付与剤。 The sealing sheet according to any one of claims 1 to 4 , wherein the adhesive composition further contains the following component (C).
Component (C): A tackifier having a softening point of 80 ° C or higher.
(D)成分:イミダゾール系硬化触媒 The sealing sheet according to any one of claims 1 to 6 , wherein the adhesive composition further contains the following component (D).
(D) Component: Imidazole-based curing catalyst
(E)成分:シランカップリング剤 The sealing sheet according to any one of claims 1 to 8 , wherein the adhesive composition further contains the following component (E).
(E) component: Silane coupling agent
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