KR20200015450A - Adhesive sheet, and encapsulation - Google Patents
Adhesive sheet, and encapsulation Download PDFInfo
- Publication number
- KR20200015450A KR20200015450A KR1020197026345A KR20197026345A KR20200015450A KR 20200015450 A KR20200015450 A KR 20200015450A KR 1020197026345 A KR1020197026345 A KR 1020197026345A KR 20197026345 A KR20197026345 A KR 20197026345A KR 20200015450 A KR20200015450 A KR 20200015450A
- Authority
- KR
- South Korea
- Prior art keywords
- adhesive
- adhesive sheet
- bond layer
- shear
- adhesive bond
- Prior art date
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 219
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 212
- 238000005538 encapsulation Methods 0.000 title description 3
- 239000010410 layer Substances 0.000 claims abstract description 96
- 239000004593 Epoxy Substances 0.000 claims abstract description 43
- 150000001875 compounds Chemical class 0.000 claims abstract description 39
- 239000012790 adhesive layer Substances 0.000 claims abstract description 21
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 7
- 229920005672 polyolefin resin Polymers 0.000 claims description 44
- 238000012360 testing method Methods 0.000 claims description 34
- 238000005259 measurement Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 20
- 239000003513 alkali Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 150000002460 imidazoles Chemical class 0.000 claims description 12
- 238000003475 lamination Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000004973 liquid crystal related substance Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 abstract description 26
- 239000003566 sealing material Substances 0.000 abstract description 9
- 238000010008 shearing Methods 0.000 abstract description 3
- -1 1, 6- hexanediol diglycidyl ether Hexahydrophthalic acid diglycidyl ester Chemical compound 0.000 description 23
- 239000000203 mixture Substances 0.000 description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 238000000576 coating method Methods 0.000 description 13
- 229920005989 resin Polymers 0.000 description 12
- 239000011347 resin Substances 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000000178 monomer Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 239000003822 epoxy resin Substances 0.000 description 10
- 229920000647 polyepoxide Polymers 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 150000001244 carboxylic acid anhydrides Chemical group 0.000 description 7
- 229920001971 elastomer Polymers 0.000 description 7
- 229910000077 silane Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 6
- 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 5
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000123 paper Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000005060 rubber Substances 0.000 description 5
- 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 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000007334 copolymerization reaction Methods 0.000 description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229920001684 low density polyethylene Polymers 0.000 description 4
- 239000004702 low-density polyethylene Substances 0.000 description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 4
- 229920000058 polyacrylate Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 4
- 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
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000005038 ethylene vinyl acetate Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229920000092 linear low density polyethylene Polymers 0.000 description 3
- 239000004707 linear low-density polyethylene Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229920013716 polyethylene resin Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- 229920001862 ultra low molecular weight polyethylene Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-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
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical class CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 125000005370 alkoxysilyl group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 150000001733 carboxylic acid esters Chemical group 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 125000005462 imide group Chemical group 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 229920001179 medium density polyethylene Polymers 0.000 description 2
- 239000004701 medium-density polyethylene Substances 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 2
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- 239000003381 stabilizer Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
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- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 1
- RUEBPOOTFCZRBC-UHFFFAOYSA-N (5-methyl-2-phenyl-1h-imidazol-4-yl)methanol Chemical compound OCC1=C(C)NC(C=2C=CC=CC=2)=N1 RUEBPOOTFCZRBC-UHFFFAOYSA-N 0.000 description 1
- 239000001124 (E)-prop-1-ene-1,2,3-tricarboxylic acid Substances 0.000 description 1
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2,2'-azo-bis-isobutyronitrile Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- KUAUJXBLDYVELT-UHFFFAOYSA-N 2-[[2,2-dimethyl-3-(oxiran-2-ylmethoxy)propoxy]methyl]oxirane Chemical compound C1OC1COCC(C)(C)COCC1CO1 KUAUJXBLDYVELT-UHFFFAOYSA-N 0.000 description 1
- AJHINEHNXSBERZ-UHFFFAOYSA-N 2-[[2-(oxiran-2-ylmethoxy)-5-[2-[4-(oxiran-2-ylmethoxy)-3-(oxiran-2-ylmethyl)phenyl]propan-2-yl]phenyl]methyl]oxirane Chemical compound CC(C)(C1=CC=C(OCC2CO2)C(CC2CO2)=C1)C1=CC=C(OCC2CO2)C(CC2CO2)=C1 AJHINEHNXSBERZ-UHFFFAOYSA-N 0.000 description 1
- YTWBFUCJVWKCCK-UHFFFAOYSA-N 2-heptadecyl-1h-imidazole Chemical compound CCCCCCCCCCCCCCCCCC1=NC=CN1 YTWBFUCJVWKCCK-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
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- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 description 1
- LLEASVZEQBICSN-UHFFFAOYSA-N 2-undecyl-1h-imidazole Chemical compound CCCCCCCCCCCC1=NC=CN1 LLEASVZEQBICSN-UHFFFAOYSA-N 0.000 description 1
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- IFDVQVHZEKPUSC-UHFFFAOYSA-N cyclohex-3-ene-1,2-dicarboxylic acid Chemical compound OC(=O)C1CCC=CC1C(O)=O IFDVQVHZEKPUSC-UHFFFAOYSA-N 0.000 description 1
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- FEHYCIQPPPQNMI-UHFFFAOYSA-N ethenyl(triphenoxy)silane Chemical compound C=1C=CC=CC=1O[Si](OC=1C=CC=CC=1)(C=C)OC1=CC=CC=C1 FEHYCIQPPPQNMI-UHFFFAOYSA-N 0.000 description 1
- NNBRCHPBPDRPIT-UHFFFAOYSA-N ethenyl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)C=C NNBRCHPBPDRPIT-UHFFFAOYSA-N 0.000 description 1
- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 description 1
- VYJZXBZFLIBVQA-UHFFFAOYSA-N ethenyl-tris(phenylmethoxy)silane Chemical compound C=1C=CC=CC=1CO[Si](OCC=1C=CC=CC=1)(C=C)OCC1=CC=CC=C1 VYJZXBZFLIBVQA-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 239000011086 glassine Substances 0.000 description 1
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- 239000004220 glutamic acid Substances 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 description 1
- IBHBKWKFFTZAHE-UHFFFAOYSA-N n-[4-[4-(n-naphthalen-1-ylanilino)phenyl]phenyl]-n-phenylnaphthalen-1-amine Chemical compound C1=CC=CC=C1N(C=1C2=CC=CC=C2C=CC=1)C1=CC=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=C1 IBHBKWKFFTZAHE-UHFFFAOYSA-N 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- JBLSZOJIKAQEKG-UHFFFAOYSA-N phenyl hypobromite Chemical compound BrOC1=CC=CC=C1 JBLSZOJIKAQEKG-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- UFDHBDMSHIXOKF-UHFFFAOYSA-N tetrahydrophthalic acid Natural products OC(=O)C1=C(C(O)=O)CCCC1 UFDHBDMSHIXOKF-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- QYJYJTDXBIYRHH-UHFFFAOYSA-N trimethoxy-[8-(oxiran-2-ylmethoxy)octyl]silane Chemical compound C(C1CO1)OCCCCCCCC[Si](OC)(OC)OC QYJYJTDXBIYRHH-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229920001866 very low density polyethylene Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/871—Self-supporting sealing arrangements
- H10K59/8722—Peripheral sealing arrangements, e.g. adhesives, sealants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
-
- 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
- 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
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
-
- H01L27/32—
-
- H01L51/50—
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
-
- C09J2201/622—
-
- C09J2205/10—
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
Abstract
본 발명은, 다관능 에폭시 화합물을 함유하는 열경화성의 접착제층을 갖는 접착 시트로서, 다관능 에폭시 화합물의 함유량이, 접착제층 전체 중 5 ∼ 50 질량％ 이며, 특정 전단 특성을 갖는 것을 특징으로 하는 접착 시트이다. 본 발명에 의하면, 봉지성이 우수한 접착제층을 갖는 접착 시트, 및, 봉지물이 상기 접착 시트로 봉지되어 이루어지는 봉지체가 제공된다. This invention is an adhesive sheet which has a thermosetting adhesive bond layer containing a polyfunctional epoxy compound, The content of a polyfunctional epoxy compound is 5-50 mass% in the whole adhesive layer, and has specific shearing characteristics Sheet. According to this invention, the adhesive sheet which has the adhesive bond layer excellent in sealing property, and the sealing body by which the sealing material is sealed with the said adhesive sheet are provided.
Description
본 발명은, 봉지성이 우수한 접착제층을 갖는 접착 시트, 및, 봉지물이 상기 접착 시트로 봉지되어 이루어지는 봉지체에 관한 것이다.This invention relates to the adhesive sheet which has the adhesive bond layer excellent in sealing property, and the sealing body by which the sealing material is sealed by the said adhesive sheet.
최근, 유기 EL 소자는, 저전압 직류 구동에 의한 고휘도 발광이 가능한 발광소자로서 주목받고 있다.In recent years, the organic EL element has attracted attention as a light emitting element capable of high luminance light emission by low voltage direct current driving.
그러나, 유기 EL 소자에는, 시간의 경과와 함께, 발광 휘도, 발광 효율, 발광 균일성 등의 발광 특성이 저하하기 쉽다는 문제가 있었다.However, the organic EL device has a problem that light emission characteristics such as light emission luminance, light emission efficiency, light emission uniformity, and the like tend to decrease with time.
이 발광 특성 저하의 문제의 원인으로서, 산소나 수분 등이 유기 EL 소자의 내부에 침입하여, 전극이나 유기층을 열화시키는 것이 생각되어 왔다. 이 때문에, 이 문제를 해결하기 위해서, 수분 차단성이 우수한 점착 시트를 봉지재로서 사용하는 것이 제안되어 왔다.As a cause of the problem of the deterioration of the luminescence property, it has been considered that oxygen, moisture, or the like penetrates into the interior of the organic EL element and deteriorates the electrode or the organic layer. For this reason, in order to solve this problem, using the adhesive sheet which is excellent in moisture barrier property as a sealing material has been proposed.
또, 액정 디스플레이 (LCD) 나 터치 패널 등의 표시 장치를 제조할 때는, 광학 부재를 첩합 (貼合) 할 목적으로 점착 시트가 사용되지만, 최근, 광학 부재의 기계적 열화를 억제하기 위해서, 수분 차단성이 우수한 점착 시트가 요구되고 있다.Moreover, when manufacturing display apparatuses, such as a liquid crystal display (LCD) and a touch panel, although the adhesive sheet is used for the purpose of bonding together an optical member, in order to suppress mechanical deterioration of an optical member in recent years, moisture blocking is carried out. The adhesive sheet excellent in the property is calculated | required.
이와 같은 특성을 갖는 점착 시트로서, 특허문헌 1 에는, 특정 점착 특성 등을 갖는, 고무계 수지를 주성분으로 하는 점착 시트가 제안되어 있다.As an adhesive sheet which has such a characteristic, in patent document 1, the adhesive sheet which has rubber-based resin which has specific adhesive characteristics etc. as a main component is proposed.
이 문헌에는, 그 점착 시트가 수증기 투과도가 낮은 점착 시트이고, 습열 경과 시에 있어서도 충분한 점착력을 갖고, 또한 습열 경과 시의 황변이 억제된 것인 점이나, 이들 특성을 발현하기 쉬운 점에서, 점착 시트는, 고무계 수지에 더하여 실란 커플링제를 함유하는 것이 바람직한 것 등이 기재되어 있다. In this document, the adhesive sheet is a pressure-sensitive adhesive sheet having low water vapor permeability, and has sufficient adhesive strength even in the course of moist heat, and yellowing at the time of elapsed moist heat, and in that it is easy to express these characteristics. It is described that the sheet preferably contains a silane coupling agent in addition to the rubber-based resin.
특허문헌 1 에 기재된 바와 같이, 고무계 수지를 주성분으로 하는 점착제 조성물을 사용함으로써, 수분 차단성이 우수한 점착 시트가 얻어지는 경향이 있다.As described in Patent Literature 1, an adhesive sheet excellent in moisture barrier property tends to be obtained by using an adhesive composition containing rubber-based resin as a main component.
그러나, 본 발명자들의 검토에 의하면, 이와 같은 점착제 조성물이어도, 고습 조건하에 놓인 후에 점착력이 저하하는 경우가 있어, 봉지재의 형성 재료로서 사용할 수 없는 것도 있는 것을 알 수 있었다.However, according to the examination of the present inventors, even if it is such an adhesive composition, after putting under high humidity conditions, adhesive force may fall and it turned out that it may not be used as a formation material of a sealing material.
따라서, 봉지성이 우수하고, 또한, 고습 조건하에 놓인 후여도, 그 성능이 유지되는 봉지재 형성 재료가 요구되고 있었다.Therefore, the sealing material formation material which is excellent in sealing property and maintains the performance even after putting under high humidity conditions was calculated | required.
본 발명은, 상기 실정을 감안하여 이루어진 것으로, 봉지성이 우수한 접착제층을 갖는 접착 시트, 및, 봉지물이 상기 접착 시트로 봉지되어 이루어지는 봉지체를 제공하는 것을 목적으로 한다.This invention is made | formed in view of the said situation, and an object of this invention is to provide the adhesive sheet which has the adhesive bond layer excellent in sealing property, and the sealing body by which the sealing material is sealed by the said adhesive sheet.
본 발명자들은 상기 과제를 해결하기 위하여, 접착제층에 대해 예의 검토하였다.The present inventors earnestly examined about an adhesive bond layer in order to solve the said subject.
그 결과, 다관능 에폭시 화합물을 특정 비율로 함유하는 열경화성의 접착제층으로서, 특정 전단 특성을 갖는 것은, 봉지성이 우수하고, 또한, 고습 조건하에 놓인 후여도, 그 성능이 유지되는 것을 알아내어, 본 발명을 완성하기에 이르렀다.As a result, as a thermosetting adhesive layer containing a polyfunctional epoxy compound at a specific ratio, it has been found that having a specific shearing property is excellent in encapsulation and is maintained even after being placed under high humidity conditions. The present invention has been completed.
이렇게 하여 본 발명에 의하면, 하기 (1) ∼ (10) 의 접착 시트, 및 (11), (12) 의 봉지체가 제공된다.In this way, according to this invention, the adhesive sheet of following (1)-(10) and the sealing body of (11) and (12) are provided.
(1) 다관능 에폭시 화합물을 함유하는 열경화성의 접착제층을 갖는 접착 시트로서, 다관능 에폭시 화합물의 함유량이, 접착제층 전체 중 5 ∼ 50 질량％ 이며, 하기 조건으로 전단 시험 (A) 를 실시했을 때에, 하기 요건〔1〕 ∼ 〔3〕을 만족하는 것을 특징으로 하는 접착 시트.(1) As an adhesive sheet which has a thermosetting adhesive bond layer containing a polyfunctional epoxy compound, content of a polyfunctional epoxy compound is 5-50 mass% in the whole adhesive layer, and the shear test (A) was performed on condition of the following. The adhesive sheet which satisfy | fills the following requirements [1]-[3] at the time.
〔전단 시험 (A)〕[Shear Test (A)]
단변이 10 mm 인 장방형의 무알칼리 유리를 2 장 준비하고, 이들 중의 1 장의 무알칼리 유리 상에, 1 변이 10 mm 인 정방형의 접착제층을 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 배치하고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트한다. 이어서, 상기 접착제층의, 무알칼리 유리와 접하고 있지 않은 측의 면에, 다른 1 장의 무알칼리 유리를 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 겹치고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트하여 적층체를 얻는다. 이어서, 이 적층체를 100 ℃ 에서 2 시간 가열하여 그 접착제층을 경화시킨다. 그 후, 적층체를 23 ℃, 상대습도 50 ％ 의 조건하에서 24 시간 정치하여, 측정 시료를 얻는다. 얻어진 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정한다.Two rectangular alkali free glasses having 10 mm short sides were prepared, and on one of these alkali free glasses, a square adhesive layer having a side of 10 mm was bonded to a surface area of 100 mm 2 (10 mm × 10 mm). It arrange | positions and laminates these on the conditions of the temperature of 60 degreeC, the pressure of 0.2 MPa, and a lamination rate of 0.2 m / min. Subsequently, another sheet of non-alkali glass is laminated on the surface of the side of the adhesive layer that is not in contact with the alkali-free glass so that the adhesion area is 100 mm 2 (10 mm × 10 mm), and these are bonded at a temperature of 60 ° C. and a pressure of 0.2 MPa. And lamination under the conditions of a lamination rate of 0.2 m / min to obtain a laminate. Next, this laminated body is heated at 100 degreeC for 2 hours, and the adhesive bond layer is hardened. Thereafter, the laminate is allowed to stand for 24 hours under the conditions of 23 ° C and a relative humidity of 50% to obtain a measurement sample. Using the obtained measurement sample, the shear load is measured under conditions of a shear rate of 0.1 mm / minute.
〔요건〕 〔Requirements〕
요건〔1〕 : 최대 전단 하중 (P1 max) 이 전단 변형 10,000 ％ 미만일 때에 측정된다.Requirement [1]: Measured when the maximum shear load (P 1 max ) is less than 10,000% shear deformation.
요건〔2〕 : 최대 전단 하중 (P1 max) 의 값이 100 N 이상이다.Requirement [2]: The value of the maximum shear load (P 1 max ) is 100 N or more.
요건〔3〕 : 전단 변형 10,000 ％ 일 때의 전단 하중 (P1 10000％) 의 값이, 최대 전단 하중 (P1 max) 의 값의 50 ％ 이상이다.Requirement [3]: The value of the shear load (P 1 10000% ) when the shear strain is 10,000% is 50% or more of the value of the maximum shear load (P 1 max ).
(2) 하기 조건으로 전단 시험 (B) 를 실시했을 때에, 하기 요건〔4〕를 만족하는 것을 특징으로 하는, (1) 에 기재된 접착 시트.(2) The adhesive sheet according to (1), which satisfies the following requirement [4] when the shear test (B) is performed under the following conditions.
〔전단 시험 (B)〕[Shear Test (B)]
전단 시험 (A) 에 있어서의 측정 시료의 제작 방법과 마찬가지로 하여 측정 시료를 제작한다.A measurement sample is produced in the same manner as the production method of the measurement sample in the shear test (A).
얻어진 측정 시료를, 온도 60 ℃, 상대습도 90 ％ 의 조건하에 100 시간, 이어서, 온도 23 ℃, 상대습도 50 ％ 의 조건하에 24 시간 정치시킨 후에, 이 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정한다.After the obtained measurement sample was allowed to stand for 100 hours under conditions of a temperature of 60 ° C and a relative humidity of 90%, and then for 24 hours under a condition of a temperature of 23 ° C and a relative humidity of 50%, a shear rate of 0.1 mm / was used using this measurement sample. Measure the shear load in minutes.
〔요건〕 〔Requirements〕
요건〔4〕: 전단 시험 (B) 에 있어서의 최대 전단 하중 (P2 max) 의 값이, 전단 시험 (1) 에 있어서의 최대 전단 하중 (P1 max) 의 값의 70 ％ 이상이다.Requirement [4]: The value of the maximum shear load (P 2 max ) in the shear test (B) is 70% or more of the value of the maximum shear load (P 1 max ) in the shear test (1).
(3) 상기 접착제층이, 추가로 변성 폴리올레핀계 수지를 함유하는 것인, (1) 또는 (2) 에 기재된 접착 시트.(3) The adhesive sheet according to (1) or (2), wherein the adhesive layer further contains a modified polyolefin resin.
(4) 변성 폴리올레핀계 수지의 함유량이, 접착제층 전체 중 40 ∼ 90 질량％ 인, (3) 에 기재된 접착 시트.(4) Adhesive sheet as described in (3) whose content of modified polyolefin resin is 40-90 mass% in the whole adhesive bond layer.
(5) 상기 접착제층이, 추가로 이미다졸계 경화 촉매를 함유하는 것인, (1) ∼ (4) 중 어느 하나에 기재된 접착 시트.(5) The adhesive sheet in any one of (1)-(4) in which the said adhesive bond layer contains an imidazole series hardening catalyst further.
(6) 이미다졸계 경화 촉매의 함유량이, 상기 접착제층 중에 포함되는 상기 다관능 에폭시 화합물 100 질량부에 대해, 0.1 ∼ 10 질량부인, (5) 에 기재된 접착 시트.(6) The adhesive sheet as described in (5) whose content of the imidazole series curing catalyst is 0.1-10 mass parts with respect to 100 mass parts of said polyfunctional epoxy compounds contained in the said adhesive bond layer.
(7) 상기 접착제층이, 추가로 실란 커플링제를 함유하는 것인, (1) ∼ (6) 중 어느 하나에 기재된 접착 시트. (7) The adhesive sheet in any one of (1)-(6) whose said adhesive bond layer contains a silane coupling agent further.
(8) 실란 커플링제의 함유량이, 접착제층 전체 중 0.01 ∼ 2 질량％ 인, (7) 에 기재된 접착 시트.(8) The adhesive sheet as described in (7) whose content of a silane coupling agent is 0.01-2 mass% in the whole adhesive bond layer.
(9) 접착제층의 두께가 1 ∼ 25 ㎛ 인, (1) ∼ (8) 중 어느 하나에 기재된 접착 시트.(9) The adhesive sheet in any one of (1)-(8) whose thickness of an adhesive bond layer is 1-25 micrometers.
(10) 추가로 박리 필름을 갖는, (1) ∼ (9) 중 어느 하나에 기재된 접착 시트.(10) The adhesive sheet according to any one of (1) to (9), further having a release film.
(11) 피봉지물이, (1) ∼ (10) 중 어느 하나에 기재된 접착 시트를 사용하여 봉지되어 이루어지는 봉지체.(11) The sealed body in which the to-be-sealed | blocked object is sealed using the adhesive sheet in any one of (1)-(10).
(12) 상기 피봉지물이, 유기 EL 소자, 유기 EL 디스플레이 소자, 액정 디스플레이 소자, 또는 태양전지 소자인, (11) 에 기재된 봉지체.(12) The sealing body as described in (11) whose said to-be-enclosed object is an organic electroluminescent element, an organic electroluminescent display element, a liquid crystal display element, or a solar cell element.
본 발명에 의하면, 봉지성이 우수한 접착제층을 갖는 접착 시트, 및, 피봉지물이 상기 접착 시트로 봉지되어 이루어지는 봉지체가 제공된다. According to this invention, the adhesive sheet which has the adhesive bond layer excellent in sealing property, and the sealing body by which the to-be-sealed | blocked object are sealed by the said adhesive sheet are provided.
이하, 본 발명을, 1) 접착 시트, 및, 2) 봉지체로 항목 분류하여 상세하게 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is classified in detail by 1) adhesive sheet and 2) sealing body, and it demonstrates in detail.
1) 접착 시트 1) adhesive sheet
본 발명의 접착 시트는, 다관능 에폭시 화합물을 함유하는 열경화성의 접착제층을 갖는 접착 시트로서, 다관능 에폭시 화합물의 함유량이, 접착제층 전체 중 5 ∼ 50 질량％ 이며, 상기 전단 시험 (A) 를 실시했을 때에, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 것을 특징으로 하는 것이다.The adhesive sheet of this invention is an adhesive sheet which has a thermosetting adhesive bond layer containing a polyfunctional epoxy compound, and content of a polyfunctional epoxy compound is 5-50 mass% in the whole adhesive layer, and the said shear test (A) When it implements, it is characterized by the said requirements [1]-[3] being satisfied.
〔접착제층〕 [Adhesive layer]
본 발명의 접착 시트를 구성하는 접착제층은, 다관능 에폭시 화합물을 함유한다.The adhesive bond layer which comprises the adhesive sheet of this invention contains a polyfunctional epoxy compound.
다관능 에폭시 화합물이란, 분자 내에 에폭시기를 2 개 이상 갖는 화합물을 말한다.A polyfunctional epoxy compound means the compound which has 2 or more of epoxy groups in a molecule | numerator.
다관능 에폭시 화합물을 함유하는 접착제를 사용함으로써, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 접착제층을 효율적으로 형성할 수 있다.By using the adhesive agent containing a polyfunctional epoxy compound, the adhesive bond layer which satisfy | fills the said requirements [1]-[3] can be formed efficiently.
다관능 에폭시 화합물로는, 비스페놀 A 형 에폭시 수지, 비스페놀 F 형 에폭시 수지, 비스페놀 S 형 에폭시 수지, 수소 첨가 비스페놀 A 형 에폭시 수지, 수소 첨가 비스페놀 F 형 에폭시 수지, 수소 첨가 비스페놀 S 형 에폭시 수지, 비스페놀 A 디글리시딜에테르, 비스페놀 F 디글리시딜에테르, 비스페놀 S 디글리시딜에테르, 브롬화비스페놀 A 디글리시딜에테르, 브롬화비스페놀 F 디글리시딜에테르, 브롬화비스페놀 S 디글리시딜에테르, 수소 첨가 비스페놀 A 디글리시딜에테르, 수소 첨가 비스페놀 F 디글리시딜에테르, 수소 첨가 비스페놀 S 디글리시딜에테르, 펜타에리트리톨폴리글리시딜에테르, 1,6-헥산디올디글리시딜에테르, 헥사하이드로프탈산디글리시딜에스테르, 네오펜틸글리콜디글리시딜에테르, 트리메틸올프로판폴리글리시딜에테르, 2,2-비스(3-글리시딜-4-글리시딜옥시페닐)프로판, 디메틸올트리시클로데칸디글리시딜에테르 등을 들 수 있다.As the polyfunctional epoxy compound, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, hydrogenated bisphenol A type epoxy resin, hydrogenated bisphenol F type epoxy resin, hydrogenated bisphenol S type epoxy resin, bisphenol A diglycidyl ether, bisphenol F diglycidyl ether, bisphenol S diglycidyl ether, brominated bisphenol A diglycidyl ether, brominated bisphenol F diglycidyl ether, brominated bisphenol S diglycidyl ether, Hydrogenated bisphenol A diglycidyl ether, Hydrogenated bisphenol F diglycidyl ether, Hydrogenated bisphenol S diglycidyl ether, Pentaerythritol polyglycidyl ether, 1, 6- hexanediol diglycidyl ether Hexahydrophthalic acid diglycidyl ester, neopentyl glycol diglycidyl ether, trimethylolpropanepolyglycidyl ether, 2,2-bis (3- Glycidyl-4- glycidyloxyphenyl) propane, dimethylol tricyclodecane diglycidyl ether, etc. are mentioned.
다관능 에폭시 화합물은, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.A polyfunctional epoxy compound can be used individually by 1 type or in combination of 2 or more type.
다관능 에폭시 화합물의 분자량은, 바람직하게는 50 ∼ 10,000, 보다 바람직하게는 100 ∼ 5,000 이다.The molecular weight of the polyfunctional epoxy compound is preferably 50 to 10,000, more preferably 100 to 5,000.
다관능 에폭시 화합물의 에폭시 당량은, 바람직하게는 100 g/eq 이상 500 g/eq 이하, 보다 바람직하게는 150 g/eq 이상 300 g/eq 이하이다. 다관능 에폭시 화합물의 에폭시 당량이 100 g/eq 이상 500 g/eq 이하인 접착제를 사용함으로써, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 접착제층을 갖는 접착 시트가 보다 얻어지기 쉬워진다.The epoxy equivalent of a polyfunctional epoxy compound becomes like this. Preferably it is 100 g / eq or more and 500 g / eq or less, More preferably, it is 150 g / eq or more and 300 g / eq or less. By using the adhesive whose epoxy equivalent of a polyfunctional epoxy compound is 100 g / eq or more and 500 g / eq or less, the adhesive sheet which has an adhesive bond layer which satisfy | fills the said requirements [1]-[3] becomes easier to be obtained.
다관능 에폭시 화합물의 함유량은, 접착제층 전체 중 5 ∼ 50 질량％ 이며, 바람직하게는 10 ∼ 40 질량％ 이다.Content of a polyfunctional epoxy compound is 5-50 mass% in the whole adhesive bond layer, Preferably it is 10-40 mass%.
다관능 에폭시 화합물의 함유량이 지나치게 적은 접착제층은, 상기 요건〔1〕,〔2〕를 만족하기 어려워져, 접착성이 열등하다. 한편, 다관능 에폭시 화합물의 함유량이 지나치게 많은 접착제층은, 상기 요건〔3〕을 만족하기 어려워져, 경화 후의 유연성이 열등하다.The adhesive layer with too little content of a polyfunctional epoxy compound becomes difficult to satisfy said requirements [1] and [2], and is inferior to adhesiveness. On the other hand, the adhesive bond layer with much content of a polyfunctional epoxy compound becomes difficult to satisfy the said requirement [3], and is inferior to the flexibility after hardening.
접착제층은, 다관능 에폭시 화합물 이외의 성분으로서, 변성 폴리올레핀계 수지를 함유하고 있어도 된다.An adhesive bond layer may contain modified polyolefin resin as components other than a polyfunctional epoxy compound.
변성 폴리올레핀계 수지를 함유하는 접착제를 사용함으로써, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 접착제층을 갖는 접착 시트가 보다 얻어지기 쉬워진다.By using the adhesive agent containing modified polyolefin resin, the adhesive sheet which has the adhesive bond layer which satisfy | fills the said requirements [1]-[3] becomes it easier to be obtained.
변성 폴리올레핀계 수지는, 전구체로서의 폴리올레핀 수지에, 변성제를 사용하여 변성 처리를 실시하여 얻어지는, 관능기가 도입된 폴리올레핀 수지이다.The modified polyolefin resin is a polyolefin resin having a functional group introduced therein obtained by performing a modification treatment on a polyolefin resin as a precursor using a modifier.
폴리올레핀 수지란, 올레핀계 단량체 유래의 반복 단위를 포함하는 중합체를 말한다. 폴리올레핀 수지는, 올레핀계 단량체 유래의 반복 단위만으로 이루어지는 중합체여도 되고, 올레핀계 단량체 유래의 반복 단위와, 올레핀계 단량체와 공중합 가능한 단량체 유래의 반복 단위로 이루어지는 중합체여도 된다.A polyolefin resin means the polymer containing the repeating unit derived from an olefin monomer. The polymer which consists only of the repeating unit derived from an olefinic monomer may be sufficient as polyolefin resin, and the polymer which consists of the repeating unit derived from the olefinic monomer and the repeating unit derived from the monomer copolymerizable with an olefinic monomer may be sufficient as it.
올레핀계 단량체로는, 탄소수 2 ∼ 8 의 α-올레핀이 바람직하고, 에틸렌, 프로필렌, 1-부텐, 이소부틸렌, 또는 1-헥센이 보다 바람직하며, 에틸렌 또는 프로필렌이 더욱 바람직하다. 이들 올레핀계 단량체는, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.As an olefin monomer, a C2-C8 alpha olefin is preferable, Ethylene, propylene, 1-butene, isobutylene, or 1-hexene is more preferable, Ethylene or propylene is further more preferable. These olefinic monomers can be used individually by 1 type or in combination of 2 or more type.
올레핀계 단량체와 공중합 가능한 단량체로는, 아세트산비닐, (메트)아크릴산에스테르, 스티렌 등을 들 수 있다. 여기서, 「(메트)아크릴산」은, 아크릴산 또는 메타크릴산의 의미이다 (이하에서 동일.).As a monomer copolymerizable with an olefinic monomer, vinyl acetate, (meth) acrylic acid ester, styrene, etc. are mentioned. Here, "(meth) acrylic acid" is the meaning of acrylic acid or methacrylic acid (it is the same below.).
이들 올레핀계 단량체와 공중합 가능한 단량체는, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.The monomer copolymerizable with these olefinic monomers can be used individually by 1 type or in combination of 2 or more type.
폴리올레핀 수지로는, 초저밀도 폴리에틸렌 (VLDPE), 저밀도 폴리에틸렌 (LDPE), 중밀도 폴리에틸렌 (MDPE), 고밀도 폴리에틸렌 (HDPE), 직사슬형 저밀도 폴리에틸렌, 폴리프로필렌 (PP), 에틸렌-프로필렌 공중합체, 올레핀계 엘라스토머 (TPO), 에틸렌-아세트산비닐 공중합체 (EVA), 에틸렌-(메트)아크릴산 공중합체, 에틸렌-(메트)아크릴산에스테르 공중합체 등을 들 수 있다.As the polyolefin resin, ultra low density polyethylene (VLDPE), low density polyethylene (LDPE), medium density polyethylene (MDPE), high density polyethylene (HDPE), linear low density polyethylene, polypropylene (PP), ethylene-propylene copolymer, olefin System elastomers (TPO), ethylene-vinyl acetate copolymers (EVA), ethylene- (meth) acrylic acid copolymers, ethylene- (meth) acrylic acid ester copolymers, and the like.
폴리올레핀 수지의 변성 처리에 사용하는 변성제는, 분자 내에, 관능기를 갖는 화합물이다.The modifier used for the modification process of polyolefin resin is a compound which has a functional group in a molecule | numerator.
관능기로는, 카르복실기, 카르복실산 무수물기, 카르복실산에스테르기, 수산기, 에폭시기, 아미드기, 암모늄기, 니트릴기, 아미노기, 이미드기, 이소시아네이트기, 아세틸기, 티올기, 에테르기, 티오에테르기, 술폰기, 포스폰기, 니트로기, 우레탄기, 할로겐 원자 등을 들 수 있다. 이들 중에서도, 카르복실기, 카르복실산 무수물기, 카르복실산에스테르기, 수산기, 암모늄기, 아미노기, 이미드기, 이소시아네이트기가 바람직하고, 카르복실산 무수물기, 알콕시실릴기가 보다 바람직하며, 카르복실산 무수물기가 특히 바람직하다.As a functional group, a carboxyl group, a carboxylic anhydride group, a carboxylic ester group, a hydroxyl group, an epoxy group, an amide group, an ammonium group, a nitrile group, an amino group, an imide group, an isocyanate group, an acetyl group, a thiol group, an ether group, a thioether group And sulfone groups, phosphone groups, nitro groups, urethane groups, halogen atoms 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, and a carboxylic anhydride group and an alkoxysilyl group are more preferable, and a carboxylic anhydride group is particularly desirable.
관능기를 갖는 화합물은, 분자 내에 2 종 이상의 관능기를 가지고 있어도 된다.The compound which has a functional group may have 2 or more types of functional groups in a molecule | numerator.
변성 폴리올레핀계 수지로는, 산 변성 폴리올레핀계 수지, 실란 변성 폴리올레핀계 수지를 들 수 있고, 본 발명의 보다 우수한 효과가 얻어지는 관점에서, 산 변성 폴리올레핀계 수지가 바람직하다.Examples of the modified polyolefin-based resin include acid-modified polyolefin-based resins and silane-modified polyolefin-based resins. Acid-modified polyolefin-based resins are preferable from the viewpoint of obtaining more excellent effects of the present invention.
산 변성 폴리올레핀계 수지란, 폴리올레핀 수지에 대해 산으로 그래프트 변성한 것을 말한다. 예를 들어, 폴리올레핀 수지에, 불포화 카르복실산 또는 불포화 카르복실산 무수물 (이하, 이들을 일괄하여 「불포화 카르복실산 등」이라고 하는 경우가 있다.) 을 반응시켜, 카르복실기 또는 카르복실산 무수물기를 도입 (그래프트 변성) 한 것을 들 수 있다.Acid-modified polyolefin resin means what graft-modified the acid with respect to polyolefin resin. For example, unsaturated carboxylic acid or unsaturated carboxylic anhydride (hereinafter, these may be collectively called "unsaturated carboxylic acid", etc.) is made to react with polyolefin resin, and a carboxyl group or a carboxylic anhydride group is introduce | transduced. (Graft degeneration) is mentioned.
폴리올레핀 수지에 반응시키는 불포화 카르복실산 등으로는, 말레산, 푸마르산, 이타콘산, 시트라콘산, 글루타콘산, 테트라하이드로프탈산, 아코니트산 등의 불포화 카르복실산 ; 무수 말레산, 무수 이타콘산, 무수 글루타콘산, 무수 시트라콘산, 무수 아코니트산, 노르보르넨디카르복실산 무수물, 테트라하이드로프탈산 무수물 등의 불포화 카르복실산 무수물 ; 을 들 수 있다.As unsaturated carboxylic acid etc. made to react with a polyolefin resin, Unsaturated carboxylic acid, such as maleic acid, a fumaric acid, itaconic acid, a citraconic acid, glutamic acid, tetrahydrophthalic acid, aconitic acid; Unsaturated carboxylic anhydrides such as maleic anhydride, itaconic anhydride, glutaconic anhydride, citraconic anhydride, aconic acid anhydride, norbornene dicarboxylic anhydride, tetrahydrophthalic anhydride and the like; Can be mentioned.
이들은, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다. 이들 중에서도, 접착 강도가 보다 우수한 접착제가 얻어지기 쉬운 점에서, 무수 말레산이 바람직하다.These can be used individually by 1 type or in combination of 2 or more type. Among these, maleic anhydride is preferable at the point which the adhesive which is more excellent in adhesive strength is easy to be obtained.
폴리올레핀 수지에 반응시키는 불포화 카르복실산 등의 양은, 폴리올레핀 수지 100 질량부에 대해, 바람직하게는 0.1 ∼ 5 질량부, 보다 바람직하게는 0.2 ∼ 3 질량부, 더욱 바람직하게는 0.2 ∼ 1.0 질량부이다. 이와 같이 하여 얻어진 산 변성 폴리올레핀계 수지를 함유하는 접착제는, 접착 강도가 보다 우수하다.The amount of unsaturated carboxylic acid or the like reacting with the polyolefin resin is preferably 0.1 to 5 parts by mass, more preferably 0.2 to 3 parts by mass, still more preferably 0.2 to 1.0 parts by mass with respect to 100 parts by mass of the polyolefin resin. . Thus, the adhesive agent containing the acid-modified polyolefin resin obtained is more excellent in adhesive strength.
산 변성 폴리올레핀계 수지로는, 시판품을 사용할 수도 있다. 시판품으로는, 예를 들어, 아드머 (등록상표) (미츠이 화학사 제조), 유니스톨 (등록상표) (미츠이 화학사 제조), BondyRam (Polyram 사 제조), orevac (등록상표) (ARKEMA 사 제조), 모딕 (등록상표) (미츠비시 화학사 제조) 등을 들 수 있다.A commercial item can also be used as acid-modified polyolefin resin. As a commercial item, For example, Admer (trademark) (made by Mitsui Chemicals Corporation), Unistol (registered trademark) (made by Mitsui Chemicals), BondyRam (made by Polyram), orevac (registered trademark) (made by ARKEMA), Modic (trademark) (made by Mitsubishi Chemical Corporation), etc. are mentioned.
실란 변성 폴리올레핀계 수지란, 폴리올레핀 수지에 대해 불포화 실란 화합물로 그래프트 변성한 것을 말한다. 실란 변성 폴리올레핀계 수지는, 주사슬인 폴리올레핀 수지에 측사슬인 불포화 실란 화합물이 그래프트 공중합한 구조를 갖는다. 예를 들어, 실란 변성 폴리에틸렌 수지 및 실란 변성 에틸렌-아세트산비닐 공중합체를 들 수 있다. 그 중에서도, 실란 변성 저밀도 폴리에틸렌, 실란 변성 초저밀도 폴리에틸렌, 실란 변성 직사슬형 저밀도 폴리에틸렌 등의 실란 변성 폴리에틸렌 수지가 바람직하다.Silane-modified polyolefin resin means what graft-modified with an unsaturated silane compound with respect to polyolefin resin. The silane-modified polyolefin resin has a structure obtained by graft copolymerization of a side chain unsaturated silane compound to a polyolefin resin which is a main chain. For example, a silane modified polyethylene resin and a silane modified ethylene-vinyl acetate copolymer are mentioned. Especially, silane modified polyethylene resins, such as a silane modified low density polyethylene, a silane modified ultra low density polyethylene, and a silane modified linear low density polyethylene, are preferable.
상기 폴리올레핀 수지에 반응시키는 불포화 실란 화합물로는, 비닐실란 화합물이 바람직하고, 예를 들어, 비닐트리메톡시실란, 비닐트리에톡시실란, 비닐트리프로폭시실란, 비닐트리이소프로폭시실란, 비닐트리부톡시실란, 비닐트리펜틸옥시실란, 비닐트리페녹시실란, 비닐트리벤질옥시실란, 비닐트리메틸렌디옥시실란, 비닐트리에틸렌디옥시실란, 비닐프로피오닐옥시실란, 비닐트리아세톡시실란, 비닐트리카르복시실란 등을 들 수 있다. 이들은, 1 종을 단독으로, 또는 2 종 이상을 조합하여 사용할 수 있다.As an unsaturated silane compound made to react with the said polyolefin resin, a vinylsilane compound is preferable, For example, a vinyl trimethoxysilane, a vinyl triethoxysilane, a vinyl tripropoxy silane, a vinyl triisopropoxy silane, and a vinyl tree Butoxysilane, vinyltripentyloxysilane, vinyltriphenoxysilane, vinyltribenzyloxysilane, vinyltrimethylenedioxysilane, vinyltriethylenedioxysilane, vinylpropionyloxysilane, vinyltriacetoxysilane, vinyltri Carboxysilane, etc. are mentioned. These can be used individually by 1 type or in combination of 2 or more type.
불포화 실란 화합물을 주사슬인 폴리올레핀 수지에 그래프트 중합시키는 경우의 조건은, 공지된 그래프트 중합법을 채용하면 된다.What is necessary is just to employ | adopt a well-known graft polymerization method as the conditions in the case of graft-polymerizing an unsaturated silane compound to polyolefin resin which is a principal chain.
폴리올레핀 수지에 반응시키는 불포화 실란 화합물의 양은, 폴리올레핀 수지 100 질량부에 대해, 0.1 ∼ 10 질량부인 것이 바람직하고, 0.3 ∼ 7 질량부인 것이 바람직하고, 0.5 ∼ 5 질량부인 것이 보다 바람직하다. 반응시키는 불포화 실란 화합물의 양이 상기 범위에 있음으로써, 얻어지는 실란 변성 폴리올레핀계 수지를 함유하는 접착제는, 접착 강도가 보다 우수한 것이 된다.It is preferable that it is 0.1-10 mass parts with respect to 100 mass parts of polyolefin resin, It is preferable that it is 0.3-7 mass parts, and, as for the quantity of the unsaturated silane compound made to react with polyolefin resin, it is more preferable that it is 0.5-5 mass parts. When the amount of the unsaturated silane compound to be reacted is in the above range, the adhesive agent containing the silane-modified polyolefin resin obtained is more excellent in adhesive strength.
실란 변성 폴리올레핀계 수지로는, 시판품을 사용할 수도 있다. 시판품으로는, 예를 들어, 링크론 (등록상표) (미츠비시 화학사 제조) 등을 들 수 있다. 그 중에서도, 저밀도 폴리에틸렌계의 링크론, 직사슬형 저밀도 폴리에틸렌계의 링크론, 초저밀도 폴리에틸렌계의 링크론, 및 에틸렌-아세트산비닐 공중합체계의 링크론을 바람직하게 사용할 수 있다.A commercial item can also be used as a silane modified polyolefin resin. As a commercial item, Linkron (trademark) (made by Mitsubishi Chemical Corporation) etc. is mentioned, for example. Especially, the low density polyethylene linkron, the linear low density polyethylene linkon, the ultra low density polyethylene linkon, and the ethylene-vinyl acetate copolymerization linkon can be used preferably.
변성 폴리올레핀계 수지는, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.Modified polyolefin resin can be used individually by 1 type or in combination of 2 or more type.
변성 폴리올레핀계 수지의 수평균 분자량 (Mn) 은 바람직하게는 10,000 ∼ 2,000,000, 보다 바람직하게는, 20,000 ∼ 1,500,000 이다.The number average molecular weight (Mn) of the modified polyolefin resin is preferably 10,000 to 2,000,000, more preferably 20,000 to 1,500,000.
변성 폴리올레핀계 수지의 수평균 분자량 (Mn) 은, 테트라하이드로푸란 (THF) 을 용매로서 사용하여 겔 퍼미에이션 크로마토그래피 (GPC) 를 실시하여, 표준 폴리스티렌 환산값으로서 구할 수 있다.The number average molecular weight (Mn) of modified polyolefin resin can be calculated | required as a standard polystyrene conversion value by performing gel permeation chromatography (GPC) using tetrahydrofuran (THF) as a solvent.
접착제층이 변성 폴리올레핀계 수지를 함유할 때, 변성 폴리올레핀계 수지의 함유량은, 접착제층 전체 중, 바람직하게는 40 ∼ 90 질량％, 보다 바람직하게는 50 ∼ 80 질량％ 이다.When an adhesive bond layer contains modified polyolefin resin, content of modified polyolefin resin is in the whole adhesive layer, Preferably it is 40-90 mass%, More preferably, it is 50-80 mass%.
변성 폴리올레핀계 수지의 함유량이 상기 범위 내임으로써, 그 접착제층은 상기 요건〔1〕 ∼ 〔3〕을 보다 만족하기 쉬워진다.When content of modified polyolefin resin exists in the said range, this adhesive bond layer will become easier to satisfy said requirements [1]-[3].
접착제층은, 다관능 에폭시 화합물 이외의 성분으로서, 이미다졸계 경화 촉매를 함유하고 있어도 된다.The adhesive layer may contain an imidazole series curing catalyst as components other than the polyfunctional epoxy compound.
이미다졸계 경화 촉매를 함유하는 접착제를 사용함으로써, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 접착제층을 갖는 접착 시트가 보다 얻어지기 쉬워진다.By using the adhesive agent containing an imidazole series hardening catalyst, the adhesive sheet which has an adhesive bond layer which satisfy | fills the said requirements [1]-[3] becomes easy to be obtained.
이미다졸계 경화 촉매로는, 2-메틸이미다졸, 2-페닐이미다졸, 2-운데실이미다졸, 2-헵타데실이미다졸, 2-에틸-4-메틸이미다졸, 2-페닐-4-메틸이미다졸, 2-페닐-4-메틸-5-하이드록시메틸이미다졸, 2-페닐-4,5-디하이드록시메틸이미다졸 등을 들 수 있다. 이들 중에서도, 2-에틸-4-메틸이미다졸이 바람직하다.As an imidazole series curing catalyst, 2-methylimidazole, 2-phenylimidazole, 2-undecyl imidazole, 2-heptadecyl imidazole, 2-ethyl-4-methylimidazole, 2 -Phenyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2-phenyl-4,5-dihydroxymethylimidazole, etc. are mentioned. Among these, 2-ethyl-4-methylimidazole is preferable.
이들 이미다졸계 경화 촉매는, 1 종을 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.These imidazole series curing catalysts can be used individually by 1 type or in combination of 2 or more type.
접착제층이 이미다졸계 경화 촉매를 함유할 때, 이미다졸계 경화 촉매의 함유량은, 상기 다관능 에폭시 화합물 100 질량부에 대해, 바람직하게는 0.1 ∼ 10 질량부, 보다 바람직하게는 0.2 ∼ 5 질량부이다. 이미다졸계 경화 촉매의 함유량이 상기 범위 내임으로써, 그 접착제층은 상기 요건〔1〕 ∼ 〔3〕을 보다 만족하기 쉬워진다.When an adhesive bond layer contains an imidazole series curing catalyst, content of an imidazole series curing catalyst becomes like this. Preferably it is 0.1-10 mass parts, More preferably, 0.2-5 mass with respect to 100 mass parts of said polyfunctional epoxy compounds. It is wealth. When content of an imidazole series hardening catalyst exists in the said range, this adhesive bond layer will become easier to satisfy said requirements [1]-[3].
접착제층은, 다관능 에폭시 화합물 이외의 성분으로서, 실란 커플링제를 함유하고 있어도 된다.The adhesive layer may contain a silane coupling agent as a component other than the polyfunctional epoxy compound.
실란 커플링제를 함유하는 접착제를 사용함으로써, 상기 요건〔1〕 ∼ 〔3〕을 만족하는 접착제층을 갖는 접착 시트가 보다 얻어지기 쉬워진다.By using the adhesive agent containing a silane coupling agent, the adhesive sheet which has an adhesive bond layer which satisfy | fills the said requirements [1]-[3] becomes easier to be obtained.
실란 커플링제로는, 공지된 실란 커플링제를 사용할 수 있다. 그 중에서도, 분자 내에 알콕시실릴기를 적어도 1 개 갖는 유기 규소 화합물이 바람직하다. As a silane coupling agent, a well-known silane coupling agent can be used. Especially, the organosilicon compound which has at least 1 alkoxysilyl group in a molecule | numerator is preferable.
실란 커플링제로는, 비닐트리메톡시실란, 비닐트리에톡시실란, 메타크릴옥시프로필트리메톡시실란 등의 중합성 불포화기 함유 규소 화합물 ; 3-글리시독시프로필트리메톡시실란, 2-(3,4-에폭시시클로헥실)에틸트리메톡시실란 등의 에폭시 구조를 갖는 규소 화합물 ; 3-아미노프로필트리메톡시실란, N-(2-아미노에틸)-3-아미노프로필트리메톡시실란, N-(2-아미노에틸)-3-아미노프로필메틸디메톡시실란 등의 아미노기 함유 규소 화합물 ; 3-클로로프로필트리메톡시실란 ; 3-이소시아네이트프로필트리에톡시실란 ; 등을 들 수 있다.As a silane coupling agent, Polymerizable unsaturated-group containing silicon compounds, such as vinyl trimethoxysilane, vinyl triethoxysilane, and methacryloxypropyl trimethoxysilane; Silicon compounds having an epoxy structure such as 3-glycidoxypropyltrimethoxysilane and 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane; Amino group-containing silicon compounds such as 3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane ; 3-chloropropyltrimethoxysilane; 3-isocyanate propyl triethoxysilane; Etc. can be mentioned.
이들 실란 커플링제는, 1 종 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.These silane coupling agents can be used individually by 1 type or in combination of 2 or more type.
접착제층이 실란 커플링제를 함유할 때, 실란 커플링제의 함유량은, 접착제층 전체 중, 바람직하게는 0.01 ∼ 2 질량％, 보다 바람직하게는 0.05 ∼ 1 질량％ 이다.When an adhesive bond layer contains a silane coupling agent, content of a silane coupling agent becomes like this. Preferably it is 0.01-2 mass%, More preferably, it is 0.05-1 mass% in the whole adhesive layer.
실란 커플링제의 함유량이 상기 범위 내임으로써, 그 접착제층은 상기 요건〔1〕 ∼ 〔3〕을 보다 만족하기 쉬워진다.When content of a silane coupling agent exists in the said range, this adhesive bond layer will become easier to satisfy said requirements [1]-[3].
접착제층은, 본 발명의 효과를 방해하지 않는 범위에서, 기타 성분을 함유해도 된다.An adhesive bond layer may contain another component in the range which does not prevent the effect of this invention.
기타 성분으로는, 자외선 흡수제, 대전 방지제, 광 안정제, 산화 방지제, 수지 안정제, 충전제, 안료, 증량제, 연화제 등의 첨가제를 들 수 있다.As another component, additives, such as a ultraviolet absorber, an antistatic agent, an optical stabilizer, antioxidant, a resin stabilizer, a filler, a pigment, an extender, and a softener, are mentioned.
이들은 1 종 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.These can be used individually by 1 type or in combination of 2 or more type.
접착제층이 이들 첨가제를 함유하는 경우, 그 함유량은, 목적에 맞춰 적절히 결정할 수 있다.When an adhesive bond layer contains these additives, the content can be suitably determined according to the objective.
접착제층의 두께는, 바람직하게는 1 ∼ 25 ㎛, 보다 바람직하게는 3 ∼ 20 ㎛ 이다.The thickness of an adhesive bond layer becomes like this. Preferably it is 1-25 micrometers, More preferably, it is 3-20 micrometers.
접착제층은 열경화성을 갖는 것이다. 즉, 접착제층을 가열함으로써, 적어도 다관능 에폭시 화합물의 에폭시기가 반응하여, 접착제층이 경화된다.An adhesive bond layer is thermosetting. That is, by heating an adhesive bond layer, the epoxy group of a polyfunctional epoxy compound reacts at least, and an adhesive bond layer hardens.
접착제층을 열경화시킬 때의 조건은 특별히 한정되지 않는다.The conditions at the time of thermosetting an adhesive bond layer are not specifically limited.
가열 온도는, 통상, 80 ∼ 200 ℃, 바람직하게는 90 ∼ 150 ℃ 이다.Heating temperature is 80-200 degreeC normally, Preferably it is 90-150 degreeC.
가열 시간은, 통상, 30 분 내지 12 시간, 바람직하게는 1 ∼ 6 시간이다.The heating time is usually 30 minutes to 12 hours, preferably 1 to 6 hours.
경화 후의 접착제층의 수증기 투과율은, 통상, 0.1 ∼ 200 g·m-2·day-1, 바람직하게는 1 ∼ 150 g·m-2·day-1 이다. The water vapor transmittance of the adhesive layer after curing is usually 0.1 to 200 g · m −2 · day −1 , preferably 1 to 150 g · m −2 · day −1 .
수증기 투과율은, 공지된 가스 투과율 측정 장치를 사용하여 측정할 수 있다.The water vapor transmission rate can be measured using a known gas transmittance measuring device.
접착제층은, 하기 조건으로 전단 시험 (A) 를 실시했을 때에, 하기 요건〔1〕 ∼ 〔3〕을 만족하는 것이다.The adhesive bond layer satisfies the following requirements [1] to [3] when the shear test (A) was performed under the following conditions.
〔전단 시험 (A)〕[Shear Test (A)]
단변이 10 mm 인 장방형의 무알칼리 유리를 2 장 준비하고, 이들 중의 1 장의 무알칼리 유리 상에, 1 변이 10 mm 인 정방형의 접착제층을 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 배치하고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트한다. 이어서, 상기 접착제층의, 무알칼리 유리와 접하고 있지 않은 측의 면에, 다른 1 장의 무알칼리 유리를 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 겹치고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트하여 적층체를 얻는다. 이어서, 이 적층체를 100 ℃ 에서 2 시간 가열하여 그 접착제층을 경화시킨다. 그 후, 적층체를 23 ℃, 상대습도 50 ％ 의 조건하에서 24 시간 정치하여, 측정 시료를 얻는다. 얻어진 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건, 및 실온 23 ℃, 상대습도 50 ％ 의 분위기하에서 전단 하중을 측정한다.Two rectangular alkali free glasses having 10 mm short sides were prepared, and on one of these alkali free glasses, a square adhesive layer having a 10 mm square was applied so that the adhesive area was 100 mm 2 (10 mm × 10 mm). It arrange | positions and laminates these on the conditions of the temperature of 60 degreeC, the pressure of 0.2 MPa, and a lamination rate of 0.2 m / min. Subsequently, another sheet of non-alkali glass is laminated on the surface of the side of the adhesive layer which is not in contact with the alkali-free glass so that the bonding area becomes 100 mm 2 (10 mm × 10 mm), and these are bonded at a temperature of 60 ° C. and a pressure of 0.2 MPa. And lamination under the conditions of a lamination rate of 0.2 m / min to obtain a laminate. Next, this laminated body is heated at 100 degreeC for 2 hours, and the adhesive bond layer is hardened. Thereafter, the laminate is allowed to stand for 24 hours under the conditions of 23 ° C and a relative humidity of 50% to obtain a measurement sample. Using the obtained measurement sample, the shear load is measured under a condition of a shear rate of 0.1 mm / min, and an atmosphere of a room temperature of 23 ° C. and a relative humidity of 50%.
요건〔1〕 : 최대 전단 하중 (P1 max) 이 전단 변형 10,000 ％ 미만일 때에 측정된다.Requirement [1]: Measured when the maximum shear load (P 1 max ) is less than 10,000% shear deformation.
요건〔2〕 : 최대 전단 하중 (P1 max) 의 값이 100 N 이상이다.Requirement [2]: The value of the maximum shear load (P 1 max ) is 100 N or more.
요건〔3〕 : 전단 변형 10,000 ％ 일 때의 전단 하중 (P1 10000％) 의 값이, 최대 전단 하중 (P1 max) 의 값의 50 ％ 이상이다. Requirement [3]: The value of the shear load (P 1 10000% ) when the shear strain is 10,000% is 50% or more of the value of the maximum shear load (P 1 max ).
전단 변형이란, 접착제층의 두께에 대한 수평 방향의 변위량을 의미하는 것이며, 하기 식에 의해 산출되는 것이다.Shear strain means the displacement amount of the horizontal direction with respect to the thickness of an adhesive bond layer, and is computed by the following formula.
예를 들어, 접착제층의 두께가 10 ㎛ 일 때는, 전단 변형이 10,000 ％ 란, 접착제층의 상면이 하면에 대해 수평으로 1000 ㎛ 어긋난 상태를 나타낸다.For example, when the thickness of an adhesive bond layer is 10 micrometers, a shear deformation of 10,000% shows the state which shifted 1000 micrometers horizontally with respect to the lower surface of the upper surface of an adhesive bond layer.
전단 시험 (A) 는, 통상적인 조건하에 있어서의 접착제의 전단 특성을 평가하는 시험이다.Shear test (A) is a test which evaluates the shear property of an adhesive agent under normal conditions.
본 발명의 접착 시트의 접착제층은, 전단 시험 (A) 를 실시했을 때에 상기 요건〔1〕을 만족하는 것이다. 즉, 본 발명의 접착 시트의 접착제층은, 최대 전단 하중 (P1 max) 이 전단 변형 10,000 ％ 미만일 때에 측정되는 것이다.The adhesive bond layer of the adhesive sheet of this invention satisfies the said requirement [1] when a shear test (A) is performed. That is, the adhesive bond layer of the adhesive sheet of this invention is measured when the maximum shear load (P 1 max ) is less than 10,000% of shear deformation.
요건〔1〕을 만족하는 접착제층은, 봉지성의 관점에서 바람직하다.The adhesive bond layer which satisfy | fills requirement [1] is preferable from a sealing viewpoint.
접착제층 중에 다관능 에폭시 수지를 5 ∼ 50 질량％ 함유시킴으로써, 요건〔1〕을 만족하는 접착제층이 얻어지기 쉬워진다.By containing 5-50 mass% of polyfunctional epoxy resins in an adhesive bond layer, the adhesive bond layer which satisfy | fills requirement [1] becomes easy to be obtained.
본 발명의 접착 시트의 접착제층은, 전단 시험 (A) 를 실시했을 때에 상기 요건〔2〕를 만족하는 것이다. 즉, 본 발명의 접착 시트의 접착제층은, 최대 전단 하중 (P1 max) 의 값이 100 N 이상인 것이다.The adhesive bond layer of the adhesive sheet of this invention satisfies the said requirement [2] when a shear test (A) is performed. That is, the value of the maximum shear load (P 1 max ) of the adhesive bond layer of the adhesive sheet of this invention is 100 N or more.
요건〔2〕를 만족하는 접착제층은, 봉지성의 관점에서 바람직하다.The adhesive bond layer which satisfies the requirement [2] is preferable from the viewpoint of sealing property.
접착제층 중에 다관능 에폭시 수지를 5 ∼ 50 질량％ 함유시킴으로써, 요건〔2〕를 만족하는 접착제층이 얻어지기 쉬워진다.By containing 5-50 mass% of polyfunctional epoxy resins in an adhesive bond layer, the adhesive bond layer which satisfy | fills requirement [2] becomes easy to be obtained.
본 발명의 접착 시트의 접착제층은, 전단 시험 (A) 를 실시했을 때에 상기 요건〔3〕을 만족하는 것이다. 즉, 본 발명의 접착 시트의 접착제층은, 전단 변형 10,000 ％ 일 때의 전단 하중 (P1 10000％) 의 값이, 최대 전단 하중 (P1 max) 의 값의 50 ％ 이상인 것이다.The adhesive bond layer of the adhesive sheet of this invention satisfies the said requirement [3] when a shear test (A) is performed. That is, in the adhesive bond layer of the adhesive sheet of this invention, the value of the shear load (P 1 10000% ) at the time of 10,000% of a shear deformation is 50% or more of the value of the maximum shear load (P 1 max ).
요건〔3〕을 만족하는 접착제층은, 피봉지물을 봉지했을 때의 유연성의 관점에서 바람직하다.The adhesive bond layer which satisfies the requirement [3] is preferable from the viewpoint of flexibility when encapsulating the sealed object.
접착제층 중에 다관능 에폭시 수지를 5 ∼ 50 질량％ 함유시킴으로써, 요건〔3〕을 만족하는 접착제층이 얻어지기 쉬워진다.By containing 5-50 mass% of polyfunctional epoxy resins in an adhesive bond layer, the adhesive bond layer which satisfy | fills requirement [3] becomes easy to be obtained.
또한, 접착제층에 변성 폴리올레핀계 수지를 함유시킴으로써, 요건〔3〕을 만족하는 접착제층이 보다 얻어지기 쉬워진다.Moreover, by containing modified polyolefin resin in an adhesive bond layer, the adhesive bond layer which satisfy | fills requirement [3] becomes easy to be obtained more.
본 발명의 접착 시트의 접착제층은, 하기 조건으로 전단 시험 (B) 를 실시했을 때에, 하기 요건〔4〕를 만족하는 것이 바람직하다.When the adhesive bond layer of the adhesive sheet of this invention performs a shear test (B) on condition of the following, it is preferable to satisfy the following requirements [4].
〔전단 시험 (B)〕[Shear Test (B)]
전단 시험 (A) 에 있어서의 측정 시료의 제작 방법과 마찬가지로 하여 측정 시료를 제작한다.A measurement sample is produced in the same manner as the production method of the measurement sample in the shear test (A).
얻어진 측정 시료를, 온도 60 ℃, 상대습도 90 ％ 의 조건하에 100 시간, 이어서, 온도 23 ℃, 상대습도 50 ％ 의 조건하에 24 시간 정치시킨 후에, 이 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건, 및 실온 23 ℃, 상대습도 50 ％ 의 분위기하에서 전단 하중을 측정한다.After the obtained measurement sample was allowed to stand for 100 hours under conditions of a temperature of 60 ° C and a relative humidity of 90%, and then for 24 hours under a condition of a temperature of 23 ° C and a relative humidity of 50%, a shear rate of 0.1 mm / The shear load is measured under the conditions of minutes and at an ambient temperature of 23 ° C. and a relative humidity of 50%.
요건〔4〕 : 전단 시험 (B) 에 있어서의 최대 전단 하중 (P2 max) 의 값이, 전단 시험 (A) 에 있어서의 최대 전단 하중 (P1 max) 의 값의 70 ％ 이상이다.Requirement [4]: The value of the maximum shear load (P 2 max ) in the shear test (B) is 70% or more of the value of the maximum shear load (P 1 max ) in the shear test (A).
전단 시험 (B) 는, 고습 조건하에 놓인 후의 접착제층의 전단 특성을 평가하는 시험이다.Shear test (B) is a test which evaluates the shear property of the adhesive bond layer after placing under high humidity conditions.
요건〔4〕를 만족하는 접착제층은, 피봉지물을 봉지한 후의 내구성이 우수한 점에서 바람직하다.The adhesive bond layer which satisfies the requirement [4] is preferable at the point which is excellent in durability after sealing a to-be-sealed object.
접착제층에 실란 커플링제를 함유시킴으로써, 요건〔4〕를 만족하는 접착제층이 얻어지기 쉬워진다.By containing a silane coupling agent in an adhesive bond layer, the adhesive bond layer which satisfy | fills requirement [4] becomes easy to be obtained.
〔박리 필름〕 [Release film]
본 발명의 접착 시트는, 박리 필름을 가지고 있어도 된다.The adhesive sheet of this invention may have a peeling film.
박리 필름은, 접착 시트의 제조 공정에 있어서는 지지체로서 기능함과 함께, 접착 시트를 사용할 때까지의 동안에는, 접착제층의 보호 시트로서 기능하는 것이다.A release film functions as a support body in the manufacturing process of an adhesive sheet, and functions as a protective sheet of an adhesive bond layer until it uses an adhesive sheet.
본 발명의 접착 시트를 사용할 때는, 통상, 박리 필름은 박리 제거된다.When using the adhesive sheet of this invention, a peeling film is peeled off normally.
박리 필름으로는, 종래 공지된 것을 이용할 수 있다. 예를 들어, 박리 필름용 기재 상에, 박리제에 의해 박리 처리된 박리층을 갖는 것을 들 수 있다.As a release film, a conventionally well-known thing can be used. For example, what has a peeling layer peeled by the peeling agent on the base material for peeling films is mentioned.
박리 필름용 기재로는, 글라신지, 코트지, 상질지 등의 종이 기재 ; 이들 종이 기재에 폴리에틸렌 등의 열가소성 수지를 라미네이트한 라미네이트지 ; 폴리에틸렌테레프탈레이트 수지, 폴리부틸렌테레프탈레이트 수지, 폴리에틸렌나프탈레이트 수지, 폴리프로필렌 수지, 폴리에틸렌 수지 등의 플라스틱 필름 ; 등을 들 수 있다.As a base material for release films, Paper base materials, such as glassine paper, a coated paper, and a quality paper; Laminated paper which laminated thermoplastic resins, such as polyethylene, on these paper base materials; Plastic films such as polyethylene terephthalate resin, polybutylene terephthalate resin, polyethylene naphthalate resin, polypropylene resin and polyethylene resin; Etc. can be mentioned.
박리제로는, 실리콘계 수지, 올레핀계 수지, 이소프렌계 수지, 부타디엔계 수지 등의 고무계 엘라스토머, 장사슬 알킬계 수지, 알키드계 수지, 불소계 수지 등을 들 수 있다.Examples of the release agent include rubber-based elastomers such as silicone resins, olefin resins, isoprene resins, butadiene resins, long chain alkyl resins, alkyd resins, and fluorine resins.
본 발명의 접착 시트가 박리 필름을 가질 ?, 박리 필름의 장수는 1 장이어도 되고 2 장이어도 되지만, 통상은, 접착제층의 양측에 각각 1 장, 합계 2 장의 박리 필름을 갖는다. 이때 2 장의 박리 필름은 동일해도 되고, 상이해도 되지만, 2 장의 박리 필름은 상이한 박리력을 갖는 것이 바람직하다. 2 장의 박리 필름의 박리력이 상이함으로써, 접착 시트의 사용 시에 문제가 발생하기 어려워진다. 즉, 2 장의 박리 필름의 박리력을 상이하게 함으로써, 최초에 박리 필름을 박리하는 공정을 보다 효율적으로 실시할 수 있다.Although the adhesive sheet of this invention may have a peeling film, and the longevity of a peeling film may be one piece, or two sheets may be sufficient, Usually, each has 1 piece and 2 pieces of peeling films in total on both sides of an adhesive bond layer. At this time, although two peeling films may be the same and may differ, it is preferable that two peeling films have a different peeling force. When the peeling force of two peeling films differs, a problem will hardly arise at the time of use of an adhesive sheet. That is, the process of peeling a peeling film at the first time can be performed more efficiently by making the peeling force of two peeling films different.
〔접착 시트〕 [Adhesion sheet]
접착 시트의 제조 방법은 특별히 한정되지 않는다. 예를 들어, 캐스트법을 사용하여, 접착 시트를 제조할 수 있다.The manufacturing method of an adhesive sheet is not specifically limited. For example, an adhesive sheet can be manufactured using the cast method.
접착 시트를 캐스트법에 의해 제조하는 경우, 예를 들어, 접착제층의 성분과 용매를 함유하는 도공액을 조제하고, 얻어진 도공액을 박리 필름의 박리 처리면에 도공하고, 얻어진 도막을 건조함으로써, 박리 필름이 형성된 접착제층을 제조하고, 이어서, 다른 1 장의 박리 필름을 접착제층 상에 겹침으로써, 접착 시트를 얻을 수 있다.When manufacturing an adhesive sheet by the casting method, for example, by preparing the coating liquid containing the component of an adhesive bond layer, and a solvent, coating the obtained coating liquid on the peeling process surface of a peeling film, and drying the obtained coating film, An adhesive sheet can be obtained by manufacturing the adhesive bond layer in which the peeling film was formed, and then laminating another one peeling film on an adhesive bond layer.
도공액의 조제에 사용하는 용매로는, 벤젠, 톨루엔 등의 방향족 탄화수소계 용매 ; 아세트산에틸, 아세트산부틸 등의 에스테르계 용매 ; 아세톤, 메틸에틸케톤, 메틸이소부틸케톤 등의 케톤계 용매 ; n-펜탄, n-헥산, n-헵탄 등의 지방족 탄화수소계 용매 ; 시클로펜탄, 시클로헥산, 메틸시클로헥산 등의 지환형 탄화수소계 용매 ; 등을 들 수 있다.As a solvent used for preparation of a coating liquid, 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; aliphatic hydrocarbon solvents such as n-pentane, n-hexane and n-heptane; Alicyclic hydrocarbon solvents such as cyclopentane, cyclohexane and methylcyclohexane; Etc. can be mentioned.
이들 용매는, 1 종 단독으로, 혹은 2 종 이상을 조합하여 사용할 수 있다.These solvent can be used individually by 1 type or in combination of 2 or more type.
용매의 함유량은, 도공성 등을 고려하여 적절히 결정할 수 있다.Content of a solvent can be suitably determined in consideration of coating property etc.
도공액을 도공하는 방법으로는, 예를 들어, 스핀 코트법, 스프레이 코트법, 바 코트법, 나이프 코트법, 롤 코트법, 블레이드 코트법, 다이 코트법, 그라비어 코트법 등을 들 수 있다.As a method of coating a coating liquid, the spin coating method, the spray coating method, the bar coating method, the knife coating method, the roll coating method, the blade coating method, the die coating method, the gravure coating method etc. are mentioned, for example.
도막을 건조할 때의 건조 조건으로는, 예를 들어, 건조 온도 80 ∼ 150 ℃, 건조 시간 30 초 내지 5 분간을 들 수 있다.As drying conditions at the time of drying a coating film, drying temperature 80-150 degreeC, drying time 30 second-5 minutes are mentioned, for example.
상기와 같이, 본 발명의 접착 시트의 접착제층은, 상기 전단 특성을 갖는 것이며, 봉지성이 우수한 것이다. 따라서, 본 발명의 접착 시트를 사용하여 봉지재를 형성함으로써, 유기 EL 소자 등의 장수명화를 달성할 수 있다.As mentioned above, the adhesive bond layer of the adhesive sheet of this invention has the said shear characteristic, and is excellent in sealing property. Therefore, long life of organic electroluminescent element etc. can be achieved by forming sealing material using the adhesive sheet of this invention.
3) 봉지체 3) Encapsulation
본 발명의 봉지체는, 피봉지물이, 본 발명의 접착 시트를 사용하여 봉지되어 이루어지는 것이다.In the sealing body of this invention, a to-be-enclosed object is sealed using the adhesive sheet of this invention.
본 발명의 봉지체로는, 예를 들어, 기판과, 그 기판 상에 형성된 소자 (피봉지물) 와, 그 소자를 봉지하기 위한 봉지재를 구비하는 것으로서, 상기 봉지재가 본 발명의 접착 시트의 접착제층 유래의 것 (접착제층의 경화물) 인 것을 들 수 있다.As the sealing body of this invention, it is equipped with the board | substrate, the element (encapsulated object) formed on the board | substrate, and the sealing material for sealing the element, for example, The said sealing material is the adhesive bond layer of the adhesive sheet of this invention. The thing of the origin (hardened | cured material of an adhesive bond layer) is mentioned.
기판은, 특별히 한정되는 것이 아니고, 여러 가지 기판 재료를 사용할 수 있다. 특히 가시광의 투과율이 높은 기판 재료를 사용하는 것이 바람직하다. 또, 소자 외부로부터 침입하려고 하는 수분이나 가스를 저지하는 차단 성능이 높고, 내용제성이나 내후성이 우수한 재료가 바람직하다. 구체적으로는, 석영이나 유리 등의 투명 무기 재료 ; 폴리에틸렌테레프탈레이트, 폴리에틸렌나프탈레이트, 폴리카보네이트, 폴리스티렌, 폴리에틸렌, 폴리프로필렌, 폴리페닐렌술파이드, 폴리불화비닐리덴, 아세틸셀룰로오스, 브롬화페녹시, 아라미드류, 폴리이미드류, 폴리스티렌류, 폴리아릴레이트류, 폴리술폰류, 폴리올레핀류 등의 투명 플라스틱, 전술한 가스 배리어성 필름 ; 을 들 수 있다.The substrate is not particularly limited, and various substrate materials can be used. It is particularly preferable to use a substrate material having a high transmittance of visible light. Moreover, the material which is high in the blocking performance which interrupts the moisture and gas which try to penetrate from the exterior of an element, and is excellent in 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, phenoxy bromide, aramids, polyimides, polystyrenes, polyarylates, poly Transparent plastics such as sulfones and polyolefins, and the above-described gas barrier films; Can be mentioned.
기판의 두께는 특별히 제한되지 않고, 광의 투과율이나, 소자 내외를 차단하는 성능을 감안하여, 적절히 선택할 수 있다.The thickness of the substrate is not particularly limited and can be appropriately selected in consideration of light transmittance and the ability to block the inside and outside of the device.
피봉지물로는, 유기 EL 소자, 유기 EL 디스플레이 소자, 액정 디스플레이 소자, 태양전지 소자 등을 들 수 있다.Examples of the encapsulated product include organic EL elements, organic EL display elements, liquid crystal display elements, and solar cell elements.
본 발명의 봉지체의 제조 방법은 특별히 한정되지 않는다. 예를 들어, 본 발명의 접착 시트의 접착제층을 피봉지물 상에 겹친 후, 가열함으로써, 접착 시트의 접착제층과 피봉지물을 접착시킨다.The manufacturing method of the sealing body of this invention is not specifically limited. For example, after the adhesive layer of the adhesive sheet of this invention is piled up on the to-be-encapsulated object, it heats, and the adhesive bond layer and the to-be-enclosed object of an adhesive sheet are adhere | attached.
이어서, 이 접착제층을 경화시킴으로써, 본 발명의 봉지체를 제조할 수 있다.Subsequently, the sealing body of this invention can be manufactured by hardening this adhesive bond layer.
접착 시트의 접착제층과 피봉지물을 접착시킬 때의 접착 조건은 특별히 한정되지 않는다. 접착 온도는, 예를 들어, 23 ∼ 100 ℃, 바람직하게는 40 ∼ 80 ℃ 이다. 이 접착 처리는, 가압하면서 실시해도 된다.The adhesion conditions at the time of adhering the adhesive bond layer of the adhesive sheet and the to-be-encapsulated object are not specifically limited. Adhesion temperature is 23-100 degreeC, for example, Preferably it is 40-80 degreeC. This adhesion treatment may be performed while pressing.
접착제층을 경화시킬 때의 경화 조건으로는, 앞서 설명한 조건을 이용할 수 있다.As hardening conditions at the time of hardening an adhesive bond layer, the conditions demonstrated above can be used.
본 발명의 봉지체는, 피봉지물이, 본 발명의 접착 시트로 봉지되어 이루어지는 것이다.In the sealing body of this invention, a to-be-enclosed object is sealed by the adhesive sheet of this invention.
따라서, 본 발명의 봉지체에 있어서는, 장기에 걸쳐 피봉지물의 성능이 유지된다.Therefore, in the sealing body of this invention, the performance of a to-be-encapsulated object is maintained over a long term.
실시예Example
이하, 실시예를 들어 본 발명을 더욱 상세하게 설명한다. 단, 본 발명은, 이하의 실시예로 조금도 한정되는 것이 아니다.Hereinafter, an Example is given and this invention is demonstrated in detail. However, this invention is not limited to a following example at all.
각 예 중의 부 및 ％ 는, 특별히 기재가 없는 한, 질량 기준이다.Parts and% in each example are mass references | standards unless there is particular notice.
〔실시예 1〕 EXAMPLE 1
산 변성 폴리올레핀계 수지 (산 변성 α-올레핀 중합체, 미츠이 화학사 제조, 상품명 : 유니스톨 H-200, 수평균 분자량 : 47,000) 76.6 부, 다관능 에폭시 화합물 (1) (수소 첨가 비스페놀 A 형 에폭시 수지, 미츠비시 화학사 제조, 상품명 : YX8034, 에폭시 당량 270 g/eq) 23.0 부, 이미다졸계 경화 촉매 (시코쿠 화성사 제조, 상품명 : 큐어졸 2E4MZ, 2-에틸-4-메틸이미다졸) 0.3 부, 및, 실란 커플링제 (1) (8-글리시독시옥틸트리메톡시실란, 신에츠 화학 공업사 제조, 상품명 : KBM4803) 0.1 부를 메틸에틸케톤에 용해하여, 고형분 농도 18 ％ 의 접착제 조성물 1 을 조제하였다.Acid-modified polyolefin resin (acid-modified alpha-olefin polymer, the Mitsui Chemicals company make, brand name: Unistol H-200, number average molecular weight: 47,000) 76.6 parts, polyfunctional epoxy compound (1) (hydrogenated bisphenol A type epoxy resin, 23.0 parts of Mitsubishi Chemical Corporation, brand name: YX8034, epoxy equivalent 270 g / eq), 0.3 part of imidazole series curing catalysts (manufactured by Shikoku Chemical Co., Ltd., brand name: Curazole 2E4MZ, 2-ethyl-4-methylimidazole), and And 0.1 parts of silane coupling agent (1) (8-glycidoxy octyltrimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd., brand name: KBM4803) were dissolved in methyl ethyl ketone to prepare an adhesive composition 1 having a solid content concentration of 18%.
이 접착제 조성물 1 을 박리 필름 (린텍사 제조, 상품명 : SP-PET382150) 의 박리 처리면 상에 도공하고, 얻어진 도막을 100 ℃ 에서 2 분간 건조하여, 두께가 10 ㎛ 인 접착제층을 형성하고, 그 위에, 다른 1 장의 박리 필름 (린텍사 제조, 상품명 : SP-PET381031) 의 박리 처리면을 첩합하여 접착 시트 1 을 얻었다.Coating this adhesive composition 1 on the peeling process surface of the peeling film (The Lintec make, brand name: SP-PET382150), The obtained coating film is dried at 100 degreeC for 2 minutes, the adhesive bond layer of thickness 10micrometer is formed, Above, the peeling process surface of another one peeling film (The Lintec make, brand name: SP-PET381031) was bonded together, and the adhesive sheet 1 was obtained.
〔실시예 2〕 EXAMPLE 2
실시예 1 에 있어서, 다관능 에폭시 화합물 (1) 대신에, 다관능 에폭시 화합물 (2) (수소 첨가 비스페놀 A 형 에폭시 수지, 미츠비시 화학사 제조, 상품명 : YX8000, 에폭시 당량 205 g/eq) 를 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여, 접착제 조성물 2 를 조제하고, 이것을 사용하여 접착 시트 2 를 얻었다.In Example 1, what used the polyfunctional epoxy compound (2) (hydrogenated bisphenol-A epoxy resin, Mitsubishi Chemical Corporation make, brand name: YX8000, epoxy equivalent 205 g / eq) instead of the polyfunctional epoxy compound (1) Except for Example 1, the adhesive composition 2 was prepared like this and the adhesive sheet 2 was obtained using this.
〔실시예 3〕 EXAMPLE 3
실시예 1 에 있어서, 다관능 에폭시 화합물 (1) 대신에, 다관능 에폭시 화합물 (3) (수소 첨가 비스페놀 A 형 에폭시 수지, 미츠비시 화학사 제조, 상품명 : YX8040, 에폭시 당량 1100 g/eq) 을 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여, 접착제 조성물 3 을 조제하고, 이것을 사용하여 접착 시트 3 을 얻었다.In Example 1, what used the polyfunctional epoxy compound (3) (hydrogenated bisphenol-A epoxy resin, the Mitsubishi Chemical Corporation make, brand name: YX8040, epoxy equivalent 1100 g / eq) instead of the polyfunctional epoxy compound (1) Except for Example 1, the adhesive composition 3 was prepared like this and the adhesive sheet 3 was obtained using this.
〔실시예 4〕 EXAMPLE 4
실시예 1 에 있어서, 실란 커플링제 (1) 대신에, 실란 커플링제 (2) (3-글리시독시프로필트리메톡시실란, 신에츠 화학 공업사 제조, 상품명 : KBM403) 를 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여, 접착제 조성물 4 를 조제하고, 이것을 사용하여 접착 시트 4 를 얻었다.Example 1 WHEREIN: Except having used the silane coupling agent (2) (3-glycidoxy propyl trimethoxysilane, the Shin-Etsu Chemical Co., Ltd. brand name: KBM403) instead of the silane coupling agent (1), Example The adhesive composition 4 was prepared like 1 and the adhesive sheet 4 was obtained using this.
〔실시예 5〕 [Example 5]
실시예 1 에 있어서, 다관능 에폭시 화합물 (1) 대신에, 다관능 에폭시 화합물 (4) (수소 첨가 비스페놀 A 디글리시딜에테르, 쿄에이샤 화학사 제조, 상품명 : 에포라이트 4000, 에폭시 당량 215 ∼ 245 g/eq) 를 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여, 접착제 조성물 5 를 조제하고, 이것을 사용하여 접착 시트 5 를 얻었다.In Example 1, instead of the polyfunctional epoxy compound (1), a polyfunctional epoxy compound (4) (hydrogenated bisphenol A diglycidyl ether, the Kyoeisha Chemical Co., Ltd. make, brand name: Eporite 4000, epoxy equivalent 215- Except having used 245 g / eq), the adhesive composition 5 was prepared like Example 1 and the adhesive sheet 5 was obtained using this.
〔실시예 6〕 EXAMPLE 6
실시예 5 에 있어서, 실란 커플링제 (1) 대신에, 실란 커플링제 (2) (3-글리시독시프로필트리메톡시실란, 신에츠 화학 공업사 제조, 상품명 : KBM403) 를 사용한 것을 제외하고, 실시예 5 와 마찬가지로 하여, 접착제 조성물 6 을 조제하고, 이것을 사용하여 접착 시트 6 을 얻었다.Example 5 WHEREIN: Except that the silane coupling agent (2) (3-glycidoxy propyl trimethoxysilane, the Shin-Etsu Chemical Co., Ltd. make, brand name: KBM403) was used instead of the silane coupling agent (1). The adhesive composition 6 was prepared like 5 and the adhesive sheet 6 was obtained using this.
〔비교예 1〕 [Comparative Example 1]
실시예 1 에 있어서, 다관능 에폭시 화합물 (1) 을 사용하지 않은 것을 제외하고, 실시예 1 과 마찬가지로 하여, 접착제 조성물 7 을 조제하고, 이것을 사용하여 접착 시트 7 을 얻었다. In Example 1, except that the polyfunctional epoxy compound (1) was not used, the adhesive composition 7 was prepared like Example 1, and the adhesive sheet 7 was obtained using this.
〔비교예 2〕 [Comparative Example 2]
교반기, 온도계, 환류 냉각기, 적하 장치 및 질소 도입관을 구비한 반응 용기에, n-부틸아크릴레이트 77 부, 메틸아크릴레이트 20 부, 아크릴산 3 부, 아세트산에틸 200 부, 2,2'-아조비스이소부티로니트릴 0.16 부를 주입하고, 질소 가스 분위기하, 70 ℃ 에서 공중합 반응을 실시하여, 중량 평균 분자량 (Mw) 800,000 의 아크릴계 중합체 (1) 을 얻었다.77 parts of n-butyl acrylates, 20 parts of methyl acrylates, 3 parts of acrylic acid, 200 parts of ethyl acetate, 2,2'- azobis to the reaction container provided with a stirrer, a thermometer, a reflux condenser, a dripping apparatus, and a nitrogen inlet tube. 0.16 parts of isobutyronitrile were injected | thrown-in, and copolymerization reaction was performed at 70 degreeC in nitrogen gas atmosphere, and the acrylic polymer (1) of 800,000 of weight average molecular weights (Mw) was obtained.
아크릴계 중합체 (1) 97.4 부, 톨릴렌디이소시아네이트의 트리메틸올프로판 어덕트체 2.3 부, 알루미늄트리스아세틸아세토네이트 0.3 부를, 톨루엔/아세트산에틸의 혼합 용매〔혼합 비율 (체적비) : 3/2〕에 용해시켜, 고형분 농도 21 ％ 의 접착제 조성물 8 을 조제하였다. 접착제 조성물 8 을 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여 접착 시트 8 을 얻었다.97.4 parts of acrylic polymer (1), 2.3 parts of trimethylolpropane adducts of tolylene diisocyanate, and 0.3 parts of aluminum trisacetylacetonate are dissolved in a mixed solvent of [toluene / ethyl acetate] (mixing ratio (volume ratio): 3/2] And the adhesive composition 8 of 21% of solid content concentration was prepared. Except having used the adhesive composition 8, it carried out similarly to Example 1, and obtained the adhesive sheet 8.
〔비교예 3〕 [Comparative Example 3]
교반기, 온도계, 환류 냉각기, 적하 장치 및 질소 도입관을 구비한 반응 용기에, 2-에틸헥실아크릴레이트 60 부, 메틸메타크릴레이트 20 부, 하이드록시에틸아크릴레이트 20 부, 아세트산에틸 200 부, 2,2'-아조비스이소부티로니트릴 0.16 부를 주입하고, 질소 가스 분위기하, 70 ℃ 에서 공중합 반응을 실시하여, 중량 평균 분자량 (Mw) 700,000 의 아크릴계 중합체 (2) 를 얻었다.60 parts 2-ethylhexyl acrylate, 20 parts methyl methacrylate, 20 parts hydroxyethyl acrylate, 200 parts ethyl acetate, to the reaction container provided with a stirrer, a thermometer, a reflux condenser, a dripping apparatus, and a nitrogen inlet tube. 0.16 parts of, 2'-azobisisobutyronitrile were injected | thrown-in, and copolymerization reaction was performed at 70 degreeC in nitrogen gas atmosphere, and the acrylic polymer (2) of 700,000 of weight average molecular weights (Mw) was obtained.
아크릴계 중합체 (2) 99.5 부, 톨릴렌디이소시아네이트의 트리메틸올프로판 어덕트체 0.2 부, 3-글리시독시프로필트리메톡시실란 0.3 부를 아세트산에틸/메틸에틸케톤의 혼합 용매〔혼합 비율 (체적비) : 4/1〕에 용해시켜, 고형분 농도 35 ％ 의 접착제 조성물 9 를 조제하였다. 접착제 조성물 9 를 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여 접착 시트 9 를 얻었다.99.5 parts of acrylic polymer (2), 0.2 parts of trimethylolpropane adducts of tolylene diisocyanate, and 0.3 parts of 3-glycidoxypropyltrimethoxysilane were mixed solvents of ethyl acetate / methyl ethyl ketone [mixing ratio (volume ratio): 4 / 1], and the adhesive composition 9 of 35% of solid content concentration was prepared. Except having used the adhesive composition 9, it carried out similarly to Example 1, and obtained the adhesive sheet 9.
〔비교예 4〕 (Comparative Example 4)
이소부틸렌과 이소프렌의 공중합체 (닛폰 부틸사 제조, Exxon Butyl 268, 수평균 분자량 260,000, 이소프렌의 함유율 1.7 몰％) 100 부에 대해, 카르복실산계 관능기를 갖는 폴리이소프렌 고무 (쿠라레사 제조, LIR410, 수평균 분자량 30,000, 1 분자당의 평균 카르복실기수 : 10) 5 부, 지방족계 석유 수지 (닛폰 제온사 제조, 퀸톤 A100, 연화점 100 ℃) 20 부, 가교제 (에폭시 화합물, 미츠비시 화학사 제조, TC-5) 1 부를 톨루엔에 용해하여, 고형분 농도 25 ％ 의 접착제 조성물 10 을 얻었다. 접착제 조성물 10 을 사용한 것을 제외하고, 실시예 1 과 마찬가지로 하여 접착 시트 10 을 얻었다.Polyisoprene rubber having a carboxylic acid-based functional group to 100 parts by weight of isobutylene and isoprene copolymer (manufactured by Nippon Butyl, Exxon Butyl 268, number average molecular weight 260,000, isoprene content of 1.7 mol%) , Number average molecular weight 30,000, average number of carboxyl groups per molecule: 10) 5 parts, aliphatic petroleum resin (manufactured by Nippon Xeon, Quinton A100, softening point 100 ° C) 20 parts, crosslinking agent (epoxy compound, manufactured by Mitsubishi Chemical Corporation, TC-5 1 part was melt | dissolved in toluene, and the adhesive composition 10 of 25% of solid content concentration was obtained. Except having used the adhesive composition 10, it carried out similarly to Example 1, and obtained the adhesive sheet 10.
실시예 1 ∼ 6, 비교예 1 ∼ 4 에서 얻은 접착 시트 1 ∼ 10 에 대해, 이하의 시험을 실시하였다.The following tests were done about the adhesive sheets 1-10 obtained in Examples 1-6 and Comparative Examples 1-4.
〔전단 시험 (A)〕[Shear Test (A)]
실시예 또는 비교예에서 얻은 접착 시트를, 1 변이 10 mm 인 정방형으로 가공하였다.The adhesive sheet obtained in the Example or the comparative example was processed into the square whose one side is 10 mm.
단변이 10 mm 인 장방형의 무알칼리 유리를 2 장 준비하였다. 상기 정방형의 접착 시트의 박리 필름을 1 장 박리하고, 남은 접착 시트를, 노출된 접착제층이 무알칼리 유리에 대향하고, 또한, 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 무알칼리 유리 상에 배치하고, 가압 롤러를 사용하여, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트하였다. 이어서, 다른 1 장의 박리 필름을 박리하고, 노출된 접착제층 상에 다른 1 장의 무알칼리 유리를 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 겹치고, 가압 롤러를 사용하여, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트하여 적층체를 얻었다.Two rectangular alkali free glass with a short side of 10 mm were prepared. One peeling film of the said square adhesive sheet is peeled off, and the remaining adhesive sheet is an alkali free glass so that the exposed adhesive bond layer may be opposed to an alkali free glass, and an adhesive area may be set to 100 mm <2> (10 mm x 10 mm). It was arrange | positioned, and it laminated using the pressure roller on condition of the temperature of 60 degreeC, the pressure of 0.2 MPa, and the lamination rate of 0.2 m / min. Subsequently, another one peeling film is peeled off, and the other one alkali free glass is laminated | stacked on the exposed adhesive bond layer so that an adhesive area may be set to 100 mm <2> (10mm * 10mm), and these pressures were used, and they were temperature 60 degreeC. The laminate was obtained by laminating under the condition of a pressure of 0.2 MPa and a lamination rate of 0.2 m / min.
이어서, 이 적층체를 100 ℃ 에서 2 시간 가열하여 그 접착제층을 경화시켰다. 그 후, 적층체를 23 ℃, 상대습도 50 ％ 의 조건하에서 24 시간 정치하여, 측정 시료를 얻었다.Next, this laminated body was heated at 100 degreeC for 2 hours, and the adhesive bond layer was hardened. Then, the laminated body was left to stand on 23 degreeC and the conditions of 50% of a relative humidity for 24 hours, and the measurement sample was obtained.
얻어진 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정하였다.Using the obtained measurement sample, the shear load was measured under conditions of a shear rate of 0.1 mm / minute.
〔전단 시험 (B)〕 [Shear Test (B)]
전단 시험 (A) 에 있어서의 측정 시료의 제작 방법과 마찬가지로 하여 측정 시료를 제작하였다.The measurement sample was produced like the manufacturing method of the measurement sample in a shear test (A).
얻어진 측정 시료를, 온도 60 ℃, 상대습도 90 ％ 의 조건하에 100 시간, 이어서, 온도 23 ℃, 상대습도 50 ％ 의 조건하에 24 시간 정치시킨 후에, 이 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정하였다.After the obtained measurement sample was allowed to stand for 100 hours under conditions of a temperature of 60 ° C and a relative humidity of 90%, and then for 24 hours under a condition of a temperature of 23 ° C and a relative humidity of 50%, a shear rate of 0.1 mm / was used using this measurement sample. Shear load was measured under conditions of minutes.
〔유기 EL 소자의 평가 시험〕 [Evaluation Test of Organic EL Device]
산화인듐주석 (ITO) 막 (두께 : 100 nm, 시트 저항 : 50 Ω/□ (옴 퍼 스퀘어) 이 성막된 유리 기판을 양극 (陽極) 으로서 갖는 유기 EL 소자를, 이하의 방법에 의해 제작하였다.An organic EL device having, as an anode, a glass substrate on which an indium tin oxide (ITO) film (thickness: 100 nm, sheet resistance: 50 Ω / square (ohm per square)) was formed was produced by the following method.
먼저, 상기 유리 기판의 ITO 막 상에, N,N'-비스(나프탈렌-1-일)-N,N'-비스(페닐)-벤지딘) (Luminescence Technology 사 제조) 을 50 nm, 트리스(8-하이드록시-퀴놀리네이트)알루미늄 (Luminescence Technology 사 제조) 을 50 nm, 0.1 ∼ 0.2 nm/분의 속도로 순차 증착시켜, 발광층을 형성하였다.First, on an ITO film of the glass substrate, N, N'-bis (naphthalen-1-yl) -N, N'-bis (phenyl) benzidine) (manufactured by Luminescence Technology) was 50 nm and Tris (8 -Hydroxy-quinolinate) aluminum (manufactured by Luminescence Technology) was sequentially deposited at a rate of 50 nm and 0.1 to 0.2 nm / min to form a light emitting layer.
얻어진 발광층 상에, 전자 주입 재료로서, 불화리튬 (LiF) (고순도 화학 연구소사 제조) 을 0.1 nm/분의 속도로 4 nm, 이어서 알루미늄 (Al) (고순도 화학 연구소사 제조) 을 0.1 nm/분의 속도로 100 nm 증착시켜 음극을 형성하여, 유기 EL 소자를 얻었다.On the obtained light emitting layer, lithium fluoride (LiF) (manufactured by High Purity Chemical Research Institute) was 4 nm at a rate of 0.1 nm / min, followed by aluminum (Al) (manufactured by High Purity Chemical Research Institute) by 0.1 nm / min as an electron injection material. The anode was formed by evaporating 100 nm at a speed of to obtain an organic EL device.
또한, 증착 시의 진공도는, 모두 1 × 10-4 Pa 이하였다.In addition, the vacuum degree at the time of vapor deposition was all 1 * 10 <-4> Pa or less.
실시예 또는 비교예에서 얻은 접착 시트의 박리 필름을 1 장 박리하고, 노출된 접착제층을 금속박 필름 상에 겹치고, 히트 라미네이터를 사용하여 이들을 60 ℃ 에서 접착하였다. 이어서, 다른 1 장의 박리 필름을 박리하고, 노출된 접착제층을, 유리 기판 상에 형성된 유기 EL 소자를 덮도록 겹치고, 히트 라미네이터를 사용하여 이들을 60 ℃ 에서 접착하였다. 이어서, 100 ℃ 에서 2 시간 가열하여 접착제층을 경화시켜, 유기 EL 소자가 봉지된 보텀 이미션형의 전자 디바이스를 얻었다.One peeling film of the adhesive sheet obtained in the Example or the comparative example was peeled off, the exposed adhesive bond layer was laminated | stacked on the metal foil film, and these were bonded at 60 degreeC using the heat laminator. Next, the other peeling film was peeled off, the exposed adhesive bond layer was overlapped so that the organic electroluminescent element formed on the glass substrate might be covered, and they were bonded at 60 degreeC using the heat laminator. Subsequently, it heated at 100 degreeC for 2 hours, hardening an adhesive bond layer, and obtained the bottom emission type electronic device in which the organic electroluminescent element was sealed.
이 전자 디바이스를, 온도 60 ℃, 상대습도 90 ％ 의 환경하에 250 시간 정치시킨 후, 유기 EL 소자를 기동시켜, 다크 스폿 (비발광 지점) 의 유무를 관찰하고, 이하의 기준으로 평가하였다.After letting this electronic device stand for 250 hours in the environment of the temperature of 60 degreeC, and 90% of a relative humidity, organic electroluminescent element was started, the presence or absence of a dark spot (non-luminescent point) was observed, and the following references | standards evaluated.
◎ : 다크 스폿이 발광 면적의 40 ％ 미만 ◎: dark spot is less than 40% of the light emitting area
△ : 다크 스폿이 발광 면적의 40 ％ 이상 50 ％ 미만(Triangle | delta): 40% or more and less than 50% of a light-emitting area
× : 다크 스폿이 발광 면적의 50 ％ 이상 X: 50% or more of the light emission area of a dark spot
평가 결과를 표 1 에 나타낸다.The evaluation results are shown in Table 1.
표 1 로부터 이하를 알 수 있다.Table 1 shows the following.
실시예 1 ∼ 6 에서 얻어진 접착 시트의 접착제층은 봉지성이 우수한 것이며, 이들을 사용하여 유기 EL 소자를 봉지함으로써, 다크 스폿의 발생을 억제할 수 있다.The adhesive bond layer of the adhesive sheets obtained in Examples 1-6 is excellent in sealing property, and can generate | occur | produce dark spot by sealing organic electroluminescent element using these.
한편, 비교예 1 ∼ 4 에서 얻어진 접착 시트의 접착제층은, 소정의 전단 특성을 가지지 않는 것이고, 이들은 봉지성이 열등하다.On the other hand, the adhesive bond layer of the adhesive sheets obtained in Comparative Examples 1-4 does not have predetermined | prescribed shearing property, and these are inferior to sealing property.
Claims (12)
다관능 에폭시 화합물의 함유량이, 접착제층 전체 중 5 ∼ 50 질량％ 이며,
하기 조건으로 전단 시험 (A) 를 실시했을 때에, 하기 요건 (1) ∼ (3) 을 만족하는 것을 특징으로 하는 접착 시트.
〔전단 시험 (A)〕
단변이 10 mm 인 장방형의 무알칼리 유리를 2 장 준비하고, 이들 중의 1 장의 무알칼리 유리 상에, 1 변이 10 mm 인 정방형의 접착제층을 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 배치하고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트한다. 이어서, 상기 접착제층의, 무알칼리 유리와 접하고 있지 않은 측의 면에, 다른 1 장의 무알칼리 유리를 접착 면적이 100 ㎟ (10 mm × 10 mm) 가 되도록 겹치고, 이들을 온도 60 ℃, 압력 0.2 MPa, 라미네이트 속도 0.2 m/분의 조건으로 라미네이트하여 적층체를 얻는다. 이어서, 이 적층체를 100 ℃ 에서 2 시간 가열하여 그 접착제층을 경화시킨다. 그 후, 적층체를 23 ℃, 상대습도 50 ％ 의 조건하에서 24 시간 정치하여, 측정 시료를 얻는다. 얻어진 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정한다.
〔요건〕
요건〔1〕 : 최대 전단 하중 (P1 max) 이 전단 변형 10,000 ％ 미만일 때에 측정된다.
요건〔2〕 : 최대 전단 하중 (P1 max) 의 값이 100 N 이상이다.
요건〔3〕 : 전단 변형 10,000 ％ 일 때의 전단 하중 (P1 10000％) 의 값이, 최대 전단 하중 (P1 max) 의 값의 50 ％ 이상이다.An adhesive sheet having a thermosetting adhesive layer containing a polyfunctional epoxy compound,
Content of a polyfunctional epoxy compound is 5-50 mass% in the whole adhesive layer,
When the shear test (A) is performed under the following conditions, the following requirements (1) to (3) are satisfied.
[Shear Test (A)]
Two rectangular alkali free glasses having 10 mm short sides were prepared, and on one of these alkali free glasses, a square adhesive layer having a side of 10 mm was bonded to a surface area of 100 mm 2 (10 mm × 10 mm). It arrange | positions and laminates these on the conditions of the temperature of 60 degreeC, the pressure of 0.2 MPa, and a lamination rate of 0.2 m / min. Subsequently, another sheet of non-alkali glass is laminated on the surface of the side of the adhesive layer that is not in contact with the alkali-free glass so that the adhesion area is 100 mm 2 (10 mm × 10 mm), and these are bonded at a temperature of 60 ° C. and a pressure of 0.2 MPa. And lamination under the conditions of a lamination rate of 0.2 m / min to obtain a laminate. Next, this laminated body is heated at 100 degreeC for 2 hours, and the adhesive bond layer is hardened. Thereafter, the laminate is allowed to stand for 24 hours under the conditions of 23 ° C and a relative humidity of 50% to obtain a measurement sample. Using the obtained measurement sample, the shear load is measured under conditions of a shear rate of 0.1 mm / minute.
〔Requirements〕
Requirement [1]: Measured when the maximum shear load (P 1 max ) is less than 10,000% shear deformation.
Requirement [2]: The value of the maximum shear load (P 1 max ) is 100 N or more.
Requirement [3]: The value of the shear load (P 1 10000% ) when the shear strain is 10,000% is 50% or more of the value of the maximum shear load (P 1 max ).
하기 조건으로 전단 시험 (B) 를 실시했을 때에, 하기 요건〔4〕를 만족하는 것을 특징으로 하는 접착 시트.
〔전단 시험 (B)〕
전단 시험 (A) 에 있어서의 측정 시료의 제작 방법과 마찬가지로 하여 측정 시료를 제작한다.
얻어진 측정 시료를, 온도 60 ℃, 상대습도 90 ％ 의 조건하에 100 시간, 이어서, 온도 23 ℃, 상대습도 50 ％ 의 조건하에 24 시간 정치시킨 후에, 이 측정 시료를 사용하여, 전단 속도 0.1 mm/분의 조건으로 전단 하중을 측정한다.
〔요건〕
요건〔4〕 : 전단 시험 (B) 에 있어서의 최대 전단 하중 (P2 max) 의 값이, 전단 시험 (A) 에 있어서의 최대 전단 하중 (P1 max) 의 값의 70 ％ 이상이다.The method of claim 1,
The adhesive sheet which satisfy | fills following requirement [4] when the shear test (B) is performed on the following conditions.
[Shear Test (B)]
A measurement sample is produced in the same manner as the production method of the measurement sample in the shear test (A).
After the obtained measurement sample was allowed to stand for 100 hours under conditions of a temperature of 60 ° C and a relative humidity of 90%, and then for 24 hours under a condition of a temperature of 23 ° C and a relative humidity of 50%, a shear rate of 0.1 mm / was used using this measurement sample. Measure the shear load in minutes.
〔Requirements〕
Requirement [4]: The value of the maximum shear load (P 2 max ) in the shear test (B) is 70% or more of the value of the maximum shear load (P 1 max ) in the shear test (A).
상기 접착제층이, 추가로 변성 폴리올레핀계 수지를 함유하는 것인, 접착 시트.The method according to claim 1 or 2,
The adhesive sheet in which the said adhesive bond layer contains modified polyolefin resin further.
변성 폴리올레핀계 수지의 함유량이, 접착제층 전체 중 40 ∼ 90 질량％ 인, 접착 시트. The method of claim 3, wherein
Adhesive sheet whose content of modified polyolefin resin is 40-90 mass% in the whole adhesive bond layer.
상기 접착제층이, 추가로 이미다졸계 경화 촉매를 함유하는 것인, 접착 시트. The method according to any one of claims 1 to 4,
The adhesive sheet in which the said adhesive bond layer contains an imidazole series hardening catalyst further.
이미다졸계 경화 촉매의 함유량이, 상기 접착제층 중에 포함되는 상기 다관능 에폭시 화합물 100 질량부에 대해, 0.1 ∼ 10 질량부인, 접착 시트.The method of claim 5, wherein
The adhesive sheet whose content of an imidazole series hardening catalyst is 0.1-10 mass parts with respect to 100 mass parts of said polyfunctional epoxy compounds contained in the said adhesive bond layer.
상기 접착제층이, 추가로 실란 커플링제를 함유하는 것인, 접착 시트.The method according to any one of claims 1 to 6,
The adhesive sheet in which the said adhesive bond layer contains a silane coupling agent further.
실란 커플링제의 함유량이, 접착제층 전체 중 0.01 ∼ 2 질량％ 인, 접착 시트. The method of claim 7, wherein
The adhesive sheet whose content of a silane coupling agent is 0.01-2 mass% in the whole adhesive bond layer.
접착제층의 두께가 1 ∼ 25 ㎛ 인, 접착 시트.The method according to any one of claims 1 to 8,
The adhesive sheet whose thickness of an adhesive bond layer is 1-25 micrometers.
추가로 박리 필름을 갖는, 접착 시트.The method according to any one of claims 1 to 9,
The adhesive sheet which has a peeling film further.
상기 피봉지물이, 유기 EL 소자, 유기 EL 디스플레이 소자, 액정 디스플레이 소자, 또는 태양전지 소자인, 봉지체.The method of claim 11,
The said sealed object is an organic electroluminescent element, an organic electroluminescent display element, a liquid crystal display element, or a solar cell element.
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| JP2017107485 | 2017-05-31 | ||
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| PCT/JP2018/020731 WO2018221571A1 (en) | 2017-05-31 | 2018-05-30 | Adhesive sheet, and sealed body |
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| TWI729034B (en) * | 2015-12-01 | 2021-06-01 | 日商琳得科股份有限公司 | Adhesive composition, sealing plate and sealing body |
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| JP2008163344A (en) * | 2008-01-22 | 2008-07-17 | Nitto Denko Corp | Reactive adhesive composition for fixing electronic component and its adhesive sheet |
| KR20150092187A (en) * | 2012-11-30 | 2015-08-12 | 린텍 가부시키가이샤 | Adhesive agent composition, adhesive sheet, and electronic device |
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