CN108353475A - composition for sealing - Google Patents
composition for sealing Download PDFInfo
- Publication number
- CN108353475A CN108353475A CN201680067352.6A CN201680067352A CN108353475A CN 108353475 A CN108353475 A CN 108353475A CN 201680067352 A CN201680067352 A CN 201680067352A CN 108353475 A CN108353475 A CN 108353475A
- Authority
- CN
- China
- Prior art keywords
- sealing
- ingredient
- mentioned
- group
- organic electroluminescent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000203 mixture Substances 0.000 title claims abstract description 155
- 238000007789 sealing Methods 0.000 title claims abstract description 152
- 239000004615 ingredient Substances 0.000 claims abstract description 89
- 150000001875 compounds Chemical class 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 69
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 20
- 238000010538 cationic polymerization reaction Methods 0.000 claims abstract description 20
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical group C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 15
- 239000003505 polymerization initiator Substances 0.000 claims abstract description 15
- 125000001046 glycoluril group Chemical class [H]C12N(*)C(=O)N(*)C1([H])N(*)C(=O)N2* 0.000 claims abstract 3
- 125000003566 oxetanyl group Chemical group 0.000 claims abstract 2
- 239000000835 fiber Substances 0.000 claims description 123
- 239000000126 substance Substances 0.000 claims description 92
- 239000002245 particle Substances 0.000 claims description 87
- 239000011248 coating agent Substances 0.000 claims description 77
- 238000000576 coating method Methods 0.000 claims description 77
- 238000000034 method Methods 0.000 claims description 61
- 238000005286 illumination Methods 0.000 claims description 25
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 19
- 238000011049 filling Methods 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 11
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 10
- 238000005401 electroluminescence Methods 0.000 claims description 9
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 8
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 7
- 238000005253 cladding Methods 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 5
- 238000010422 painting Methods 0.000 claims description 2
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 claims 1
- 238000013022 venting Methods 0.000 abstract description 9
- -1 episulfide compounds Chemical class 0.000 description 95
- 239000002585 base Substances 0.000 description 61
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 27
- 239000002904 solvent Substances 0.000 description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 23
- 239000004593 Epoxy Substances 0.000 description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 21
- 238000007711 solidification Methods 0.000 description 19
- 230000008023 solidification Effects 0.000 description 19
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 18
- VPVSTMAPERLKKM-UHFFFAOYSA-N glycoluril Chemical class N1C(=O)NC2NC(=O)NC21 VPVSTMAPERLKKM-UHFFFAOYSA-N 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 17
- 229910052799 carbon Inorganic materials 0.000 description 16
- 125000000217 alkyl group Chemical group 0.000 description 15
- 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 14
- 235000013339 cereals Nutrition 0.000 description 14
- 239000004215 Carbon black (E152) Substances 0.000 description 13
- 229930195733 hydrocarbon Natural products 0.000 description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 12
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 12
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 11
- 150000001768 cations Chemical class 0.000 description 11
- 229960000834 vinyl ether Drugs 0.000 description 11
- 125000001118 alkylidene group Chemical group 0.000 description 10
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 10
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 10
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 10
- 150000002921 oxetanes Chemical group 0.000 description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 9
- 239000005977 Ethylene Substances 0.000 description 9
- 150000001721 carbon Chemical group 0.000 description 9
- 150000002430 hydrocarbons Chemical class 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 9
- 239000001294 propane Substances 0.000 description 9
- 125000004450 alkenylene group Chemical group 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 125000005843 halogen group Chemical group 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 8
- 125000004430 oxygen atom Chemical group O* 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000004305 biphenyl Substances 0.000 description 7
- 235000010290 biphenyl Nutrition 0.000 description 7
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 229920001577 copolymer Polymers 0.000 description 7
- 229940052303 ethers for general anesthesia Drugs 0.000 description 7
- 125000005842 heteroatom Chemical group 0.000 description 7
- 239000002070 nanowire Substances 0.000 description 7
- 229920002554 vinyl polymer Polymers 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 230000035515 penetration Effects 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 125000004646 sulfenyl group Chemical group S(*)* 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 229940106691 bisphenol a Drugs 0.000 description 5
- 150000002118 epoxides Chemical class 0.000 description 5
- 150000002170 ethers Chemical class 0.000 description 5
- 125000000623 heterocyclic group Chemical group 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 5
- 229920003986 novolac Polymers 0.000 description 5
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 5
- 150000002927 oxygen compounds Chemical class 0.000 description 5
- 125000001424 substituent group Chemical group 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 3
- 125000006374 C2-C10 alkenyl group Chemical group 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 3
- 125000006267 biphenyl group Chemical group 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
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 150000003983 crown ethers Chemical class 0.000 description 3
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N n-Butanol Substances CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 125000006340 pentafluoro ethyl group Chemical group FC(F)(F)C(F)(F)* 0.000 description 3
- 125000000538 pentafluorophenyl group Chemical group FC1=C(F)C(F)=C(*)C(F)=C1F 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910052701 rubidium Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- DNVXWIINBUTFEP-UHFFFAOYSA-N 2-[(2-phenylphenoxy)methyl]oxirane Chemical compound C1OC1COC1=CC=CC=C1C1=CC=CC=C1 DNVXWIINBUTFEP-UHFFFAOYSA-N 0.000 description 2
- CQOZJDNCADWEKH-UHFFFAOYSA-N 2-[3,3-bis(2-hydroxyphenyl)propyl]phenol Chemical compound OC1=CC=CC=C1CCC(C=1C(=CC=CC=1)O)C1=CC=CC=C1O CQOZJDNCADWEKH-UHFFFAOYSA-N 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 2
- CGRJJOYCFCCGPX-UHFFFAOYSA-N 3-ethyloxetane Chemical compound CCC1COC1 CGRJJOYCFCCGPX-UHFFFAOYSA-N 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 125000004453 alkoxycarbonyl group Chemical group 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 125000005587 carbonate group Chemical group 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229930003836 cresol Natural products 0.000 description 2
- 150000001896 cresols Chemical class 0.000 description 2
- 125000000596 cyclohexenyl group Chemical group C1(=CCCCC1)* 0.000 description 2
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000006735 epoxidation reaction Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 150000002220 fluorenes Chemical class 0.000 description 2
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 2
- 238000010191 image analysis Methods 0.000 description 2
- 125000001041 indolyl group Chemical group 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N methyl cyanide Natural products CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 2
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N methylene hexane Natural products CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000000466 oxiranyl group Chemical group 0.000 description 2
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 2
- RMVRSNDYEFQCLF-UHFFFAOYSA-O phenylsulfanium Chemical compound [SH2+]C1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-O 0.000 description 2
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
- 229920001197 polyacetylene Polymers 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 229920000123 polythiophene Polymers 0.000 description 2
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- 238000003756 stirring Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- WHLUQAYNVOGZST-UHFFFAOYSA-N tifenamil Chemical group C=1C=CC=CC=1C(C(=O)SCCN(CC)CC)C1=CC=CC=C1 WHLUQAYNVOGZST-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 150000003852 triazoles Chemical group 0.000 description 1
- ZFEAYIKULRXTAR-UHFFFAOYSA-M triphenylsulfanium;chloride Chemical compound [Cl-].C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 ZFEAYIKULRXTAR-UHFFFAOYSA-M 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- QVTVDJWJGGEOGX-UHFFFAOYSA-N urea;cyanide Chemical group N#[C-].NC(N)=O QVTVDJWJGGEOGX-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/21—Urea; Derivatives thereof, e.g. biuret
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/04—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
- C08G65/16—Cyclic ethers having four or more ring atoms
- C08G65/18—Oxetanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1515—Three-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Epoxy Resins (AREA)
- Electroluminescent Light Sources (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Sealing Material Composition (AREA)
- Polyethers (AREA)
Abstract
The present invention provides a kind of organic EL element composition for sealing, it is not necessary that organic EL element to be directly exposed in UV, and can effectively utilize the solidfied material with low venting quality and moisture resistance and be sealed.The organic EL element composition for sealing of the present invention contains following compositions (A), ingredient (B) and ingredient (C).Ingredient (A)：With 2 or more the cation-curable compounds selected from one or more of alicyclic epoxy group, the group containing oxetanes ring, epithio base and vinyl ether group group in 1 molecule；Ingredient (B)：Light cationic polymerization initiator；Ingredient (C)：Glycoluril compounds.
Description
Technical field
The present invention relates to can be sealed against in the case where not damaging organic EL element, can protect organic EL element not
The composition for sealing deteriorated caused by moisture occurs.The day that the application is filed an application based on November 30th, 2015 in Japan
This Patent 2015-233349 claims priority, and its content is incorporated herein.
Background technology
Organic electroluminescent (hereinafter also referred to " organic EL ") element has sandwiches luminescent layer using a pair of of opposite electrode
It constitutes, the electrode injection electronics from side, the electrode injection hole from the other side.The injected electrons and hole are in luminescent layer
In conjunction with when generate shine.Including the organic EL device of above-mentioned organic EL element because its high-impact, visibility and
The diversity of illuminant colour and as the flat-panel monitor of full color or as substitute LED equipment and receive expectation.Organic EL devices
The light extraction mode of part include top emission type and bottom emission type both, the aperture opening ratio of top emission type is big, therefore goes out light efficiency
Rate is excellent, is preferred in this regard.
However, compared with other electronic units, organic EL element is easier to be influenced by moisture, and existing can be because immersion has
Moisture in machine EL element and the problem of cause the oxidation of electrode, the denaturation of organic matter etc., the characteristics of luminescence caused to be remarkably decreased.Make
For the method for solving the problems, such as this, it is known to using the solidfied material of composition for sealing by the peripheral sealing of organic EL element (or packet
Cover) method.
As above-mentioned encapsulating method, it is known to：Periphery to being formed in the organic EL element on substrate, which utilizes, to be shone in UV
It penetrates the lower cured composition for sealing of generation to be filled, then cures above-mentioned composition for sealing, be thus sealed
Method (1)；To head cover (lid) coating composition for sealing and after carrying out UV irradiations, is fitted in and be formed with organic EL element
Substrate and the method (2) being sealed.
The above method (1) is due to making organic EL element be directly exposed in UV, thus presence causes the characteristics of luminescence to reduce
Problem.In addition, configuring colour filter on the top of organic EL element to form the organic EL device with high contrast
In the case of, can because colour filter there are due to shield UV, therefore existing causes what the solidification of composition for sealing became inadequate to ask
Topic.
On the other hand, in the above method (2), although can prevent due to making organic EL element be directly exposed in UV
The caused characteristics of luminescence reduces, but since the solidification of composition for sealing under uv illumination can carry out rapidly, if presence is pasted
Closing operation is slow, can cause fitting become difficult, yield rate reduce the problem of.
Following the description has been recorded in patent document 1：Containing epoxide, polymerization initiator and as cure retarder
Crown ether, polyethers composition for sealing, even if with that can carry out and complete cured if shielding UV reactions after UV irradiations
Therefore characteristic if using above-mentioned composition in the above method (2), can inhibit the organic EL element caused by UV
Deterioration while realize sealing.It can decompose in the presence of cation however, crown ether, polyethers exist and generate exhaust,
And the problem of causing organic EL element to deteriorate because of the exhaust.
Existing technical literature
Patent document
Patent document 1：No. 4384509 bulletins of Japanese Patent No.
Invention content
Problems to be solved by the invention
Therefore, the purpose of the present invention is to provide a kind of organic EL element composition for sealing, it is not necessary that organic EL is first
Part is directly exposed in UV, and can be effectively utilized the solidfied material with low venting quality and moisture resistance and be sealed.
The other of the present invention are designed to provide a kind of organic EL element composition for sealing, are not necessarily to organic EL element
It is directly exposed in UV, and the solidfied material with low venting quality, moisture resistance and electric conductivity can be effectively utilized and be sealed.
Solution to the problem
The present inventor has made intensive studies to solve the above subject, as a result, it has been found that：Relative to by light cationic polymerization
Weakly alkaline glycoluril compounds are equivalent to for the cation that initiator generates, having can capture due to carrying out UV irradiations by light sun
Cation that cation polymerization initiator generates, to inhibit the progress of cationic polymerization, and the release sun when implementing to heat
Ion and make cationic polymerization carry out effect；Above-mentioned glycoluril compounds will not become the producing cause of exhaust；Addition can be passed through
Glycoluril compounds and the service life for freely controlling composition for sealing, by being irradiated to the film of the composition for sealing
Conformed to after UV organic EL element then implement heat treatment, can organic EL element is not directly exposed in UV,
And sealing is realized in the case of not causing fitting to become difficult, so as to yield rate well using with low venting quality and anti-
Moist solidfied material sealing organic el element.
In addition, it is found that when adding specific conducting fibre coating particles into composition for sealing, it can utilize and remove
Also conductive solidfied material seals organic EL element other than features described above.
It is completed the present invention is based on these opinions.
That is, the present invention contains following compositions (A), ingredient (B) for a kind of sealing organic electroluminescent element composition
And ingredient (C).
Ingredient (A)：There are 2 or more in 1 molecule and be selected from alicyclic epoxy group, the group containing oxetanes ring, epithio
The cation-curable compound of one kind or two or more group in base and vinyl ether group；
Ingredient (B)：Light cationic polymerization initiator；
Ingredient (C)：Glycoluril compounds.
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, wherein ingredient (C) be containing
The glycoluril compounds of glycidyl or allyl.
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, wherein relative to ingredient (B) 1
Parts by weight contain 0.05~3 parts by weight of ingredient (C).
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, wherein also containing following compositions
(D)。
Ingredient (D)：The compound with 1 or more glycidyl ether (is contained in the change in ingredient (A) in 1 molecule
Except conjunction object).
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, wherein also containing average grain diameter
For 0.001~30 μm of inorganic filling material.
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, wherein also containing following conductions
Property fiber coating particles.
Conducting fibre coating particles：Include the electric conductivity object of the threadiness of particle-like substance and the cladding particle-like substance
The conducting fibre coating particles of matter.
In addition, the present invention provides above-mentioned sealing organic electroluminescent element composition, it is that top emission type is organic
Electroluminescent cell composition for sealing.
In addition, the present invention provides a kind of manufacturing method of organic electroluminescence device, have via following processes 1 and 2 pairs
Electro-luminescence element is sealed.
Process 1：Illumination is implemented to the film formed by above-mentioned sealing organic electroluminescent element composition；
Process 2：Make the element setting that the substrate for being provided with element is fitted in via the film after illumination obtained from process 1
Simultaneously implement to heat in face.
In addition, the present invention provides a kind of organic electroluminescence device, has above-mentioned sealing organic electroluminescent element and use
The solidfied material of composition.
That is, the present invention relates to following technical proposals.
[1] a kind of sealing organic electroluminescent element composition contains following compositions (A), ingredient (B) and ingredient
(C)。
Ingredient (A)：There are 2 or more in 1 molecule and be selected from alicyclic epoxy group, the group containing oxetanes ring, epithio
The cation-curable compound of one or more of base and vinyl ether group group；
Ingredient (B)：Light cationic polymerization initiator；
Ingredient (C)：Glycoluril compounds.
[2] the sealing organic electroluminescent element composition described in above-mentioned [1], wherein ingredient (A) contains in 1 molecule
Compound with 2 or more epoxycyclohexyls.
[3] the sealing organic electroluminescent element composition described in above-mentioned [1], wherein ingredient (A) contains formula (a) institute
The compound shown.
[4] the sealing organic electroluminescent element composition described in above-mentioned [1], wherein ingredient (A), which contains, to be selected from the group
At least one of compound：(3,4,3 ', 4 '-diepoxy) joins hexamethylene, bis- (3,4- epoxycyclohexyl-methyls) ethers, 1,2- rings
Bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) ethane of oxygen-1,2-, bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) propane of 2,2- and 1,2- are bis-
(3,4- 7-oxa-bicyclo[4.1.0-1- bases) ethane.
[5] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[4], wherein ingredient
(A) contain and at least one of be selected from the group compound：4,4 '-bis- [(3- ethyl -3- oxetanylmethoxies) methoxies] join
Bis- [(3- ethyl -3- oxetanylmethoxies methoxyl group) methyl] benzene of benzene, 1,4-, bis- { [1- ethyls (3- oxetanylmethoxies)] methyl }
Ether, 4,4 '-bis- [(3- ethyl -3- oxetanylmethoxies) methoxies] connection hexamethylene, the bis- [(3- ethyl -3- oxa- ring fourths of 1,4-
Base) methoxy] hexamethylene, 3- ethyls -3 { [(3- Ethyloxetane -3- bases) methoxyl group] methyl } oxetanes,
And phenol novolak type oxetanes.
[6] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[5], wherein ingredient
(A) contain the episulfide compounds with fluorene skeleton.
[7] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[6], wherein ingredient
(A) contain cyclic annular ether type vinyl ether compound.
[8] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[7], wherein sealing
With in the cation-curable total amount of compound (100 weight %) for including in composition, the ratio shared by ingredient (A) is 30~80
Weight %.
[9] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[8], wherein relative to
The content of 100 parts by weight of cation-curable compound for including in composition for sealing, ingredient (B) is 0.05~4 parts by weight.
[10] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[9], wherein ingredient
(C) it is formula (c) compound represented.
[11] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[9], wherein ingredient
(C) it is the glycoluril compounds containing glycidyl or allyl.
[12] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[11], wherein opposite
In 1 parts by weight of ingredient (B), contain 0.05~3 parts by weight of ingredient (C).
[13] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[12], wherein also containing
There are following compositions (D).
Ingredient (D)：The compound with 1 or more glycidyl ether (is contained in the change in ingredient (A) in 1 molecule
Except conjunction object)
[14] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[13], wherein close
In the cation-curable total amount of compound (100 weight %) for including in envelope composition, ratio shared by ingredient (D) is 20~
70 weight %.
[15] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[14], wherein close
In the cation-curable total amount of compound (100 weight %) for including in envelope composition, ingredient (A) and ingredient (D) it is total
The shared ratio of amount is 70 weight % or more.
[16] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[15], wherein also containing
It is 0.001~30 μm of inorganic filling material to have average grain diameter.
[17] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[16], wherein also containing
There are following conducting fibre coating particles.
Conducting fibre coating particles：Include the electric conductivity object of the threadiness of particle-like substance and the cladding particle-like substance
The conducting fibre coating particles of matter.
[18] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[17], is top
Emission type organic electro luminescent component seal composition.
[19] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[18], viscosity (25
DEG C, shear velocity:20 (1/s)) it is 10~10000mPas.
[20] the sealing organic electroluminescent element composition described in any one of above-mentioned [1]~[19], wherein from photograph
Penetrate ultraviolet light (exposure:2000mJ/cm2) just terminate viscosity the risings degree started until after irradiation 30 minutes for 1.5 times with
Under.
[21] a kind of manufacturing method of organic electroluminescence device, via following processes 1 and 2 pairs of organic electroluminescent members
Part is sealed.
Process 1：Painting to being formed with composition by the sealing organic electroluminescent element described in any one of [1]~[20]
Film implements illumination；
Process 2：Make to fit in the base for being provided with organic electroluminescent device via the film after illumination obtained from process 1
The element setting face of plate simultaneously is implemented to heat.
[22] a kind of organic electroluminescence device has the organic electroluminescent member described in any one of [1]~[20]
The solidfied material of part composition for sealing.
[23] organic electroluminescence device described in above-mentioned [22], wherein above-mentioned solidfied material (thickness:100 μm) moisture-inhibiting
Amount is 150g/m2Dayatm or less.
The effect of invention
The organic EL element composition for sealing of the present invention is due to above-mentioned composition, even if irradiating UV to film,
It can also inhibit cured progress before implementing to heat, it, will not be viscous because losing even if the progress of fitting operation is sluggish
Connecing property and cause fitting become difficult.In turn, by the implementation heat treatment after fitting, solidification can be made to carry out, it can be not
Sealing is realized in the case that organic EL element is directly exposed in UV.In addition, the organic EL element sealing combination of the present invention
Object can form the solidfied material with moisture resistance while also with low venting quality, can prevent organic caused by moisture, exhaust
The deterioration of EL element.Further, contain conducting fibre coating particles in the organic EL element composition for sealing of the present invention
In the case of, the solidfied material for also having both electric conductivity can be formed.
Therefore, organic EL element composition for sealing of the invention, by the present invention organic EL element composition for sealing
The piece or film of formation, can be suitable for the seal applications of top emission type organic EL element.
In addition, using the present invention organic EL element composition for sealing, by the present invention organic EL element sealing group
The piece that object is formed or the organic EL device that film is sealed are closed, there is the excellent characteristics of luminescence, long lifespan and reliability height.
Description of the drawings
An example of the scanning electron microscope image (SEM image) of conducting fibre coating particles in [Fig. 1] present invention.
[Fig. 2] shows to have used the manufacturing method of the organic EL device of the organic EL element composition for sealing of the present invention
The schematic diagram of an example.
Symbol description
1 head cover (lid)
2 box dams (dam)
3 distributors
4 composition for sealing
5 substrates
6 cathodes
7 luminescent layers
8 anodes
Specific implementation mode
[organic EL element composition for sealing]
The organic EL element composition for sealing (hereinafter also referred to " composition for sealing ") of the present invention contains following compositions
(A), ingredient (B) and ingredient (C).
Ingredient (A)：There are 2 or more in 1 molecule and be selected from alicyclic epoxy group, the group containing oxetanes ring, epithio
The cation-curable compound of one or more of base and vinyl ether group group；
Ingredient (B)：Light cationic polymerization initiator；
Ingredient (C)：Glycoluril compounds.
(ingredient (A))
The ingredient (A) of the present invention is that there are 2 or more to be selected from alicyclic epoxy group (by adjacent 2 that constitute alicyclic ring in 1 molecule
The epoxy group that carbon atom and oxygen atom are constituted, such as epoxycyclohexyl etc.), the group containing oxetanes ring, epithio base and
The cation-curable compound of one or more of vinyl ether group group.The compound being contained in ingredient (C)
Except.
As the compound (hereinafter also referred to " alicyclic epoxy with 2 or more above-mentioned alicyclic epoxy groups in 1 molecule
Close object "), following formula (a) compound represented can be enumerated.
[chemical formula 1]
In above-mentioned formula (a), R1~R18It is identical or different, it indicates hydrogen atom, halogen atom, optionally include oxygen atom or halogen atom
Alkyl or optionally with substituent group alkoxy.
As R1~R18In halogen atom, it can be mentioned, for example：Fluorine atom, chlorine atom, bromine atom, iodine atom etc..
As R1~R18In alkyl, it can be mentioned, for example：Aliphatic alkyl, alicyclic type hydrocarbon, aromatic hydrocarbyl, Yi Jiyou
Group made of 2 or more bondings in them.
As above-mentioned aliphatic alkyl, it can be mentioned, for example：It is methyl, ethyl, propyl, isopropyl, butyl, hexyl, octyl, different
The C such as octyl, decyl, dodecyl1-20Alkyl (preferably C1-10Alkyl, particularly preferably C1-4Alkyl)；Vinyl, allyl,
Methacrylic, 1- acrylic, isopropenyl, 1- cyclobutenyls, 2- cyclobutenyls, 3- cyclobutenyls, 1- pentenyls, 2- pentenyls, 3-
The C such as pentenyl, 4- pentenyls, 5- hexenyls2-20Alkenyl (preferably C2-10Alkenyl, particularly preferably C2-4Alkenyl)；Acetenyl, third
The C such as alkynyl2-20Alkynyl (preferably C2-10Alkynyl, particularly preferably C2-4Alkynyl) etc..
As above-mentioned alicyclic type hydrocarbon, it can be mentioned, for example：Cyclopropyl, cyclobutyl, cyclopenta, cyclohexyl, cyclo-dodecyl
Equal C3-12Naphthenic base；The C such as cyclohexenyl group3-12Cycloalkenyl group；The C such as bicycloheptyl, bicycloheptene base4-15Endocyclic alkyl etc..
As above-mentioned aromatic hydrocarbyl, it can be mentioned, for example：The C such as phenyl, naphthalene6-14Aryl (preferably C6-10Aryl) etc..
In addition, as by 2 or more in the group selected from above-mentioned aliphatic alkyl, alicyclic type hydrocarbon and aromatic hydrocarbyl
Group made of bonding, it can be mentioned, for example：The C such as cyclohexyl methyl3-12Naphthenic base replaces C1-20Alkyl；The C such as methylcyclohexyl1-20
Alkyl replaces C3-12Naphthenic base；The C such as benzyl, phenethyl7-18Aralkyl is (in particular, C7-10Aralkyl)；The C such as cinnamyl6-14Aryl
Replace C2-20Alkenyl；The C such as tolyl1-20Alkyl replaces C6-14Aryl；The C such as styryl2-20Alkenyl replaces C6-14Aryl etc..
As R1~R18In the optionally alkyl comprising oxygen atom or halogen atom, at least one in above-mentioned alkyl can be enumerated
Hydrogen atom by with oxygen atom group or halogen atom replace made of group etc..It, can as the above-mentioned group with oxygen atom
It enumerates for example：Hydroxyl；Hydroperoxy；The C such as methoxyl group, ethyoxyl, propoxyl group, isopropoxy, butoxy, isobutoxy1-10Alkane
Oxygroup；The C such as allyloxy2-10Alkenyloxy group；Optionally have and is selected from C1-10Alkyl, C2-10Alkenyl, halogen atom and C1-10In alkoxy
The C of substituent group6-14Aryloxy group (for example, toloxyl, naphthoxy etc.)；The C such as benzyloxy, benzene ethyoxyl7-18Aralkoxy；Acetyl
The C such as oxygroup, propionyloxy, (methyl) acryloxy, benzoyloxy1-10Acyloxy；Methoxycarbonyl, ethoxy carbonyl,
The C such as propoxycarbonyl, butoxy carbonyl1-10Alkoxy carbonyl；Optionally have and is selected from C1-10Alkyl, C2-10Alkenyl, halogen atom and
C1-10The C of substituent group in alkoxy6-14Aryloxycarbonyl is (for example, phenyloxycarbonyl, toloxyl carbonyl, naphthoxycarbonyl
Deng)；The C such as benzyloxycarbonyl7-18Aromatic alkoxy carbonyl；The group containing epoxy group such as glycidyl oxygroup；Ethyl oxa- ring fourth
The group of the oxygen heterocycle butyl such as oxygroup；The C such as acetyl group, propiono, benzoyl1-10Acyl group；Isocyanate group；Sulfo group；Ammonia
Base formoxyl；Oxo base；By 2 or more in these via singly-bound or C1-10Group etc. made of the bondings such as alkylidene.
As R1~R18In alkoxy, it can be mentioned, for example：Methoxyl group, ethyoxyl, propoxyl group, isopropoxy, butoxy,
The C such as isobutoxy1-10Alkoxy.
As the substituent group that above-mentioned alkoxy optionally has, it can be mentioned, for example：Halogen atom, hydroxyl, C1-10Alkoxy,
C2-10Alkenyloxy group, C6-14Aryloxy group, C1-10Acyloxy, sulfydryl, C1-10Alkylthio group, C2-10Alkenylthio group, C6-14Arylthio, C7-18Aralkyl
Sulfenyl, carboxyl, C1-10Alkoxy carbonyl, C6-14Aryloxycarbonyl, C7-18Aromatic alkoxy carbonyl, amino, list or two C1-10Alkyl ammonia
Base, C1-10Acyl amino, the group containing epoxy group, the group of oxygen heterocycle butyl, C1-10Acyl group, oxo base and by these
2 or more via singly-bound or C1-10Group etc. made of the bondings such as alkylidene.
In above-mentioned formula (a), X indicates singly-bound or links group (bivalent group with 1 or more atom).As above-mentioned company
Group is tied, it can be mentioned, for example：Epoxidised alkenylene, carbonyl, ether has occurred in some or all of bivalent hydrocarbon radical, carbon-to-carbon double bond
Key, ester bond, carbonate group, amide groups and by multiple groups etc. to link in them.
As above-mentioned bivalent hydrocarbon radical, it can be mentioned, for example：The straight-chain of carbon atom number 1~18 or the alkylidene of branched, carbon
The alicyclic type hydrocarbon etc. of the divalent of atomicity 3~18.It, can as the straight-chain of carbon atom number 1~18 or the alkylidene of branched
It enumerates for example：Methylene, methylmethylene, dimethylated methylene base, ethylidene, propylidene, trimethylene etc..As carbon atom number
3~18 divalent alicyclic type hydrocarbon, it can be mentioned, for example：1,2- cyclopentylenes, 1,3- cyclopentylenes, cyclopentylidene, the Asias 1,2- hexamethylene
Cycloalkylidenes such as base, 1,3- cyclohexylidenes, 1,4- cyclohexylidenes, cyclohexylidene (including cycloalkanes fork) etc..
Epoxidised alkenylene (also referred to as " epoxidation Asia alkene has occurred as some or all of above-mentioned carbon-to-carbon double bond
Base ") in alkenylene, it can be mentioned, for example：Ethenylidene, allylidene, 1- butenylidenes, 2- butenylidenes, Aden's dialkylene,
The alkenylene etc. of the straight or brancheds of carbon atom numbers 2~8 such as inferior pentenyl, sub- hexenyl, heptene base, sub- octenyl.It is special
It is not that, as above-mentioned epoxidation alkenylene, epoxidised alkenylene has occurred in the whole of preferably carbon-to-carbon double bond, more preferably
The alkenylene of epoxidised carbon atom number 2~4 has occurred in the whole of carbon-to-carbon double bond.
As above-mentioned connection group X, the particularly preferably connection group containing oxygen atom is specific enumerable：-CO-、-O-
CO-O-、-COO-、-O-、-CONH-；By multiple groups to link in these groups；By 1 or 2 in these groups
A above 1 or 2 or more group etc. to link with above-mentioned bivalent hydrocarbon radical.
As the typical example of cycloaliphatic epoxy shown in above-mentioned formula (a), it can be mentioned, for example：(3,4,3 ', 4 '-two
Epoxy) join hexamethylene, bis- (3,4- epoxycyclohexyl-methyls) ethers, bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) second of 1,2- epoxies-1,2-
Bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) propane of alkane, 2,2-, bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) ethane of 1,2- or following formula
(1)~(10) compound represented etc..It should be noted that the L in following formula (5) is the alkylidene of carbon atom number 1~8,
In preferably carbon atom number 1~3 straight-chain or branched alkylidene.N in following formula (5), (7), (9), (10)1~n8
It is identical or different, indicate 1~30 integer.
[chemical formula 2]
[chemical formula 3]
As cycloaliphatic epoxy, wherein curability, heat resistance (glass transition temperature from composition for sealing
Degree), low-shrinkage, from the perspective of low linear expansion, it is preferable to use (3,4,3 ', 4 '-diepoxy) connection hexamethylene and/or double
(3,4- epoxycyclohexyl-methyls) ether.From the viewpoint of the moisture resistance of solidfied material, particularly preferably (3,4,3 ', 4 '-two rings
Oxygen) connection hexamethylene.
(hereinafter also referred to as the compound with 2 or more the above-mentioned groups containing oxetanes ring in 1 molecule
" oxetane compound "), it can be mentioned, for example：4,4 '-bis- [(3- ethyl -3- oxetanylmethoxies) methoxy] biphenyl,
Bis- [(3- ethyl -3- oxetanylmethoxies methoxyl group) methyl] benzene of 1,4-, bis- { [1- ethyls (3- oxetanylmethoxies)] methyl } ethers, 4,
4 '-bis- [(3- ethyl -3- oxetanylmethoxies) methoxies] join hexamethylene, bis- [(3- ethyl -3- oxetanylmethoxies) first of 1,4-
Oxygroup methyl] hexamethylene, 3- ethyls -3 { [(3- Ethyloxetane -3- bases) methoxyl group] methyl } oxetanes, phenol
Phenolic varnish type oxetanes etc..It can use such as trade name " ETERNACOLL OXBP " (the emerging production (strain) in space portion is made)
Commercially available product.
As in 1 molecule with 2 or more above-mentioned epithio bases compound, it can be mentioned, for example：Bis- (the β-epithio rosickyite of 1,3-
Base) hexamethylene, bis- (β-epithio propylsulfanylmethyl) hexamethylenes of 1,3-, bis- [4- (β-epithio rosickyite base) cyclohexyl] methane, 2,2-
Bis- [4- (β-epithio rosickyite base) cyclohexyl] propane, bis- [4- (β-epithio rosickyite base) cyclohexyl] thioethers, the bis- (β-epithios third of 2,5-
Sulfenyl) epithio with alicyclic ring such as -1,4- dithiane, bis- (β-epithio rosickyite base the Ethylsulfanylmethyl) -1,4- dithiane of 2,5-
Close object；Bis- (β-epithio rosickyite base) benzene of 1,3-, bis- (β-epithio propylsulfanylmethyl) benzene of 1,3-, bis- [4- (β-epithio rosickyite base) benzene
Base] methane, bis- [4- (β-epithio rosickyite base) phenyl] propane of 2,2-, bis- [4- (β-epithio rosickyite base) phenyl] thioethers, bis- [4-
(β-epithio rosickyite base) phenyl] episulfide compounds with aromatic ring such as sulfonium compound, bis- (β-epithio rosickyite base) biphenyl of 4,4-；2-
Bis- [(2- β-epithio rosickyite base ethyl) sulphur of bis- (β-epithio rosickyite base) propane of (2- β-epithio rosickyite base ethylmercapto group) -1,3-, 1,2-
Base] -3- (β-epithio rosickyite base) propane, four (β-epithio propylsulfanylmethyl) methane, 1,1,1- tri- (β-epithio propylsulfanylmethyl)
The alkyl thioethers type ring sulphur compound such as propane；Bis- { 4- [2- (the 2,3- epithios propoxyl group) ethyoxyl] phenyl } fluorenes of 9,9-, 9,9- are bis-
{ 4- [2- (2,3- epithios propoxyl group) ethyoxyl] -3- aminomethyl phenyls } fluorenes, bis- { 4- [2- (the 2,3- epithios propoxyl group) ethoxies of 9,9-
Base] -3,5- 3,5-dimethylphenyls fluorenes, bis- { 4- [2- (2,3- epithios propoxyl group) the ethyoxyl] -3- phenyls } fluorenes of 9,9-, 9,9-
Bis- { 6- [2- (2,3- epithios propoxyl group) ethyoxyl] -2- naphthalenes } fluorenes, bis- { 5- [2- (the 2,3- epithios propoxyl group) ethoxies of 9,9-
Base] -1- naphthalenes } episulfide compounds etc. with fluorene skeleton such as fluorenes.
As compound (hereinafter also referred to " the vinyl ethers chemical combination with 2 or more above-mentioned vinyl ether groups in 1 molecule
Object "), it can be mentioned, for example：The ring-type ether type vinyl ethers such as isobide divinyl ether, hydroxy norbomene divinyl ether
Close object (oxirane ring, oxetanes ring, tetrahydrofuran ring etc. have the vinyl ether compound of cyclic ether group)；Quinhydrones
The aryl divinyl ether compounds such as divinyl ether；1,4- butanediol divinyl ethers etc. have the vinyl ethers of chain alkyl
Compound；The chains ether type vinyl ether compound such as triethyleneglycol divinylether；Hexamethylene divinyl ether, hexamethylene diformazan
Alcohol divinyl ether etc. has the vinyl ether compound of cyclic hydrocarbon group.
Ingredient (A) can be used alone, or two or more is applied in combination.In the composition for sealing of the present invention
Including cation-curable total amount of compound (100 weight %) in, the ratio shared by ingredient (A) is, for example, 30~80 weight %
Left and right, preferably 40~60 weight %.When containing ingredient (A) with above range, it can inhibit during wishing solidification delay
Cured progress, and rapidly solidification can be realized after implementing heat treatment, it is preferred in this regard.Ingredient
(A) when content is less than above range, exists and be difficult to obtain the tendency of sufficient curing rate implementing heat treatment.Separately
On the one hand, when the content of ingredient (A) is more than above range, there is the tendency for being difficult to obtain sufficient solidification delay effect.
(ingredient (B))
The ingredient (B) of the present invention is to generate cation kind, by illumination to cause cation-curable compound
The light cationic polymerization initiator of curing reaction.Light cationic polymerization initiator is comprising light absorbing cation portion and as acid
The anion portion of occurring source.
As the present invention light cationic polymerization initiator, it can be mentioned, for example：DiazoniumSalt compounds, iodineSalt
Compound, sulfonium salt compounds,Salt compounds, selenium salt compounds, oxygenSalt compounds, ammonium salt compounds, bromine
Salt compounds etc..Wherein, from can be formed from the aspect of excellent curability solidfied material, it is preferable to use sulfonium salt class chemical combination
Object.
As the cationic portion of sulfonium salt compounds, it can be mentioned, for example：Triphenylsulfonium ion, diphenyl [4- (thiophenyl)
Phenyl] the aryl sulfonium cation (in particular, triaryl matte ion) such as sulfonium cation, tri-p-tolylsulfonium ion.
As the anion portion of light cationic polymerization initiator, it can be mentioned, for example：BF4 -、B(C6F5)4 -、PF6 -、[(Rf)nPF6-n]-(Rf：Alkyl, n made of 80% or more of hydrogen atom is replaced by fluorine atoms：1~5 integer), AsF6 -、SbF6 -、
SbF5OH-Deng.
As the present invention light cationic polymerization initiator, it can be mentioned, for example：4- (4- xenyls sulfenyl) phenyl -4- biphenyl
Base phenyl sulfonium four (pentafluorophenyl group) borate, 4- (4- xenyls sulfenyl) phenyl -4- xenyl phenyl sulfoniums hexafluoro antimonate, hexichol
Base [4- (phenylsulfartyl) phenyl] sulfonium four (pentafluorophenyl group) borate, diphenyl [4- (phenylsulfartyl) phenyl] sulfonium hexafluorophosphoric acid
Salt, three fluorophosphate of diphenyl [4- (phenylsulfartyl) phenyl] sulfonium three (pentafluoroethyl group), 4- (4- xenyls sulfenyl) phenyl -4- connection
Three fluorophosphate of phenyl sulfonium three (pentafluoroethyl group), trade name " CYRACURE UVI-6970 ", " CYRACURE UVI-
6974 ", " CYRACURE UVI-6990 ", " CYRACURE UVI-950 " (above by U.S. combinating carbide corporation),
" IRGACURE 250 ", " IRGACURE 261 ", " IRGACURE 264 " (above by BASF AG's system), " Optomer SP-
150 ", " Optomer SP-151 ", " Optomer SP-170 ", " Optomer SP-171 " (above by (strain) ADEKA systems),
" CG-24-61 " (Ciba Japan corporations), " DAICAT II " ((strain) Daicel systems), " UVAC1590 ", " UVAC1591 "
(above by Daicel-Cytec (strain) make), " CI-2064 ", " CI-2639 ", " CI-2624 ", " CI-2481 ", " CI-2734 ",
" CI-2855 ", " CI-2823 ", " CI-2758 ", " CIT-1682 " (being made above up to (strain) by Japanese Cao), " PI-2074 "
(Rhodia corporations, four (pentafluorophenylboronic acid salt) tolyl cumenyl iodineSalt), " FFC509 " (3M corporations),
“BBI-102”、“BBI-101”、“BBI-103”、“MPI-103”、“TPS-103”、“MDS-103”、“DTS-103”、“NAT-
103 ", " NDS-103 " (being made above by Midori Kagaku (strain)), " CD-1010 ", " CD-1011 ", " CD-1012 "
(Sartomer America corporations), " CPI-100P ", " CPI-101A " (being made above by SAN-APRO (strain)) etc..These can
To be used alone a kind, or two or more is applied in combination.
The cation-curable compound that composition for sealing relative to the present invention includes is (containing situation of more than two kinds
Under, it is its total amount) 100 parts by weight, the usage amount (use level) of ingredient (B) is, for example, 0.05~4 parts by weight or so, preferably
0.2~2 parts by weight.
(ingredient (C))
Contain glycoluril compounds as ingredient (C) in the composition for sealing of the present invention.Glycoluril compounds are relative to by light
The cation that cationic polymerization initiators generate shows alkalescent, therefore has capture due to implementing illumination by light cationic polymerization
The effect for the cation that initiator generates can inhibit cured progress after illumination until implementing the until of heating.That is, hair
Shoot solidification delay effect.Also, with by implementing to discharge captured cation, by heat treatment to make after illumination
The effect that the solidification of composition for sealing carries out.Thereby, it is possible to cured to control by adjusting the opportunity heated is implemented
Start, so as to prevent because fitting operation it is slow due to cause fitting become difficult the case where generation.Glycoluril compounds can
To be used alone a kind, or two or more is applied in combination.
As the glycoluril compounds in the present invention, it can be mentioned, for example：Following formula (c) compound represented.
[chemical formula 4]
In above-mentioned formula (c), Ra、Rb、Rc、RdIt is identical or different, indicate hydrogen atom, alkyl, hetero ring type group and by being selected from
2 or more groups in alkyl and hetero ring type group are via group made of singly-bound or connection group bonding.
As above-mentioned connection group, it can be mentioned, for example：Epoxy has occurred in some or all of bivalent hydrocarbon radical, carbon-to-carbon double bond
The alkenylene of change, carbonyl, ehter bond, ester bond, carbonate group, amide groups and by multiple groups to link in these groups
Deng.
Above-mentioned alkyl includes：Aliphatic alkyl, alicyclic type hydrocarbon and aromatic hydrocarbyl and by these groups via list
Group made of key bonding.
As above-mentioned aliphatic alkyl, preferably C1-20Aliphatic alkyl, it can be mentioned, for example：C1-20(preferably C1-10, it is special
It You Xuanwei not C1-3) left and right alkyl；The C such as vinyl, allyl2-20(preferably C2-10, particularly preferably C2-3) left and right alkene
Base；C2-20(preferably C2-10, particularly preferably C2-3) left and right alkynyl etc..
As above-mentioned alicyclic type hydrocarbon, preferably C3-20Alicyclic type hydrocarbon, it can be mentioned, for example：The C such as cyclopenta, cyclohexyl3-20
(preferably C3-15, particularly preferably C5-8) left and right naphthenic base；The C such as cyclopentenyl, cyclohexenyl group3-20(preferably C3-15, especially
Preferably C5-8) left and right cycloalkenyl group；Endocyclics alkyl such as norborny etc..
As above-mentioned aromatic hydrocarbyl, preferably C6-14(especially C6-10) aromatic hydrocarbyl, it can be mentioned, for example phenyl etc..
The heterocycle for constituting above-mentioned hetero ring type group includes aromatic series heterocycle and non-aromatic heterocycle.As such miscellaneous
Ring, can enumerate the atom for constituting ring has carbon atom and at least one kind of hetero atom (for example, oxygen atom, sulphur atom, nitrogen-atoms etc.)
3~10 membered rings (preferably 3~6 membered rings) and their fused rings.It is specific enumerable：Including oxygen atom is as heteroatomic miscellaneous
Ring (for example, oxirane ring, oxetanes ring, furan nucleus, morpholine ring etc.), comprising sulphur atom as heteroatomic heterocycle
(for example, thiphene ring, thiazole ring etc.), comprising nitrogen-atoms as heteroatomic heterocycle (for example, pyrrole ring, pyrrolidine ring, pyrazoles
Ring, imidazole ring, triazole ring, isocyanide urea ring, pyridine ring, pyridazine ring, pyrimidine ring, pyridine ring, piperidine ring, piperazine ring etc., indole ring,
Indole ring, quinoline ring, acridine ring, naphthyridines ring, quinazoline ring, purine ring etc.) etc..Hetero ring type group is the knot from above-mentioned heterocycle
Group made of 1 hydrogen atom is removed in structure formula.
As group made of above-mentioned 2 or more the group bondings by alkyl and hetero ring type group, example can be enumerated
Such as glycidyl.
Above-mentioned alkyl, hetero ring type group and the group made of 2 or more the group bondings in them can also have
Having various substituent groups, [halogen atom, oxo base, hydroxyl, substituted oxy are (for example, C1-4Alkoxy, C6-10Aryloxy group, C7-16Aralkyl oxygen
Base, C1-4Acyloxy etc.), carboxyl, substituted oxy carbonyl is (for example, C1-4Alkoxy carbonyl, C6-10Aryloxycarbonyl, C7-16Aralkyl oxygen
Base carbonyl etc.), substituted or unsubstituted carbamoyl is (for example, carbamoyl, C1-4Alkyl-substituted amino formoxyl, C6-10Virtue
Base substituted-amino formoxyl), cyano, nitro, sulfo group, sulfydryl etc.].In addition, alicyclic type hydrocarbon, aromatic hydrocarbyl ring on
It can be with fused aromatic or the heterocycle of non-aromatic.
As above-mentioned Ra、Rb、Rc、Rd, wherein preferably hydrogen atom or containing with cation-curable group have react
The group of the group (hereinafter also referred to " reactive group ") of property.Above-mentioned cation-curable group includes：Fat in ingredient (A)
Other epoxies in ring epoxy group, the group containing oxetanes ring, epithio base, vinyl ether group and aftermentioned ingredient (D)
Base, vinyl, allyl.In the present invention, particularly preferably above-mentioned Ra、Rb、Rc、RdIn 2 or more (especially 4) be containing
There is the group (especially glycidyl or allyl) of reactive group.
As the glycoluril compounds in the present invention, wherein the preferably glycoluril with glycidyl and/or allyl
Close object, the R in particularly preferred formula (c)a、Rb、Rc、RdIn 2 or more (especially 4) be glycidyl and/or allyl
Multifunctional glycoluril compounds.
As glycoluril compounds, for example, with glycidyl glycoluril compounds can by make epoxychloropropane with it is sweet
Urea is reacted and is manufactured.In the present invention, (work can also be melted by four countries above using such as trade name " TA-G ", " TG-G "
Industry (strain) make) etc. commercially available products.
Include in composition for sealing relative to the present invention ingredient (B) (containing in the case of two or more for it always
Amount) 1 parts by weight, the usage amount (use level) of ingredient (C) is, for example, 0.05~3 parts by weight, and the upper limit is preferably 2.5 parts by weight, spy
It You Xuanwei not 2.0 parts by weight, most preferably 1.5 parts by weight.Lower limit be preferably 0.1 parts by weight, particularly preferably 0.3 parts by weight,
Most preferably 0.5 parts by weight, especially preferably 0.8 parts by weight.From sufficient solidification delay effect aspect can be obtained,
It is preferred that containing ingredient (C) with above range.When the content of ingredient (C) is less than above range, exists and be difficult to obtain sufficient solidification
The tendency of carryover effects.On the other hand, when the content of ingredient (C) is more than above range, it is difficult implementing to heat to exist
To obtain the tendency of sufficient curing rate, it some times happens that solidification is bad.
(ingredient (D))
The composition for sealing of the present invention can also include the one kind or two or more cation in addition to mentioned component (A)
Curability compound is as ingredient (D).
As the cation-curable compound in addition to mentioned component (A), it can be mentioned, for example：In addition to ingredient (A)
Compound (hereinafter also referred to " other epoxides ") with epoxy group, the compound with vinyl, with allyl
Compound etc..
Above-mentioned other epoxides include：Directly there are compound, the glycidol of epoxy group on alicyclic ring with singly bound
Base ether type epoxy compound, glycidyl esters epoxide, glycidyl amine epoxide etc..
As the compound for directly having epoxy group on above-mentioned alicyclic ring with singly bound, it can be mentioned, for example：Bis- (the hydroxyl first of 2,2-
Base)-n-butyl alcohol 1,2- epoxies -4- (2- epoxy ethyls) hexamethylene addition product (trade name " EHPE3150 ", (strain) Daicel
System) etc..
As above-mentioned glycidyl ethers epoxide, it can be mentioned, for example：1,6-HD-diglycidyl
Aliphatic obtained from ether, trimethylolpropane-triglycidyl group ether etc. makes epoxychloropropane be reacted with aliphatic polyol
Glycidyl ethers epoxide；Bisphenol A type epoxy compound, bisphenol F type epoxy compound, bisphenol E-type epoxy compound
Object, o-phenyl phenol glycidyl ether, biphenyl phenolic epoxide, phenol novolak-type epoxy compound, cresols phenol
Novolac type ring oxygen compound, the cresol novolak type epoxy compound of bisphenol-A, naphthalene type ring oxygen compound, triphenol methane type
The aromatic glycidyls ether type epoxy compound such as epoxide；Hydrogenated bisphenol A type epoxide (2,2- it is bis- [4- (2,
3- glycidoxies) cyclohexyl] propane, bis- [3,5- dimethyl -4- (2,3- glycidoxies) cyclohexyl] propane of 2,2- and it
The bisphenol A type epoxy compounds such as polymer it is hydrogenated made of compound), A Hydrogenated Bisphenol A F type rings oxygen compound (it is bis- [it is adjacent,
O- (2,3- glycidoxies) cyclohexyl] methane, bis- [adjacent, p- (2,3- glycidoxies) cyclohexyl] methane, it is bis- [it is right, it is p-
(2,3- glycidoxies) cyclohexyl] methane, bis- [3,5- dimethyl -4- (2,3- glycidoxies) cyclohexyl] methane and it
Polymer etc.), hydrogenated biphenyl phenolic epoxide, hydrogenation phenol novolak-type epoxy compound, hydrogenation cresols phenol
Novolac type ring oxygen compound, the hydrogenation cresol novolak type epoxy compound of bisphenol-A, hydrogenated naphthalene type ring oxygen compound, hydrogen
Ester ring type contracts obtained from the aromatic glycidyls ether type epoxy compounds such as change triphenol methane type epoxy compound are hydrogenated
Water glyceryl ether type epoxy compound etc..It is, for example, possible to use trade name " YL-983U " (Mitsubishi Chemical's (strain) system), " R1710 "
The commercially available products such as (Printec (strain) systems), " SY-OPG ", " PEG " (above by slope this pharmaceutical industries (strain) system).
As the above-mentioned compound with vinyl, it can be mentioned, for example：Styrene, p-methylstyrene, ethyl styrene,
The styrene compounds such as propylstyrene, isopropyl styrene, p-tert-butylstyrene；N- vinyl carbazoles, N- vinyl
Nitrogen vinyl compound such as pyrrolidones etc..
As the above-mentioned compound with allyl, it can be mentioned, for example：(methyl) allyl acrylate, Malaysia diene acid third
Ester, triallyl cyanurate, diallyl phthalate etc..
In the present invention, wherein from the viewpoint of curing rate at room temperature is slow, (especially using other epoxides
There is the compound of 1 or more glycidyl ether, having 1 or more in most preferably 1 molecule shrinks in preferably 1 molecule
Glyceryl ether and the compound for not having ester bond and polyether structure；It is contained in except the compound in ingredient (A)) when, it can be with
Obtain makes solidification delay become more stable effect while inhibiting the generation of exhaust, therefore preferably.
Ingredient in the cation-curable total amount of compound (100 weight %) for including in the composition for sealing of the present invention
(D) ratio shared by is, for example, 20~70 weight % or so, and the upper limit is preferably 65 weight %, particularly preferably 60 weight %.Under
Limit is preferably 30 weight %, particularly preferably 40 weight %, is most preferably 50 weight %.From solidification delay can be made to become steady
From the perspective of fixed, ingredient (D) is preferably contained with above range.
In addition, in the cation-curable total amount of compound (100 weight %) for including in the composition for sealing of the present invention
Ingredient (A) and ingredient (D) (compound with 1 or more glycidyl ether in particularly preferably 1 molecule, most preferably 1
Compound in molecule with 1 or more glycidyl ether and without ester bond and polyether structure) total amount shared by
Ratio is, for example, 50 weight % or more, preferably 70 weight % or more, particularly preferably 80 weight % or more, is most preferably 90 weights
Measure % or more.It should be noted that the upper limit is 100 weight %.
(additive)
In the composition for sealing of the present invention other than mentioned component, one or two can also be contained as needed
The above additive.As above-mentioned additive, it can be mentioned, for example：It is conductive material, inorganic filling material, polymerization inhibitor, silane coupled
It is agent, antioxidant, light stabilizer, plasticizer, levelling agent, antifoaming agent, solvent, ultra-violet absorber, ionic adsorption body, pigment, glimmering
Body of light, releasing agent etc..
For the composition for sealing of the present invention, in the case where requiring higher moisture resistance, inorganic fill out is preferably comprised
Fill material.As above-mentioned inorganic filling material, it can be mentioned, for example：The inorganic oxygen such as silica, aluminium oxide, zinc oxide, magnesia
Compound；The carbonate such as calcium carbonate, magnesium carbonate；Silicates such as calcium silicates, bead, talcum, clay, mica etc..
The shape of inorganic filling material is not particularly limited, it can be mentioned, for example：Spherical (just spherical, close just spherical, ellipsoid
Deng), polyhedral, rodlike (cylindric, prism-shaped etc.), tabular, flakey, irregular shape etc..Wherein, from can assign
, it is preferable to use flat inorganic filling material from the perspective of superior moisture resistance.
In the present invention, wherein coating pressure when from due to relative to distribution has linear response therefore coating
, it is preferable to use the silicates such as talcum, mica from the perspective of excellent.
The average grain diameter (being based on laser diffraction/scattering method (micro- tracing)) of inorganic filling material is, for example, 0.001~30 μ
M, it is preferably 0.1~10 μm.
As the additive amount of above-mentioned inorganic filling material, relative to the cation-curable for including in composition for sealing
Close 100 parts by weight of object, for example, 10~60 parts by weight or so, preferably 20~45 parts by weight.By the nothing for adding above range
Machine packing material can further increase moisture resistance.When the content of inorganic filling material is higher than above range, existing leads to viscosity
Become the tendency of excessively high coating reduction.
It is required that in the case that sealing material is conductive, electric conductivity material is preferably comprised in composition for sealing of the invention
Material preferably comprises following conducting fibres in particular, from the viewpoint of the sealing material for obtaining having both electric conductivity and the transparency
Coating particles.
(conducting fibre coating particles)
Conducting fibre coating particles are comprising particle-like substance and to coat the fibrous electric conductivity object of the particle-like substance
The conducting fibre coating particles of matter (in this specification, also referred to as " conducting fibre ").It should be noted that in electric conductivity fibre
It ties up in coating particles, " conducting fibre coating particles shape substance " refers to, conducting fibre covers the surface of particle-like substance
All or part of state.In conducting fibre coating particles, at least the one of the surface of conducting fibre coating particles shape substance
Part, for example, uncoated part can also more exist than the part coated.In addition, particle-like substance with lead
Conductive fiber also will not necessarily contact, in general, a part for conducting fibre is contacted with the surface of particle-like substance.
Fig. 1 is an example of the scanning electron microscope image of the conducting fibre coating particles in the present invention.Such as Fig. 1 institutes
Show, the conducting fibre coating particles in the present invention have at least part of particle-like substance (the spherical substance in Fig. 1)
The composition coated by conducting fibre (substance of the threadiness in Fig. 1).
(particle-like substance)
The particle-like substance for constituting the conducting fibre coating particles in the present invention is the structure of particle shape.
The material (raw material) of above-mentioned particle-like substance is not particularly limited, it can be mentioned, for example：Metal, plastics, rubber, pottery
Known in porcelain, glass, silica etc. or usual material.In the present invention, it is preferred to use transparent plastic therein, glass, two
The transparent material such as silica particularly preferably uses transparent plastic.
Above-mentioned transparent plastic includes thermosetting resin and thermoplastic resin etc..As above-mentioned thermosetting resin, example can be enumerated
Such as：Poly- (methyl) acrylate；Polystyrene resin；Polycarbonate resin；Polyester resin；Polyurethane resin；Asphalt mixtures modified by epoxy resin
Fat；Polysulfone resin；Amorphous polyolefins resin；By divinylbenzene, hexatriene, divinyl ether, divinylsulfone, two allyls
Base methanol, alkylidene two (methyl) acrylate, oligomeric or polyalkylene glycol two (methyl) acrylate, three (first of alkylidene
Base) acrylate, alkylidene four (methyl) acrylate, bis- (methyl) acrylamides of alkylidene, two terminal acrylic acid be modified it is poly-
The multi-functional monomer such as butadiene oligomer be polymerized alone or with network polymers obtained from other monomer polymerizations；Phenolic aldehyde tree
Fat, melamine resin, benzoguanamin formaldehyde resin, Lauxite etc..As above-mentioned thermoplastic resin, example can be enumerated
Such as：Ethylene/vinyl acetate, Ethylene/vinyl acetate/copolymers of unsaturated carboxylic acids, ethylene/ethyl acrylate copolymerization
Object, ethylene/methacrylic acid methyl terpolymer, ethylene/(methyl) acrylic copolymer, ethylene/copolymer-maleic anhydride, second
Alkene/amino alkyl methacrylate copolymer, ethylene/vinyl base silane copolymer, ethylene/methacrylic acid ethylene oxidic ester
Copolymer, ethylene/methacrylic acid hydroxy methacrylate copolymer, (methyl) methyl acrylate/styrol copolymer, acrylonitrile/benzene
Ethylene copolymer etc..
The shape of above-mentioned particle-like substance is not particularly limited, it can be mentioned, for example：Spherical (just spherical, close just spherical, ellipsoid
Shape etc.), polyhedral, rodlike (cylindric, prism-shaped etc.), tabular, flakey, irregular shape etc..In the present invention,
In from can manufacture conducting fibre coating particles with high productivity, be easy to be uniformly dispersed in the composition for sealing of the present invention
In, be easy from the perspective of integrally assigning electric conductivity for solidfied material, it is preferably spherical.
The average aspect ratio of above-mentioned particle-like substance is not particularly limited, but preferably shorter than 20 (for example, 1 less than
20), particularly preferably 1~10.When average aspect ratio is higher than above range, it is difficult to sometimes by coordinating a small amount of conducting fibre
Coating particles and make the present invention composition for sealing show excellent electric conductivity.It should be noted that above-mentioned particle shape object
The average aspect ratio of matter (can be, for example, for example 100 or more, excellent to sufficient amount by using electron microscope (SEM, TEM)
It is selected as 300 or more；Especially 100,300) particle-like substance shooting electron microscope image, calculate these particle shapes
The aspect ratio of substance simultaneously carries out arithmetic average and measures.
In addition, above-mentioned particle-like substance is constructed without particular determination, it can be the composition of single layer, can also be multilayer
The composition of (plural layer).In addition, above-mentioned particle-like substance can be any in solid particle, hollow-particle, porous granule etc.
Particle.
The average grain diameter of above-mentioned particle-like substance is not particularly limited, but preferably 0.1~100 μm, particularly preferably 1~
50 μm, most preferably 5~30 μm.When average grain diameter is less than above range, a small amount of conducting fibre is only coordinated to coat grain sometimes
Son is difficult to that it is made to show excellent electric conductivity.When average grain diameter is higher than above range, average grain diameter is more than organic EL element
There is the tendency for the film for being difficult to be formed homogeneous thickness in the thickness of sealant.It should be noted that above-mentioned particle-like substance is flat
Equal grain size is the median particle diameter (d50) using laser diffraction/scattering method.
It is preferred that above-mentioned particle-like substance is transparent.Specifically, above-mentioned particle-like substance is in visible wavelength range
Total light penetration be not particularly limited, but preferably 70% or more, particularly preferably 80% or more.Total light penetration is low
When above range, the transparency of solidfied material (including conducting fibre coating particles) may be caused to reduce.
It should be noted that total light penetration of the above-mentioned particle-like substance in visible wavelength range can be by such as
It is measured and finds out lowerly：Make the monomer of the raw material as the particle-like substance between glass, in 80~150 DEG C of temperature model
Crowd around conjunction, obtains the tablet of thick 1mm, it is saturating to measure total light of the tablet in visible wavelength range based on JIS K7361-1
Cross rate.In addition, similarly measure be only glass total light penetration, and obtained value is set as blank value (total light is saturating
Cross rate 100%).
Additionally, it is preferred that above-mentioned particle-like substance has flexibility, 10% compressive strength of each particle is, for example, 10kgf/mm2
Below, it is preferably 5kgf/mm2Below, it is particularly preferably 3kgf/mm2Below.For comprising 10% compressive strength in above range
Particle-like substance conducting fibre coating particles, it can be made to follow fine concaveconvex structure and occur by being pressurizeed
Deformation.Therefore, by containing the conducting fibre coating particles the present invention composition for sealing be cured as having it is fine recessed
In the case of the shape of male structure, the particle-like substance can be made to spread all over to discreet portions, so as to prevent electric conductivity undesirable
Partial generation.
The refractive index of above-mentioned particle-like substance is not particularly limited, but preferably 1.4~2.7, particularly preferably 1.5~
1.8.It should be noted that in the case where the particle-like substance is plastic pellet, the refractive index of above-mentioned particle-like substance can be with
It finds out as follows：The monomer of the raw material as particle-like substance is set to polymerize between glass, in 80~150 DEG C of temperature ranges, system
Make in the state of making prism closely sealed with the test film using single bromonaphthalene as intermediate fluid at the test film of vertical 20mm × horizontal 6mm
With the refractive index under 25 DEG C of multi-wavelength Abbe refractometer (trade name " DR-M2 ", (strain) Atago systems) measurement, sodium D-line.
In addition, for above-mentioned particle-like substance, preferably it (it is fine not include electric conductivity with the composition for sealing of the present invention
Tie up coating particles) solidfied material refractive index (25 DEG C, wavelength 589.3nm under) difference it is small, preferably comprise conducting fibre cladding
The folding of the particle-like substance of particle and the solidfied material of the composition for sealing (not including conducting fibre coating particles) of the present invention
The absolute value of the difference for penetrating rate is such as 0.1 or less (preferably 0.05 or less, particularly preferably 0.02 or less).
That is, it is preferred that under the conducting fibre coating particles satisfaction for including in the organic EL element composition for sealing of the present invention
Formula.
| the refractive index of particle-like substance-organic EL element composition for sealing (does not include conducting fibre coating particles)
Solidfied material refractive index |≤0.1
(do not included by the particle-like substance and the composition for sealing of the present invention that make composition conducting fibre coating particles
Conducting fibre coating particles) solidfied material specific refractivity in above range, can obtain that the transparency is excellent, for mist degree
As 10% or less (preferably 6% or less, further preferably 3% or less), total light penetration (are preferably for 90% or more
93% or more) solidfied material.It should be noted that the mist degree of solidfied material can be measured based on JIS K7136.In addition, solidification
Total light penetration (thickness of the object in visible wavelength range:10 μm, wavelength:JIS K7361-1 450nm) can be based on to carry out
It measures.
Further, from the viewpoint of it can assign excellent electric conductivity with less usage amount, the structure preferably in the present invention
There is sharp size distribution (deviation of=grain size is few), preferably its variation at the particle-like substance of conducting fibre coating particles
Coefficient (CV values) is 50% or less.It should be noted that the coefficient of variation is obtained with standard deviation divided by average grain diameter
Value, be as particle size homogeneity finger target value.
Above-mentioned particle-like substance can be manufactured using known or customary way, and manufacturing method is not particularly limited.Example
Such as, it for for the metallic the case where, is reacted using vapor phase methods such as CVD method, spray heating decompositions, based on chemical reduction
Damp process etc. manufactured.In addition, for for the plastic pellet the case where, such as using passing through suspension polymerization, lotion
Polymerization well known to polymerization, seeded polymerization, dispersion copolymerization method etc. makes the list of foregoing illustrative composition resin (polymer)
The method etc. of body polymerization is manufactured.
Commercially available product can also be used in the present invention.As the particle-like substance formed by thermosetting resin, can be used for example：
Trade name " Techpolymer MBX series ", " Techpolymer BMX series ", " Techpolymer ABX series ",
" Techpolymer ARX series ", " Techpolymer AFX series " (being made above by ponding finished industrial (strain)), commodity
Name " Micro-pearl SP ", " Micro-pearl SI " (being made above by ponding chemical industry (strain))；As by thermoplastic resin
The particle-like substance that fat is formed can be used for example：Trade name " Softbeads " (Sumitomo refine (strain) system), trade name
" DUOMASTER " (ponding finished industrial (strain) system) etc..
(fibrous conductive material (conducting fibre))
The conducting fibre for constituting conducting fibre coating particles is structure (the threadiness knot of conductive threadiness
Structure body).The shape of above-mentioned conducting fibre is fibrous (filiform), is not particularly limited, but its average aspect ratio is for example
It is 10 or more, preferably 20~5000, particularly preferably 50~3000, most preferably 100~1000.Average aspect ratio is less than upper
When stating range, a small amount of conducting fibre coating particles is only coordinated to be difficult to that it is made to show excellent electric conductivity sometimes.It is above-mentioned to lead
The available method same as the average aspect ratio of particle-like substance of average aspect ratio of conductive fiber is found out.It needs to illustrate
It is that the concept of " threadiness " in above-mentioned conducting fibre also includes the shape of the various linear structure bodies such as " threadiness ", " rodlike ".
In addition, being also that 1000nm fibers below are known as " nano wire " by average boldness in the present specification.
The average boldness (average diameter) of above-mentioned conducting fibre is not particularly limited, but preferably 1~400nm, especially
Preferably 10~200nm, it is most preferably 50~150nm.When average boldness is less than above range, easily occur between conducting fibre
Cohesion, may cause the manufacture of conducting fibre coating particles to become difficult.On the other hand, average boldness is higher than above range
When, the cladding of particle-like substance becomes difficult, and can not effectively manufacture conducting fibre coating particles sometimes.Above-mentioned electric conductivity is fine
The average boldness of dimension can measure as follows：Using electron microscope (SEM, TEM), for sufficient amount (for example, 100 with
Above, preferably 300 or more；Especially 100,300) conducting fibre shoot electron microscope image, and measure this
The rugosity (diameter) of a little conducting fibres, finds out their arithmetic average.
The average length of above-mentioned conducting fibre is not particularly limited, but preferably 1~100 μm, particularly preferably 5~80
μm, be most preferably 10~50 μm.When average length is less than above range, the cladding of particle-like substance becomes difficult, and possibly can not
Effectively manufacture conducting fibre coating particles.On the other hand, when average length is higher than above range, conducting fibre is to each other
It is easy to happen winding.The average length of above-mentioned conducting fibre can measure as follows：Using electron microscope (SEM, TEM),
For sufficient amount (for example, 100 or more, preferably 300 or more；Especially 100,300) conducting fibre clap
Electron microscope image is taken the photograph, and measures the length of these conducting fibres, finds out their arithmetic average.It should be noted that
It for the length of conducting fibre, should be measured with extending to linear state, but actually its bending that mostly occurs,
Therefore, using image analysis apparatus, diameter projected and the projected area of conducting fibre are calculated according to electron microscope image,
And it is assumed to cylinder, its length is calculated by following formula.
Length=projected area/diameter projected
The material (raw material) for constituting above-mentioned conducting fibre is conductive material, it can be mentioned, for example：Gold
Category, semiconductor, carbon material, electroconductive polymer etc..
As above-mentioned metal, it can be mentioned, for example：It is known in gold, silver, copper, iron, nickel, cobalt, tin and their alloy etc. or usual
Metal.In the present invention, from the aspect of excellent electric conductivity, wherein it is preferred that silver.
As above-mentioned semiconductor, it can be mentioned, for example：Known in cadmium sulfide, cadmium selenide etc. or usual semiconductor.
As above-mentioned carbon material, it can be mentioned, for example：Known in carbon fiber, carbon nanotube etc. or usual carbon material.
It is upper to be used as above-mentioned electroconductive polymer, it can be mentioned, for example：Polyacetylene, gathers to benzene, p-phenylene vinylene polyacene
(polyparaphenylene vinylene), polypyrrole, polyaniline, polythiophene and their derivative are (for example, common
Polymer backbone on the electroconductive polymer with the substituent groups such as alkyl, hydroxyl, carboxyl, ethylenedioxy；It is specific enumerable
Poly- Ethylenedioxy Thiophene etc.) etc..In the present invention, polyacetylene preferably among the above, Polyaniline and its derivative, polypyrrole and its
Derivative, polythiophene and its derivative.It should be noted that above-mentioned electroconductive polymer can also include known or usual mixes
Miscellaneous dose (for example, the receptors such as halogen, halide, lewis acid；Donors such as alkali metal, alkaline-earth metal etc.).
As the conducting fibre of the present invention, preferably conductive nanometer line, particularly preferably it is selected from metal nanometer line, partly leads
At least one of body nano wire, carbon fiber, carbon nanotube and electroconductive polymer nano wire conductive nanometer line, especially from
From the aspect of excellent electric conductivity, most preferably nano silver wire.
Above-mentioned conducting fibre can be manufactured by known or usual manufacturing method.For example, above-mentioned metal nanometer line can lead to
Liquid phase method, vapor phase method etc. is crossed to be manufactured.More specifically, nano silver wire can for example, by Mater.Chem.Phys.2009,
114,333-338, Adv.Mater.2002,14, P833-837, Chem.Mater.2002,14, P4736-4745, Japanese Unexamined Patent Application Publication
Method described in 2009-505358 bulletins manufactures.In addition, nanowires of gold can be for example, by Japanese Unexamined Patent Publication 2006-
Method described in No. 233252 bulletins manufactures.In addition, copper nano-wire can be for example, by Japanese Unexamined Patent Publication 2002-266007 public affairs
Method described in report manufactures.In addition, cobalt nanowire can be for example, by described in Japanese Unexamined Patent Publication 2004-149871 bulletins
Method manufactures.In addition, semiconductor nanowires can come for example, by the method described in Japanese Unexamined Patent Publication 2010-208925 bulletins
Manufacture.Above-mentioned carbon fiber can be manufactured for example, by the method described in Japanese Unexamined Patent Publication 06-081223 bulletins.Above-mentioned carbon is received
Mitron can be manufactured for example, by the method described in Japanese Unexamined Patent Publication 06-157016 bulletins.Above-mentioned electroconductive polymer is received
Rice noodles can be for example, by the method described in Japanese Unexamined Patent Publication 2006-241334 bulletins, Japanese Unexamined Patent Publication 2010-76044 bulletins
To manufacture.As above-mentioned conducting fibre, commercially available product can also be used.
Conducting fibre coating particles in the present invention can by by above-mentioned particle-like substance and conducting fibre in solvent
It is middle to mix to manufacture.As the manufacturing method of conducting fibre coating particles, the method etc. of specific enumerable following (1)~(4).
(1) above-mentioned particle-like substance will be made to be scattered in dispersion liquid made of solvent (being known as " particle dispersion ") and make above-mentioned
Conducting fibre is scattered in dispersion liquid made of solvent and (is known as " fiber dispersion ") mixing, and removes solvent as needed, from
And obtain the conducting fibre coating particles in the present invention (or dispersion liquid of conducting fibre coating particles).
(2) it after coordinating above-mentioned conducting fibre in above-mentioned particle dispersion and being mixed, removes as needed molten
Agent, to obtain conducting fibre coating particles (or dispersion liquid of conducting fibre coating particles).
(3) it after coordinating above-mentioned particle-like substance in above-mentioned fiber dispersion and being mixed, removes as needed molten
Agent, to obtain conducting fibre coating particles (or dispersion liquid of conducting fibre coating particles).
(4) after coordinating above-mentioned particle-like substance and above-mentioned conducting fibre in a solvent and being mixed, as needed
Solvent is removed, to obtain conducting fibre coating particles (or dispersion liquid of conducting fibre coating particles).
The solvent that uses when as conducting fibre coating particles in the manufacture present invention, it can be mentioned, for example：Water；Methanol,
The alcohol such as ethyl alcohol, propyl alcohol, isopropanol, butanol；The ketone such as acetone, methyl ethyl ketone (MEK), methyl iso-butyl ketone (MIBK) (MIBK)；Benzene, toluene, two
The aromatic hydrocarbons such as toluene, ethylbenzene；The ethers such as ether, dimethoxy-ethane, tetrahydrofuran, dioxane；Methyl acetate, acetic acid
The esters such as ethyl ester, isopropyl acetate, butyl acetate；The amides such as N,N-dimethylformamide, DMAC N,N' dimethyl acetamide；Acetonitrile, third
Nitriles such as nitrile, benzonitrile etc..These solvents can be used alone, or two or more combinations (mixed solvent is made) are made
With.In the present invention, alcohol, ketone preferably among the above.
In addition, if above-mentioned cation-curable compound (ingredient (A) etc.) is liquefied compound, can also be made
It is used for solvent.It, can be not via the process for removing solvent in the case where using the curability compound of liquid as solvent
Obtain the composition for sealing for including curability compound and conducting fibre coating particles.
The viscosity of above-mentioned solvent is not particularly limited, but is gone out from the viewpoint for effectively manufacturing conducting fibre coating particles
Hair, as the viscosity at 25 DEG C, preferably 10cP or less (for example, 0.1~10cP), particularly preferably 0.5~5cP.It needs
Bright, E types viscosimeter (trade name " VISCONIC ", (strain) Tokimec systems) for example can be used in the viscosity at 25 DEG C of solvent
It is measured (rotor:1 ° of 34 ' × R24, rotating speed:0.5rpm, measuring temperature:25℃).
For the boiling point under 1 atmospheric pressure of above-mentioned solvent, from conducting fibre coating particles can be effectively manufactured
From the perspective of, preferably 200 DEG C or less, particularly preferably 150 DEG C or less, most preferably 120 DEG C or less.
When in a solvent mixing particle-like substance and conducting fibre, relative to 100 parts by weight of solvent, above-mentioned particle shape
The content of substance is, for example, 0.1~50 parts by weight or so, preferably 1~30 parts by weight.By by the content control of particle-like substance
System can more effectively generate conducting fibre coating particles in above range.
When in a solvent mixing particle-like substance and conducting fibre, relative to 100 parts by weight of solvent, above-mentioned electric conductivity
The content of fiber is, for example, 0.1~50 parts by weight or so, preferably 1~30 parts by weight.By by the content control of conducting fibre
System can more effectively generate conducting fibre coating particles in above range.
When particle-like substance and conducting fibre being mixed in a solvent, above-mentioned particle-like substance and above-mentioned conducting fibre
Ratio be preferably that the ratio between the projected area [surface area/projected area] of the surface area and conducting fibre of particle-like substance is made to reach
To such as 100/1~100/100 or so, preferably 100/10~100/50 ratio.By controlling above-mentioned ratio in above range,
Conducting fibre coating particles can more effectively be manufactured.It should be noted that the surface area of above-mentioned particle-like substance is available
The specific surface area found out (based on JIS Z8830) by BET method is multiplied by the method for the quality (usage amount) of particle-like substance come
It finds out.In addition, for the projected area of above-mentioned conducting fibre, as set forth above, it is possible to by using electron microscope (SEM,
TEM sufficient amount) is directed to (for example, 100 or more, preferably 300 or more；Especially 100,300) electric conductivity it is fine
Dimension shooting electron microscope image, calculates the projected area of these conducting fibres using image analysis apparatus and carries out arithmetic
It is average to find out.
By removing solvent after mixing particle-like substance and conducting fibre, the present invention of solid form can be obtained
In conducting fibre coating particles.The removing of solvent is not particularly limited, for example, can be by known in heating, be evaporated under reduced pressure etc.
Or customary way is implemented.It should be noted that solvent is it is not always necessary that remove, such as it can also be directly in the present invention
The form of the dispersion liquid of conducting fibre coating particles uses.
Conducting fibre coating particles in the present invention can be as described above by by raw material (particle-like substance and conduction
Property fiber) mix manufacture in a solvent, do not need cumbersome process, therefore be advantageous in terms of manufacturing cost.As picture
It the reason of manufacture, can be speculated as using such short-cut method is mixed in a solvent in this wise：It is used as raw material
Threadiness conductive material (especially average aspect ratio be 10 or more conducting fibre) surface energy it is big, in order to reduce
Surface energy and realize stabilisation, can preferentially adhere to or be adsorbed in particle surface.
In particular, the combination as particle-like substance and conducting fibre, by using the particle shape of average grain diameter A [μm]
It more than substance and average length A × 0.5 [μm] (preferably more than A × 1.0 [μm], is particularly preferably A × 1.5 [μm] or more)
Conducting fibre can more effectively manufacture the conducting fibre coating particles in the present invention.In particular, for it is just spherical or it is close just
For the case where spherical particle-like substance, it is preferable to use particle-like substance and average length (B × 1/ of average perimeter B [μm]
6) conducting fibre of (preferably B [μm] or more) more than [μm].It should be noted that the average perimeter of above-mentioned particle-like substance
It can find out as follows：Using electron microscope (SEM, TEM), for sufficient amount (for example, 100 or more, preferably 300
More than a；Especially 100,300 etc.) particle-like substance shoot electron microscope image, measure these particle-like substances
Perimeter and carry out arithmetic average.
The ratio of the particle-like substance and conducting fibre that constitute the conducting fibre coating particles in the present invention is to make grain
The ratio between the surface area of sub- shape substance and the projected area of conducting fibre [surface area/projected area] reach such as 100/1~
When the ratio of 100/100 or so (especially 100/10~100/50), can more have while the transparency for ensuring solidfied material
Effect ground assigns electric conductivity, is preferred in this regard.It should be noted that the surface area and conduction of above-mentioned particle-like substance
Property fiber projected area respectively can utilize the above method measure.
Conducting fibre coating particles in the present invention by adding on a small quantity due to that with above-mentioned composition, can be assigned
The composition for sealing of the present invention with excellent electric conductivity (electric conductivity especially in a thickness direction), can be formed the transparency and
The solidfied material of excellent electric conductivity.
In addition, conducting fibre coating particles in the present invention there is flexibility in the case of (for example, 10% compression is strong
Degree is 3kgf/mm2In the case of below), will include that the composition for sealing of the conducting fibre coating particles is shaped to have
When having the shape of micro concavo-convex, conducting fibre coating particles can follow above-mentioned concaveconvex structure and deform to spread all over subtle
Part, therefore the generation of the undesirable part of electric conductivity can be prevented, the excellent solidfied material of electric conductivity can be formed.
Particle-like substance (conducting fibre particles coated contained in particle-like substance) in composition for sealing contains
(use level) is measured relative to 100 parts by weight of cation-curable compound, for example, 0.09~6.0 parts by weight or so.Above-mentioned grain
When the content of sub- shape substance is less than above range, according to purposes difference, the electric conductivity of gained solidfied material may be caused to become insufficient.
On the other hand, when the content of above-mentioned particle-like substance is higher than above range, there is the transparency reduction for leading to gained solidfied material
Tendency.
Total amount (100 bodies of the content of above-mentioned particle-like substance in composition for sealing relative to composition for sealing
Product %), for example, 0.02~7 volume % or so.
The content (use level) of conducting fibre in composition for sealing relative to 100 parts by weight of curability compound,
For example, 0.01~1.0 parts by weight or so.It, can according to purposes difference when the content of above-mentioned conducting fibre is less than above range
The electric conductivity of gained solidfied material can be caused to become insufficient.On the other hand, when the content of above-mentioned conducting fibre is higher than above range,
In the presence of the tendency for causing the transparency of gained solidfied material to reduce.
Total amount (100 bodies of the content of above-mentioned conducting fibre in composition for sealing relative to composition for sealing
Product %), for example, 0.01~1.1 volume %.
The composition for sealing of the present invention can be by making ingredient (A), ingredient (B), ingredient (C) and as needed
Ingredient (D), additive (for example, conducting fibre coating particles etc.) utilize rotation-revolution formula churning deaerator, homogenizing
The commonly known mixing such as device, planetary mixer, three-roll grinder, ball mill is mixed with equipment to be manufactured to uniform.It needs
Bright, each ingredient can mix simultaneously, can also gradually mix.
The composition for sealing of the present invention is (especially as filling material when using box dam completion method sealing organic el element
Expect use in the case of) viscosity (25 DEG C, shear velocity:20 (1/s)) it is, for example, 10~10000mPas or so, is preferably
20~3000mPas, particularly preferably 30~2500mPas, it is most preferably 30~1000mPas.
For the composition for sealing of the present invention, by can be consolidated by implementing heat treatment after implementing illumination
Change.For illumination, for 100 μm of thickness film the case where, irradiate 500mJ/cm preferably by mercury vapor lamp etc.2Above
Light.In addition, heat treatment (is particularly preferably 60~180 DEG C, is most preferably preferably by baking oven etc. at such as 40~200 DEG C
80~150 DEG C) under heat 10~200 minutes (being particularly preferably 30~120 minutes).
The composition for sealing of the present invention due to containing the mentioned component (C) with cationic capture effect, even if
Implement illumination, by cationic polymerization initiators generate cation can also capture by ingredient (C), thus can after illumination up to
Inhibit the progress of cationic polymerization before implementing heat treatment.That is, solidification delay effect can be played.Then, by illumination
Implement heat treatment afterwards, is released by the cation that ingredient (C) is captured, so as to make cation-curable compound
Cationic polymerization be able to carry out and complete to cure.That is, can be controlled by adjusting the opportunity for implementing heat treatment and freely solid
The progress of change.
Ultraviolet light (exposure is irradiated to the composition for sealing of the present invention using the mercury vapor lamp of 200W/cm:2000mJ/
cm2) just after viscosity (25 DEG C, shear velocity:20 (1/s)) it is, for example, 10~150000mPas or so, preferably 20
~50000mPas, particularly preferably 30~30000mPas.
Ultraviolet light (exposure is irradiated to the composition for sealing of the present invention using the mercury vapor lamp of 200W/cm:2000mJ/
cm2) 30 minutes viscosity (25 DEG C, shear velocities afterwards:20 (1/s)) it is, for example, 10~5000000mPas or so, preferably 20
~300000mPas, particularly preferably 30~100000mPas.
Ultraviolet light (exposure is irradiated to the composition for sealing of the present invention using the mercury vapor lamp of 200W/cm:2000mJ/
cm2) the viscosity rising degree since just terminating until after irradiation 30 minutes be, for example, 10 times or less (such as 1~10 times),
Preferably 8 times or less, more preferably 3 times or less, particularly preferably 2 times or less, most preferably 1.5 times or less.
In addition, the water vapo(u)r transmission of solidfied material obtained from being cured as the above method is low (that is, moisture resistance is excellent), Gu
Compound (thickness:100 μm) vapor transfer rate be, for example, 150g/m2Dayatm or less, preferably 100g/m2Dayatm with
Under, particularly preferably 80g/m2Dayatm or less, it is most preferably 50g/m2Dayatm or less.On it should be noted that
It is to be based on JIS L 1099 and JIS Z0208 to state vapor transfer rate, and thickness is measured under conditions of 60 DEG C, 90%RH and is adjusted to 100 μ
It is worth obtained from the vapor transfer rate of the solidfied material of m.
In addition, the capacity from cure retarder of solidfied material obtained from being cured as the above method (60mg) is
90ppm or less degree (preferably 70ppm or less, particularly preferably 50ppm or less), shows low venting quality.It needs to illustrate
It is that capacity can be measured by headspace GC/MS.
In addition, the present invention composition for sealing containing above-mentioned conducting fibre coating particles, consolidate
The excellent electric conductivity of solidfied material obtained from change, resistivity (25 DEG C, 1 atmospheric pressure under) are that 0.1 Ω cm~10M Ω cm are left
Right, preferably 0.1 Ω cm~1M Ω cm.
The composition for sealing of the present invention has solidification delay, can arbitrarily be adjusted to solidification beginning period.
Therefore, it is heated by so that it is fitted in organic EL element after carrying out illumination to composition for sealing, it can be not
Organic EL element is exposed in UV and is realized to organic EL members in the case of occurring the case where fitting will not be caused to become difficult
The sealing of part.In addition, the composition for sealing of the present invention can form while have low venting quality and the solidfied material of moisture resistance.Cause
This, composition for sealing of the invention for example can be suitable for use as filling material using box dam completion method when sealing organic el element
If material can protect organic EL element not encroached on by moisture, exhaust using the composition for sealing of the present invention, can
Prevent the deterioration of the organic EL element caused by moisture, exhaust.
[organic EL device]
The organic EL device of the present invention is the organic electroluminescence for the solidfied material for having the composition for sealing of the present invention
Part is obtained using the composition for sealing sealing organic el element of the present invention.
If using the composition for sealing of the present invention, by (special come sealing organic el element via following processes
It is top emission type organic EL element), it can be realized to the close of element while preventing the deterioration of the element caused by illumination
Envelope, so as to provide long-life and the high organic EL device of reliability.It should be noted that illumination and heating treatment method can
It is carried out by the above method.
Process 1：Illumination is implemented to the film that the organic EL element composition for sealing by the present invention is formed；
Process 2：Make the member that the substrate for being provided with organic EL element is fitted in via the film after illumination obtained from process 1
Part setting face simultaneously is implemented to heat.
The encapsulating method of organic EL element as the present invention, more specifically, following methods 1,2 can be enumerated.
<Method 1：Referring to Fig. 2>
Process 1-1：It is coated with the composition for sealing of the present invention on head cover and forms film/head cover laminated body；
Process 1-2：Illumination is implemented to film；
Process 2-1：Organic EL element is set on substrate, and in organic EL element setting face so that coated surface is set with element
Set film/head cover laminated body after the opposite mode in face is bonded illumination；
Process 2-2：By implementing to make curing of coating by heat treatment.
<Method 2>
Process 1-1 '：Sheet for sealing or film are formed in the composition for sealing of the surface of processing release paper etc. the coating present invention；
Process 1-2 '：Illumination is implemented to sheet for sealing or film；
Process 2-1：Organic EL element, and the sealing in organic EL element setting surface side after illumination are set on substrate
It is bonded head cover with piece or film；
Process 2-2：By implementing to make sheet for sealing or film cure by heat treatment.
As above-mentioned head cover (lid), substrate, it is preferable to use moisture resistance base material, it can be mentioned, for example：Soda-lime glass, alkali-free glass etc.
Glass baseplate；The metal bases such as stainless steel, aluminium；Trifluoro polyethylene, polytrifluorochloroethylene (PCTFE), Kynoar (PVDF),
The poly- ethylene fluoride Type of Collective object such as the copolymer of PCTFE and PVDF, PVDF and the copolymer of poly- fluorination vinyl chloride, polyimides,
Polyester, polyethylene, the polystyrene such as the cyclenes such as makrolon, dicyclopentadiene hydrocarbon resins, polyethylene terephthalate
Equal resin base materials etc..It should be noted that organic EL element is provided on substrate, and not it is arranged on head cover (lid).
Above-mentioned organic EL element may include the laminated body of anode/luminescent layer/cathode.SiN can also be set as desired
The passivating films such as film.
Can be for example, by head cover (Cover by the film that is formed of composition for sealing of the present invention) on coating box dam material
(dam material) and form box dam, and be discharged into the box dam using distributor etc. the present invention composition for sealing and shape
At.The thickness of film is as long as in the range of can achieve the purpose that protect the components from the infringements such as moisture without special limit
System.
In addition, will be discharged containing the composition for sealing of conducting fibre coating particles machine is discharged using distributor etc.
When, conducting fibre coating particles are preferably dissipated to the discharge of the state in composition for sealing with high score, for example, it is preferable to use tool
The screw discharge of composition for sealing is discharged in the discharge machine for having the rotary drive structures such as screw rod by the rotation based on screw rod
Method etc., is discharged while stirring.For rotary speed, the vane size of screw rod etc. of screw rod, preferably combined according to sealing
The size etc. of conducting fibre coating particles contained in the viscosity of object, composition is suitably adjusted.
According to the above method, the sealing to organic EL element can be realized in the case where being not exposed in UV, is not had
The deterioration because caused by being exposed in UV organic EL element.Also, it utilizes while there is low venting quality and the solidfied material of moisture resistance
Organic EL element is sealed, it is thus possible to protect organic EL element.Therefore, using above method sealing organic el element and
Obtained organic EL device, long lifespan and reliability are high.
Embodiment
Hereinafter, the present invention is described in more detail in conjunction with the embodiments, but the present invention is not limited to these implementations
Example.It should be noted that viscosity is measured using rheometer (trade name " Physica MCR301 ", Anton Paar corporations)
At 25 DEG C, shear velocity be 20 (1/s) when viscosity.
Embodiment 1
Each ingredient is put into rotation-revolution mixing machine (trade name " Awa-tori Rentaro according to the formula described in table
(あ わ と り Practice Taros) ARE-310 ", (strain) Thinky systems) in and be stirred, obtained composition for sealing (1).
It is coated with gained composition for sealing (1) on the glass substrate and forms film (1) (thickness:100 μm), and utilize water
Silver-colored light irradiation ultraviolet light (exposure:1600mJ/cm2).Before measuring irradiation ultraviolet light, after ultraviolet light irradiation just, it is purple
30 minutes viscosity after outside line irradiation has been calculated after being irradiated to ultraviolet light since just terminating ultraviolet light irradiation 30 points by following formula
Viscosity rising degree during clock.
The viscosity after viscosity/ultraviolet light irradiation just when 30 minutes after viscosity rising degree=ultraviolet light irradiation
Then, the film (1) after ultraviolet light being irradiated heats 1 hour in 100 DEG C, has obtained solidfied material (1) (rear solidification).
For gained solidfied material (1), capacity and water vapo(u)r transmission are had rated using following methods.
Embodiment 2~9, the Comparative Examples 1 to 5
Other than changing formula as described in table, composition for sealing is obtained similarly to Example 1, is obtained
To film and solidfied material is obtained.It should be noted that in embodiment 6, rear cured temperature 150 DEG C have been altered to.
For gained solidfied material, capacity and water vapo(u)r transmission are had rated using following methods.
<Capacity>
Capacity (the unit from cure retarder for the solidfied material obtained in Examples and Comparative Examples:Ppm) such as
It is determined lowerly：Solidfied material 60mg is added in phial, carries out UV irradiations (2000mJ/cm2), in 100 DEG C of condition
Lower standing was determined the capacity in phial after 1 hour.Wherein, using toluene titer [as standard substance
Toluene:100ppm, the hexane as solvent:60mg] make standard curve.In addition, as sensing equipment, trade name has been used
" HP-6890N " (Hewlett-Packard corporations), chromatographic column have used trade name " DB-624 " (Agilent corporations).
<Water vapo(u)r transmission>
Water vapo(u)r transmission for the solidfied material obtained in Examples and Comparative Examples is based on JIS L 1099 and JIS Z
0208 (Kapp Method) measures under the conditions of 60 DEG C, 90%RH and has rated solidfied material (thickness:100 μm) vapor transfer rate (g/m2·
day·atm)。
[table 1]
[table 2]
The compound used in Examples and Comparative Examples is as described below.
(cation-curable compound)
a-1：(3,4,3 ', 4 '-diepoxy) joins hexamethylene
a-2：Bis- (3,4- epoxycyclohexyl-methyls) ethers
a-3：4,4 '-bis- [(3- ethyl -3- oxetanylmethoxies) methoxy] biphenyl, trade name " ETERNACOLL
OXBP ", emerging production (strain) system in space portion
a-4：Epithio end fluorene compound, trade name " CS-500 ", Osaka Gas Chemicals (strain) systems
a-5：Hydroxy norbomene divinyl ether, trade name " ONB-DVE ", (strain) Daicel systems
(light cationic polymerization initiator)
b-1：Four (pentafluorophenyl group) borate of 4- (4- xenyls sulfenyl) phenyl -4- xenyl phenyl sulfonium
b-2：Three fluorophosphate of diphenyl [4- (phenylsulfartyl) phenyl] sulfonium three (pentafluoroethyl group)
b-3：4- (4- xenyls sulfenyl) phenyl -4- xenyl phenyl sulfonium hexafluoro antimonates
(cure retarder)
c-1：1,3,4,6- four glycidyl groups glycoluril, trade name " TG-G ", four countries' chemical conversion industry (strain) system
c-2：1,3,4,6- tetraallyls glycoluril, trade name " TA-G ", four countries' chemical conversion industry (strain) system
c-3：Crown ether, trade name " 18-Crown-6 ", Japanese Cao make up to (strain)
c-4：Bis- (triethylene glycol glycidyl ether) ethers of bisphenol-A, trade name " RIKARESIN BEO-60E ", new Japan
Physics and chemistry (strain) is made
c-5：1,3,5- tri- (4,5- epoxypentyls) -1,3,5- triazine -2,4,6- triketones, trade name " TEPIC-VL ", day
Chemical industry (strain) is produced to make
(other cation-curable compounds)
d-1：Liquid bisphenol F diglycidyl ethers, trade name " YL-983U ", Mitsubishi Chemical's (strain) system
d-2：Bis-phenol E diglycidyl ethers, trade name " R1710 ", Printec (strain) systems
d-3：O-phenyl phenol glycidyl ether, trade name " SY-OPG ", slope this pharmaceutical industries (strain) system
Industrial applicibility
For the organic EL element composition for sealing of the present invention, even if irradiating UV to film, implementing to heat
Cured progress can also be inhibited before, even if the progress of fitting operation is sluggish, will not cause to be bonded because losing cementability
It becomes difficult.In turn, by the implementation heat treatment after fitting, solidification can be made to carry out, it can be straight not by organic EL element
It connects and realizes sealing in the case of being exposed in UV.Have in addition, the organic EL element composition for sealing of the present invention can be formed
Moisture resistance also has the solidfied material of low venting quality simultaneously, can prevent the deterioration of the organic EL element caused by moisture, exhaust.
Therefore, organic EL element composition for sealing of the invention, by the present invention organic EL element composition for sealing
The piece or film of formation can be suitable for the seal applications of top emission type organic EL element.
Claims (9)
1. a kind of sealing organic electroluminescent element composition, containing following compositions (A), ingredient (B) and ingredient (C),
Ingredient (A)：In 1 molecule have 2 or more be selected from alicyclic epoxy group, the group containing oxetanes ring, epithio base and
The cation-curable compound of one or more of vinyl ether group group；
Ingredient (B)：Light cationic polymerization initiator；
Ingredient (C)：Glycoluril compounds.
2. sealing organic electroluminescent element composition according to claim 1, wherein ingredient (C) is to contain shrink
The glycoluril compounds of glyceryl or allyl.
3. sealing organic electroluminescent element composition according to claim 1 or 2, wherein relative to ingredient (B) 1
Parts by weight contain 0.05~3 parts by weight of ingredient (C).
4. sealing organic electroluminescent element composition described in any one of claim 1 to 3, further contains
Following compositions (D),
Ingredient (D)：The compound with 1 or more glycidyl ether (is contained in the compound in ingredient (A) in 1 molecule
Except).
5. sealing organic electroluminescent element composition according to any one of claims 1 to 4, further contains
The inorganic filling material that average grain diameter is 0.001~30 μm.
6. sealing organic electroluminescent element composition according to any one of claims 1 to 5, further contains
Following conducting fibre coating particles,
Conducting fibre coating particles：Including the conductive material of the threadiness of particle-like substance and the cladding particle-like substance
Conducting fibre coating particles.
7. it is top light emitting according to sealing organic electroluminescent element composition according to any one of claims 1 to 6
Type sealing organic electroluminescent element composition.
8. a kind of manufacturing method of organic electroluminescence device is carried out via following processes 1 and 2 pairs of organic electroluminescent devices
Sealing,
Process 1：Painting to being formed by sealing organic electroluminescent element according to any one of claims 1 to 7 composition
Film implements illumination；
Process 2：Make to fit in the substrate for being provided with organic electroluminescent device via the film after illumination obtained from process 1
Element setting face simultaneously is implemented to heat.
9. it is close to have organic electroluminescent device according to any one of claims 1 to 7 for a kind of organic electroluminescence device
The solidfied material of envelope composition.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015233349 | 2015-11-30 | ||
| JP2015-233349 | 2015-11-30 | ||
| PCT/JP2016/085653 WO2017094809A1 (en) | 2015-11-30 | 2016-11-24 | Sealing composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108353475A true CN108353475A (en) | 2018-07-31 |
Family
ID=58796964
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201680067352.6A Pending CN108353475A (en) | 2015-11-30 | 2016-11-24 | composition for sealing |
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| Country | Link |
|---|---|
| JP (1) | JPWO2017094809A1 (en) |
| KR (1) | KR102624114B1 (en) |
| CN (1) | CN108353475A (en) |
| TW (1) | TW201738291A (en) |
| WO (1) | WO2017094809A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6665136B2 (en) * | 2017-07-28 | 2020-03-13 | 株式会社ダイセル | Monomer mixture and curable composition containing the same |
| JP6538774B2 (en) * | 2017-07-28 | 2019-07-03 | 株式会社ダイセル | Monomer mixture and curable composition containing the same |
| WO2019203123A1 (en) * | 2018-04-20 | 2019-10-24 | 積水化学工業株式会社 | Sealant for organic el display element and top emission type organic el display element |
| TWI691521B (en) | 2018-12-10 | 2020-04-21 | 新應材股份有限公司 | Flexible encapsulating material, process for preparing the same and encapsulating method using the same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102414617A (en) * | 2009-04-27 | 2012-04-11 | 太阳控股株式会社 | Photo-curable and heat-curable resin composition |
| CN104718579A (en) * | 2012-07-24 | 2015-06-17 | 株式会社大赛璐 | Conductive fiber-coated particle, curable composition and cured article derived from curable composition |
| JP2015120889A (en) * | 2013-11-20 | 2015-07-02 | 四国化成工業株式会社 | Epoxy resin composition and optical semiconductor device |
| WO2015111525A1 (en) * | 2014-01-23 | 2015-07-30 | 株式会社ダイセル | Sealing composition |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4384509B2 (en) | 2003-01-09 | 2009-12-16 | 積水化学工業株式会社 | Method for sealing organic electroluminescent element and organic electroluminescent element |
| KR20160096538A (en) * | 2013-12-09 | 2016-08-16 | 세키스이가가쿠 고교가부시키가이샤 | Sealant for display element |
| JP6560985B2 (en) * | 2014-01-23 | 2019-08-14 | デンカ株式会社 | Resin composition |
-
2016
- 2016-11-24 KR KR1020187016231A patent/KR102624114B1/en active IP Right Grant
- 2016-11-24 CN CN201680067352.6A patent/CN108353475A/en active Pending
- 2016-11-24 JP JP2017554164A patent/JPWO2017094809A1/en active Pending
- 2016-11-24 WO PCT/JP2016/085653 patent/WO2017094809A1/en active Application Filing
- 2016-11-28 TW TW105139070A patent/TW201738291A/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102414617A (en) * | 2009-04-27 | 2012-04-11 | 太阳控股株式会社 | Photo-curable and heat-curable resin composition |
| CN104718579A (en) * | 2012-07-24 | 2015-06-17 | 株式会社大赛璐 | Conductive fiber-coated particle, curable composition and cured article derived from curable composition |
| JP2015120889A (en) * | 2013-11-20 | 2015-07-02 | 四国化成工業株式会社 | Epoxy resin composition and optical semiconductor device |
| WO2015111525A1 (en) * | 2014-01-23 | 2015-07-30 | 株式会社ダイセル | Sealing composition |
Also Published As
| Publication number | Publication date |
|---|---|
| KR102624114B1 (en) | 2024-01-12 |
| KR20180088413A (en) | 2018-08-03 |
| TW201738291A (en) | 2017-11-01 |
| JPWO2017094809A1 (en) | 2018-09-13 |
| WO2017094809A1 (en) | 2017-06-08 |
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