JP2015225785A - Sealing method for organic electroluminescence element - Google Patents
Sealing method for organic electroluminescence element Download PDFInfo
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- JP2015225785A JP2015225785A JP2014110488A JP2014110488A JP2015225785A JP 2015225785 A JP2015225785 A JP 2015225785A JP 2014110488 A JP2014110488 A JP 2014110488A JP 2014110488 A JP2014110488 A JP 2014110488A JP 2015225785 A JP2015225785 A JP 2015225785A
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- JP
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- Prior art keywords
- sealing
- organic
- layer
- film
- organic electroluminescence
- Prior art date
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- Pending
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- 238000007789 sealing Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005401 electroluminescence Methods 0.000 title claims description 10
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 8
- 238000010828 elution Methods 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 229920001187 thermosetting polymer Polymers 0.000 claims description 5
- 239000012943 hotmelt Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004020 luminiscence type Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 45
- 239000000243 solution Substances 0.000 description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- -1 titania alkoxide Chemical class 0.000 description 8
- 239000000178 monomer Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-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
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- CSUFEOXMCRPQBB-UHFFFAOYSA-N 1,1,2,2-tetrafluoropropan-1-ol Chemical compound CC(F)(F)C(O)(F)F CSUFEOXMCRPQBB-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 1
- COWKRCCNQSQUGJ-UHFFFAOYSA-N 1,1,2,2,3-pentafluoropropan-1-ol Chemical compound OC(F)(F)C(F)(F)CF COWKRCCNQSQUGJ-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- KZVBBTZJMSWGTK-UHFFFAOYSA-N 1-[2-(2-butoxyethoxy)ethoxy]butane Chemical compound CCCCOCCOCCOCCCC KZVBBTZJMSWGTK-UHFFFAOYSA-N 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- RECMXJOGNNTEBG-UHFFFAOYSA-N 1-phenylmethoxyethanol Chemical compound CC(O)OCC1=CC=CC=C1 RECMXJOGNNTEBG-UHFFFAOYSA-N 0.000 description 1
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 101000679365 Homo sapiens Putative tyrosine-protein phosphatase TPTE Proteins 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 102100022578 Putative tyrosine-protein phosphatase TPTE Human genes 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- TUVYSBJZBYRDHP-UHFFFAOYSA-N acetic acid;methoxymethane Chemical compound COC.CC(O)=O TUVYSBJZBYRDHP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000007611 bar coating method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- ZZHNUBIHHLQNHX-UHFFFAOYSA-N butoxysilane Chemical compound CCCCO[SiH3] ZZHNUBIHHLQNHX-UHFFFAOYSA-N 0.000 description 1
- 125000000609 carbazolyl group Chemical class C1(=CC=CC=2C3=CC=CC=C3NC12)* 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229940116333 ethyl lactate Drugs 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- MYEJNNDSIXAGNK-UHFFFAOYSA-N ethyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](CC)(OC(C)C)OC(C)C MYEJNNDSIXAGNK-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 1
- HLXDKGBELJJMHR-UHFFFAOYSA-N methyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](C)(OC(C)C)OC(C)C HLXDKGBELJJMHR-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- FABOKLHQXVRECE-UHFFFAOYSA-N phenyl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)C1=CC=CC=C1 FABOKLHQXVRECE-UHFFFAOYSA-N 0.000 description 1
- VPLNCHFJAOKWBT-UHFFFAOYSA-N phenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C1=CC=CC=C1 VPLNCHFJAOKWBT-UHFFFAOYSA-N 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- SZEGZMUSBCXNLO-UHFFFAOYSA-N propan-2-yl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)C(C)C SZEGZMUSBCXNLO-UHFFFAOYSA-N 0.000 description 1
- YHNFWGSEMSWPBF-UHFFFAOYSA-N propan-2-yl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C(C)C YHNFWGSEMSWPBF-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical class C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- OQTSOKXAWXRIAC-UHFFFAOYSA-N tetrabutan-2-yl silicate Chemical compound CCC(C)O[Si](OC(C)CC)(OC(C)CC)OC(C)CC OQTSOKXAWXRIAC-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- MQVCTPXBBSKLFS-UHFFFAOYSA-N tri(propan-2-yloxy)-propylsilane Chemical compound CCC[Si](OC(C)C)(OC(C)C)OC(C)C MQVCTPXBBSKLFS-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- BJDLPDPRMYAOCM-UHFFFAOYSA-N triethoxy(propan-2-yl)silane Chemical compound CCO[Si](OCC)(OCC)C(C)C BJDLPDPRMYAOCM-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- LGROXJWYRXANBB-UHFFFAOYSA-N trimethoxy(propan-2-yl)silane Chemical compound CO[Si](OC)(OC)C(C)C LGROXJWYRXANBB-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 125000006617 triphenylamine group Chemical group 0.000 description 1
- VUWVDNLZJXLQPT-UHFFFAOYSA-N tripropoxy(propyl)silane Chemical compound CCCO[Si](CCC)(OCCC)OCCC VUWVDNLZJXLQPT-UHFFFAOYSA-N 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
Description
本発明は、本発明は有機エレクトロルミネッセンス素子（以下、有機ＥＬ素子という）の封止方法に関する。 The present invention relates to a method for sealing an organic electroluminescence element (hereinafter referred to as an organic EL element).
有機ＥＬ素子は、薄膜面発光デバイスであり、さらなる高付加価値化が求められている。特に、フィルム、薄膜ガラス、金属フォイル等からなるフレキシブル基板を用いたフレキシブル有機ＥＬが注目を集めている。フレキシブル有機ＥＬは、軽く、アンブレイカブルであり、可撓性があるという特長を有しており、これまでにない商品を生み出す可能性がある。 The organic EL element is a thin film surface emitting device, and further high added value is required. In particular, a flexible organic EL using a flexible substrate made of a film, thin film glass, metal foil or the like has attracted attention. Flexible organic EL is light, unbreakable, and has the characteristics of being flexible, and has the potential to produce unprecedented products.
しかしながら、フレキシブル有機ＥＬパネルにおける封止方法は、ガラス等のリジッド基板とは異なる。一般的に、ガラス基板での封止においては、中空の封止キャップ等が用いられるが、フレキシブル基板では、中空の封止キャップを用いることはできず、ＣＶＤ法やスパッタ法等の真空成膜による膜封止方法が用いられることが報告されている（特許文献１、非特許文献１参照）。 However, the sealing method in the flexible organic EL panel is different from a rigid substrate such as glass. In general, a hollow sealing cap or the like is used for sealing with a glass substrate, but a hollow sealing cap cannot be used for a flexible substrate, and a vacuum film formation such as a CVD method or a sputtering method is possible. It has been reported that the film sealing method according to the above is used (see Patent Document 1 and Non-Patent Document 1).
しかしながら、ＣＶＤ法やスパッタ法による膜封止方法では、成膜スピードが遅いため、生産性が悪く、高コストとなる。封止膜として窒化酸化ケイ素膜や酸化ケイ素膜が用いられるが、成膜スピードを上げると、緻密な膜が得られない、有機ＥＬ素子にダメージを与える等の課題を有していた。また、無機酸膜内部に応力が発生するため、ひび割れや有機ＥＬ素子にダメージを与える場合もある。 However, in the film sealing method by the CVD method or the sputtering method, since the film formation speed is slow, the productivity is low and the cost is high. A silicon nitride oxide film or a silicon oxide film is used as the sealing film. However, when the film formation speed is increased, a dense film cannot be obtained, and the organic EL element is damaged. In addition, since stress is generated inside the inorganic acid film, there are cases where cracks and organic EL elements are damaged.
本発明は、上記技術的課題を解決するためになされたものであり、フレキシブル有機ＥＬパネルを低コストで提供するための新たな有機ＥＬ素子の封止方法を提供することを目的とするものである。 The present invention has been made to solve the above technical problem, and an object of the present invention is to provide a new organic EL element sealing method for providing a flexible organic EL panel at a low cost. is there.
本発明に係る有機ＥＬ素子の封止方法は、有機ＥＬ素子上に、無機酸化物からなる封止膜を塗布成膜により形成することを特徴とする。 The organic EL element sealing method according to the present invention is characterized in that a sealing film made of an inorganic oxide is formed on an organic EL element by coating.
前記封止方法においては、前記封止膜をアルコールにて塗布成膜することが好ましい。 In the sealing method, the sealing film is preferably formed by coating with alcohol.
前記アルコールは、フッ素系アルコールであることが好ましい。 The alcohol is preferably a fluorinated alcohol.
また、有機ＥＬ素子を構成する有機ＥＬ層と前記封止膜の間に、有機ＥＬ層溶出防止層を形成してもよい。 Moreover, you may form an organic EL layer elution prevention layer between the organic EL layer which comprises an organic EL element, and the said sealing film.
また、前記封止膜は複数層であることが好ましい。 Further, the sealing film is preferably a plurality of layers.
また、前記封止膜の少なくとも１層が酸化チタンであることが好ましい。 Moreover, it is preferable that at least one layer of the sealing film is titanium oxide.
上記封止方法は、ダムフィル構造による封止、又は、ＵＶ硬化樹脂、熱硬化樹脂又はホットメルト樹脂を用いた封止と併用してもよい。 The sealing method may be used in combination with sealing with a dam-fill structure or sealing using a UV curable resin, a thermosetting resin, or a hot melt resin.
本発明に係る有機ＥＬ素子の封止方法は、非常に簡便であり、フレキシブルなデバイスにも対応が可能でありながら、有機ＥＬ素子を外気の水分、酸素から保護し、有機ＥＬの保存性を向上させることができる。
上記方法による封止膜を備えた有機ＥＬ素子は、表示素子や光源等としての有効利用が期待される。
The organic EL element sealing method according to the present invention is very simple and can be applied to a flexible device, while protecting the organic EL element from moisture and oxygen in the outside air, and thus improving the storage stability of the organic EL element. Can be improved.
The organic EL element provided with the sealing film by the above method is expected to be effectively used as a display element or a light source.
以下、本発明について詳細に説明する。
本発明に係る有機ＥＬ素子の封止方法は、有機ＥＬ素子上に、無機酸化物からなる封止膜を塗布成膜により形成するものである。
塗布型膜による封止は、塗布した際に有機ＥＬ層が溶出するという問題がある。これに対して、本発明においては、塗布液としてアルコール、好ましくは、フッ素系アルコールを用い、また、前記塗布液に溶解しないバッファ層として有機ＥＬ層溶出防止層を電極の上に形成することにより、下層の有機ＥＬ層の溶解を抑制することができる。
Hereinafter, the present invention will be described in detail.
In the organic EL device sealing method according to the present invention, a sealing film made of an inorganic oxide is formed on an organic EL device by coating.
Sealing with a coating-type film has a problem that the organic EL layer elutes when coated. In contrast, in the present invention, an alcohol, preferably a fluorinated alcohol, is used as the coating solution, and an organic EL layer elution preventing layer is formed on the electrode as a buffer layer that does not dissolve in the coating solution. The dissolution of the lower organic EL layer can be suppressed.
前記封止膜の形成には、無機酸化物のゾルゲル法を用いる。例えば、フッ素系アルコールに溶解したチタニアアルコキシドを塗布後、焼成することにより、封止膜が得られる。 An inorganic oxide sol-gel method is used to form the sealing film. For example, a sealing film can be obtained by applying titania alkoxide dissolved in a fluorinated alcohol and then baking.
ゾルゲル法により形成される無機酸化物の封止膜は、金属塩又は金属アルコキシドの加水分解により得られる。
具体的は、まず、塗布液として、金属アルコキシドのゾルゲル液を調製する。金属種としては、Ｓｉが好ましく、それ以外には、Ｔｉ、Ｓｎ、Ａｌ、Ｚｎ、Ｚｒ、Ｉｎ等や、これらの混合物等が挙げられるが、これらに限定されるものではない。上記金属の酸化物の前駆体を適宜混合したものを用いることもできる。中でも、シリカ（ＳｉＯ2）、チタニア（ＴｉＯ2）が好ましい。
例えば、シリカの場合は、シリカ前駆体としては、テトラメトキシシラン（ＴＭＯＳ）、テトラエトキシシラン（ＴＥＯＳ）、テトラ−ｉ−プロポキシシラン、テトラ−ｎ−プロポキシシラン、テトラ−ｉ−ブトキシシラン、テトラ−ｎ−ブトキシシラン、テトラ−ｓｅｃ−ブトキシシラン、テトラ−ｔ−ブトキシシラン等のテトラアルコキシドモノマーや、メチルトリメトキシシラン、エチルトリメトキシシラン、プロピルトリメトキシシラン、イソプロピルトリメトキシシラン、フェニルトリメトキシシラン、メチルトリエトキシシラン（ＭＴＥＳ）、エチルトリエトキシシラン、プロピルトリエトキシシラン、イソプロピルトリエトキシシラン、フェニルトリエトキシシラン、メチルトリプロポキシシラン、エチルトリプロポキシシラン、プロピルトリプロポキシシラン、イソプロピルトリプロポキシシラン、フェニルトリプロポキシシラン、メチルトリイソプロポキシシラン、エチルトリイソプロポキシシラン、プロピルトリイソプロポキシシラン、イソプロピルトリイソプロポキシシラン、フェニルトリイソプロポキシシラン等のトリアルコキシドモノマーや、これらのモノマーを少量重合したポリマー、前記モノマー又はポリマーの一部に官能基やポリマーを導入した複合材料等のシリコンアルコキシドが挙げられる。
さらに、金属アルコキシド以外に、金属アセチルアセトネート、金属カルボキシレート、オキシ塩化物、塩化物や、これらの混合物等が挙げられるが、これらに限定されるものではない。
An inorganic oxide sealing film formed by a sol-gel method is obtained by hydrolysis of a metal salt or a metal alkoxide.
Specifically, first, a metal alkoxide sol-gel solution is prepared as a coating solution. As the metal species, Si is preferable, and other than that, Ti, Sn, Al, Zn, Zr, In, and the like, a mixture thereof, and the like can be mentioned, but are not limited thereto. What mixed suitably the precursor of the said metal oxide can also be used. Of these, silica (SiO 2 ) and titania (TiO 2 ) are preferable.
For example, in the case of silica, the silica precursors include tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), tetra-i-propoxysilane, tetra-n-propoxysilane, tetra-i-butoxysilane, tetra- tetraalkoxide monomers such as n-butoxysilane, tetra-sec-butoxysilane, tetra-t-butoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, isopropyltrimethoxysilane, phenyltrimethoxysilane, Methyltriethoxysilane (MTES), ethyltriethoxysilane, propyltriethoxysilane, isopropyltriethoxysilane, phenyltriethoxysilane, methyltripropoxysilane, ethyltripropoxysila Trialkoxide monomers such as propyltripropoxysilane, isopropyltripropoxysilane, phenyltripropoxysilane, methyltriisopropoxysilane, ethyltriisopropoxysilane, propyltriisopropoxysilane, isopropyltriisopropoxysilane, phenyltriisopropoxysilane And silicon alkoxide such as a polymer obtained by polymerizing these monomers in a small amount, or a composite material in which a functional group or polymer is introduced into a part of the monomer or polymer.
Further, in addition to metal alkoxide, metal acetylacetonate, metal carboxylate, oxychloride, chloride, a mixture thereof, and the like are exemplified, but not limited thereto.
前記ゾルゲル液の溶媒としては、例えば、メタノール、エタノール、イソプロピルアルコール（ＩＰＡ）、ブタノール等のアルコール類、ヘキサン、ヘプタン、オクタン、デカン、シクロヘキサン等の脂肪族炭化水素類、ベンゼン、トルエン、キシレン、メシチレン等の芳香族炭化水素類、ジエチルエーテル、テトラヒドロフラン、ジオキサン等のエーテル類、アセトン、メチルエチルケトン、イソホロン、シクロヘキサノン等のケトン類、ブトキシエチルエーテル、ヘキシルオキシエチルアルコール、メトキシ−２−プロパノール、ベンジルオキシエタノール等のエーテルアルコール類、エチレングリコール、プロピレングリコール等のグリコール類、エチレングリコールジメチルエーテル、ジエチレングリコールジメチルエーテル、プロピレングリコールモノメチルエーテルアセテート等のグリコールエーテル類、酢酸エチル、乳酸エチル、γ−ブチロラクトン等のエステル類、フェノール、クロロフェノール等のフェノール類、Ｎ，Ｎ−ジメチルホルムアミド、Ｎ，Ｎ−ジメチルアセトアミド、Ｎ−メチルピロリドン等のアミド類、クロロホルム、塩化メチレン、テトラクロロエタン、モノクロロベンゼン、ジクロロベンゼン等のハロゲン系溶媒、二硫化炭素等の含ヘテロ元素化合物、水、及び、これらの混合溶媒が挙げられる。特に、アルコール類であるエタノール又はイソプロピルアルコールが好ましい。より好ましくは、フッ素系アルコールが挙げられる。テトラフルオロプロパノール、ペンタフルオロプロパノール、ヘキサフルオロイソプロパノール等である。 Examples of the solvent for the sol-gel solution include alcohols such as methanol, ethanol, isopropyl alcohol (IPA) and butanol, aliphatic hydrocarbons such as hexane, heptane, octane, decane and cyclohexane, benzene, toluene, xylene and mesitylene. Aromatic hydrocarbons such as diethyl ether, tetrahydrofuran, dioxane, etc., ketones such as acetone, methyl ethyl ketone, isophorone, cyclohexanone, butoxyethyl ether, hexyloxyethyl alcohol, methoxy-2-propanol, benzyloxyethanol, etc. Ether alcohols, glycols such as ethylene glycol and propylene glycol, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, Glycol ethers such as lenglycol monomethyl ether acetate, esters such as ethyl acetate, ethyl lactate and γ-butyrolactone, phenols such as phenol and chlorophenol, N, N-dimethylformamide, N, N-dimethylacetamide, N- Examples thereof include amides such as methylpyrrolidone, halogen-based solvents such as chloroform, methylene chloride, tetrachloroethane, monochlorobenzene and dichlorobenzene, hetero element compounds such as carbon disulfide, water, and mixed solvents thereof. In particular, alcohols such as ethanol or isopropyl alcohol are preferred. More preferably, a fluorine-type alcohol is mentioned. Tetrafluoropropanol, pentafluoropropanol, hexafluoroisopropanol and the like.
前記ゾルゲル液には、添加物を混合してもよい。例えば、アミン系化合物や界面活性剤等を混合することができる。 An additive may be mixed in the sol-gel solution. For example, an amine compound or a surfactant can be mixed.
有機ＥＬ素子は、水分に弱いため、水分濃度１００ｐｐｍ以下、好ましくは１０ｐｐｍ以下で、ゾルゲル液を調液する。塗布の際には、ゾルゲル反応の進行を促進させるために、水分や触媒を含んでいてもよいが、水分を含む場合には、脱水溶媒にて、上記範囲内の水分濃度の不活性雰囲気下でゾルゲル液を調液した後、大気に１０秒〜５分程度開放して、水分を混入させてもよい。 Since the organic EL element is vulnerable to moisture, the sol-gel solution is prepared at a moisture concentration of 100 ppm or less, preferably 10 ppm or less. In application, in order to promote the progress of the sol-gel reaction, water or a catalyst may be included. When water is included, a dehydrating solvent is used in an inert atmosphere having a water concentration within the above range. After preparing the sol-gel solution, the mixture may be opened to the atmosphere for about 10 seconds to 5 minutes to mix water.
前記ゾルゲル液は、スピンコート法、インクジェット法、キャスティング法、ディップコート法、バーコート法、ブレードコート法、ロールコート法、グラビアコート法、フレキソ印刷法、スプレーコート法、スリットダイコート法等のウェットプロセスにより成膜されるが、塗布成膜方法はこれに限定されるものではない。 The sol-gel solution is a wet process such as spin coating method, ink jet method, casting method, dip coating method, bar coating method, blade coating method, roll coating method, gravure coating method, flexographic printing method, spray coating method, slit die coating method, etc. However, the coating film forming method is not limited to this.
塗布成膜後、加熱プロセス、光焼成プロセス等により緻密な膜形成を行うことが好ましい。
加熱プロセスを用いる場合は、有機ＥＬ素子に熱ダメージを与えない温度範囲で行う必要があり、１５０℃以下で行うことが好ましい。
また、光焼成プロセスを用いる場合は、無機酸化物の光吸収がある光であることが好ましく、例えば、高圧水銀灯、低圧水銀灯、エキシマーランプ等を用いることができるが、これに限定されるものではない。波長３００ｎｍ以下の光が好ましく、特に、波長２５４ｎｍ又は１７２ｎｍの光が好ましい。
加熱プロセス及び光焼成プロセスは、同時に行ってもよい。
After the coating film formation, it is preferable to form a dense film by a heating process, a light baking process, or the like.
When using a heating process, it is necessary to carry out in the temperature range which does not give a thermal damage to an organic EL element, and it is preferable to carry out at 150 degrees C or less.
Moreover, when using a photo-baking process, it is preferable that it is light which has the light absorption of an inorganic oxide, for example, a high pressure mercury lamp, a low pressure mercury lamp, an excimer lamp etc. can be used, However, It is not limited to this. Absent. Light having a wavelength of 300 nm or less is preferable, and light having a wavelength of 254 nm or 172 nm is particularly preferable.
The heating process and the light baking process may be performed simultaneously.
前記封止膜の膜厚は５ｎｍ〜１０μｍであることが好ましい。 The thickness of the sealing film is preferably 5 nm to 10 μm.
また、有機ＥＬ素子を構成する有機ＥＬ層と前記封止膜の間に、有機ＥＬ層溶出防止層を形成してもよい。有機ＥＬ層溶出防止層は、有機ＥＬ素子上に塗布成膜されるゾルゲル液が有機ＥＬ素子に与えるダメージを抑制するための層であり、また、有機ＥＬ自体もしくはパーティクルによる凹凸を平坦化することができる。 Moreover, you may form an organic EL layer elution prevention layer between the organic EL layer which comprises an organic EL element, and the said sealing film. The organic EL layer elution prevention layer is a layer for suppressing the damage caused to the organic EL element by the sol-gel solution applied and formed on the organic EL element, and also planarizes the unevenness caused by the organic EL itself or particles. Can do.
前記有機ＥＬ層溶出防止層は、ゾルゲル液であるアルコール溶媒に不溶な有機材料を蒸着法にて形成してもよい。該有機材料としては、トリフェニルアミン誘導体、カルバゾール誘導体、スチルベン誘導体等の多くの有機ＥＬ材料を適用することができ、特に限定されるものではない。
また、前記有機ＥＬ層溶出防止層は、塗布にて形成してもよい。塗布により形成する材料としては、熱硬化型又はＵＶ硬化型の無溶剤モノマーが好ましく、特に、硬化型シリコーンモノマーが好ましい。無溶剤モノマーを塗布後、熱硬化及び／又はＵＶ硬化により固体薄膜化させ、有機ＥＬ層溶出防止層を形成する。
前記有機ＥＬ層溶出防止層には、水分・酸素を吸収するゲッター剤を混合してもよい。
The organic EL layer elution preventing layer may be formed by vapor deposition of an organic material insoluble in an alcohol solvent that is a sol-gel solution. As the organic material, many organic EL materials such as a triphenylamine derivative, a carbazole derivative, and a stilbene derivative can be applied, and the organic material is not particularly limited.
The organic EL layer elution preventing layer may be formed by coating. As a material to be formed by coating, a thermosetting or UV curable solventless monomer is preferable, and a curable silicone monomer is particularly preferable. After applying the solventless monomer, the organic EL layer elution preventing layer is formed by forming a solid thin film by heat curing and / or UV curing.
A getter agent that absorbs moisture and oxygen may be mixed in the organic EL layer elution preventing layer.
本発明に係る封止方法は、他の封止方法と併用してもよい。すなわち、上記のような塗布方法により形成した無機酸化物からなる封止膜の上に、さらに、封止構造を設けてもよい。
該封止構造としては、封止基板を用いたダムフィル構造や、封止基板をＵＶ硬化樹脂、熱硬化樹脂又は熱可塑性樹脂（ホットメルト樹脂）による封止構造が挙げられる。前記封止基板は、高い水分バリア性、フレキシブル性を有していることが好ましい。
前記ダムフィル構造におけるフィル剤、ＵＶ硬化樹脂、熱硬化樹脂又は熱可塑性樹脂には、水分・酸素を吸収するゲッター剤を混合してもよい。
The sealing method according to the present invention may be used in combination with other sealing methods. That is, you may provide a sealing structure further on the sealing film which consists of an inorganic oxide formed with the above application | coating methods.
Examples of the sealing structure include a dam fill structure using a sealing substrate, and a sealing structure using a UV curable resin, a thermosetting resin, or a thermoplastic resin (hot melt resin). The sealing substrate preferably has high moisture barrier properties and flexibility.
A getter agent that absorbs moisture and oxygen may be mixed with the filling agent, UV curable resin, thermosetting resin, or thermoplastic resin in the dam fill structure.
本発明における有機ＥＬ素子は、特に限定されるものではなく、様々な層構造、蛍光方式やリン光方式や熱活性遅延蛍光方式等の様々な発光方式のものでよい。発光ユニットを多段に配置し、電荷発生層を直列に介したマルチフォトン（タンデム）素子であってもよい。
また、前記有機ＥＬ素子は、真空成膜方式や塗布成膜方式、真空と塗布成膜方式を混合したハイブリット素子のいずれの成膜方式によって形成されたものでもよい。さらに、有機ＥＬ素子の２つの電極は、封止膜側の電極が透明であり、封止膜方向に光を取り出すものであってもよい。
The organic EL element in the present invention is not particularly limited, and may have various layer structures, various light emission methods such as a fluorescence method, a phosphorescence method, and a thermally activated delayed fluorescence method. A multi-photon (tandem) element in which the light emitting units are arranged in multiple stages and the charge generation layer is connected in series may be used.
Further, the organic EL element may be formed by any film forming method of a vacuum film forming method, a coating film forming method, and a hybrid element in which a vacuum and a coating film forming method are mixed. Further, the two electrodes of the organic EL element may be ones in which the electrode on the sealing film side is transparent and light is extracted in the direction of the sealing film.
以下、本発明を実施例に基づいて、さらに具体的に説明する。
図１に記載したような封止構造の有機ＥＬ素子を作製した。基板１上に電極（陽極）２としてＩＴＯを成膜した基板に、有機ＥＬ層３として、正孔注入層ＭｏＯ3を膜厚５ｎｍ、正孔輸送層ＮＰＤを膜厚４０ｎｍ、発光層兼電子輸送層Ａｌｑ3を膜厚６０ｎｍ、電子注入層ＬｉＦを膜厚１ｎｍ、さらに、電極（陰極）４としてＡｌを膜厚１００ｎｍ、有機ＥＬ層溶出防止層５としてＴＰＴＥを膜厚１００ｎｍで真空成膜した有機ＥＬ素子を作製した。
Hereinafter, the present invention will be described more specifically based on examples.
An organic EL element having a sealing structure as described in FIG. 1 was produced. A substrate in which ITO is formed as an electrode (anode) 2 on a substrate 1, an organic EL layer 3, a hole injection layer MoO 3 with a film thickness of 5 nm, a hole transport layer NPD with a film thickness of 40 nm, and a light emitting layer / electron transport Layer Alq 3 having a film thickness of 60 nm, electron injection layer LiF having a film thickness of 1 nm, further, an electrode (cathode) 4 having an Al film thickness of 100 nm, and an organic EL layer elution preventing layer 5 having a TPTE film having a film thickness of 100 nm. An EL element was produced.
水分濃度１ｐｐｍ以下の乾燥窒素雰囲気下のグローブボックス内で、チタニウムテトライソプロポキシド（Ｔｉ（ＯｉＰｒ）4）の２ｗｔ％脱水テトラフルオロプロパノール溶液を調液し、湿度３０％の大気に１分間開放し、すぐにグローブボックス内に戻した溶液をゾルゲル液−１とした。 In a glove box under a dry nitrogen atmosphere with a moisture concentration of 1 ppm or less, a 2 wt% dehydrated tetrafluoropropanol solution of titanium tetraisopropoxide (Ti (OiPr) 4 ) is prepared and opened to the atmosphere with a humidity of 30% for 1 minute. The solution immediately returned to the glove box was designated as sol-gel solution-1.
同様に、水分濃度１ｐｐｍ以下の乾燥窒素雰囲気下のグローブボックス内で、チタニウムテトライソプロポキシド（Ｔｉ（ＯｉＰｒ）4）の２ｗｔ％脱水ｎ−ブタノール溶液を調液し、湿度４０％の大気に１分間開放し、すぐにグローブボックス内に戻した溶液をゾルゲル液−２とした。 Similarly, a 2 wt% dehydrated n-butanol solution of titanium tetraisopropoxide (Ti (OiPr) 4 ) was prepared in a glove box under a dry nitrogen atmosphere with a moisture concentration of 1 ppm or less, and 1% was added to the atmosphere with a humidity of 40%. The solution which was opened for a minute and immediately returned to the glove box was designated as sol-gel solution-2.
ゾルゲル液−１，２を下記表１に示すような各条件で３層塗布成膜して封止膜６を形成し、２３℃、湿度４０％で２か月間放置した後の発光状態を観察し、封止性能の評価を行った。
図２〜５に、各有機ＥＬ素子の発光状態の写真を示す。
なお、加熱は、グローブボックス内でホットプレートを用いて行った。また、ＵＶ照射は、グローブボックス内で、低圧水銀灯を３７ｍＷ／ｃｍ2の強度で照射した。
Three layers of sol-gel solutions-1 and 2 are formed under the conditions shown in Table 1 to form a sealing film 6, and the light emission state is observed after being left for 2 months at 23 ° C. and a humidity of 40%. Then, the sealing performance was evaluated.
In FIGS. 2-5, the photograph of the light emission state of each organic EL element is shown.
The heating was performed using a hot plate in the glove box. Further, UV irradiation was performed with a low-pressure mercury lamp at an intensity of 37 mW / cm 2 in a glove box.
上記評価結果から、本発明に係る塗布成膜による封止膜により高い封止性能が得られることが認められた。 From the above evaluation results, it was confirmed that high sealing performance can be obtained by the sealing film formed by the coating film formation according to the present invention.
１ 基板
２，４ 電極
３ 有機ＥＬ層
５ 有機ＥＬ溶出防止層
６ 封止膜
DESCRIPTION OF SYMBOLS 1 Substrate 2, 4 Electrode 3 Organic EL layer 5 Organic EL elution prevention layer 6 Sealing film
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