JP3261945B2 - Electroluminescent element sealing laminate and electroluminescent element sealing structure - Google Patents
Electroluminescent element sealing laminate and electroluminescent element sealing structureInfo
- Publication number
- JP3261945B2 JP3261945B2 JP26108595A JP26108595A JP3261945B2 JP 3261945 B2 JP3261945 B2 JP 3261945B2 JP 26108595 A JP26108595 A JP 26108595A JP 26108595 A JP26108595 A JP 26108595A JP 3261945 B2 JP3261945 B2 JP 3261945B2
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- electroluminescent element
- layer
- fluoride
- laminate
- 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.)
- Expired - Fee Related
Links
- 238000007789 sealing Methods 0.000 title claims description 53
- 239000010409 thin film Substances 0.000 claims description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 45
- 238000000034 method Methods 0.000 claims description 32
- 235000012245 magnesium oxide Nutrition 0.000 claims description 22
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical class [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 22
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 19
- 239000000853 adhesive Substances 0.000 claims description 18
- 230000001070 adhesive effect Effects 0.000 claims description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- 239000002985 plastic film Substances 0.000 claims description 14
- 229920006255 plastic film Polymers 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- 229920003023 plastic Polymers 0.000 claims description 10
- 239000004033 plastic Substances 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 6
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 5
- 150000002894 organic compounds Chemical class 0.000 claims description 4
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims description 3
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 3
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 claims description 3
- 229910001637 strontium fluoride Inorganic materials 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 106
- 239000010408 film Substances 0.000 description 46
- 239000000463 material Substances 0.000 description 31
- -1 polyethylene terephthalate Polymers 0.000 description 31
- 238000002347 injection Methods 0.000 description 28
- 239000007924 injection Substances 0.000 description 28
- 229910052814 silicon oxide Inorganic materials 0.000 description 24
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 22
- 230000004888 barrier function Effects 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 229920000139 polyethylene terephthalate Polymers 0.000 description 12
- 239000005020 polyethylene terephthalate Substances 0.000 description 12
- 239000011347 resin Substances 0.000 description 11
- 229920005989 resin Polymers 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000007738 vacuum evaporation Methods 0.000 description 7
- 238000007740 vapor deposition Methods 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000001771 vacuum deposition Methods 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000010549 co-Evaporation Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- WCPAKWJPBJAGKN-UHFFFAOYSA-N oxadiazole Chemical compound C1=CON=N1 WCPAKWJPBJAGKN-UHFFFAOYSA-N 0.000 description 5
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 5
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000004695 Polyether sulfone Substances 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000005401 electroluminescence Methods 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 229920000092 linear low density polyethylene Polymers 0.000 description 4
- 239000004707 linear low-density polyethylene Substances 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920006393 polyether sulfone Polymers 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 239000005083 Zinc sulfide Substances 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007733 ion plating Methods 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 3
- MKZHJJQCUIZEDE-UHFFFAOYSA-N 1-[(2-hydroxy-3-naphthalen-1-yloxypropyl)-propan-2-ylamino]-3-naphthalen-1-yloxypropan-2-ol Chemical compound C1=CC=C2C(OCC(O)CN(CC(O)COC=3C4=CC=CC=C4C=CC=3)C(C)C)=CC=CC2=C1 MKZHJJQCUIZEDE-UHFFFAOYSA-N 0.000 description 2
- MUNFOTHAFHGRIM-UHFFFAOYSA-N 2,5-dinaphthalen-1-yl-1,3,4-oxadiazole Chemical compound C1=CC=C2C(C3=NN=C(O3)C=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 MUNFOTHAFHGRIM-UHFFFAOYSA-N 0.000 description 2
- OGGKVJMNFFSDEV-UHFFFAOYSA-N 3-methyl-n-[4-[4-(n-(3-methylphenyl)anilino)phenyl]phenyl]-n-phenylaniline Chemical compound CC1=CC=CC(N(C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=C(C)C=CC=2)=C1 OGGKVJMNFFSDEV-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 2
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 2
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 2
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- WDECIBYCCFPHNR-UHFFFAOYSA-N chrysene Chemical compound C1=CC=CC2=CC=C3C4=CC=CC=C4C=CC3=C21 WDECIBYCCFPHNR-UHFFFAOYSA-N 0.000 description 2
- VPUGDVKSAQVFFS-UHFFFAOYSA-N coronene Chemical compound C1=C(C2=C34)C=CC3=CC=C(C=C3)C4=C4C3=CC=C(C=C3)C4=C2C3=C1 VPUGDVKSAQVFFS-UHFFFAOYSA-N 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 208000028659 discharge Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005566 electron beam evaporation Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 229910052839 forsterite Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- LKKPNUDVOYAOBB-UHFFFAOYSA-N naphthalocyanine Chemical class N1C(N=C2C3=CC4=CC=CC=C4C=C3C(N=C3C4=CC5=CC=CC=C5C=C4C(=N4)N3)=N2)=C(C=C2C(C=CC=C2)=C2)C2=C1N=C1C2=CC3=CC=CC=C3C=C2C4=N1 LKKPNUDVOYAOBB-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 125000001037 p-tolyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)C([H])([H])[H] 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000548 poly(silane) polymer Polymers 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 229920001230 polyarylate Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229920000123 polythiophene Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000005033 polyvinylidene chloride Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- AHLATJUETSFVIM-UHFFFAOYSA-M rubidium fluoride Chemical compound [F-].[Rb+] AHLATJUETSFVIM-UHFFFAOYSA-M 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 2
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- FKASFBLJDCHBNZ-UHFFFAOYSA-N 1,3,4-oxadiazole Chemical compound C1=NN=CO1 FKASFBLJDCHBNZ-UHFFFAOYSA-N 0.000 description 1
- KLCLIOISYBHYDZ-UHFFFAOYSA-N 1,4,4-triphenylbuta-1,3-dienylbenzene Chemical compound C=1C=CC=CC=1C(C=1C=CC=CC=1)=CC=C(C=1C=CC=CC=1)C1=CC=CC=C1 KLCLIOISYBHYDZ-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- UVHXEHGUEKARKZ-UHFFFAOYSA-N 1-ethenylanthracene Chemical compound C1=CC=C2C=C3C(C=C)=CC=CC3=CC2=C1 UVHXEHGUEKARKZ-UHFFFAOYSA-N 0.000 description 1
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- 125000001637 1-naphthyl group Chemical group [H]C1=C([H])C([H])=C2C(*)=C([H])C([H])=C([H])C2=C1[H] 0.000 description 1
- GUPMCMZMDAGSPF-UHFFFAOYSA-N 1-phenylbuta-1,3-dienylbenzene Chemical compound C=1C=CC=CC=1[C](C=C[CH2])C1=CC=CC=C1 GUPMCMZMDAGSPF-UHFFFAOYSA-N 0.000 description 1
- NIDFGXDXQKPZMA-UHFFFAOYSA-N 14h-benz[4,5]isoquino[2,1-a]perimidin-14-one Chemical compound C1=CC(N2C(=O)C=3C4=C(C2=N2)C=CC=C4C=CC=3)=C3C2=CC=CC3=C1 NIDFGXDXQKPZMA-UHFFFAOYSA-N 0.000 description 1
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- YTQQIHUQLOZOJI-UHFFFAOYSA-N 2,3-dihydro-1,2-thiazole Chemical compound C1NSC=C1 YTQQIHUQLOZOJI-UHFFFAOYSA-N 0.000 description 1
- SNTWKPAKVQFCCF-UHFFFAOYSA-N 2,3-dihydro-1h-triazole Chemical compound N1NC=CN1 SNTWKPAKVQFCCF-UHFFFAOYSA-N 0.000 description 1
- PQYIVUDIIIJJDM-UHFFFAOYSA-N 2,5-dinaphthalen-1-yl-1,3,4-thiadiazole Chemical compound C1=CC=C2C(C3=NN=C(S3)C=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 PQYIVUDIIIJJDM-UHFFFAOYSA-N 0.000 description 1
- ZGNCKIDXVHSMJL-UHFFFAOYSA-N 2-methylquinoline-8-carboxylic acid Chemical compound C1=CC=C(C(O)=O)C2=NC(C)=CC=C21 ZGNCKIDXVHSMJL-UHFFFAOYSA-N 0.000 description 1
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 1
- MGADZUXDNSDTHW-UHFFFAOYSA-N 2H-pyran Chemical compound C1OC=CC=C1 MGADZUXDNSDTHW-UHFFFAOYSA-N 0.000 description 1
- CAAMSDWKXXPUJR-UHFFFAOYSA-N 3,5-dihydro-4H-imidazol-4-one Chemical compound O=C1CNC=N1 CAAMSDWKXXPUJR-UHFFFAOYSA-N 0.000 description 1
- GOLORTLGFDVFDW-UHFFFAOYSA-N 3-(1h-benzimidazol-2-yl)-7-(diethylamino)chromen-2-one Chemical compound C1=CC=C2NC(C3=CC4=CC=C(C=C4OC3=O)N(CC)CC)=NC2=C1 GOLORTLGFDVFDW-UHFFFAOYSA-N 0.000 description 1
- RIERSGULWXEJKL-UHFFFAOYSA-N 3-hydroxy-2-methylbenzoic acid Chemical compound CC1=C(O)C=CC=C1C(O)=O RIERSGULWXEJKL-UHFFFAOYSA-N 0.000 description 1
- GQUDMCXNHNALEP-UHFFFAOYSA-N 3-n-(4-methylphenyl)benzene-1,3-diamine Chemical compound C1=CC(C)=CC=C1NC1=CC=CC(N)=C1 GQUDMCXNHNALEP-UHFFFAOYSA-N 0.000 description 1
- UAPNUNDZDVNTDQ-UHFFFAOYSA-N 4,5-diphenyl-1,2,3-triazole Chemical compound C1=CC=CC=C1C1=NNN=C1C1=CC=CC=C1 UAPNUNDZDVNTDQ-UHFFFAOYSA-N 0.000 description 1
- YOPJQOLALJLPBS-UHFFFAOYSA-N 4,5-diphenyloxadiazole Chemical compound C1=CC=CC=C1C1=C(C=2C=CC=CC=2)ON=N1 YOPJQOLALJLPBS-UHFFFAOYSA-N 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- HTPBWAPZAJWXKY-UHFFFAOYSA-L zinc;quinolin-8-olate Chemical compound [Zn+2].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 HTPBWAPZAJWXKY-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Electroluminescent Light Sources (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、フラットディスプ
レイを構成する表示材料のうち、エレクトロルミネッセ
ンス（以下、ＥＬという）素子を封止するための積層体
およびＥＬ素子封止構造体、特に有機ＥＬ素子構造体に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a laminate for sealing an electroluminescent (hereinafter, referred to as EL) element and an EL element sealing structure, particularly an organic EL element, among display materials constituting a flat display. Related to the structure.
【０００２】[0002]
【従来の技術】エレクトロニクスの飛躍的な進歩によ
り、液晶，プラズマディスプレイ，ＥＬ，蛍光表示管，
発光ダイオ−ドなどのフラットディスプレイと呼ばれる
様々なディスプレイが実用化されている。このうちＥＬ
は、液晶表示素子や時計、計器類のバックライト、制御
／計測機器やＯＡ機器あるいは自動車等の移動体用機器
のディスプレイモニターおよび光源、複写機の除電光
源、インテリアやエクステリアの各種装飾用光源、屋内
や夜間の安全灯、交通標識の光源などとして実用化ある
いは開発され、特に注目されている。ＥＬ素子には、発
光物質が無機化合物である無機ＥＬ素子と、有機化合物
薄膜から構成される有機ＥＬ素子がある。このうち、無
機ＥＬ素子の光源部は硫化亜鉛等の発光物質で構成さ
れ、水分により発光物質自体の発光機能が低下する。ま
た有機ＥＬ素子では、有機薄膜も水分により影響を受け
るが、それと同時に陰極として用いた金属が水分によっ
て酸化し有機層との界面が剥離する、あるいは酸化物に
なった結果、導電性の低下のために発光機能が著しく低
下する。そのため、ＥＬ素子光源部は、フッ素フィルム
等の防湿性の高い熱融着性プラスチックで封止されてい
る。しかし、フッ素フィルムは非常に生産性が悪いため
価格が高く、ＥＬの普及を妨げる原因の一つとなってい
る。また、ＥＬ素子光源部を保護するためには高い防湿
性が要求され、フッ素フィルムを厚くする必要があるた
め、フィルム自体の透明性（光線透過性）が低下し、Ｅ
Ｌ素子光源部の発光能力が十分に発揮されないという欠
点があった。2. Description of the Related Art With the rapid progress of electronics, liquid crystals, plasma displays, ELs, fluorescent display tubes,
Various displays called flat displays such as light emitting diodes have been put to practical use. EL
Are liquid crystal display elements, clocks, backlights of instruments, display monitors and light sources for control / measurement equipment, OA equipment, and mobile equipment such as automobiles, static elimination light sources for copiers, various decoration light sources for interiors and exteriors, It has been put to practical use or developed as a safety light for indoors or at night, a light source for traffic signs, and the like, and is particularly attracting attention. EL elements include an inorganic EL element in which a light emitting substance is an inorganic compound and an organic EL element formed of an organic compound thin film. Among them, the light source section of the inorganic EL element is formed of a light emitting substance such as zinc sulfide, and the light emitting function of the light emitting substance itself is reduced by moisture. In the organic EL device, the organic thin film is also affected by moisture, but at the same time, the metal used as the cathode is oxidized by moisture and the interface with the organic layer is peeled off or becomes an oxide. Therefore, the light emitting function is significantly reduced. Therefore, the EL element light source section is sealed with a heat-fusible plastic having high moisture resistance such as a fluorine film. However, the fluorine film has a very low productivity and therefore has a high price, which is one of the factors preventing the spread of EL. Further, in order to protect the light source of the EL element, a high moisture-proof property is required, and it is necessary to increase the thickness of the fluorine film.
There is a disadvantage that the light emitting ability of the L element light source unit is not sufficiently exhibited.
【０００３】けい素酸化物単独の蒸着フィルムに接着剤
を介して熱融着性プラスチックを積層してなる積層体を
ＥＬ素子の封止材にすることも考えられるが、けい素酸
化物単独の蒸着フィルム単枚では防湿性が不足している
ため、２枚以上を重ねて用いる必要がある。しかし、け
い素酸化物単独の蒸着フィルムは濃い褐色を呈してお
り、２枚以上重ねることにより、この褐色はより濃くな
る。ＥＬ素子の発光部から放たれる光は、褐色の積層体
を透過することにより、光量，色相ともに低下，変化し
てしまう。そのため、けい素酸化物単独の蒸着フィルム
を用いた積層体は、ＥＬ素子封止用には使用できなかっ
た。It is conceivable to use a laminate formed by laminating a heat-fusible plastic on a vapor-deposited film of silicon oxide alone via an adhesive as an encapsulating material for an EL element. Since a single vapor-deposited film lacks moisture resistance, it is necessary to use two or more films in a stack. However, the vapor deposited film of silicon oxide alone has a dark brown color, and the brown color becomes darker by stacking two or more sheets. The light emitted from the light emitting portion of the EL element passes through the brown laminate, so that both the light amount and the hue are reduced or changed. Therefore, a laminate using a vapor-deposited film of silicon oxide alone could not be used for sealing an EL element.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は、湿度
依存性の殆どないガスバリヤー性，水蒸気バリヤー性，
高透明性を同時に付加した、ＥＬ素子を封止するための
積層体およびＥＬ素子封止構造体、特に有機ＥＬ素子封
止構造体を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a gas barrier having almost no humidity dependency, a water vapor barrier, and the like.
An object of the present invention is to provide a laminate for sealing an EL element and an EL element sealing structure, particularly an organic EL element sealing structure, to which high transparency is added at the same time.
【０００５】[0005]
【課題を解決するための手段】本発明は、プラスチック
フィルム（Ａ）の片面または両面に、真空薄膜形成技術
によって、けい素酸化物を必須成分とし、これに金属フ
ッ化物およびマグネシウム酸化物類から選ばれる一種ま
たは二種以上の成分を含有する薄膜層（Ｂ）を形成し、
接着剤（Ｃ）を介し、さらに熱融着性プラスチック
（Ｄ）を積層してなるエレクトロルミネッセンス素子封
止用積層体である。本発明は、また、上記積層体の熱融
着性プラスチック（Ｄ）どうしを２枚の重ね合わせ、そ
の間にエレクトロルミネッセンス素子を設けてなるエレ
クトロルミネッセンス素子封止構造体である。本発明
は、さらに、陽極および陰極間に発光層もしくは発光層
を含む有機化合物薄膜層を備えた有機エレクトロルミネ
ッセンス素子を上記積層体間に設けてなる有機エレクト
ロルミネッセンス素子封止構造体である。According to the present invention, silicon oxide is used as an essential component on one or both sides of a plastic film (A) by a vacuum thin film forming technique, and metal oxide and magnesium oxide are used. Forming a thin film layer (B) containing one or more selected components,
This is a laminate for encapsulating an electroluminescent element, which is obtained by further laminating a heat-fusible plastic (D) via an adhesive (C). The present invention is also an electroluminescence element sealing structure in which two sheets of the heat-fusible plastic (D) of the above-mentioned laminate are superimposed and an electroluminescence element is provided therebetween. The present invention further provides an organic electroluminescence element sealing structure in which an organic electroluminescence element having a light emitting layer or an organic compound thin film layer including a light emitting layer between an anode and a cathode is provided between the laminates.
【０００６】[0006]
【発明の実施の形態】本発明におけるプラスチックフィ
ルム（Ａ）としては、ポリエチレンテレフタレ−ト，ポ
リエチレン−２，６−ナフタレート，ポリカ−ボネ−
ト，ポリサルフォン，ポリエ−テルサルフォン，ポリエ
−テルエ−テルケトン，ポリフェノキシエ−テル，ポリ
アリレ−ト，フッ素樹脂，ポリプロピレン等のフィルム
が適用できる。プラスチックフィルム（Ａ）の片面また
は両面に薄膜層（Ｂ）を形成することにより、水蒸気バ
リヤ−性が付加されるため、プラスチックフィルム
（Ａ）自体の水蒸気バリヤ−性は多少悪くても構わな
い。また、真空薄膜形成に使用できるフィルムであれば
特に制限なく用いることができ、ニ軸延伸フィルム等の
ように熱固定されたフィルムでも良い。なお、プラスチ
ックフィルム（Ａ）の表面には何も付与されていない方
が望ましいが、薄膜層（Ｂ）との接着性を向上させるた
めの易接着層やポリ塩化ビニリデン等の有機バリヤ−層
が片面または両面に付与されていても構わない。プラス
チックフィルム（Ａ）の厚さは、６〜５００μｍ、特に
１２〜５０μｍが適当である。BEST MODE FOR CARRYING OUT THE INVENTION The plastic film (A) in the present invention includes polyethylene terephthalate, polyethylene-2,6-naphthalate, polycarbonate and the like.
, Polysulfone, polyethersulfone, polyetheretheroketone, polyphenoxyether, polyarylate, fluororesin, polypropylene and the like. By forming the thin film layer (B) on one side or both sides of the plastic film (A), a water vapor barrier property is added. Therefore, the plastic film (A) itself may have a somewhat poor water vapor barrier property. In addition, any film can be used without particular limitation as long as it can be used for forming a vacuum thin film, and a heat-fixed film such as a biaxially stretched film may be used. It is preferable that nothing is provided on the surface of the plastic film (A). However, an easy-adhesion layer for improving the adhesion to the thin film layer (B) or an organic barrier layer such as polyvinylidene chloride is preferably used. It may be provided on one side or both sides. The thickness of the plastic film (A) is suitably from 6 to 500 μm, especially from 12 to 50 μm.
【０００７】薄膜層（Ｂ）は、特に高い水蒸気バリヤ−
性，ガスバリヤ−性を有し、温湿度に対し膨張が少な
く、かつプラスチックフィルム（Ａ）と強固に密着して
いなければならない。薄膜層（Ｂ）は、けい素酸化物を
必須成分とし、これに金属フッ化物およびマグネシウム
酸化物類から選ばれる一種または二種以上の成分を含有
する。いずれの組み合わせにおいても、ガスバリヤ−性
と水蒸気バリヤ−性は得られるが、高い光線透過性（透
明性）をあわせて付加したい場合には、けい素酸化物と
金属フッ化物とからなる薄膜層（Ｂ）を形成することが
有効である。また、特に水蒸気バリヤ−性を高度にした
い場合には、けい素酸化物とマグネシウム酸化物類とか
らなる薄膜層（Ｂ）を形成することが有効である。The thin film layer (B) has a particularly high water vapor barrier.
It must have properties and gas barrier properties, have little expansion with respect to temperature and humidity, and be firmly adhered to the plastic film (A). The thin film layer (B) contains silicon oxide as an essential component, and contains one or more components selected from metal fluorides and magnesium oxides. In any combination, gas barrier properties and water vapor barrier properties can be obtained, but when it is desired to add high light transmittance (transparency) together, a thin film layer composed of silicon oxide and metal fluoride ( Forming B) is effective. In particular, when a high water vapor barrier property is desired, it is effective to form a thin film layer (B) composed of silicon oxide and magnesium oxides.
【０００８】薄膜層（Ｂ）を構成するけい素酸化物は、
ＳｉＯx （ｘ＝１以上，２未満）であり、ＳｉＯ，Ｓｉ
2 Ｏ3 ，Ｓｉ3 Ｏ4 等はこの中に含まれる。中でもＳｉ
Ｏxのｘが１．８より大きく、かつ２．０未満である
と、けい素酸化物は無色透明のＳｉＯ2 に近づくため、
得られる薄膜層（Ｂ）の光線透過性（透明性）が高くな
る。反対にＳｉＯx のｘが１．８以下であると、けい素
酸化物はやや褐色と呈し、更にＳｉＯx のｘが１．５以
下になると完全に褐色を呈してしまう。The silicon oxide constituting the thin film layer (B) is
SiO x (x = 1 or more, less than 2), and SiO, Si
2 O 3 , Si 3 O 4 and the like are included in this. Among them, Si
If x of O x is greater than 1.8 and less than 2.0, the silicon oxide approaches colorless and transparent SiO 2 ,
The light transmittance (transparency) of the obtained thin film layer (B) is increased. Conversely, if x of SiO x is 1.8 or less, the silicon oxide is slightly brown, and if x of SiO x is 1.5 or less, the silicon oxide is completely brown.
【０００９】薄膜層（Ｂ）を構成する金属フッ化物とし
ては、アルカリ土類金属のフッ化物，アルカリ金属のフ
ッ化物およびフッ化アルミニウムが挙げられる。具体的
には、フッ化マグネシウム，フッ化カルシウム，フッ化
ストロンチウム，フッ化バリウム，フッ化リチウム，フ
ッ化ナトリウム，フッ化カリウム，フッ化ルビジウム，
フッ化セシウム，フッ化フランシウム等が挙げられる。
この中でも、フッ化マグネシウム，フッ化カルシウム，
フッ化ストロンチウムおよびフッ化バリウムが好まし
く、特にフッ化マグネシウムおよびフッ化カルシウムが
優れている。金属フッ化物がアルカリ土類金属のフッ化
物である場合は、高度なバリヤ−性と高透明性を両立で
き好ましい。アルカリ金属のフッ化物である場合は、ア
ルカリ土類金属のフッ化物の場合と透明性は同等である
が、バリヤー性は若干劣る。Examples of the metal fluoride constituting the thin film layer (B) include an alkaline earth metal fluoride, an alkali metal fluoride and aluminum fluoride. Specifically, magnesium fluoride, calcium fluoride, strontium fluoride, barium fluoride, lithium fluoride, sodium fluoride, potassium fluoride, rubidium fluoride,
Cesium fluoride, furanium fluoride and the like can be mentioned.
Among them, magnesium fluoride, calcium fluoride,
Strontium fluoride and barium fluoride are preferred, and magnesium fluoride and calcium fluoride are particularly excellent. When the metal fluoride is a fluoride of an alkaline earth metal, both high barrier properties and high transparency can be achieved, which is preferable. In the case of an alkali metal fluoride, the transparency is the same as that of an alkaline earth metal fluoride, but the barrier property is slightly inferior.
【００１０】薄膜層（Ｂ）を構成するマグネシウム酸化
物類としては、酸化マグネシウム、酸化マグネシウムと
二酸化けい素との共酸化物（フォルステライトやステア
タイトと呼称される共酸化物）、酸化マグネシウムと金
属フッ化物との複合化合物が挙げられる。薄膜層（Ｂ）
を構成するけい素酸化物：金属フッ化物またはマグネシ
ウム酸化物類の組成比は、９８〜８０モル％：２〜２０
モル％の範囲、特に９５〜９０モル％：５〜１０モル％
の範囲が望ましい。また、薄膜層（Ｂ）がけい素酸化
物、金属フッ化物およびマグネシウム酸化物類からなる
場合は、けい素酸化物：金属フッ化物：マグネシウム酸
化物類の組成比は、９７．５〜８０モル％：２〜１９．
５モル％：０．５〜１８モル％の範囲、特に９３〜８８
モル％：５〜１０モル％：２〜１７モル％の範囲が望ま
しい。The magnesium oxides constituting the thin film layer (B) include magnesium oxide, a co-oxide of magnesium oxide and silicon dioxide (a co-oxide called forsterite or steatite), and magnesium oxide. A composite compound with a metal fluoride is exemplified. Thin film layer (B)
The composition ratio of silicon oxide: metal fluoride or magnesium oxides is 98 to 80 mol%: 2 to 20
Mol% range, especially 95-90 mol%: 5-10 mol%
Is desirable. When the thin film layer (B) is composed of silicon oxide, metal fluoride and magnesium oxide, the composition ratio of silicon oxide: metal fluoride: magnesium oxide is 97.5 to 80 mol. %: 2-19.
5 mol%: in the range of 0.5-18 mol%, especially 93-88
Mole%: 5 to 10 mol%: The range of 2 to 17 mol% is desirable.
【００１１】薄膜層（Ｂ）の原料は、金属酸化物，金属
フッ化物，金属，有機金属化合物等の無機化合物，有機
化合物の単独または混合物の何れでも構わないが、特に
けい素酸化物と金属フッ化物の混合物、またはけい素酸
化物，金属フッ化物及び二酸化けい素と酸化マグネシウ
ムの共酸化物の混合物を原料とし、真空蒸着等により直
接プラスチックフィルム上に薄膜層（Ｂ）を形成するこ
とが望ましい。原料の組成比は、けい素酸化物と金属フ
ッ化物を用いる場合、けい素酸化物：金属フッ化物＝９
８〜７０モル％：２〜３０モル％の範囲、特に９５〜８
５モル％：５〜１５モル％の範囲が望ましい。The raw material of the thin film layer (B) may be an inorganic compound such as a metal oxide, a metal fluoride, a metal, an organometallic compound, or an organic compound alone or a mixture. It is possible to form a thin film layer (B) directly on a plastic film by vacuum deposition or the like using a mixture of fluorides or a mixture of silicon oxide, metal fluoride, and a co-oxide of silicon dioxide and magnesium oxide as raw materials. desirable. When silicon oxide and metal fluoride are used, the composition ratio of the raw materials is as follows: silicon oxide: metal fluoride = 9
8 to 70 mol%: in the range of 2 to 30 mol%, especially 95 to 8 mol%
5 mol%: a range of 5 to 15 mol% is desirable.
【００１２】また、けい素酸化物とマグネシウム酸化物
類を用いる場合は、けい素酸化物：マグネシウム酸化物
類＝９９．５〜７０モル％：０．５〜３０モル％の範
囲、特に９９．５〜９０モル％：０．５〜１０モル％の
範囲が望ましい。さらに、けい素酸化物，金属フッ化物
およびマグネシウム酸化物類を用いる場合は、けい素酸
化物：金属フッ化物：マグネシウム酸化物類＝９７．５
〜７０モル％：２〜２９．５モル％：０．５〜２８モル
％の範囲、特に９５〜９０モル％：４．５〜９．５モル
％：０．５〜５．５モル％の範囲が望ましい。When silicon oxide and magnesium oxide are used, silicon oxide: magnesium oxide = 99.5 to 70 mol%: in the range of 0.5 to 30 mol%, particularly 99.70 mol%. 5 to 90 mol%: a range of 0.5 to 10 mol% is desirable. Further, when silicon oxide, metal fluoride and magnesium oxides are used, silicon oxide: metal fluoride: magnesium oxides = 97.5.
７０70 mol%: 2 to 29.5 mol%: 0.5 to 28 mol%, especially 95 to 90 mol%: 4.5 to 9.5 mol%: 0.5 to 5.5 mol% Range is desirable.
【００１３】原料として用いるけい素酸化物の例として
は、けい素と二酸化けい素の混合物，一酸化けい素単
体、及びけい素と二酸化けい素と一酸化けい素の混合物
が挙げられる。けい素（Ｓｉ）と二酸化けい素（ＳｉＯ
2 ）の混合物を用いる場合、その組成比は基本的には等
モルが好ましいが、Ｓｉ：ＳｉＯ2 ＝４０〜６０モル
％：６０〜４０モル％の範囲ならよい。また、原料とし
て用いるけい素酸化物が、Ｓｉ、ＳｉＯ、ＳｉＯ2 の混
合物である場合は、Ｓｉ：ＳｉＯ2 をほぼ等モルにす
れば良く、（Ｓｉ＋ＳｉＯ2 ）：ＳｉＯの比率は特に限
定されない。Examples of the silicon oxide used as a raw material include a mixture of silicon and silicon dioxide, silicon monoxide alone, and a mixture of silicon, silicon dioxide and silicon monoxide. Silicon (Si) and silicon dioxide (SiO
When the mixture of 2 ) is used, the composition ratio is basically preferably equimolar, but may be in the range of Si: SiO 2 = 40-60 mol%: 60-40 mol%. When the silicon oxide used as a raw material is a mixture of Si, SiO, and SiO 2 , the ratio of Si: SiO 2 may be approximately equal, and the ratio of (Si + SiO 2 ): SiO is not particularly limited.
【００１４】プラスチックフィルム（Ａ）に薄膜層
（Ｂ）を形成する真空薄膜形成技術の方式は巻き取り連
続方式，枚葉方式のどちらでもよく、また形成する方法
としては、真空蒸着，イオンプレ−ティング，スパッタ
リングなどを用いることができる。さらに、真空蒸着の
加熱方法としては、その蒸着中にスプラッシュと呼称さ
れる蒸着飛沫が発生しなければ、あるいは支障なく取り
除ける程度に少なければ特に制限はなく、高周波誘導加
熱，抵抗加熱，電子線加熱などの公知の加熱方法を用い
ることができる。蒸着飛沫が多量に発生すると、飛沫が
蒸着フィルム上に異物として残り、ＥＬ素子封止構造体
を製造した時にその異物が黒点になるため、ＥＬ素子封
止構造体自体が不良となってしまう。The vacuum thin film forming technique for forming the thin film layer (B) on the plastic film (A) may be either a continuous winding method or a single-wafer method. The forming method may be vacuum evaporation, ion plating. , Sputtering or the like can be used. Further, there is no particular limitation on the heating method of the vacuum evaporation, as long as the evaporation splash called "splash" does not occur during the evaporation or is small enough to remove it without any trouble. High frequency induction heating, resistance heating, electron beam heating A known heating method such as a heating method can be used. When a large amount of vapor deposition droplets is generated, the droplets remain as foreign substances on the vapor deposition film, and the foreign substances become black spots when the EL element sealing structure is manufactured, so that the EL element sealing structure itself becomes defective.
【００１５】真空蒸着の蒸発源としては一般的なルツボ
方式でもかまわないが、異なる昇華点，融点の物質が常
時均一に真空蒸着できる特開平１−２５２７８６号公報
や特開平２−２７７７７４号公報に記載される蒸発原料
を連続的に供給排出する方式も用いることができる。プ
ラスチックフィルム（Ａ）に薄膜層（Ｂ）を形成する場
合、真空蒸着等の方法により原料組成をそのまま薄膜層
（Ｂ）の組成に反映させてもよいが、反応蒸着により２
種以上の原料を反応させながら、薄膜層（Ｂ）を形成し
ても良い。As an evaporation source for vacuum deposition, a general crucible method may be used. However, Japanese Patent Application Laid-Open Nos. 1-252786 and 2-277774 which can uniformly vapor-deposit substances having different sublimation points and melting points can be used. A method of continuously supplying and discharging the described evaporation raw material can also be used. When the thin film layer (B) is formed on the plastic film (A), the raw material composition may be directly reflected on the composition of the thin film layer (B) by a method such as vacuum evaporation.
The thin film layer (B) may be formed while reacting more than one kind of raw material.
【００１６】反応蒸着による薄膜層（Ｂ）の形成方法と
しては、金属または有機金属酸化物のような金属を含む
化合物を酸化またはフッ化させながら真空蒸着する方
法、金属フッ化物をプラスチックフィルム上に蒸着し後
工程でその蒸着層を酸化処理する方法が挙げられる。酸
化処理の方法としては、プラスチックフィルムの使用可
能温度範囲内で処理を行う方法なら特に限定されず、蒸
着中の酸素ガス導入法，放電処理法，酸素プラズマ法，
熱酸化法等が挙げられる。薄膜層（Ｂ）の厚さは、使用
するプラスチックフィルム（Ａ）に合わせて選定される
が、片面あたり５〜２００ｎｍ、特に１０〜１００ｎｍ
が望ましい。また、薄膜層（Ｂ）は、二層以上の積層構
造であってもよく、その時、異種類の金属フッ化物，マ
グネシウム酸化物類を積層してもよい。As a method of forming the thin film layer (B) by reactive vapor deposition, a method of vacuum-depositing while oxidizing or fluorinating a compound containing a metal such as a metal or an organic metal oxide, and a method of depositing a metal fluoride on a plastic film There is a method in which the deposited layer is oxidized in a later step after the deposition. The method of the oxidation treatment is not particularly limited as long as the treatment is performed within a usable temperature range of the plastic film, and an oxygen gas introduction method during vapor deposition, a discharge treatment method, an oxygen plasma method,
Thermal oxidation method and the like can be mentioned. The thickness of the thin film layer (B) is selected according to the plastic film (A) to be used.
Is desirable. Further, the thin film layer (B) may have a laminated structure of two or more layers, and at that time, different kinds of metal fluorides and magnesium oxides may be laminated.
【００１７】接着剤（Ｃ）としては、特に制限はなく、
ウレタン系接着剤，エポキシアミン系接着剤，エポキシ
系接着剤，アクリル系接着剤，シアノアクリレート系接
着剤等，ウレタン系アンカーコート剤，アルキルチタネ
ート系アンカーコート剤，ポリエチレンイミン系アンカ
ーコート剤，ブタジエン系アンカーコート剤が挙げら
れ、有機溶剤タイプ，水性タイプ，無溶剤タイプいずれ
でも構わない。接着剤（Ｃ）は、接着助剤としてエポキ
シシランやアミノシラン等のシランカップラーを含むこ
とが望ましい。接着剤（Ｃ）の塗布量については限定は
ない。ただし、ＥＬ封止構造体を常時屋外で使用する場
合は、耐候性の高い接着剤を使用しなければならない。The adhesive (C) is not particularly limited.
Urethane-based adhesives, epoxyamine-based adhesives, epoxy-based adhesives, acrylic-based adhesives, cyanoacrylate-based adhesives, etc., urethane-based anchor coating agents, alkyl titanate-based anchor coating agents, polyethyleneimine-based anchor coating agents, butadiene-based An anchor coating agent may be used, and any of an organic solvent type, an aqueous type, and a non-solvent type may be used. The adhesive (C) desirably contains a silane coupler such as epoxysilane or aminosilane as an adhesion aid. There is no limitation on the amount of the adhesive (C) applied. However, when the EL sealing structure is always used outdoors, an adhesive having high weather resistance must be used.
【００１８】熱融着性プラスチック（Ｄ）としては、熱
融着性（ヒートシール性）があれば制限はなく、ポリエ
チレン，ポリプロピレン等のポリオレフィンやエチレン
−酢酸ビニル共重合体，エチレン−アクリル酸共重合
体，アイオノマー，ポリ塩化ビニル，ポリ塩化ビニリデ
ン，ポリウレタン，フッ素樹脂，ポリアクリロニトリ
ル，ポリスチレン，ポリエチレンテレフタレート等のフ
ィルムを適用できる。熱融着性プラスチック（Ｄ）の積
層方法としては、ドライラミネートの様に予めフィルム
になっているものを貼り合わせる方法や押し出しラミネ
ートの様に樹脂を溶融させフィルム化しながら貼り合わ
せる方法が挙げられる。The heat fusible plastic (D) is not limited as long as it has heat fusibility (heat sealability). Polyolefins such as polyethylene and polypropylene, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer can be used. Films such as polymers, ionomers, polyvinyl chloride, polyvinylidene chloride, polyurethane, fluororesins, polyacrylonitrile, polystyrene, and polyethylene terephthalate can be used. Examples of the method for laminating the heat-fusible plastic (D) include a method in which a film is previously bonded as in dry lamination and a method in which a resin is melted and formed into a film as in extrusion lamination.
【００１９】ＥＬ素子封止構造体を得るには、２枚の本
発明のＥＬ素子封止用積層体（基本構成：Ａ／Ｂ／Ｃ／
Ｄ）の熱融着性プラスチック（Ｄ）どうしが向き合う様
に熱融着する。その際に２枚の積層体の間にＥＬ素子を
挟み込む（基本構成：Ａ／Ｂ／Ｃ／Ｄ／ＥＬ素子／Ｄ／
Ｃ／Ｂ／Ａ）。熱融着方法はあえて限定されず、一般に
は熱ラミネートなどが利用できるが、接着剤を用いたラ
ミネートでも構わない。この時、ＥＬ素子封止用積層体
の面積はＥＬ素子の面積より大きく、２つの面積の差で
４方を熱融着する。４方が完全に熱融着できない場合
は、ＥＬ素子がＥＬ素子封止用積層体からはみ出し、封
止材の意味をなさなくなってしまう。In order to obtain an EL element sealing structure, two EL element sealing laminates of the present invention (basic constitution: A / B / C /
The heat-fusible plastics of (D) are heat-sealed so that the plastics (D) face each other. At that time, an EL element is sandwiched between the two laminates (basic configuration: A / B / C / D / EL element / D /
C / B / A). The method of heat fusion is not particularly limited, and generally a heat lamination or the like can be used, but a lamination using an adhesive may be used. At this time, the area of the EL element sealing laminate is larger than the area of the EL element, and the four sides are thermally fused with a difference between the two areas. If the four sides cannot be completely heat-sealed, the EL element will protrude from the EL element sealing laminate, and will not be meaningful as a sealing material.
【００２０】本発明のＥＬ素子封止用積層体の基本構成
は、Ａ／Ｂ／Ｃ／Ｄであるが、さらに水蒸気バリヤー性
を高めたい場合は、Ａ／Ｂ／Ｃ／Ａ／Ｂ／Ｃ／Ｄ，Ａ／
Ｂ／Ｃ／Ｂ／Ａ／Ｃ／Ｄの様に蒸着フィルムを２枚重ね
にしたり、Ａ／Ｂ／Ｃ／Ａ／Ｂ／Ｃ／Ａ／Ｂ／Ｃ／Ｄの
様に蒸着フィルムを３枚重ねにしてもよい。The basic structure of the laminate for sealing an EL element of the present invention is A / B / C / D, but if it is desired to further enhance the water vapor barrier property, A / B / C / A / B / C / D, A /
Two layers of vapor deposition films like B / C / B / A / C / D, or three layers of vapor deposition films like A / B / C / A / B / C / A / B / C / D They may be stacked.
【００２１】本発明のＥＬ素子封止構造体に用いられる
無機ＥＬ素子は、ＩＴＯなどの導電性酸化物や金などの
金属の薄膜を用いた透明電極層の上に、チタン酸バリウ
ムあるいは酸化イットリウムなどの誘電体を用いた絶縁
層、マンガンあるいは希土類フッ化物などを添加した硫
化亜鉛、硫化カルシウム、硫化ストロンチウムなどの蛍
光体を含む発光層の順に形成され、必要に応じて絶縁層
を設けた後、アルミニウムやカーボンなどを用いた背面
電極が形成された構造であるが限定はされない。また吸
湿層等を素子中に設ける場合もあるが、特に限定はされ
ない。The inorganic EL element used in the EL element encapsulating structure of the present invention comprises a transparent electrode layer using a thin film of a conductive oxide such as ITO or a metal such as gold, and a barium titanate or a yttrium oxide. An insulating layer using a dielectric such as, and a luminescent layer containing a phosphor such as zinc sulfide, calcium sulfide, and strontium sulfide to which manganese or a rare earth fluoride is added, are formed in this order. , A structure in which a back electrode using aluminum, carbon, or the like is formed, but is not limited thereto. Further, a moisture absorbing layer or the like may be provided in the element, but is not particularly limited.
【００２２】本発明のＥＬ素子封止構造体に用いられる
有機ＥＬ素子は、陽極と陰極間に一層もしくは多層の有
機薄膜を形成した素子である。一層型素子の場合、陽極
と陰極との間に発光層のみを設けている。。多層型素子
は、（陽極／正孔注入層／発光層／陰極）、（陽極／発
光層／電子注入層／陰極）、（陽極／正孔注入層／発光
層／電子注入層／陰極）のいずれかの層構成からなる。
有機ＥＬ素子は、多層構成にすることにより、正孔と電
子の発光層中での再結合を効率的に起こさせることが可
能になり、さらにクエンチングによる輝度や寿命の低下
を防ぐことができる。The organic EL element used in the EL element sealing structure of the present invention is an element in which one or more organic thin films are formed between an anode and a cathode. In the case of a single-layer device, only a light-emitting layer is provided between an anode and a cathode. . The multi-layered device includes (anode / hole injection layer / light emitting layer / cathode), (anode / light emitting layer / electron injection layer / cathode), and (anode / hole injection layer / light emitting layer / electron injection layer / cathode). It has any one of the layer configurations.
When the organic EL element has a multilayer structure, recombination of holes and electrons in the light-emitting layer can be efficiently caused, and a decrease in luminance and life due to quenching can be prevented. .
【００２３】有機ＥＬ素子では、効率良く発光させるた
めに、少なくとも電極のうちの片方は素子の発光波長領
域において充分透明であることが望ましい。また、基板
も透明であることが望ましい。有機ＥＬ素子においては
通常は陽極を透明電極とするが、陰極のみあるいは陽
極、陰極ともに透明電極であっても良い。基板は、機械
的、熱的強度を有し、透明であれば限定されるものでは
ないが、例示すると、ガラス板、ポリエチレン板、ポリ
エーテルサルフォン板、ポリプロピレン板等の透明性樹
脂があげられる。In an organic EL device, it is desirable that at least one of the electrodes is sufficiently transparent in an emission wavelength region of the device in order to efficiently emit light. Further, it is desirable that the substrate is also transparent. In an organic EL element, the anode is usually a transparent electrode, but only the cathode or both the anode and the cathode may be transparent electrodes. The substrate is not limited as long as it has mechanical and thermal strength and is transparent, but examples thereof include transparent resins such as a glass plate, a polyethylene plate, a polyether sulfone plate, and a polypropylene plate. .
【００２４】有機ＥＬ素子の陽極に使用される導電性材
料は、４．０ｅＶより大きな仕事関数を持つものが好適
であり、炭素、アルミニウム、バナジウム、鉄、コバル
ト、ニッケル、タングステン、銀、金、白金、パラジウ
ム等およびそれらの合金、ＩＴＯ基板、ＮＥＳＡ基板に
使用される酸化スズ、酸化インジウム等の酸化金属、さ
らにはポリチオフェンやポリピロール等の有機導電性樹
脂が用いられるが、これらに限定されるものではない。
陽極は、必要があれば二層以上の層構成により形成され
ていても良い。透明電極は、上記の導電性材料を使用し
て、蒸着やスパッタリング等の方法で所定の透光性を確
保するように設定する。基板と陽極を合わせた光透過率
は１０％以上にすることが望ましい。The conductive material used for the anode of the organic EL device preferably has a work function greater than 4.0 eV, and includes carbon, aluminum, vanadium, iron, cobalt, nickel, tungsten, silver, gold, Platinum, palladium and their alloys, metal oxides such as tin oxide and indium oxide used for ITO and NESA substrates, and organic conductive resins such as polythiophene and polypyrrole are used, but are not limited thereto. is not.
The anode may be formed of two or more layers if necessary. The transparent electrode is set so as to secure a predetermined translucency by a method such as vapor deposition or sputtering using the above conductive material. The light transmittance of the combined substrate and anode is desirably 10% or more.
【００２５】有機ＥＬ素子の正孔注入層に用いる正孔注
入材料としては、陽極から効率よく正孔が注入され、正
孔を輸送する能力を持ち、発光層または発光層中の発光
材料に対して優れた正孔注入効果を有し、かつ薄膜形成
能の優れた化合物が挙げられる。具体的には、フタロシ
アニン系化合物、ナフタロシアニン系化合物、ポルフィ
リン系化合物、オキサジアゾール、トリアゾール、イミ
ダゾール、イミダゾロン、イミダゾールチオン、ピラゾ
リン、ピラゾロン、テトラヒドロイミダゾール、オキサ
ゾール、オキサジアゾール、ヒドラゾン、アシルヒドラ
ゾン、ポリアリールアルカン、スチルベン、ブタジエ
ン、ベンジジン型トリフェニルアミン、スチリルアミン
型トリフェニルアミン、ジアミン型トリフェニルアミン
等と、それらの誘導体、およびポリビニルカルバゾー
ル、ポリシラン、導電性高分子等の高分子材料等がある
が、これらに限定されるものではない。The hole injecting material used in the hole injecting layer of the organic EL device has a capability of efficiently injecting holes from the anode and transporting holes, and has an ability to transport the holes. Compounds having an excellent hole injection effect and excellent thin film forming ability. Specifically, phthalocyanine compounds, naphthalocyanine compounds, porphyrin compounds, oxadiazole, triazole, imidazole, imidazolone, imidazolethione, pyrazoline, pyrazolone, tetrahydroimidazole, oxazole, oxadiazole, hydrazone, acylhydrazone, poly There are arylalkane, stilbene, butadiene, benzidine-type triphenylamine, styrylamine-type triphenylamine, diamine-type triphenylamine, and derivatives thereof, and polymer materials such as polyvinylcarbazole, polysilane, and conductive polymer. However, the present invention is not limited to these.
【００２６】有機ＥＬ素子において、さらに効果的な正
孔注入材料は、芳香族三級アミン誘導体もしくはフタロ
シアニン誘導体である。具体的には、芳香族三級アミン
誘導体としては、トリフェニルアミン、トリトリルアミ
ン、トリルジフェニルアミン、Ｎ，Ｎ’−ジフェニル−
Ｎ，Ｎ’−ジ（３−メチルフェニル）−１，１’−ビフ
ェニル−４，４’−ジアミン、Ｎ，Ｎ’−ジフェニル−
Ｎ，Ｎ’−ジ（２，４−ジメチルフェニル）−１，１’
−ビフェニル−４，４’−ジアミン、Ｎ，Ｎ，Ｎ’Ｎ’
−テトラ（４−メチルフェニル）−１，１’−ジ（３−
メチルフェニル）−４，４’−ジアミン、Ｎ，Ｎ，Ｎ’
Ｎ’−テトラ（４−メチルフェニル）−１，３−フェニ
レンジアミン、Ｎ，Ｎ’−ジフェニル−Ｎ，Ｎ’−ジナ
フチル−１，１’−ビフェニル−４，４’−ジアミン、
Ｎ，Ｎ’−ジ（４−メチルフェニル）−Ｎ，Ｎ’−ジ
（４−ｎ−ブチルフェニル）−フェナントレン−９，１
０−ジアミン、１，１−ビス（４−ジ（４−メチルフェ
ニル）アミノフェニル）シクロヘキサン等、もしくはこ
れらの芳香族三級アミン骨格を有したオリゴマーもしく
はポリマー等があるが、これらに限定されるものではな
い。フタロシアニン（Ｐｃ）誘導体としては、Ｈ2 Ｐ
ｃ、ＣｕＰｃ、ＣｏＰｃ、ＮｉＰｃ、ＺｎＰｃ、ＰｄＰ
ｃ、ＦｅＰｃ、ＭｎＰｃ、ＣｌＡｌＰｃ、ＣｌＧａＰ
ｃ、ＣｌＩｎＰｃ、ＣｌＳｎＰｃ、Ｃｌ2 ＳｉＰｃ、
（ＨＯ）ＡｌＰｃ、（ＨＯ）ＧａＰｃ、ＶＯＰｃ、Ｔｉ
ＯＰｃ、ＭｏＯＰｃ、ＧａＰｃ−Ｏ−ＧａＰｃ等のフタ
ロシアニン誘導体およびナフタロシアニン誘導体等があ
るが、これらに限定されるものではない。In the organic EL device, a more effective hole injection material is an aromatic tertiary amine derivative or a phthalocyanine derivative. Specifically, as the aromatic tertiary amine derivative, triphenylamine, tolylamine, tolylphenylamine, N, N'-diphenyl-
N, N'-di (3-methylphenyl) -1,1'-biphenyl-4,4'-diamine, N, N'-diphenyl-
N, N'-di (2,4-dimethylphenyl) -1,1 '
-Biphenyl-4,4'-diamine, N, N, N'N '
-Tetra (4-methylphenyl) -1,1'-di (3-
Methylphenyl) -4,4′-diamine, N, N, N ′
N′-tetra (4-methylphenyl) -1,3-phenylenediamine, N, N′-diphenyl-N, N′-dinaphthyl-1,1′-biphenyl-4,4′-diamine,
N, N'-di (4-methylphenyl) -N, N'-di (4-n-butylphenyl) -phenanthrene-9,1
Examples include, but are not limited to, 0-diamine, 1,1-bis (4-di (4-methylphenyl) aminophenyl) cyclohexane, and the like, and oligomers or polymers having an aromatic tertiary amine skeleton. Not something. Phthalocyanine (Pc) derivatives include H 2 P
c, CuPc, CoPc, NiPc, ZnPc, PdP
c, FePc, MnPc, ClAlPc, ClGaP
c, ClInPc, ClSnPc, Cl 2 SiPc,
(HO) AlPc, (HO) GaPc, VOPc, Ti
Examples include, but are not limited to, phthalocyanine derivatives such as OPc, MoOPc, and GaPc-O-GaPc, and naphthalocyanine derivatives.
【００２７】有機ＥＬ素子の発光層は発光材料および必
要に応じてこれに添加するドーピング材料からなる。発
光材料は、薄膜形成能に優れ、薄膜状態において電極ま
たは正孔注入層、電子注入層から注入された正孔と電子
を発光層中で効率よく再結合させて、その時に発生する
エネルギーによって励起することができ、励起状態から
基底状態に戻る際のエネルギー放出である発光強度の高
い材料である。またドーピング材料は、発光層からの輝
度を向上させたり、発光色を変えたりする場合に発光層
に添加する材料である。ドーピング材料は発光層に添加
された状態で必要な特性を発揮すれば良く、薄膜形成能
に乏しかったり、単独の薄膜状態では発光しなくても良
い。発光材料またはドーピング材料の具体的な例として
は、アントラセン、ナフタレン、フェナントレン、ピレ
ン、テトラセン、コロネン、クリセン、フルオレセイ
ン、ペリレン、フタロペリレン、ナフタロペリレン、ペ
リノン、フタロペリノン、ナフタロペリノン、ジフェニ
ルブタジエン、テトラフェニルブタジエン、クマリン、
オキサジアゾール、アルダジン、ビスベンゾキサゾリ
ン、ビススチリル、ピラジン、シクロペンタジエン、キ
ノリン金属錯体、アミノキノリン金属錯体、ベンゾキノ
リン金属錯体、イミン、ジフェニルエチレン、ビニルア
ントラセン、ジアミノカルバゾール、ピラン、チオピラ
ン、ポリメチン、メロシアニン、イミダゾールキレート
化オキシノイド化合物、キナクリドン、ルブレン等およ
びそれらの誘導体があるが、これらに限定されるもので
はない。The light emitting layer of the organic EL device is composed of a light emitting material and a doping material added to the light emitting material as required. The light-emitting material has excellent thin-film forming ability. In the thin-film state, the holes and electrons injected from the electrodes or the hole injection layer and the electron injection layer efficiently recombine in the light-emitting layer, and are excited by the energy generated at that time. It is a material having high emission intensity, which is energy release when returning from the excited state to the ground state. Further, the doping material is a material added to the light emitting layer when improving the luminance from the light emitting layer or changing the light emission color. The doping material only needs to exhibit necessary characteristics in a state where it is added to the light emitting layer, and may have poor thin film forming ability or may not emit light in a single thin film state. Specific examples of the light-emitting material or the doping material include anthracene, naphthalene, phenanthrene, pyrene, tetracene, coronene, chrysene, fluorescein, perylene, phthaloperylene, naphthaloperylene, perinone, phthaloperinone, naphthaloperinone, diphenylbutadiene, tetraphenylbutadiene, coumarin,
Oxadiazole, aldazine, bisbenzoxazoline, bisstyryl, pyrazine, cyclopentadiene, quinoline metal complex, aminoquinoline metal complex, benzoquinoline metal complex, imine, diphenylethylene, vinylanthracene, diaminocarbazole, pyran, thiopyran, polymethine, merocyanine , Imidazole chelated oxinoid compounds, quinacridone, rubrene, and the like, and derivatives thereof, but are not limited thereto.
【００２８】有機ＥＬ素子の電子注入層に用いる電子注
入材料としては、電子を輸送する能力を持ち、発光層ま
たは発光材料に対して優れた電子注入効果を有し、かつ
薄膜形成能の優れた化合物が挙げられる。例えば、フル
オレノン、アントラキノジメタン、ジフェノキノン、チ
オピランジオキシド、オキサジアゾール、チアジアゾー
ル、テトラゾール、ペリレンテトラカルボン酸、フレオ
レニリデンメタン、アントラキノジメタン、アントロン
等とそれらの誘導体があるが、これらに限定されるもの
ではない。The electron injecting material used for the electron injecting layer of the organic EL element has the ability to transport electrons, has an excellent electron injecting effect on the light emitting layer or the light emitting material, and has excellent thin film forming ability. Compounds. For example, there are fluorenone, anthraquinodimethane, diphenoquinone, thiopyrandioxide, oxadiazole, thiadiazole, tetrazole, perylenetetracarboxylic acid, fluorenylidenemethane, anthraquinodimethane, anthrone and the like, and derivatives thereof. However, the present invention is not limited to this.
【００２９】有機ＥＬ素子において、さらに効果的な電
子注入材料は、金属錯体化合物もしくは含窒素五員環誘
導体である。具体的には、金属錯体化合物としては、８
−ヒドロキシキノリナートリチウム、ビス（８−ヒドロ
キシキノリナート）亜鉛、ビス（８−ヒドロキシキノリ
ナート）銅、ビス（８−ヒドロキシキノリナート）マン
ガン、トリス（８−ヒドロキシキノリナート）アルミニ
ウム、トリス（２−メチル−８−ヒドロキシキノリナー
ト）アルミニウム、トリス（８−ヒドロキシキノリナー
ト）ガリウム、ビス（１０−ヒドロキシベンゾ［ｈ］キ
ノリナート）ベリリウム、ビス（１０−ヒドロキシベン
ゾ［ｈ］キノリナート）亜鉛、ビス（２−メチル−８−
キノリナート）クロロガリウム、ビス（２−メチル−８
−キノリナート）（ｏ−クレゾラート）ガリウム、ビス
（２−メチル−８−キノリナート）（１−ナフトラー
ト）アルミニウム、ビス（２−メチル−８−キノリナー
ト）（２−ナフトラート）ガリウム等があるが、これら
に限定されるものではない。また、含窒素五員誘導体と
しては、オキサゾール、チアゾール、オキサジアゾー
ル、チアジアゾールもしくはトリアゾール誘導体が好ま
しい。具体的には、２，５−ビス（１−フェニル）−
１，３，４−オキサゾール、ジメチルＰＯＰＯＰ、２，
５−ビス（１−フェニル）−１，３，４−チアゾール、
２，５−ビス（１−フェニル）−１，３，４−オキサジ
アゾール、２−（４’−ｔｅｒｔ−ブチルフェニル）−
５−( ４”−ビフェニル) １，３，４−オキサジアゾー
ル、２，５−ビス（１−ナフチル）−１，３，４−オキ
サジアゾール、１，４−ビス［２−(５−フェニルオキ
サジアゾリル) ］ベンゼン、１，４−ビス［２−( ５−
フェニルオキサジアゾリル) −４−ｔｅｒｔ−ブチルベ
ンゼン］、２−（４’−ｔｅｒｔ−ブチルフェニル）−
５−( ４”−ビフェニル) −１，３，４−チアジアゾー
ル、２，５−ビス（１−ナフチル）−１，３，４−チア
ジアゾール、１，４−ビス［２−( ５−フェニルチアジ
アゾリル) ］ベンゼン、２−（４’−ｔｅｒｔ−ブチル
フェニル）−５−( ４”−ビフェニル) −１，３，４−
トリアゾール、２，５−ビス（１−ナフチル）−１，
３，４−トリアゾール、１，４−ビス［２−( ５−フェ
ニルトリアゾリル) ］ベンゼン等があるが、これらに限
定されるものではない。In the organic EL device, a more effective electron injecting material is a metal complex compound or a nitrogen-containing five-membered ring derivative. Specifically, as the metal complex compound, 8
Lithium hydroxyquinolinato, bis (8-hydroxyquinolinato) zinc, bis (8-hydroxyquinolinato) copper, bis (8-hydroxyquinolinato) manganese, tris (8-hydroxyquinolinato) aluminum, Tris (2-methyl-8-hydroxyquinolinato) aluminum, tris (8-hydroxyquinolinato) gallium, bis (10-hydroxybenzo [h] quinolinate) beryllium, bis (10-hydroxybenzo [h] quinolinate) Zinc, bis (2-methyl-8-
Quinolinato) chlorogallium, bis (2-methyl-8)
-Quinolinato) (o-cresolate) gallium, bis (2-methyl-8-quinolinato) (1-naphtholate) aluminum, bis (2-methyl-8-quinolinato) (2-naphtholate) gallium, and the like. It is not limited. As the nitrogen-containing five-membered derivative, an oxazole, thiazole, oxadiazole, thiadiazole or triazole derivative is preferable. Specifically, 2,5-bis (1-phenyl)-
1,3,4-oxazole, dimethyl POPOP, 2,
5-bis (1-phenyl) -1,3,4-thiazole,
2,5-bis (1-phenyl) -1,3,4-oxadiazole, 2- (4′-tert-butylphenyl)-
5- (4 "-biphenyl) 1,3,4-oxadiazole, 2,5-bis (1-naphthyl) -1,3,4-oxadiazole, 1,4-bis [2- (5- Phenyloxadiazolyl)] benzene, 1,4-bis [2- (5-
Phenyloxadiazolyl) -4-tert-butylbenzene], 2- (4'-tert-butylphenyl)-
5- (4 "-biphenyl) -1,3,4-thiadiazole, 2,5-bis (1-naphthyl) -1,3,4-thiadiazole, 1,4-bis [2- (5-phenylthiadiazo) Yl)] benzene, 2- (4'-tert-butylphenyl) -5- (4 "-biphenyl) -1,3,4-
Triazole, 2,5-bis (1-naphthyl) -1,
Examples include, but are not limited to, 3,4-triazole, 1,4-bis [2- (5-phenyltriazolyl)] benzene.
【００３０】有機ＥＬ素子における正孔注入層、発光
層、電子注入層各層では、正孔もしくは電子が効率よく
電極から注入され、層中で輸送されるよう、正孔注入材
料、発光材料、ドーピング材料、または電子注入材料を
同一層中に二種類以上混合して使用することも出来る
し、正孔注入層、発光層、電子注入層は、それぞれ二層
以上の層構成により形成されても良い。また、発光層に
は、陽極から注入した正孔もしくは陰極から注入した電
子を発光材料あるいはドーピング材料まで効率よく輸送
するために、正孔注入材料もしくは電子注入材料を添加
しても良い。さらに、正孔注入層に電子受容物質を、電
子注入材料に電子供与性物質を添加して増感させること
もできる。In each of the hole injection layer, the light-emitting layer, and the electron injection layer in the organic EL device, a hole injection material, a light-emitting material, and a doping are used so that holes or electrons are efficiently injected from the electrode and transported in the layer. Two or more kinds of materials or electron injecting materials can be mixed and used in the same layer, and the hole injecting layer, the light emitting layer, and the electron injecting layer may each be formed by two or more layers. . Further, a hole injection material or an electron injection material may be added to the light emitting layer in order to efficiently transport holes injected from an anode or electrons injected from a cathode to a light emitting material or a doping material. Further, an electron accepting substance may be added to the hole injection layer, and an electron donating substance may be added to the electron injection material to sensitize.
【００３１】本発明に係わる有機ＥＬ素子における正孔
注入層、発光層、電子注入層各層は、抵抗加熱蒸着、電
子ビーム蒸着、スパッタリング、イオンプレーティン
グ、化学反応蒸着等の乾式成膜法やスピンコーティン
グ、ディッピング等の湿式成膜法のいずれかの方法を適
用することができる。膜厚は特に限定されるものではな
いが、各層は適切な膜厚に設定する必要がある。膜厚が
厚すぎると、一定の光出力を得るために大きな印加電圧
が必要になり効率が悪くなる。膜厚が薄すぎると、薄膜
中にピンホール等が発生して、電界を印加しても充分な
発光輝度が得られない。通常の膜厚は５ｎｍから１０μ
ｍの範囲が適しているが、１０ｎｍから０．２μｍの範
囲がさらに好ましい。In the organic EL device according to the present invention, each of the hole injection layer, the light emitting layer and the electron injection layer is formed by a dry film forming method such as resistance heating evaporation, electron beam evaporation, sputtering, ion plating, chemical reaction evaporation or the like. Any of wet film forming methods such as coating and dipping can be applied. The thickness is not particularly limited, but each layer needs to be set to an appropriate thickness. If the film thickness is too large, a large applied voltage is required to obtain a constant light output, resulting in poor efficiency. If the film thickness is too small, pinholes or the like are generated in the thin film, and sufficient light emission luminance cannot be obtained even when an electric field is applied. Normal thickness is 5nm to 10μ
The range of m is suitable, but the range of 10 nm to 0.2 μm is more preferable.
【００３２】湿式成膜法の場合、各層を形成する材料
を、クロロホルム、テトラヒドロフラン、ジオキサン等
の適切な溶媒に溶解または分散して薄膜を形成するが、
その溶媒はいずれであっても良い。また、いずれの薄膜
においても、成膜性向上、膜のピンホール防止等のため
適切な樹脂や添加剤を使用しても良い。使用の可能な樹
脂としては、ポリスチレン、ポリカーボネート、ポリア
リレート、ポリエステル、ポリアミド、ポリウレタン、
ポリスルフォン、ポリメチルメタクリレート、ポリメチ
ルアクリレート、セルロース等の絶縁性樹脂、ポリ−Ｎ
−ビニルカルバゾール、ポリシラン等の光導電性樹脂、
ポリチオフェン、ポリピロール等の導電性樹脂を挙げる
ことができる。また、添加剤としては、酸化防止剤、紫
外線吸収剤、可塑剤等を挙げることができる。In the case of the wet film forming method, a material for forming each layer is dissolved or dispersed in an appropriate solvent such as chloroform, tetrahydrofuran, dioxane or the like to form a thin film.
The solvent may be any. In any of the thin films, a suitable resin or additive may be used to improve film forming properties, prevent pinholes in the film, and the like. Possible resins include polystyrene, polycarbonate, polyarylate, polyester, polyamide, polyurethane,
Insulating resin such as polysulfone, polymethyl methacrylate, polymethyl acrylate, cellulose, poly-N
-Photoconductive resins such as vinyl carbazole and polysilane,
Examples of the conductive resin include polythiophene and polypyrrole. Examples of the additive include an antioxidant, an ultraviolet absorber, and a plasticizer.
【００３３】有機ＥＬ素子において陰極に使用される導
電性物質としては、４ｅＶより小さな仕事関数を持つも
のが好適であり、セシウム、ルビジウム、カリウム、ナ
トリウム、リチウム、バリウム、ストロンチウム、、カ
ルシウム、マグネシウム、ユーロピウム、イッテルビウ
ム、サマリウム、セリウム、エルビウム、ガドリニウ
ム、イットリウム、ネオジム、ランタン、スカンジウム
等およびそれらと４ｅＶ以上の金属元素との合金が用い
られるが、これらに限定されるものではない。製膜法と
しては、抵抗加熱蒸着、電子ビーム蒸着、直流スパッ
タ、ＲＦスパッタ、イオンプレーティングなどの方法が
挙げられる。As the conductive material used for the cathode in the organic EL device, those having a work function of less than 4 eV are preferable, and cesium, rubidium, potassium, sodium, lithium, barium, strontium, calcium, magnesium, Examples include, but are not limited to, europium, ytterbium, samarium, cerium, erbium, gadolinium, yttrium, neodymium, lanthanum, scandium, and alloys thereof with metal elements of 4 eV or more. Examples of the film forming method include methods such as resistance heating evaporation, electron beam evaporation, direct current sputtering, RF sputtering, and ion plating.
【００３４】本発明は、陰極の安定性あるいは他の特性
を改善するために、多元合金にすることを妨げない。ま
た、陰極は必要に応じて二層以上の金属または合金によ
り構成されても良く、層の下部と上部でその組成や成分
比率が連続的に変化しても良い。また、水分や酸素に対
するバリア性のさらに高い絶縁性の酸化物や窒化物を陰
極を覆うように形成しても良い。The present invention does not preclude the use of multiple alloys to improve the stability or other properties of the cathode. The cathode may be composed of two or more layers of metals or alloys, if necessary, and the composition and component ratio of the lower layer and the upper layer may be continuously changed. Further, an insulating oxide or nitride having a higher barrier property against moisture or oxygen may be formed so as to cover the cathode.
【００３５】本発明により得られた有機ＥＬ素子封止構
造体においては、温度、湿度、雰囲気等に対する安定性
のさらなる向上のために、封止構造体の内部または外部
に別の封止フイルムや封止樹脂等を用いることも可能で
ある。また、封止構造体の内部にシリコンオイル等を封
入して素子を保護することも可能である。本発明におけ
る封止用積層体とこれらの封止樹脂またはシリコンオイ
ルを併用する場合には、樹脂またはオイルは発光面とは
反対側の陰極側のみに塗布あるいは封入するのが好まし
い。In the organic EL device sealing structure obtained according to the present invention, another sealing film or a sealing film is provided inside or outside the sealing structure in order to further improve the stability against temperature, humidity, atmosphere and the like. It is also possible to use a sealing resin or the like. Further, it is also possible to protect the element by enclosing silicone oil or the like inside the sealing structure. When the sealing laminate and the sealing resin or silicone oil in the present invention are used in combination, it is preferable that the resin or oil is applied or sealed only on the cathode side opposite to the light emitting surface.
【００３６】[0036]
【実施例】以下、実施例に基づいて本発明をさらに詳細
に説明するが、本発明はその要旨を越えない限り、以下
の実施例に限定されるものではない。なお、実施例にお
ける試験方法は以下の通りである。 水蒸気バリヤー性：ＡＳＴＭ Ｆ １２４９に準拠し、
米国モダンコントロールズ社製「ＰＥＲＭＡＴＲＡＮ−
Ｗ−ＴＷＩＮ」を用いて水蒸気透過率を測定した。この
値が小さいほど、水蒸気バリヤー性は優れている。 透明性：分光光度計（日本分光社製「Ｕ−ｂｅｓｔ３
０」）を用い、リファレンスを空気とし４００ｎｍでの
透過率を測定した。この値が大きいほど、透明性は優れ
ている。 ＥＬ素子封止構造体試験：無機および有機ＥＬ素子封止
構造体を４０℃９０％ＲＨの環境下で１００００時間暴
露した。その後両ＥＬ素子を発光させ、ＥＬ素子がダメ
ージを受けていないか評価した。無機ＥＬ素子について
は目視で、有機ＥＬ素子については発光輝度の低下度お
よび目視により評価した。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist. In addition, the test method in an Example is as follows. Steam barrier property: based on ASTM F 1249,
"PERMATRAN-" manufactured by Modern Controls, USA
The water vapor transmission rate was measured using "W-TWIN". The smaller the value, the better the water vapor barrier property. Transparency: Spectrophotometer (“U-best3 manufactured by JASCO Corporation”
0 "), and the transmittance at 400 nm was measured using air as a reference. The higher this value, the better the transparency. EL element sealing structure test: The inorganic and organic EL element sealing structures were exposed at 40 ° C. and 90% RH for 10,000 hours. Thereafter, both EL elements were allowed to emit light, and it was evaluated whether the EL elements were damaged. The inorganic EL element was evaluated visually, and the organic EL element was evaluated visually by the degree of decrease in emission luminance and visually.
【００３７】〔実施例１〕特開平１−２５２７８６号公
報に記載された蒸発原料を連続的に供給排出する方式の
連続巻き取り式抵抗加熱方式の真空蒸着装置を用い、厚
さ２５μｍのポリエ−テルサルフォン（ＰＥＳ）フィル
ムの片面に、けい素、二酸化けい素およびフッ化マグネ
シウムの混合物（混合比４６モル％：４６モル％：８モ
ル％）を加熱真空蒸着した（薄膜層の厚みは約６０ｎ
ｍ）。得られた蒸着フィルムを、２５μｍのフッ素樹脂
フィルム（ダイキン社製「ＦＥＰ」）と接着剤（東洋モ
ートン社製「ＡＤ７６Ｐ１／ＣＡＴ−１０」）を用いて
ドライラミネートし、ＥＬ素子封止用積層体を得た。EXAMPLE 1 A continuous winding type resistance heating type vacuum evaporation apparatus of the type described in Japanese Patent Application Laid-Open No. 1-252786, which continuously supplies and discharges the evaporation raw material, was used. On one side of a tersulfone (PES) film, a mixture of silicon, silicon dioxide and magnesium fluoride (mixing ratio: 46 mol%: 46 mol%: 8 mol%) was heated and vacuum-deposited (thickness of the thin film layer was about 60 n).
m). The obtained vapor-deposited film is dry-laminated using a 25 μm fluororesin film (“FEP” manufactured by Daikin) and an adhesive (“AD76P1 / CAT-10” manufactured by Toyo Morton Co., Ltd.) to form a laminate for sealing an EL element. I got
【００３８】〔実施例２〕実施例１と同様の真空蒸着装
置を用い、厚さ１２μｍのポリエチレンテレフタレート
（ＰＥＴ）フィルムの片面に、一酸化けい素および二酸
化けい素とマグネシウム酸化物の共酸化物（フォルステ
ライト：ＳｉＯ2 ・２ＭｇＯ）の混合物（混合比９０モ
ル％：１０モル％）を加熱真空蒸着した（薄膜層の厚み
は約６０ｎｍ）。得られた蒸着フィルムを、４０μｍの
線状低密度ポリエチレン（Ｌ−ＬＤＰＥ）と接着剤（東
洋モートン社製「ＡＤ５８５／ＣＡＴ−１０」）を用い
てドライラミネートし、ＥＬ素子封止用積層体を得た。Example 2 Using a vacuum deposition apparatus similar to that of Example 1, one side of a 12 μm-thick polyethylene terephthalate (PET) film was coated with silicon monoxide and a co-oxide of silicon dioxide and magnesium oxide. A mixture of (forsterite: SiO 2 .2MgO) (mixing ratio 90 mol%: 10 mol%) was heated and vacuum-deposited (thickness of the thin film layer was about 60 nm). The obtained vapor-deposited film was dry-laminated using 40 μm linear low-density polyethylene (L-LDPE) and an adhesive (“AD585 / CAT-10” manufactured by Toyo Morton Co., Ltd.) to obtain a laminate for sealing an EL element. Obtained.
【００３９】〔実施例３〕実施例１と同様の真空蒸着装
置を用い、厚さ２５μｍのポリエチレンテレフタレート
（ＰＥＴ）フィルムの片面に、けい素、二酸化けい素、
フッ化マグネシウおよび二酸化けい素とマグネシウム酸
化物の共酸化物（ステアタイト：２ＳｉＯ 2 ・２Ｍｇ
Ｏ）の混合物（混合比４０モル％：４０モル％：１０モ
ル％：１０モル％）を加熱真空蒸着した（薄膜層の厚み
は約６０ｎｍ）。得られた蒸着フィルムを、４０μｍの
線状低密度ポリエチレン（Ｌ−ＬＤＰＥ）と実施例２と
同様にしてドライラミネートし、ＥＬ素子封止用積層体
を得た。[Embodiment 3] The same vacuum deposition apparatus as in Embodiment 1
25 μm thick polyethylene terephthalate
(PET) One side of the film, silicon, silicon dioxide,
Magnesium fluoride and silicon dioxide and magnesium acid
Oxide (steatite: 2SiO) Two・ 2Mg
O) (mixing ratio 40 mol%: 40 mol%: 10 mol)
%: 10 mol%) was heated and vacuum-deposited (thickness of thin film layer)
Is about 60 nm). The obtained vapor-deposited film was
Linear low density polyethylene (L-LDPE) and Example 2
Dry-laminated in the same manner, and laminate for EL element sealing
I got
【００４０】〔実施例４〕加熱蒸発源を電子ビーム式に
切り替えた以外は実施例と同様の真空蒸着装置を用い、
厚さ１２μｍのポリエチレンテレフタレート（ＰＥＴ）
フィルムの片面に、けい素、二酸化けい素およびフッ化
カルシウムの混合物（混合比４５モル％：４５モル％：
１０モル％）を加熱真空蒸着した（薄膜層の厚みは約６
０ｎｍ）。得られた蒸着フィルム２枚と、４０μｍのポ
リプロピレン（ＣＰＰ）とを接着剤（東洋モートン社製
「ＡＤ５９０／ＣＡＴ−５５」）を用いてドライラミネ
ートし（構成はＰＥＴ／薄膜層／接着剤／ＰＥＴ／薄膜
層／接着剤／ＣＰＰ）、ＥＬ素子封止用積層体を得た。Example 4 The same vacuum evaporation apparatus as in Example 4 was used except that the heating evaporation source was changed to an electron beam type.
12 μm thick polyethylene terephthalate (PET)
On one side of the film, a mixture of silicon, silicon dioxide and calcium fluoride (mixing ratio: 45 mol%: 45 mol%:
10 mol%) was heated and vacuum-deposited (the thickness of the thin film layer was about 6).
0 nm). The two obtained vapor-deposited films and 40 μm polypropylene (CPP) were dry-laminated using an adhesive (“AD590 / CAT-55” manufactured by Toyo Morton Co., Ltd.) (the composition was PET / thin film layer / adhesive / PET). / Thin film layer / adhesive / CPP) to obtain a laminate for sealing an EL element.
【００４１】〔比較例１〕ポリエ−テルサルフォン（Ｐ
ＥＳ）フィルムに真空蒸着しない（薄膜層を形成しな
い）以外は、実施例１と同様にしてＥＬ素子封止用積層
体を得た。 〔比較例２〕ポリエチレンテレフタレート（ＰＥＴ）フ
ィルムに真空蒸着しない（薄膜層を形成しない）以外
は、実施例２と同様にしてＥＬ素子封止用積層体を得
た。 〔比較例３〕蒸着原料を一酸化けい素だけにした以外
は、実施例２と同様にしてＥＬ素子封止用積層体を得
た。Comparative Example 1 Polyethersulfone (P
ES) An EL element sealing laminate was obtained in the same manner as in Example 1, except that vacuum deposition was not performed on the film (no thin film layer was formed). [Comparative Example 2] An EL element sealing laminate was obtained in the same manner as in Example 2 except that a vacuum deposition was not performed on a polyethylene terephthalate (PET) film (a thin film layer was not formed). Comparative Example 3 An EL element sealing laminate was obtained in the same manner as in Example 2 except that silicon monoxide was used only as a deposition material.
【００４２】実施例１〜４および比較例１〜３で得られ
たＥＬ素子封止用積層体について、水蒸気バリヤー性と
透明性の試験を行った。また、実施例および比較例で得
られたＥＬ素子封止用積層体と、無機および有機ＥＬ素
子を用いて熱圧着によりＥＬ素子封止構造体を製造し、
ＥＬ素子封止構造体試験を行った。結果は表１に示す。
本実施例および比較例で用いた無機ＥＬ素子は、ＩＴ
Ｏ電極上にチタン酸バリウムからなる絶縁層と硫化亜
鉛：マンガンからなる発光層を形成し、その上に背面電
極としてアルミニウムを形成したものを用いた。また有
機ＥＬ素子は以下のようにして作成したものを用いた。
洗浄したＩＴＯ電極付きガラス板上に、オリゴ（ｐ−ト
リルイミノ−１，４−フェニレン−１，１−シクロヘキ
シレン−１，４−フェニレン）を真空蒸着して、膜厚５
０ｎｍの正孔注入層を得た。次いで、トリス（８−ヒド
ロキシキノリン）アルミニウム錯体を発光材料として真
空蒸着して膜厚５０ｎｍの発光層を作成した。その上
に、共蒸着によりＭｇ：Ａｇ＝１０：１の合金で膜厚２
００ｎｍの膜厚の陰極を形成した。正孔注入層、発光層
および陰極は、１０-6Ｔｏｒｒの真空中で、基板温度室
温の条件下で蒸着した。The laminate for sealing an EL element obtained in Examples 1 to 4 and Comparative Examples 1 to 3 was subjected to a test of water vapor barrier property and transparency. Further, an EL element sealing structure obtained by thermocompression bonding using the EL element sealing laminate obtained in Examples and Comparative Examples, and inorganic and organic EL elements,
An EL element sealing structure test was performed. The results are shown in Table 1.
The inorganic EL element used in this example and the comparative example was IT
An insulating layer made of barium titanate and a light emitting layer made of zinc sulfide: manganese were formed on the O electrode, and an aluminum layer was formed thereon as a back electrode. The organic EL device used was prepared as follows.
Oligo (p-tolylimino-1,4-phenylene-1,1-cyclohexylene-1,4-phenylene) was vacuum-deposited on the washed glass plate with the ITO electrode to form a film having a thickness of 5 μm.
A hole injection layer of 0 nm was obtained. Next, a tris (8-hydroxyquinoline) aluminum complex was used as a light-emitting material to form a light-emitting layer having a thickness of 50 nm by vacuum evaporation. On top of that, an alloy of Mg: Ag = 10: 1 with a film thickness of 2 by co-evaporation.
A cathode having a thickness of 00 nm was formed. The hole injection layer, the light emitting layer, and the cathode were deposited in a vacuum of 10 -6 Torr at a substrate temperature of room temperature.
【００４３】[0043]
【表１】 [Table 1]
【００４４】〔実施例５〕洗浄したＩＴＯ電極付きガラ
ス板上に、Ｈ2 Ｐｃを真空蒸着して、膜厚１０ｎｍの第
一正孔注入層を得た。さらに、１，１−ビス（４−ジ−
ｐ−トリルアミノフェニル）シクロヘキサンを真空蒸着
して、膜厚４０ｎｍの第二正孔注入層を得た。次いで、
トリス（８−ヒドロキシキノリン）アルミニウム錯体を
発光材料として真空蒸着して膜厚５０ｎｍの発光層を作
成した。その上に、共蒸着によりＭｇ：Ｉｎ＝１０：１
の合金で膜厚２００ｎｍの膜厚の陰極を形成した。正孔
注入層、発光層および陰極は、１０-6Ｔｏｒｒの真空中
で、基板温度室温の条件下で蒸着した。このようにして
作成した有機ＥＬ素子と、実施例２の積層体を用いて熱
圧着により有機ＥＬ素子封止構造体を製造した。この有
機ＥＬ素子封止構造体を４０℃９０％ＲＨの環境下で１
００００時間暴露した後、発光させた結果を表２に示
す。Example 5 H 2 Pc was vacuum-deposited on a cleaned glass plate with an ITO electrode to obtain a 10-nm-thick first hole injection layer. Further, 1,1-bis (4-di-
(p-Tolylaminophenyl) cyclohexane was vacuum-deposited to obtain a second hole injection layer having a thickness of 40 nm. Then
A tris (8-hydroxyquinoline) aluminum complex was used as a light emitting material and vacuum-deposited to form a light emitting layer having a thickness of 50 nm. On top of that, Mg: In = 10: 1 by co-evaporation.
A cathode having a film thickness of 200 nm was formed from the above alloy. The hole injection layer, the light emitting layer, and the cathode were deposited in a vacuum of 10 -6 Torr at a substrate temperature of room temperature. An organic EL element sealing structure was manufactured by thermocompression bonding using the organic EL element thus produced and the laminate of Example 2. This organic EL element sealing structure is placed in an environment of 40 ° C. and 90% RH for 1 hour.
After exposure for 0000 hours, the results of light emission are shown in Table 2.
【００４５】〔実施例６〕洗浄したＩＴＯ電極付きガラ
ス板上に、Ｎ，Ｎ’−ジフェニル−Ｎ，Ｎ’−ジ（３−
メチルフェニル）−１，１’−ビフェニル−４，４’−
ジアミンを真空蒸着して、膜厚５０ｎｍの正孔注入層を
得た。次いで、トリス（８−ヒドロキシキノリン）アル
ミニウム錯体に対してキナクリドンを１モル％の割合で
共蒸着して膜厚５０ｎｍの発光層を作成した。その上
に、共蒸着によりＡｌ：Ｌｉ＝３：２の合金で膜厚２０
０ｎｍの膜厚の陰極を形成した。正孔注入層、発光層お
よび陰極は、１０-6Ｔｏｒｒの真空中で、基板温度室温
の条件下で蒸着した。このようにして作成した有機ＥＬ
素子と、実施例２の積層体を用いて熱圧着により有機Ｅ
Ｌ素子封止構造体を製造した。この有機ＥＬ素子封止構
造体を４０℃９０％ＲＨの環境下で１００００時間暴露
した後、発光させた結果を表２に示す。Example 6 N, N'-diphenyl-N, N'-di (3-
Methylphenyl) -1,1′-biphenyl-4,4′-
Diamine was vacuum deposited to obtain a hole injection layer having a thickness of 50 nm. Then, quinacridone was co-evaporated at a rate of 1 mol% with respect to the tris (8-hydroxyquinoline) aluminum complex to form a 50 nm-thick light emitting layer. On top of that, an alloy of Al: Li = 3: 2 by co-evaporation to a film thickness of 20
A cathode having a thickness of 0 nm was formed. The hole injection layer, the light emitting layer, and the cathode were deposited in a vacuum of 10 -6 Torr at a substrate temperature of room temperature. Organic EL created in this way
Organic E by thermocompression bonding using the element and the laminate of Example 2.
An L element sealing structure was manufactured. After exposing this organic EL element sealing structure in an environment of 40 ° C. and 90% RH for 10,000 hours, light was emitted, and the results are shown in Table 2.
【００４６】〔実施例７〕洗浄したＩＴＯ電極付きガラ
ス板上に、オリゴ（ｐ−トリルイミノ−１，４−フェニ
レン−１，１−シクロヘキシレン−１，４−フェニレ
ン）を真空蒸着して、膜厚５０ｎｍの正孔注入層を得
た。次いで、ビス（２−メチル−８−キノリナート）
（１−ナフトラート）ガリウム錯体を発光材料として真
空蒸着して膜厚５０ｎｍの発光層を作成した。その上
に、共蒸着によりＭｇ：Ａｇ＝１０：１の合金で膜厚２
００ｎｍの膜厚の陰極を形成した。正孔注入層、発光層
および陰極は、１０-6Ｔｏｒｒの真空中で、基板温度室
温の条件下で蒸着した。このようにして作成した有機Ｅ
Ｌ素子と、実施例２の積層体を用いて熱圧着により有機
ＥＬ素子封止構造体を製造した。この有機ＥＬ素子封止
構造体を４０℃９０％ＲＨの環境下で１００００時間暴
露した後、発光させた結果を表２に示す。Example 7 Oligo (p-tolylimino-1,4-phenylene-1,1-cyclohexylene-1,4-phenylene) was vacuum-deposited on a washed glass plate with an ITO electrode to form a film. A hole injection layer having a thickness of 50 nm was obtained. Then, bis (2-methyl-8-quinolinate)
The (1-naphtholate) gallium complex was used as a light emitting material and vacuum deposited to form a light emitting layer having a thickness of 50 nm. On top of that, an alloy of Mg: Ag = 10: 1 with a film thickness of 2 by co-evaporation.
A cathode having a thickness of 00 nm was formed. The hole injection layer, the light emitting layer, and the cathode were deposited in a vacuum of 10 -6 Torr at a substrate temperature of room temperature. Organic E prepared in this way
Using the L element and the laminate of Example 2, an organic EL element sealing structure was manufactured by thermocompression bonding. After exposing this organic EL element sealing structure in an environment of 40 ° C. and 90% RH for 10,000 hours, light was emitted, and the results are shown in Table 2.
【００４７】〔実施例８〕洗浄したＩＴＯ電極付きガラ
ス板上に、オリゴ（ｐ−トリルイミノ−１，４−フェニ
レン−１，１−シクロヘキシレン−１，４−フェニレ
ン）を真空蒸着して、膜厚４０ｎｍの正孔注入層を得
た。次いで、Ｎ，Ｎ，Ｎ’，Ｎ’―テトラ（４―（２−
フェニル−２−プロピル）フェニル）アントラセン―
９，１０―ジアミンを発光材料として真空蒸着して膜厚
３０ｎｍの発光層を作成した。さらに、２，５−ビス
（１−ナフチル）−１，３，４−オキサジアゾールを真
空蒸着して膜厚３０ｎｍの電子注入層を作成した。その
上に、共蒸着によりＭｇ：Ａｇ＝１０：１の合金で膜厚
２００ｎｍの膜厚の陰極を形成した。有機各層および陰
極は、１０-6Ｔｏｒｒの真空中で、基板温度室温の条件
下で蒸着した。このようにして作成した有機ＥＬ素子
と、実施例２の積層体を用いて熱圧着により有機ＥＬ素
子封止構造体を製造した。この有機ＥＬ素子封止構造体
を４０℃９０％ＲＨの環境下で１００００時間暴露した
後、発光させた結果を表２に示す。Example 8 Oligo (p-tolylimino-1,4-phenylene-1,1-cyclohexylene-1,4-phenylene) was vacuum-deposited on a washed glass plate with an ITO electrode to form a film. A hole injection layer having a thickness of 40 nm was obtained. Then, N, N, N ', N'-tetra (4- (2-
Phenyl-2-propyl) phenyl) anthracene
Vacuum evaporation was performed using 9,10-diamine as a light emitting material to form a light emitting layer having a thickness of 30 nm. Further, 2,5-bis (1-naphthyl) -1,3,4-oxadiazole was vacuum-deposited to form an electron injection layer having a thickness of 30 nm. A cathode having a thickness of 200 nm was formed thereon by co-evaporation using an alloy of Mg: Ag = 10: 1. Each organic layer and the cathode were deposited in a vacuum of 10 -6 Torr at a substrate temperature of room temperature. An organic EL element sealing structure was manufactured by thermocompression bonding using the organic EL element thus produced and the laminate of Example 2. After exposing this organic EL element sealing structure in an environment of 40 ° C. and 90% RH for 10,000 hours, light was emitted, and the results are shown in Table 2.
【００４８】[0048]
【表２】 [Table 2]
【００４９】[0049]
【発明の効果】本発明により、高価な厚いフッ素フィル
ムを使用することなく、高度な無色透明性と高度な水蒸
気バリヤー性を有するＥＬ素子封止用積層体が得られる
ようになった。さらに、本積層体によりＥＬ素子、特に
有機ＥＬ素子を封止することで、長期間に渡って変質の
ない安定なＥＬ素子封止構造体が得られるようになっ
た。According to the present invention, a laminate for sealing an EL element having high colorless transparency and high water vapor barrier property can be obtained without using an expensive thick fluorine film. Furthermore, by sealing an EL element, particularly an organic EL element, with the present laminated body, a stable EL element sealing structure without deterioration for a long period of time can be obtained.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) H05B 33/04 H05B 33/14 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) H05B 33/04 H05B 33/14
Claims (5)
両面に、真空薄膜形成技術によって、けい素酸化物を必
須成分とし、これに金属フッ化物およびマグネシウム酸
化物類から選ばれる一種または二種以上の成分を含有す
る薄膜層（Ｂ）を形成し、接着剤（Ｃ）を介し、さらに
熱融着性プラスチック（Ｄ）を積層してなるエレクトロ
ルミネッセンス素子封止用積層体。1. A method for forming a silicon thin film on one or both sides of a plastic film (A) by a vacuum thin film forming technique, wherein one or two or more kinds selected from metal fluorides and magnesium oxides are added. A laminate for encapsulating an electroluminescent element, wherein a thin film layer (B) containing a component is formed, and a heat-fusible plastic (D) is further laminated via an adhesive (C).
フッ化マグネシウム，フッ化カルシウム，フッ化ストロ
ンチウムおよびフッ化バリウムから選ばれる一種または
二種以上である請求項１記載のエレクトロルミネッセン
ス素子封止用積層体。2. The metal fluoride constituting the thin film layer (B) comprises:
The electroluminescent element sealing laminate according to claim 1, wherein the laminate is one or more kinds selected from magnesium fluoride, calcium fluoride, strontium fluoride, and barium fluoride.
物類が、酸化マグネシウム，酸化マグネシウムと二酸化
けい素との共酸化物および酸化マグネシウムと金属フッ
化物との複合化合物から選ばれる一種または二種以上で
ある請求項１または２記載のエレクトロルミネッセンス
素子封止用積層体。3. The magnesium oxide constituting the thin film layer (B) is one or two selected from magnesium oxide, a co-oxide of magnesium oxide and silicon dioxide, and a complex compound of magnesium oxide and metal fluoride. The laminate for encapsulating an electroluminescent element according to claim 1, which is at least one kind.
性プラスチック（Ｄ）どうしを２枚重ね合わせ、その間
にエレクトロルミネッセンス素子を設けてなるエレクト
ロルミネッセンス素子封止構造体。4. An electroluminescent element encapsulating structure comprising two laminated sheets of the heat-fusible plastic (D) of the laminate according to claims 1 to 3, and an electroluminescent element provided therebetween.
ス素子が、陽極および陰極間に発光層もしくは発光層を
含む有機化合物薄膜層を備えた有機エレクトロルミネッ
センス素子であるエレクトロルミネッセンス素子封止構
造体。5. An electroluminescent element sealing structure, wherein the electroluminescent element according to claim 4 is an organic electroluminescent element including a light emitting layer or an organic compound thin film layer including a light emitting layer between an anode and a cathode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26108595A JP3261945B2 (en) | 1994-10-14 | 1995-10-09 | Electroluminescent element sealing laminate and electroluminescent element sealing structure |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24912294 | 1994-10-14 | ||
| JP6-249122 | 1994-10-14 | ||
| JP26108595A JP3261945B2 (en) | 1994-10-14 | 1995-10-09 | Electroluminescent element sealing laminate and electroluminescent element sealing structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08167475A JPH08167475A (en) | 1996-06-25 |
| JP3261945B2 true JP3261945B2 (en) | 2002-03-04 |
Family
ID=26539105
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26108595A Expired - Fee Related JP3261945B2 (en) | 1994-10-14 | 1995-10-09 | Electroluminescent element sealing laminate and electroluminescent element sealing structure |
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| Country | Link |
|---|---|
| JP (1) | JP3261945B2 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4514841B2 (en) * | 1998-02-17 | 2010-07-28 | 淳二 城戸 | Organic electroluminescent device |
| US6146225A (en) * | 1998-07-30 | 2000-11-14 | Agilent Technologies, Inc. | Transparent, flexible permeability barrier for organic electroluminescent devices |
| JP4505067B2 (en) * | 1998-12-16 | 2010-07-14 | 淳二 城戸 | Organic electroluminescent device |
| EP1112674B1 (en) * | 1999-07-09 | 2009-09-09 | Institute of Materials Research & Engineering | Laminates for encapsulating oled devices |
| US7164155B2 (en) | 2002-05-15 | 2007-01-16 | Semiconductor Energy Laboratory Co., Ltd. | Light emitting device |
| EP2538752A4 (en) | 2010-02-18 | 2014-09-24 | Mitsui Chemicals Tohcello Inc | Sealed functional element |
| CN103855316B (en) * | 2012-11-30 | 2016-08-03 | 海洋王照明科技股份有限公司 | A kind of organic electroluminescence device and preparation method thereof |
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1995
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Also Published As
| Publication number | Publication date |
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