CN104518131A - Organic electroluminescent device and preparation method - Google Patents
Organic electroluminescent device and preparation method Download PDFInfo
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- CN104518131A CN104518131A CN201310449355.4A CN201310449355A CN104518131A CN 104518131 A CN104518131 A CN 104518131A CN 201310449355 A CN201310449355 A CN 201310449355A CN 104518131 A CN104518131 A CN 104518131A
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- barrier layer
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- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 230000004888 barrier function Effects 0.000 claims abstract description 103
- 239000000463 material Substances 0.000 claims abstract description 59
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 230000005540 biological transmission Effects 0.000 claims abstract description 23
- 238000002347 injection Methods 0.000 claims abstract description 23
- 239000007924 injection Substances 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 12
- 238000005401 electroluminescence Methods 0.000 claims description 57
- 229910052757 nitrogen Inorganic materials 0.000 claims description 34
- 238000007738 vacuum evaporation Methods 0.000 claims description 31
- 238000001704 evaporation Methods 0.000 claims description 30
- 230000008020 evaporation Effects 0.000 claims description 30
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 27
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- DHDHJYNTEFLIHY-UHFFFAOYSA-N 4,7-diphenyl-1,10-phenanthroline Chemical group C1=CC=CC=C1C1=CC=NC2=C1C=CC1=C(C=3C=CC=CC=3)C=CN=C21 DHDHJYNTEFLIHY-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- 239000004411 aluminium Substances 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- 239000010931 gold Substances 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 10
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 10
- 150000004706 metal oxides Chemical class 0.000 claims description 10
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052741 iridium Inorganic materials 0.000 claims description 9
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 150000005360 2-phenylpyridines Chemical class 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 5
- YSZJKUDBYALHQE-UHFFFAOYSA-N rhenium trioxide Chemical compound O=[Re](=O)=O YSZJKUDBYALHQE-UHFFFAOYSA-N 0.000 claims description 5
- WXBOMIKEWRRKBB-UHFFFAOYSA-N rhenium(iv) oxide Chemical compound O=[Re]=O WXBOMIKEWRRKBB-UHFFFAOYSA-N 0.000 claims description 5
- IBHBKWKFFTZAHE-UHFFFAOYSA-N n-[4-[4-(n-naphthalen-1-ylanilino)phenyl]phenyl]-n-phenylnaphthalen-1-amine Chemical class C1=CC=CC=C1N(C=1C2=CC=CC=C2C=CC=1)C1=CC=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=C1 IBHBKWKFFTZAHE-UHFFFAOYSA-N 0.000 claims description 4
- 229910000423 chromium oxide Inorganic materials 0.000 claims 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 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 abstract description 5
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- HONWGFNQCPRRFM-UHFFFAOYSA-N 2-n-(3-methylphenyl)-1-n,1-n,2-n-triphenylbenzene-1,2-diamine Chemical compound CC1=CC=CC(N(C=2C=CC=CC=2)C=2C(=CC=CC=2)N(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 HONWGFNQCPRRFM-UHFFFAOYSA-N 0.000 abstract 1
- GJNUVYYGKXYCMI-UHFFFAOYSA-N C(C1=CC=CC=C1)C1=CC=NC2=C3N=CC=C(C3=CC=C12)CC1=CC=CC=C1 Chemical compound C(C1=CC=CC=C1)C1=CC=NC2=C3N=CC=C(C3=CC=C12)CC1=CC=CC=C1 GJNUVYYGKXYCMI-UHFFFAOYSA-N 0.000 abstract 1
- FIMQDWPAUNOAIR-UHFFFAOYSA-N N-benzyl-N-[4-[4-[benzyl(naphthalen-1-yl)amino]phenyl]phenyl]naphthalen-1-amine Chemical compound C1(=CC=CC2=CC=CC=C12)N(C1=CC=C(C=C1)C1=CC=C(N(CC2=CC=CC=C2)C2=CC=CC3=CC=CC=C23)C=C1)CC1=CC=CC=C1 FIMQDWPAUNOAIR-UHFFFAOYSA-N 0.000 abstract 1
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 218
- 239000011521 glass Substances 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 8
- 230000035699 permeability Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- VQGHOUODWALEFC-UHFFFAOYSA-N 2-phenylpyridine Chemical compound C1=CC=CC=C1C1=CC=CC=N1 VQGHOUODWALEFC-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- GEQBRULPNIVQPP-UHFFFAOYSA-N 2-[3,5-bis(1-phenylbenzimidazol-2-yl)phenyl]-1-phenylbenzimidazole Chemical compound C1=CC=CC=C1N1C2=CC=CC=C2N=C1C1=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=C1 GEQBRULPNIVQPP-UHFFFAOYSA-N 0.000 description 4
- DIVZFUBWFAOMCW-UHFFFAOYSA-N 4-n-(3-methylphenyl)-1-n,1-n-bis[4-(n-(3-methylphenyl)anilino)phenyl]-4-n-phenylbenzene-1,4-diamine Chemical compound CC1=CC=CC(N(C=2C=CC=CC=2)C=2C=CC(=CC=2)N(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=C(C)C=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=C(C)C=CC=2)=C1 DIVZFUBWFAOMCW-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- AWXGSYPUMWKTBR-UHFFFAOYSA-N 4-carbazol-9-yl-n,n-bis(4-carbazol-9-ylphenyl)aniline Chemical compound C12=CC=CC=C2C2=CC=CC=C2N1C1=CC=C(N(C=2C=CC(=CC=2)N2C3=CC=CC=C3C3=CC=CC=C32)C=2C=CC(=CC=2)N2C3=CC=CC=C3C3=CC=CC=C32)C=C1 AWXGSYPUMWKTBR-UHFFFAOYSA-N 0.000 description 3
- 101000837344 Homo sapiens T-cell leukemia translocation-altered gene protein Proteins 0.000 description 3
- 102100028692 T-cell leukemia translocation-altered gene protein Human genes 0.000 description 3
- 238000001994 activation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical group O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 3
- QVLNJJLJVMLHFO-UHFFFAOYSA-N [F].[O-2].[Zn+2] Chemical compound [F].[O-2].[Zn+2] QVLNJJLJVMLHFO-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
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- 239000002356 single layer Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
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- Electroluminescent Light Sources (AREA)
Abstract
The invention provides an organic electroluminescent device comprising an anode conductive substrate, a hole injection layer, a hole transmission layer, a luminescent layer, an electron transmission layer, an electron injection layer, a cathode and a packaging layer which are laminated in turn. The packaging layer comprises an organic barrier layer and an inorganic barrier layer. Material of the organic barrier layer is at least one type of copper phthalocyanine, N,N'-dibenzyl-N,N'-di(1-naphthyl)-1,1'-biphenyl-4,4'-diamine, 8-hydroxyquinoline aluminum, 4,4',4''-tri(N-3-methyl phenyl-N-phenyl amino)triphenylamine and 4,7-dibenzyl-1,10-phenanthroline. Material of the inorganic barrier layer comprises pure metal and metallic oxide, and mass percentage of pure metal is 10-30%. The packaging layer of the organic electroluminescent device is high in compactness so that erosion of oxygen and water vapor to the device can be effectively reduced, and the service life of the device can be substantially enhanced. The invention also provides a preparation method of the organic electroluminescent device.
Description
Technical field
The present invention relates to organic electroluminescence device, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is between transparent anode and metallic cathode, accompany multilayer organic material film (hole injection layer, hole transmission layer, luminescent layer, electron supplying layer and electron injecting layer), and apply certain voltage when between electrode after, luminescent layer will be luminous.In recent years, organic electroluminescence device because cost of manufacture own is low, the response time is short, luminosity is high, the feature such as wide viewing angle, low driving voltage and energy-conserving and environment-protective received extensive concern in fields such as total colouring, backlight and illuminations, and has been considered to be most likely at the device of new generation following illumination and display device market occupying dominance.
At present, there is life-span shorter problem in organic electroluminescence device, and this occurs rapidly aging mainly because organic material film is very loose after easily being infiltrated by compositions such as the steam in air and oxygen.Therefore, organic electroluminescence device must encapsulate before entering actual use, and the quality of encapsulation is directly connected to the life-span of organic electroluminescence device.
Glass cover or crown cap is adopted to encapsulate in conventional art, its edge ultraviolet polymerization resin seal, but the glass cover used in this method or crown cap volume are often comparatively large, add the weight of device, and the method can not be applied to flexible organic electroluminescence gives out light the encapsulation of device.
Summary of the invention
For overcoming the defect of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and preparation method thereof.This organic electroluminescence device is provided with encapsulated layer at cathode surface, comprise the inorganic barrier layer and inorganic barrier layer that are cascading, effectively can reduce water, oxygen isoreactivity material to the erosion of device, thus improves the life-span of organic electroluminescence device significantly.Its preparation method technique is simple, and material is cheap and easy to get, is suitable for suitability for industrialized production.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise the anode conducting substrate stacked gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode and encapsulated layer, described encapsulated layer comprises the inorganic barrier layer and inorganic barrier layer that are cascading, the material of described inorganic barrier layer comprises CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, 4'-diamines (NPB), oxine aluminium (Alq3), 4, 4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA) and 4, 7-diphenyl-1, at least one in 10-Phen (BCP),
The material of described inorganic barrier layer comprises metal simple-substance and metal oxide, mass fraction shared by described metal simple-substance is 10 ~ 30%, and described metal simple-substance is one or more in copper (Cu), aluminium (Al), indium (In), gold (Au), nickel (Ni) and silver (Ag); Described metal oxide is tungsten oxide (WO
3), chromium oxide (CrO
3), molybdenum oxide (MoO
3), manganese dioxide (MnO
2), rhenium dioxide (ReO
2) and rhenium trioxide (ReO
3) in one or more.
Preferably, the thickness of described inorganic barrier layer is 200nm ~ 300nm.
Preferably, the thickness of described inorganic barrier layer is 100nm ~ 150nm.
Preferably, described inorganic barrier layer and inorganic barrier layer are arranged alternately 4 ~ 6 layers successively.
Encapsulated layer of the present invention comprises inorganic barrier layer and inorganic barrier layer, wherein, the material of inorganic barrier layer comprises CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA) or 4,7-diphenyl-1,10-Phen (BCP); Metal simple-substance in inorganic barrier layer is one or more in copper (Cu), aluminium (Al), indium (In), gold (Au), nickel (Ni) and silver (Ag); Metal oxide is tungsten oxide (WO
3), chromium oxide (CrO
3), molybdenum oxide (MoO
3), manganese dioxide (MnO
2), rhenium dioxide (ReO
2) and rhenium trioxide (ReO
3) in one or more.One made by inorganic barrier layer and device, do not need to destroy vacuum, simultaneously as substrate and alleviation effect of stress; Simple substance and oxide make not to be needed to destroy vacuum equally, and evaporation mode all can be adopted to make, and the block of metal own is high, and the object adding metal oxide is the stress in relief layer, prevents crack performance from occurring.Thus the combination of inorganic barrier layer of the present invention and inorganic barrier layer makes encapsulated layer have excellent packaging effect, extend water Oxygen permeation path, effectively block extraneous steam, oxygen to the erosion of device, improve the useful life of device.
Preferably, anode conducting substrate comprises anode conductive layer and substrate, its substrate can be glass substrate or organic film substrate, the material of anode conductive layer can be conductive oxide, as, tin indium oxide (ITO), Al-Doped ZnO (AZO), mix indium zinc oxide (IZO) or mix fluorine zinc oxide (FTO), these conductive oxides are produced on the glass substrate, are called for short ito glass, AZO glass, IZO glass, FTO glass.Anode conducting substrate can be made by oneself, also can commercially obtain.
The material of the present invention to described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer does not make particular determination, adopts common used material in industry.
Preferably, the material of described hole injection layer comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in described N, N'-diphenyl-N, MoO in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines
3, described MoO
3doping mass fraction be 30%; The material of described hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA); The material of described luminescent layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI) and three (the 2-phenylpyridines) be entrained in described 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene close iridium (Ir (ppy)
3), the doping mass fraction that described three (2-phenylpyridines) close iridium is 5%; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen); The material of described electron injecting layer comprises 4,7-diphenyl-1,10-phenanthroline and is entrained in the CsN in described 4,7-diphenyl-1,10-phenanthrolines
3, described CsN
3doping mass fraction be 30%.
Negative electrode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed).
The thickness of the present invention to described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode does not make particular determination.
The encapsulated layer employing inorganic barrier layer of organic electroluminescence device of the present invention and inorganic barrier layer successively alternative stacked are arranged on cathode surface, whole encapsulated layer effectively can stop that extraneous steam and oxygen are to the erosion of organic electroluminescence device, thus extends device lifetime.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) provide clean anode electrically-conductive backing plate, on anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared in vacuum evaporation successively;
(2) prepare encapsulated layer on the cathode, obtain organic electroluminescence device; Wherein, described encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows: adopt the mode of vacuum evaporation to deposit inorganic barrier layer and inorganic barrier layer successively at described cathode surface, the vacuum degree in Vacuum Evaporation Process is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
The material of described inorganic barrier layer comprises CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA) and 4, at least one in 7-diphenyl-1,10-Phen (BCP);
The material of described inorganic barrier layer comprises metal simple-substance and metal oxide, mass fraction shared by described metal simple-substance is 10 ~ 30%, and described metal simple-substance is one or more in copper (Cu), aluminium (Al), indium (In), gold (Au), nickel (Ni) and silver (Ag); Described metal oxide is tungsten oxide (WO
3), chromium oxide (CrO
3), molybdenum oxide (MoO
3), manganese dioxide (MnO
2), rhenium dioxide (ReO
2) and rhenium trioxide (ReO
3) in one or more.
Preferably, the thickness of described inorganic barrier layer is 200nm ~ 300nm.
Preferably, the thickness of described inorganic barrier layer is 100nm ~ 150nm.
Preferably, described inorganic barrier layer and inorganic barrier layer are arranged alternately 4 ~ 6 layers successively.
Preferably, anode conducting substrate comprises anode conductive layer and substrate, its substrate can be glass substrate or organic film substrate, the material of anode conductive layer can be conductive oxide, as, tin indium oxide (ITO), Al-Doped ZnO (AZO), mix indium zinc oxide (IZO) or mix fluorine zinc oxide (FTO), these conductive oxides are produced on the glass substrate, are called for short ito glass, AZO glass, IZO glass, FTO glass.Anode conducting substrate can be made by oneself, also can commercially obtain.
Described anode substrate carries out following clean operation usually: carry out acetone cleaning, ethanol purge, washed with de-ionized water, ethanol purge successively, all cleans with supersonic wave cleaning machine, individual event washing cleaning 5 minutes, and then dry up with nitrogen, stove-drying is stand-by; Again surface activation process is carried out to the substrate after cleaning, to increase the oxygen content of conductive surface layer, improve the work function of conductive layer surface.
The material of the present invention to described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer does not make particular determination, adopts common used material in industry.
Preferably, the material of described hole injection layer comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in described N, N'-diphenyl-N, MoO in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines
3, described MoO
3doping mass fraction be 30%; The material of described hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA); The material of described luminescent layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI) and three (the 2-phenylpyridines) be entrained in described 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene close iridium (Ir (ppy)
3), the doping mass fraction that described three (2-phenylpyridines) close iridium is 5%; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen); The material of described electron injecting layer comprises 4,7-diphenyl-1,10-phenanthroline and is entrained in the CsN in described 4,7-diphenyl-1,10-phenanthrolines
3, described CsN
3doping mass fraction be 30%.
Negative electrode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed).
Described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared by vacuum evaporation, prepare thickness and do not make particular determination.Preferably, the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
This preparation method has obtained the encapsulating structure that multilayer material layer is arranged alternately, and preparation method is easy, and the encapsulating material of employing is less expensive, is easy to large area preparation, and the method is particularly useful for encapsulating flexible organic electroluminescent device.
The invention provides a kind of organic electroluminescence device and preparation method thereof and there is following beneficial effect:
(1) encapsulated layer of organic electroluminescence device of the present invention comprises inorganic barrier layer and the inorganic barrier layer of alternative stacked setting, encapsulation layer structure is fine and close, blocking capability is strong, thus effectively block extraneous steam and oxygen to the erosion of organic electroluminescence device, improve the life-span of organic electroluminescence device;
(2) water resistance (WVTR) of organic electroluminescence device of the present invention reaches 10
-4g/m
2day, the life-span reaches more than 3500 hours (T70@1000cd/m
2: namely starting brightness is 1000cd/m
2, brightness decay is to 70% time used);
(3) preparation method of the present invention is applicable to the organic electroluminescence device that preparation take electro-conductive glass as anode substrate, is also applicable to prepare the flexible organic electroluminescent device being anode substrate with plastics or metal; And preparation method's technique is simple, easy large area preparation, is suitable for industrialization and uses on a large scale.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) ito glass substrate is got, carry out acetone cleaning, ethanol purge, washed with de-ionized water, ethanol purge successively, all clean with supersonic wave cleaning machine, individual event washing cleaning 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then carries out surface activation process to the ito glass substrate after cleaning, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
(2) adopt the mode of vacuum evaporation in clean drying and ito glass substrate after surface activation process prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, wherein:
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3, MoO
3doping mass fraction be 30%, vacuum degree during evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 10nm;
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA), the vacuum degree 3 × 10 during evaporation
-5pa, evaporation rate is
evaporation thickness is 30nm;
The material of luminescent layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI) and is entrained in three in TPBI (2-phenylpyridine) and closes iridium (Ir (ppy)
3), Ir (ppy)
3doping mass fraction be 5%; Vacuum degree during vacuum evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), the vacuum degree 3 × 10 during vacuum evaporation
-5pa, evaporation rate is
evaporation thickness is 10nm;
The CsN that the material of electron injecting layer comprises 4,7-diphenyl-1,10-phenanthroline (Bphen) and is entrained in Bphen
3, CsN
3doping mass fraction be 30%, vacuum degree during vacuum evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
The material of metallic cathode is metallic aluminium (Al), and evaporation thickness is 100nm, and vacuum degree during vacuum evaporation is 3 × 10
-5pa, evaporation rate is
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 250nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is CuPc, and the vacuum degree of preparation process is 1 × 10
-3pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 120nm again, the material of inorganic barrier layer is Ag and ReO
3the composite material formed, mass fraction shared by Al is 15%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-3pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 4 layers.
Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains.As shown in Figure 1, the present embodiment organic electroluminescence device, comprises ito glass substrate 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, metallic cathode 7 and encapsulated layer 8 successively.Encapsulated layer 8 comprises the inorganic barrier layer 81,83,85,87 that four layers of thickness in monolayer are 250nm successively, and four layers of thickness in monolayer are the inorganic barrier layer 82,84,86,88 of 120nm.
Adopt water vapour permeability tester to measure the water vapour permeability of this organic electroluminescence device, record water vapour permeability (WVTR, the g/m of this organic electroluminescence device
2day) be 8.8 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under test this organic electroluminescence device life-span be 3500 hours.
Embodiment 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on ito glass substrate, prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, preparation method is with embodiment one;
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 250nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is NPB, and the vacuum degree of preparation process is 5 × 10
-5pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 150nm again, the material of inorganic barrier layer comprises Al and CrO
3, mass fraction shared by Al is 30%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-5pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 6 layers.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 6.9 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under life-span of testing be 3644 hours.
Embodiment 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on ito glass substrate, prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, preparation method is with embodiment one;
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 200nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is Alq3, and the vacuum degree of preparation process is 5 × 10
-5pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 100nm again, the material of inorganic barrier layer comprises In and MoO
3, mass fraction shared by In is 10%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-5pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 6 layers.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 7.3 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under life-span of testing be 3612 hours.
Embodiment 4
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on ito glass substrate, prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, preparation method is with embodiment one;
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 250nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is m-MTDATA, and the vacuum degree of preparation process is 5 × 10
-5pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 120nm again, the material of inorganic barrier layer comprises Au and MnO
2, mass fraction shared by Au is 20%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-4pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 5 layers.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 7.8 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under life-span of testing be 3574 hours.
Embodiment 5
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on ito glass substrate, prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, preparation method is with embodiment one;
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 250nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is BCP, and the vacuum degree of preparation process is 5 × 10
-5pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 130nm again, the material of inorganic barrier layer comprises Ni and ReO
2, mass fraction shared by Ni is 15%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-4pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 5 layers.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 8.2 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under life-span of testing be 3540 hours.
Embodiment 6
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on ito glass substrate, prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, preparation method is with embodiment one;
(3) on negative electrode, prepare encapsulated layer, obtain organic electroluminescence device, wherein, encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows:
Be the inorganic barrier layer of 300nm by the mode of vacuum evaporation at cathode surface deposit thickness, material is CuPc, and the vacuum degree of preparation process is 1 × 10
-5pa, evaporation rate is
Adopt the mode of vacuum evaporation to prepare on inorganic barrier layer surface the inorganic barrier layer that thickness is 150nm again, the material of inorganic barrier layer comprises Cu and WO
3, mass fraction shared by Cu is 20%; In Vacuum Evaporation Process, vacuum degree is 1 × 10
-5pa, evaporation rate is
In the present embodiment, inorganic barrier layer and inorganic barrier layer replace preparation 6 layers.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 6.4 × 10
-4g/m
2day, at T70@1000cd/m
2luminescent condition under life-span of testing be 3673 hours.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. an organic electroluminescence device, comprise the anode conducting substrate stacked gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode and encapsulated layer, it is characterized in that, described encapsulated layer comprises the inorganic barrier layer and inorganic barrier layer that are cascading, the material of described inorganic barrier layer comprises CuPc, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, 4'-diamines, oxine aluminium, 4, 4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine and 4, 7-diphenyl-1, at least one in 10-Phen,
The material of described inorganic barrier layer comprises metal simple-substance and metal oxide, and mass fraction shared by described metal simple-substance is 10 ~ 30%, and described metal simple-substance is one or more in copper, aluminium, indium, gold, nickel and silver; Described metal oxide is one or more in tungsten oxide, chromium oxide, molybdenum oxide, manganese dioxide, rhenium dioxide and rhenium trioxide.
2. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness of described inorganic barrier layer is 200nm ~ 300nm.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness of described inorganic barrier layer is 100nm ~ 150nm.
4. organic electroluminescence device as claimed in claim 1, it is characterized in that, described inorganic barrier layer and inorganic barrier layer are arranged alternately 4 ~ 6 layers successively.
5. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described hole injection layer comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines and be entrained in described N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1, MoO in 1'-biphenyl-4,4'-diamines
3, described MoO
3doping mass fraction be 30%; The material of described hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine; The material of described luminescent layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene and be entrained in described 1,3, three (2-phenylpyridines) in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene close iridium, and the doping mass fraction that described three (2-phenylpyridines) close iridium is 5%; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline; The material of described electron injecting layer comprises 4,7-diphenyl-1,10-phenanthroline and is entrained in the CsN in described 4,7-diphenyl-1,10-phenanthrolines
3, described CsN
3doping mass fraction be 30%.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
(1) provide clean anode electrically-conductive backing plate, on anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared in vacuum evaporation successively;
(2) prepare encapsulated layer on the cathode, obtain organic electroluminescence device; Wherein, described encapsulated layer comprises inorganic barrier layer and inorganic barrier layer, and concrete preparation method is as follows: adopt the mode of vacuum evaporation to deposit inorganic barrier layer and inorganic barrier layer successively at described cathode surface, the vacuum degree in Vacuum Evaporation Process is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
The material of described inorganic barrier layer comprises CuPc, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine and 4, at least one in 7-diphenyl-1,10-Phen;
The material of described inorganic barrier layer comprises metal simple-substance and metal oxide, and mass fraction shared by described metal simple-substance is 10 ~ 30%, and described metal simple-substance is one or more in copper, aluminium, indium, gold, nickel and silver; Described metal oxide is one or more in tungsten oxide, chromium oxide, molybdenum oxide, manganese dioxide, rhenium dioxide and rhenium trioxide.
7. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the thickness of described inorganic barrier layer is 200nm ~ 300nm.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the thickness of described inorganic barrier layer is 100nm ~ 150nm.
9. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, described inorganic barrier layer and inorganic barrier layer are arranged alternately 4 ~ 6 layers successively.
10. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the material of described hole injection layer comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines and be entrained in described N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1, MoO in 1'-biphenyl-4,4'-diamines
3, described MoO
3doping mass fraction be 30%; The material of described hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine; The material of described luminescent layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene and be entrained in described 1,3, three (2-phenylpyridines) in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene close iridium, and the doping mass fraction that described three (2-phenylpyridines) close iridium is 5%; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline; The material of described electron injecting layer comprises 4,7-diphenyl-1,10-phenanthroline and is entrained in the CsN in described 4,7-diphenyl-1,10-phenanthrolines
3, described CsN
3doping mass fraction be 30%.
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| CN109950424B (en) * | 2019-04-26 | 2020-05-05 | 上海大学 | A kind of OLED thin film encapsulation layer and preparation method thereof |
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