CN104124378A - Organic electroluminescent device and preparation method thereof - Google Patents
Organic electroluminescent device and preparation method thereof Download PDFInfo
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- CN104124378A CN104124378A CN201310145189.9A CN201310145189A CN104124378A CN 104124378 A CN104124378 A CN 104124378A CN 201310145189 A CN201310145189 A CN 201310145189A CN 104124378 A CN104124378 A CN 104124378A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 93
- 238000002347 injection Methods 0.000 claims abstract description 40
- 239000007924 injection Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000005401 electroluminescence Methods 0.000 claims description 49
- 239000011521 glass Substances 0.000 claims description 36
- 230000005540 biological transmission Effects 0.000 claims description 35
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 33
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 25
- 238000001704 evaporation Methods 0.000 claims description 21
- 230000008020 evaporation Effects 0.000 claims description 21
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 claims description 18
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 16
- 238000005566 electron beam evaporation Methods 0.000 claims description 15
- 238000007747 plating Methods 0.000 claims description 15
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical group O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- DHDHJYNTEFLIHY-UHFFFAOYSA-N 4,7-diphenyl-1,10-phenanthroline Chemical compound C1=CC=CC=C1C1=CC=NC2=C1C=CC1=C(C=3C=CC=CC=3)C=CN=C21 DHDHJYNTEFLIHY-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- MQCHTHJRANYSEJ-UHFFFAOYSA-N n-[(2-chlorophenyl)methyl]-1-(3-methylphenyl)benzimidazole-5-carboxamide Chemical compound CC1=CC=CC(N2C3=CC=C(C=C3N=C2)C(=O)NCC=2C(=CC=CC=2)Cl)=C1 MQCHTHJRANYSEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical class C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 6
- 239000000075 oxide glass Substances 0.000 claims description 6
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims description 4
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Natural products C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004305 biphenyl Substances 0.000 claims description 4
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 4
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical group [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 4
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- QWODREODAXFISP-UHFFFAOYSA-N n-[4-(4-anilinophenyl)phenyl]-n-phenylnaphthalen-1-amine Chemical compound C=1C=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=CC=1NC1=CC=CC=C1 QWODREODAXFISP-UHFFFAOYSA-N 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 4
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 4
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract 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 10
- 101000837344 Homo sapiens T-cell leukemia translocation-altered gene protein Proteins 0.000 description 10
- 102100028692 T-cell leukemia translocation-altered gene protein Human genes 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000003599 detergent Substances 0.000 description 6
- 229910000765 intermetallic Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000011368 organic material Substances 0.000 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910052774 Proactinium Inorganic materials 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
- HXWWMGJBPGRWRS-CMDGGOBGSA-N 4- -2-tert-butyl-6- -4h-pyran Chemical compound O1C(C(C)(C)C)=CC(=C(C#N)C#N)C=C1\C=C\C1=CC(C(CCN2CCC3(C)C)(C)C)=C2C3=C1 HXWWMGJBPGRWRS-CMDGGOBGSA-N 0.000 description 4
- ZOKIJILZFXPFTO-UHFFFAOYSA-N 4-methyl-n-[4-[1-[4-(4-methyl-n-(4-methylphenyl)anilino)phenyl]cyclohexyl]phenyl]-n-(4-methylphenyl)aniline Chemical compound C1=CC(C)=CC=C1N(C=1C=CC(=CC=1)C1(CCCCC1)C=1C=CC(=CC=1)N(C=1C=CC(C)=CC=1)C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 ZOKIJILZFXPFTO-UHFFFAOYSA-N 0.000 description 4
- RAPHUPWIHDYTKU-WXUKJITCSA-N 9-ethyl-3-[(e)-2-[4-[4-[(e)-2-(9-ethylcarbazol-3-yl)ethenyl]phenyl]phenyl]ethenyl]carbazole Chemical compound C1=CC=C2C3=CC(/C=C/C4=CC=C(C=C4)C4=CC=C(C=C4)/C=C/C=4C=C5C6=CC=CC=C6N(C5=CC=4)CC)=CC=C3N(CC)C2=C1 RAPHUPWIHDYTKU-WXUKJITCSA-N 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010893 electron trap Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- SNTWKPAKVQFCCF-UHFFFAOYSA-N 2,3-dihydro-1h-triazole Chemical class N1NC=CN1 SNTWKPAKVQFCCF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000004776 molecular orbital Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/805—Electrodes
- H10K50/82—Cathodes
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention discloses an organic electroluminescent device comprising a conductive anode substrate, a hole injection layer, a hole transporting layer, a light emitting layer, an electron transporting layer, an electron injection layer and a cathode composite layer which are stacked in sequence. The cathode composite layer is made of a mixture mixed by a silicon compound, metal having a low work function and electron transporting material according to a mass ratio of 0.01:1:2 to 0.1:1.5:3. The cathode composite layer of the organic electroluminescent device is made of a mixture mixed by a silicon compound, metal having a low work function and electron transporting material. Particles of the silicon compound are very large and in the shape of microspheres, so that microspherical structures arranged in sequence are formed in a film layer, and light encountering the shape of microspheres would be scattered so that light transmitted from two sides can be scattered back to the center of the device. Compared with a conventional organic electroluminescent device, the organic electroluminescent device is higher in light emitting efficiency. The invention further discloses a preparation method of the organic electroluminescent device.
Description
Technical field
The present invention relates to organic electroluminescent field, relate in particular to a kind of organic electroluminescence device and preparation method thereof.
Background technology
1987, the C.W.Tang of Eastman Kodak company of the U.S. and VanSlyke reported the breakthrough in organic electroluminescent research.Utilize ultrathin film technology to prepare high brightness, high efficiency double-deck organic electroluminescence device (OLED).In this double-deck device, under 10V, brightness reaches 1000cd/m2, and its luminous efficiency is 1.51lm/W, life-span to be greater than 100 hours.
The principle of luminosity of OLED is based under the effect of extra electric field, and electronics is injected into organic lowest unocccupied molecular orbital (LUMO) from negative electrode, and hole is injected into organic highest occupied molecular orbital (HOMO) from conductive anode substrate.Electronics and hole meet at luminescent layer, compound, form exciton, exciton moves under electric field action, and energy is passed to luminescent material, and excitation electron is from ground state transition to excitation state, excited energy, by Radiation-induced deactivation, produces photon, discharges luminous energy.
In traditional organic electroluminescence device, the light of device inside only has 18% left and right can be transmitted into outside to go, and other part can consume in device outside with other forms, (as the specific refractivity between glass and ITO, glass refraction is 1.5 between interface, refractive index poor, ITO is 1.8, light arrives glass from ITO, and total reflection will occur), cause the loss of total reflection, thereby cause overall bright dipping lower, thereby cause the luminous efficiency of device lower.
Summary of the invention
Based on this, be necessary the organic electroluminescence device that provides a kind of luminous efficiency higher.
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually;
The material of described cathode composite layer is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, and wherein, described low workfunction metal is that work function is-metal of 2.0eV～-3.5eV.
In one embodiment, described silicon compound is silicon monoxide, silicon dioxide or sodium metasilicate;
Described low workfunction metal is magnesium, strontium, calcium or ytterbium;
Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or N-aryl benzimidazole.
In one embodiment, the thickness of described cathode composite layer is 100nm～400nm.
In one embodiment, described conductive anode substrate is indium tin oxide glass, aluminium zinc oxide glass or indium-zinc oxide glass, and the thickness of the conductive layer of described anode conducting substrate is 80nm～150nm.
In one embodiment, the material of described hole injection layer is molybdenum trioxide, tungstic acid or vanadic oxide, and the thickness of described hole injection layer is 20nm～80nm.
In one embodiment, the material of described hole transmission layer is 1,1-, bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4''-tri-(carbazole-9-yl) triphenylamine or N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine; The thickness of described hole transmission layer is 20nm～60nm.
In one embodiment, the material of described luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, 9,10-bis--β-naphthylene anthracene, 4, two (the 9-ethyl-3-carbazole vinyl)-1 of 4'-, 1'-biphenyl or oxine aluminium, the thickness of described luminescent layer is 5nm～40nm.
In one embodiment, the material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 1,2, and 4-triazole derivative or N-aryl benzimidazole, the thickness of described electron transfer layer is 40nm～300nm.
In one embodiment, the material of described electron injecting layer is cesium carbonate, cesium fluoride, nitrine caesium or lithium fluoride, and the thickness of described electron injecting layer is 0.5nm～10nm.
A preparation method for organic electroluminescence device, comprises the steps:
Conductive anode substrate is carried out to surface preparation;
In described conductive anode substrate, evaporation forms hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
On described electron injecting layer, electron beam evaporation plating forms negative electrode, obtain described organic electroluminescence device, wherein, the material of described cathode composite layer is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, described low workfunction metal is that work function is-metal of 2.0eV～-3.5eV, and the energy density of described electron beam evaporation plating is 10W/cm
2～l00W/cm
2.
The material of the cathode composite layer of this organic electroluminescence device is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, wherein, silicon compound particle is larger, be microspheroidal, thereby make inner formation of rete arrange orderly micro-sphere structure, thereby light is encountered this microspheroidal and can be formed scattering and make to get back in the middle of device to the light scattering of both sides transmittings, with respect to traditional organic electroluminescence device, luminous efficiency is higher.
Brief description of the drawings
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is the preparation method's of the organic electroluminescence device of an execution mode flow chart;
Fig. 3 is the current density of organic electroluminescence device and the graph of a relation of current efficiency that embodiment 1 and comparative example prepare.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details are set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, and therefore the present invention is not subject to the restriction of following public concrete enforcement.
The organic electroluminescence device of an execution mode as shown in Figure 1, is characterized in that, comprises conductive anode substrate 10, hole injection layer 20, hole transmission layer 30, luminescent layer 40, electron transfer layer 50, electron injecting layer 60 and cathode composite layer 70.
Conductive anode substrate 10 can be indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).At one, preferably in embodiment, conductive anode substrate 10 is indium tin oxide glass (ITO).
The thickness of the conductive layer of anode conducting substrate 10 can be 80nm～150nm.
The material of hole injection layer 20 can be molybdenum trioxide (MoO
3), tungstic acid (WO
3) or vanadic oxide (V
2o
5).The thickness of hole injection layer 20 can be 20nm～80nm.At one, preferably in embodiment, the material of hole injection layer 20 is molybdenum trioxide (MoO
3), the thickness of hole injection layer 20 is 25nm.
The material of hole transmission layer 30 can be 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-(1-naphthyl)-N, N'-diphenyl-4,4'-benzidine (NPB).The thickness of hole transmission layer 30 can be 20nm～60nm.At one, preferably in embodiment, the material of hole transmission layer 30 is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA), and the thickness of hole transmission layer 30 is 35nm.
The material of luminescent layer 40 can be 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis--β-naphthylene anthracene (ADN), 4, two (the 9-ethyl-3-carbazole vinyl)-1 of 4'-, 1'-biphenyl (BCzVBi) or oxine aluminium (Alq
3).The thickness of luminescent layer 40 can be 5nm～40nm.At one, preferably in embodiment, the material of luminescent layer 40 is oxine aluminium (Alq
3), the thickness of luminescent layer 40 is 20nm.
The material of electron transfer layer 50 can be electron transport material.The thickness of electron transfer layer 50 can be 40nm～300nm.Electric transmission layer material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (TAZ) or N-aryl benzimidazole (TPBI).At one, preferably in embodiment, the material of electron transfer layer 50 is TAZ, and the thickness of electron transfer layer 50 is 200nm.
The material of electron injecting layer 60 can be cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) or lithium fluoride (LiF).The thickness of electron injecting layer 60 can be 0.5nm～10nm.At one, preferably in embodiment, the material of electron injecting layer 60 is LiF, and the thickness of electron injecting layer 60 is 0.7nm.
The material of cathode composite layer 70 is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio.Wherein, low workfunction metal is that work function is-metal of 2.0eV～-3.5eV.The thickness of cathode composite layer 70 is 100nm～400nm.
Silicon compound can be silicon monoxide (SiO), silicon dioxide (SiO
2) or sodium metasilicate (Na
2siO
3).
Low workfunction metal can be magnesium (Mg), strontium (Sr), calcium (Ca) or ytterbium (Yb).
Electron transport material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (TAZ) or N-aryl benzimidazole (TPBI).
The material of the cathode composite layer 70 of this organic electroluminescence device is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, wherein, silicon compound particle is larger, be microspheroidal, thereby make inner formation of rete arrange orderly micro-sphere structure, thereby light is encountered this microspheroidal and can be formed scattering and make to get back in the middle of device to the light scattering of both sides transmittings, with respect to traditional organic electroluminescence device, luminous efficiency is higher.
In addition, silicon compound is more stable in air, can improve the stability of low workfunction metal after doping.Low workfunction metal is conducive to reduce the injection barrier of electronics, can improve electron injection efficiency.Electron transport material can improve the electron density of cathode composite layer 70, thereby improves carrier transport speed, and meanwhile, electron transport material can also improve the evenness of film, and smooth surface reduces the existence of inner electron trap, thereby improves luminous efficiency.
The preparation method of above-mentioned organic electroluminescence device as shown in Figure 2, comprises the steps:
S10, conductive anode substrate 10 is carried out to surface preparation.
Conductive anode substrate 10 can be indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).At one, preferably in embodiment, conductive anode substrate 10 is indium tin oxide glass (ITO).
The thickness of the conductive layer of anode conducting substrate 10 can be 80nm～150nm.
The operation of surface preparation can be: first conductive anode substrate 10 is carried out to photoetching treatment, be cut into needed size, with liquid detergent, deionized water, acetone, ethanol and isopropyl alcohol ultrasonic cleaning 15min respectively, remove the organic pollution on conductive anode substrate 10 surfaces successively.
S20, in conductive anode substrate 10, evaporation forms hole injection layer 20, hole transmission layer 30, luminescent layer 40, electron transfer layer 50 and electron injecting layer 60 successively.
In evaporate process, operating pressure is 2 × 10
-3～5 × 10
-5pa, the evaporation speed of organic material is 0.1～1nm/s, the evaporation speed of metal and metallic compound is 1～10nm/s.
The material of hole injection layer 20 can be molybdenum trioxide (MoO
3), tungstic acid (WO
3) or vanadic oxide (V
2o
5).The thickness of hole injection layer 20 can be 20nm～80nm.At one, preferably in embodiment, the material of hole injection layer 20 is molybdenum trioxide (MoO
3), the thickness of hole injection layer 20 is 25nm.
The material of hole transmission layer 30 can be 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-(1-naphthyl)-N, N'-diphenyl-4,4'-benzidine (NPB).The thickness of hole transmission layer 30 can be 20nm～60nm.At one, preferably in embodiment, the material of hole transmission layer 30 is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA), and the thickness of hole transmission layer 30 is 35nm.
The material of luminescent layer 40 can be 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis--β-naphthylene anthracene (ADN), 4, two (the 9-ethyl-3-carbazole vinyl)-1 of 4'-, 1'-biphenyl (BCzVBi) or oxine aluminium (Alq
3).The thickness of luminescent layer 40 can be 5nm～40nm.At one, preferably in embodiment, the material of luminescent layer 40 is oxine aluminium (Alq
3), the thickness of luminescent layer 40 is 20nm.
The material of electron transfer layer 50 can be electron transport material.The thickness of electron transfer layer 50 can be 40nm～300nm.Electric transmission layer material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (TAZ) or N-aryl benzimidazole (TPBI).At one, preferably in embodiment, the material of electron transfer layer 50 is TAZ, and the thickness of electron transfer layer 50 is 200nm.
The material of electron injecting layer 60 can be cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) or lithium fluoride (LiF).The thickness of electron injecting layer 60 can be 0.5nm～10nm.At one, preferably in embodiment, the material of electron injecting layer 60 is LiF, and the thickness of electron injecting layer 60 is 0.7nm.
S30, on electron injecting layer 60 electron beam evaporation plating form cathode composite layer 70, obtain organic electroluminescence device.
In electron beam evaporation plating process, operating pressure is 2 × 10
-3～5 × 10
-5pa.The energy density of electron beam evaporation plating is 10W/cm
2～l00W/cm
2.
The material of cathode composite layer 70 is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio.Wherein, low workfunction metal is that work function is-metal of 2.0eV～-3.5eV.The thickness of cathode composite layer 70 is 100nm～400nm.
Silicon compound can be silicon monoxide (SiO), silicon dioxide (SiO
2) or sodium metasilicate (Na2SiO
3).
Low workfunction metal can be magnesium (Mg), strontium (Sr), calcium (Ca) or ytterbium (Yb).
Electron transport material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (TAZ) or N-aryl benzimidazole (TPBI).
The material of the cathode composite layer 70 of the organic electroluminescence device that the preparation method of this organic electroluminescence device prepares is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, wherein, silicon compound particle is larger, be microspheroidal, thereby make inner formation of rete arrange orderly micro-sphere structure, thereby light is encountered this microspheroidal and can be formed scattering and make to get back in the middle of device to the light scattering of both sides transmittings, with respect to traditional organic electroluminescence device, luminous efficiency is higher.
In addition, silicon compound is more stable in air, can improve the stability of low workfunction metal after doping.Low workfunction metal is conducive to reduce the injection barrier of electronics, can improve electron injection efficiency.Electron transport material can improve the electron density of cathode composite layer 70 inside, thereby improves carrier transport speed, and meanwhile, electron transport material can also improve the evenness of film, and smooth surface reduces the existence of inner electron trap, thereby improves luminous efficiency.
Be below specific embodiment and comparative example part, the test and the Preparation equipment that in embodiment, use comprise: the high vacuum coating system (evaporation) of scientific instrument development center, Shenyang Co., Ltd, the USB4000 fiber spectrometer (testing electroluminescent spectrum) of U.S. marine optics Ocean Optics, the Keithley2400(test electric property of Keithley company of the U.S.), the CS-100A colorimeter (test brightness and colourity) of Japanese Konica Minolta company.
In specific embodiment and comparative example part, "/" represents stacked, and ": " represents the mass ratio of the former with the latter.
Embodiment 1
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually, and concrete structure is expressed as: ito glass/MoO
3/ TCTA/Alq
3/ TAZ/LiF/SiO
2: Mg:Bphen(0.03:1.2:2).Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and with liquid detergent and deionized water, ito glass is carried out to ultrasonic cleaning 15min successively, removes the organic pollution of glass surface.
Be 8 × 10 in operating pressure
-5under the condition of Pa, be 0.2nm/s according to the evaporation speed of organic material, the evaporation speed of metal and metallic compound is 3nm/s, and on ito glass, evaporation is prepared hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively.The material of hole injection layer is MoO
3, thickness is 25nm.The material of hole transmission layer is TCTA, and thickness is 35nm.The material of luminescent layer is Alq
3, thickness is 20nm.The material of electron transfer layer is TAZ, and thickness is 200nm.The material of electron injecting layer is LiF, and thickness is 0.7nm.
Then be 50W/cm in the energy density of electron beam evaporation plating
2condition under, on electron injecting layer, electron beam evaporation plating is prepared cathode composite layer, obtains needed organic electroluminescence device.The material of cathode composite layer is SiO
2, Mg and Bphen be that the mixture that 0.03:1.2:2 is mixed to get (can be expressed as: SiO according to mass ratio
2: Mg:Bphen), thickness is 200nm.
Embodiment 2
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually, and concrete structure is expressed as: AZO glass/WO
3/ TCTA/ADN/Bphen/CsF/SiO:Sr:TAZ(0.01:1:2).Preparation process is:
It is the AZO glass of 80nm that conductive layer thickness is provided, and with liquid detergent and deionized water, AZO glass is carried out to ultrasonic cleaning 15min successively, removes the organic pollution of glass surface.
Be 2 × 10 in operating pressure
-3under the condition of Pa, be 0.1nm/s according to the evaporation speed of organic material, the evaporation speed of metal and metallic compound is 10nm/s, prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer at AZO evaporation successively on glass.The material of hole injection layer is WO
3, thickness is 80nm.The material of hole transmission layer is TCTA, and thickness is 60nm.The material of luminescent layer is ADN, and thickness is 5nm.The material of electron transfer layer is Bphen, and thickness is 200nm.The material of electron injecting layer is CsF, and thickness is 10nm.
Then be 10W/cm in the energy density of electron beam evaporation plating
2condition under, on electron injecting layer, electron beam evaporation plating is prepared cathode composite layer, obtains needed organic electroluminescence device.The material of cathode composite layer is that SiO, Sr and TAZ are the mixture (can be expressed as: SiO:Sr:TAZ) that 0.01:1:2 is mixed to get according to mass ratio, and thickness is 100nm.
Embodiment 3
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually, and concrete structure is expressed as: IZO glass/V
2o
5/ TAPC/BCzVBi/TAZ/Cs
2cO
3/ Na
2siO
3: Ca:TPBi(0.1:1.5:3).Preparation process is:
It is the IZO glass of 120nm that conductive layer thickness is provided, and with liquid detergent and deionized water, IZO glass is carried out to ultrasonic cleaning 15min successively, removes the organic pollution of glass surface.
Be 5 × 10 in operating pressure
-5under the condition of Pa, be 1nm/s according to the evaporation speed of organic material, the evaporation speed of metal and metallic compound is 1nm/s, prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer at IZO evaporation successively on glass.The material of hole injection layer is V
2o
5, thickness is 20nm.The material of hole transmission layer is TAPC, and thickness is 30nm.The material of luminescent layer is BCzVBi, and thickness is 40nm.The material of electron transfer layer is TAZ, and thickness is 60nm.The material of electron injecting layer is Cs
2cO
3, thickness is 0.5nm.
Then be 100W/cm in the energy density of electron beam evaporation plating
2condition under, on electron injecting layer, electron beam evaporation plating is prepared cathode composite layer, obtains needed organic electroluminescence device.The material of cathode composite layer is Na
2siO
3, Ca and TPBi be that the mixture that 0.1:1.5:3 is mixed to get (can be expressed as: Na according to mass ratio
2siO
3: Ca:TPBi), thickness is 400nm.
Embodiment 4
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually, and concrete structure is expressed as: IZO glass/MoO
3/ NPB/DCJTB/TPBi/CsN
3/ SiO
2: Yb:TAZ(0.05:1.3:2.5).Preparation process is:
It is the IZO glass of 150nm that conductive layer thickness is provided, and with liquid detergent and deionized water, IZO glass is carried out to ultrasonic cleaning 15min successively, removes the organic pollution of glass surface.
Be 5 × 10 in operating pressure
-4under the condition of Pa, be 0.2nm/s according to the evaporation speed of organic material, the evaporation speed of metal and metallic compound is 5nm/s, prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer at IZO evaporation successively on glass.The material of hole injection layer is MoO
3, thickness is 30nm.The material of hole transmission layer is NPB, and thickness is 50nm.The material of luminescent layer is DCJTB, and thickness is 5nm.The material of electron transfer layer is TPBi, and thickness is 40nm.The material of electron injecting layer is CsN
3, thickness is 1nm.
Then be 30W/cm in the energy density of electron beam evaporation plating
2condition under, on electron injecting layer, electron beam evaporation plating is prepared cathode composite layer, obtains needed organic electroluminescence device.The material of cathode composite layer is SiO
2, Yb and TAZ be that the mixture that 0.05:1.3:2.5 is mixed to get (can be expressed as: SiO according to mass ratio
2: Yb:TAZ), thickness is 150nm.
Comparative example
A kind of organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, and concrete structure is expressed as: ito glass/MoO
3/ TCTA/Alq
3/ TAZ/Li/Ag.Preparation process is
It is the ito glass of 100nm that conductive layer thickness is provided, and with liquid detergent and deionized water, ito glass is carried out to ultrasonic cleaning 15min successively, removes the organic pollution of glass surface.
Be 8 × 10 in operating pressure
-5under the condition of Pa, be 0.2nm/s according to the evaporation speed of organic material, the evaporation speed of metal and metallic compound is 3nm/s, and on ito glass, evaporation is prepared hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively.The material of hole injection layer is MoO
3, thickness is 25nm.The material of hole transmission layer is TCTA, and thickness is 35nm.The material of luminescent layer is Alq
3, thickness is 20nm.The material of electron transfer layer is TAZ, and thickness is 200nm.The material of electron injecting layer is LiF, and thickness is 0.7nm.The materials A g of negative electrode, thickness is 200nm.
Fig. 3 is the current density of organic electroluminescence device and the graph of a relation of current efficiency that embodiment 1 and comparative example prepare, and curve 1 shows the current density of organic electroluminescence device and the relation of current efficiency prepared by embodiment 1; The current density of organic electroluminescence device and the relation of current efficiency of curve 2 display comparison example preparations.As can be seen from Figure 3, under different current densities, the organic electroluminescence device that the current efficiency of the organic electroluminescence device that embodiment 1 prepares all prepares than comparative example large, the maximum current efficiency of embodiment 1 is 6.94cd/A, and that comparative example is only 4.78cd/A.
The cathode composite layer of the organic electroluminescence device that embodiment 1 prepares makes to get back in the middle of organic electroluminescence device to the light scattering of both sides transmitting, improve light extraction efficiency, improve electron injection efficiency, improve carrier transport speed, reduce the existence of inner electron trap, cathode composite layer can effectively improve the luminous efficiency of organic electroluminescence device.
Above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an organic electroluminescence device, is characterized in that, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode composite layer that stack gradually;
The material of described cathode composite layer is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, and wherein, described low workfunction metal is that work function is-metal of 2.0eV～-3.5eV.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, described silicon compound is silicon monoxide, silicon dioxide or sodium metasilicate;
Described low workfunction metal is magnesium, strontium, calcium or ytterbium;
Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or N-aryl benzimidazole.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described cathode composite layer is 100nm～400nm.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, described conductive anode substrate is indium tin oxide glass, aluminium zinc oxide glass or indium-zinc oxide glass, and the thickness of the conductive layer of described anode conducting substrate is 80nm～150nm.
5. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described hole injection layer is molybdenum trioxide, tungstic acid or vanadic oxide, and the thickness of described hole injection layer is 20nm～80nm.
6. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4''-tri-(carbazole-9-yl) triphenylamine or N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine; The thickness of described hole transmission layer is 20nm～60nm.
7. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, 9,10-bis--β-naphthylene anthracene, 4, two (the 9-ethyl-3-carbazole vinyl)-1 of 4'-, 1'-biphenyl or oxine aluminium, the thickness of described luminescent layer is 5nm～40nm.
8. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or N-aryl benzimidazole, the thickness of described electron transfer layer is 40nm～300nm.
9. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described electron injecting layer is cesium carbonate, cesium fluoride, nitrine caesium or lithium fluoride, and the thickness of described electron injecting layer is 0.5nm～10nm.
10. a preparation method for organic electroluminescence device, is characterized in that, comprises the steps:
Conductive anode substrate is carried out to surface preparation;
In described conductive anode substrate, evaporation forms hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
On described electron injecting layer, electron beam evaporation plating forms cathode composite layer, obtain described organic electroluminescence device, wherein, the material of described cathode composite layer is that silicon compound, low workfunction metal and electron transport material are the mixture that 0.01:1:2～0.1:1.5:3 is mixed to get according to mass ratio, described low workfunction metal is that work function is-metal of 2.0eV～-3.5eV, and the energy density of described electron beam evaporation plating is 10W/cm
2～l00W/cm
2.
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| WO2018120327A1 (en) * | 2016-12-26 | 2018-07-05 | 深圳市华星光电技术有限公司 | Organic light-emitting device, and organic light-emitting display |
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