CN104009176A - Organic electroluminescent device and preparation method - Google Patents
Organic electroluminescent device and preparation method Download PDFInfo
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- CN104009176A CN104009176A CN201310059562.9A CN201310059562A CN104009176A CN 104009176 A CN104009176 A CN 104009176A CN 201310059562 A CN201310059562 A CN 201310059562A CN 104009176 A CN104009176 A CN 104009176A
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- titanium dioxide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 165
- 239000000463 material Substances 0.000 claims abstract description 52
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 45
- 229910000311 lanthanide oxide Inorganic materials 0.000 claims abstract description 37
- 239000011521 glass Substances 0.000 claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 229910001954 samarium oxide Inorganic materials 0.000 claims abstract description 10
- 229940075630 samarium oxide Drugs 0.000 claims abstract description 10
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 10
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims description 41
- 230000008020 evaporation Effects 0.000 claims description 41
- 238000005401 electroluminescence Methods 0.000 claims description 40
- 230000005540 biological transmission Effects 0.000 claims description 20
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 20
- 238000010894 electron beam technology Methods 0.000 claims description 16
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 14
- CIEHQLJGGPHJPU-UHFFFAOYSA-N [Pr+3].[O-2].[O-2].[Ti+4] Chemical compound [Pr+3].[O-2].[O-2].[Ti+4] CIEHQLJGGPHJPU-UHFFFAOYSA-N 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 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
- -1 anode Substances 0.000 claims description 5
- SNTWKPAKVQFCCF-UHFFFAOYSA-N 2,3-dihydro-1h-triazole Chemical class N1NC=CN1 SNTWKPAKVQFCCF-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
- 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 4
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 4
- 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 3
- 230000001133 acceleration Effects 0.000 claims description 3
- ZVADOHBJTZCNEM-UHFFFAOYSA-N [O-2].[O-2].[Pr+4] Chemical compound [O-2].[O-2].[Pr+4] ZVADOHBJTZCNEM-UHFFFAOYSA-N 0.000 abstract 1
- 230000005525 hole transport Effects 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 abstract 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 116
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 18
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 10
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- 238000004770 highest occupied molecular orbital Methods 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000010931 gold Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 238000011010 flushing procedure Methods 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
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000010405 anode material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000011368 organic material Substances 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 239000012044 organic layer Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 238000005036 potential barrier Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 2
- 229910000024 caesium carbonate 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
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 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 2
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000004776 molecular orbital Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 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
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
An organic electroluminescent device comprises a glass substrate, an anode, a hole scattering layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a cathode which are successively laminated. Materials of the hole scattering layer contain a lanthanide oxide and titanium dioxide doped in the lanthanide oxide. Mass of titanium dioxide accounts for 10wt%-30wt% of mass of the lanthanide oxide. The lanthanide oxide is selected from at least one of praseodymium dioxide, praseodymium oxide, ytterbium trioxide and samarium oxide. Luminous efficiency of the above organic electroluminescent device is high. The invention also provides a preparation method of the organic electroluminescent device.
Description
Technical field
The present invention relates to a kind of organic electroluminescence device and preparation method thereof.
Background technology
The principle of luminosity of organic electroluminescence device 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 anode.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 luminescent device, the light of device inside only has 18% left and right can be transmitted into outside to go, and other part can consume at device outside with other forms, (as the specific refractivity between glass and ITO, glass refraction is that 1.5, ITO is 1.8 between interface, refractive index poor, light arrives glass from ITO, will there is total reflection), caused the loss of total reflection, thereby it is lower to cause integral body to go out optical property.
Summary of the invention
Based on this, be necessary to provide organic electroluminescence device that a kind of light extraction efficiency is higher and preparation method thereof.
A kind of organic electroluminescence device, comprise the substrate of glass, anode, hole scattering layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, the material of described hole scattering layer comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, and described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide.
In an embodiment, the thickness of described hole scattering layer is 10nm ~ 40nm therein.
In an embodiment, the particle diameter of described titanium dioxide is 20nm～200nm therein.
Therein in an embodiment, the material of described luminescent layer is selected from 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'-, at least one in 1'-biphenyl and oxine aluminium.
In an embodiment, the material of described electron transfer layer is selected from 4,7-diphenyl-1 therein, 10-phenanthroline, 1,2, at least one in 4-triazole derivative and N-aryl benzimidazole.
A preparation method for organic electroluminescence device, comprises the following steps:
At the back side magnetron sputtering in substrate of glass, prepare anode, the surface electronic bundle of described anode is prepared hole scattering layer, the material of described hole scattering layer comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide, and
On the surface of described hole scattering layer, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively.
In an embodiment, the thickness of described hole scattering layer is 10nm ~ 40nm therein.
In an embodiment, the particle diameter of described titanium dioxide is 20nm～200nm therein.
Therein in an embodiment, the concrete steps of described preparation hole scattering layer are, described titanium dioxide is configured to solution, the solid-to-liquid ratio of described titania solution is 20%～60%, then add dispersant, the mass ratio of described dispersant and described titanium dioxide is 1:1.5～1:25, after stirring, calcining at 400 ℃～600 ℃, time is 20 minutes～60 minutes, obtains anatase titania, and described anatase titania is mixed with lanthanide oxide, the preparation of employing electron beam, obtains hole scattering layer.
In an embodiment, described hole scattering layer adopts electron beam preparation therein, and described electron beam preparation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, energy density is 10W/cm
2～l00W/cm
2.
In an embodiment, described magnetron sputtering is 5 * 10 at vacuum pressure therein
-5pa ~ 2 * 10
-3under Pa, carry out, acceleration pressure is 300V～800V, and magnetic field is 50G～200G, and power density is 1W/cm
2~ 40W/cm
2.
Above-mentioned organic electroluminescence device and preparation method thereof, by prepare hole scattering layer at anode surface, the HOMO energy level of the lanthanide oxide in this hole scattering layer is lower,-below 6.5eV, HOMO energy level comparison match with organic layer, reduced interface potential barrier, can effectively improve hole injectability, with lanthanide oxide and titanium dioxide, adulterate, titanium dioxide anatase structured has very high specific area and stability, improve the stability of cavitation layer, in visible-range, there is higher transmitance simultaneously, can carry out scattering to light, this structure can improve the light extraction efficiency of organic electroluminescence device greatly.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is preparation method's the flow chart of the organic electroluminescence device of an execution mode;
Fig. 3 is current density and the luminous efficiency graph of a relation of the organic electroluminescence device of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, organic electroluminescence device and preparation method thereof is further illustrated.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode comprises substrate of glass 20, anode 30, hole scattering layer 40, hole transmission layer 50, luminescent layer 60, electron transfer layer 70, electron injecting layer 80 and the negative electrode 90 stacking gradually.
The glass that substrate of glass 20 is 1.8 ~ 2.2 for refractive index, in 400nm transmitance higher than 90%.Substrate of glass 20 is preferably the glass that the trade mark is N-LAF36, N-LASF31A, N-LASF41A or N-LASF44.
Anode 30 is formed at the surface of substrate of glass 20.The material of anode 30 comprises at least one in indium tin oxide (ITO), aluminium zinc oxide (AZO) and indium-zinc oxide (IZO).The thickness of anode 30 is 80nm ~ 300nm.Preferred thickness is 120nm.
Hole scattering layer 40 is formed at the surface of anode 30.The material of hole scattering layer 40 comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, and described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide.The thickness of hole scattering layer 40 is 10nm ~ 40nm, and the particle diameter of titanium dioxide is 20nm～200nm.
Hole transmission layer 50 is formed at the surface of hole scattering layer 40.The material of hole transmission layer 50 is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA) and N, N '-(1-naphthyl)-N, N '-diphenyl-4, at least one in 4 '-benzidine (NPB).The thickness of hole transmission layer 50 is 40 ~ 80nm.
Luminescent layer 60 is formed at the surface of hole transmission layer 50.The material of luminescent layer 60 is selected from 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) and oxine aluminium (Alq
3) at least one, be preferably Alq
3.The thickness of luminescent layer 60 is 5nm ~ 40nm, is preferably 15nm.
Electron transfer layer 70 is formed at the surface of luminescent layer 60.The material of electron transfer layer 70 is selected from 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2, and at least one in 4-triazole derivative (as TAZ) and N-aryl benzimidazole (TPBI), is preferably TAZ.The thickness of electron transfer layer 70 is 40nm ~ 250nm, is preferably 200nm.
Electron injecting layer 80 is formed at the surface of electron transfer layer 70.The material of electron injecting layer 80 is selected from cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) at least one, be preferably LiF.The thickness of electron injecting layer 80 is 0.5nm ~ 10nm, is preferably 0.7nm.
Negative electrode 90 is formed at the surface of electron injecting layer 80.The material of negative electrode 90 is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au), is preferably Al.The thickness of negative electrode 90 is 80nm ~ 250nm, is preferably 200nm.
Above-mentioned organic electroluminescence device 100, by prepare hole scattering layer 40 between anode 30 and hole transmission layer 50, the HOMO energy level of the lanthanide oxide in this hole scattering layer 40 is lower,-below 6.5eV, HOMO energy level comparison match with organic layer, reduced interface potential barrier, can effectively improve hole injectability, with lanthanide oxide and titanium dioxide, adulterate, titanium dioxide anatase structured has very high specific area and stability, improve the stability of cavitation layer, in visible-range, there is higher transmitance simultaneously, can carry out scattering to light, this structure can improve the light extraction efficiency of organic electroluminescence device greatly.
Be appreciated that in this organic electroluminescence device 100 and also other functional layers can be set as required.
Please refer to Fig. 2, the preparation method of the organic electroluminescence device 100 of an embodiment, it comprises the following steps:
Step S110, at the back side of substrate of glass 20, adopt magnetron sputtering method to prepare anode 30.
The glass that substrate of glass 20 is 1.8 ~ 2.2 for refractive index, in 400nm transmitance higher than 90%.Substrate of glass 20 is preferably the glass that the trade mark is N-LAF36, N-LASF31A, N-LASF41A or N-LASF44.
The material of anode 30 comprises at least one in indium tin oxide (ITO), aluminium zinc oxide (AZO) and indium-zinc oxide (IZO).The thickness of anode 30 is 80nm ~ 300nm.Preferred thickness is 120nm.
Magnetron sputtering is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, acceleration pressure is 300V～800V, and magnetic field is 50G～200G, and power density is 1W/cm
2~ 40W/cm
2.
In present embodiment, substrate of glass 20 is placed in isopropyl alcohol and soaks 1 hour ~ 5 hours after using before use distilled water, alcohol flushing totally.
Step S120, at the surface electronic bundle of anode 30, prepare hole scattering layer 40.
The material of described hole scattering layer 40 comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, and described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide.The thickness of hole scattering layer 40 is 10nm ~ 40nm, and the particle diameter of titanium dioxide is 20nm～200nm.
The concrete steps of described preparation hole scattering layer are, described titanium dioxide is configured to solution, and the solid-to-liquid ratio of described titania solution is 20%～60%, then adds dispersant, the mass ratio of described dispersant and described titanium dioxide is 1:1.5～1:25, after stirring, calcining at 400 ℃～600 ℃, the time is 20 minutes～60 minutes, obtain anatase titania, described anatase titania is mixed with lanthanide oxide, adopt electron beam preparation, obtain hole scattering layer.
Wherein, dispersant comprises acetylacetone,2,4-pentanedione, acetone or polyethylene glycol;
Wherein, the solvent of dissolving titanium dioxide comprises water, ethanol, isopropyl alcohol or n-butanol.
Described electron beam preparation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, energy density is 10W/cm
2～l00W/cm
2.
Step S130, on the surface of hole scattering layer 40, evaporation forms hole transmission layer 50, luminescent layer 60, electron transfer layer 70, electron injecting layer 80 and negative electrode 90 successively.
Hole transmission layer 50 is formed at the surface of hole scattering layer 40.The material of hole transmission layer 50 is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA) and N, N '-(1-naphthyl)-N, N '-diphenyl-4, at least one in 4 '-benzidine (NPB).The thickness of hole transmission layer 50 is 40-80nm.Evaporation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Luminescent layer 60 is formed at the surface of hole transmission layer 50.The material of luminescent layer 60 is selected from 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) and oxine aluminium (Alq
3) at least one, be preferably Alq
3.The thickness of luminescent layer 60 is 5nm ~ 40nm, is preferably 30nm.Evaporation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Electron transfer layer 70 is formed at the surface of luminescent layer 60.The material of electron transfer layer 70 is selected from 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2, and at least one in 4-triazole derivative (as TAZ) and N-aryl benzimidazole (TPBI), is preferably TAZ.The thickness of electron transfer layer 70 is 40nm ~ 250nm, is preferably 200nm.Evaporation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Electron injecting layer 80 is formed at the surface of electron transfer layer 70.The material of electron injecting layer 80 is selected from cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) at least one, be preferably LiF.The thickness of electron injecting layer 80 is 0.5nm ~ 10nm, is preferably 0.7nm.Evaporation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Negative electrode 90 is formed at the surface of electron injecting layer 80.The material of negative electrode 90 is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au), is preferably Al.The thickness of negative electrode 90 is 80nm ~ 250nm, is preferably 200nm.Evaporation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, evaporation speed is 1nm/s ~ 10nm/s.
Above-mentioned organic electroluminescence device preparation method, preparation technology is simple; The light extraction efficiency of the organic electroluminescence device of preparation is higher.
Below in conjunction with specific embodiment, the preparation method of organic electroluminescence device is elaborated.
The preparation used of the embodiment of the present invention and comparative example and tester are: high vacuum coating system (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 U.S. Keithley company, CS-100A colorimeter measuring current density and the colourity of Japanese Konica Minolta company.
Embodiment 1
The present embodiment is prepared structure
2: TiO
2/ TCTA/Alq
3the organic electroluminescence device of/TPBI/CsF/Ag.
Substrate of glass is N-LASF44, distilled water for substrate of glass, alcohol flushing is clean after, be placed in isopropyl alcohol and soak an evening.Adopt the mode of magnetron sputtering to prepare anode at glass basic surface, anode material is ITO, and thickness is 120nm, and the condition of magnetron sputtering is that pressure is 8 * 10
-4pa, accelerating voltage 400V, magnetic field 100G, power density 25W/cm
2, adopt the mode of electron beam to prepare hole scattering layer at anode surface, the material of hole scattering layer be by titania additive in titanium dioxide praseodymium, wherein, the mass percent that titanium dioxide accounts for titanium dioxide praseodymium is 20%, wherein, the particle diameter of titanium dioxide is 50nm, by titanium dioxide 3.5g, join 10ml ethanol and form titania solution, the solid-to-liquid ratio of titania solution is 35%, add again 0.15g acetylacetone,2,4-pentanedione as dispersant, stir and form suspension-turbid liquid, then calcining at 450 ℃, time is 30 minutes, obtain anatase titania, anatase titania is mixed according to mass ratio 1:4 with titanium dioxide praseodymium, adopting electron beam is 8 * 10 at pressure
-4pa, energy density be 20W/cm
2under condition, prepare hole scattering layer, the thickness that obtains hole scattering layer is 20nm, and evaporation is prepared hole transmission layer: selected materials is TCTA, and the thickness of hole transmission layer is 50nm, and evaporation is prepared luminescent layer: selected materials is Alq
3, thickness is 15nm, evaporation is prepared electron transfer layer, and material is TAZ, and thickness is 200nm, evaporation is prepared electron injecting layer, material is CsF, and thickness is 1.5nm, evaporation is prepared negative electrode, and material is Au, and thickness is 150nm, finally obtain needed electroluminescent device.The operating pressure of preparation is 8 * 10
-4pa, the evaporation speed of organic material is 0.2nm/s, the evaporation speed of metal and metal oxide materials is 2nm/s.
Refer to Fig. 3, the structure that is depicted as preparation in embodiment 1 is/substrate of glass/ITO/PrO
2: TiO
2/ TCTA/Alq
3the organic electroluminescence device of/TPBI/CsF/Ag (curve 1) with structure prepared by comparative example is: ito glass/MoO
3/ TCTA/Alq
3the luminous efficiency of the organic electroluminescence device of/TPBi/CsF/Ag (curve 2) and the relation of current density.Step and each layer thickness that comparative example is prepared with organic electroluminescence devices are all identical with embodiment 1.
From scheming, can see, the luminous efficiency of embodiment 1 is large than comparative example all, the luminous efficiency of embodiment 1 is 3.8m/W, and that comparative example is only 2.4lm/W, and the luminous efficiency of comparative example along with the increase of current density fast-descending, this explanation, in the HOMO energy level of lanthanide oxide lower,-below 6.5eV, HOMO energy level comparison match with organic layer, reduced interface potential barrier, can effectively improve hole injectability, with lanthanide oxide and titanium dioxide, adulterate, titanium dioxide anatase structured has very high specific area and stability, improve the stability of cavitation layer, in visible-range, there is higher transmitance simultaneously, can carry out scattering to light, , this structure can improve the light extraction efficiency of organic electroluminescence device greatly.
The luminous efficiency of the organic electroluminescence device that below prepared by each embodiment is all similar with embodiment 1, and each organic electroluminescence device also has similar luminous efficiency, repeats no more below.
Embodiment 2
The present embodiment is prepared structure
2o
3: TiO
2the organic electroluminescence device of/NPB/ADN/Bphen/LiF/Pt.
Substrate of glass is N-LAF36, distilled water for substrate of glass, alcohol flushing is clean after, be placed in isopropyl alcohol and soak an evening, adopt the mode of magnetron sputtering to prepare anode at glass basic surface, anode material is AZO, and thickness is 300nm, and the condition of magnetron sputtering is that pressure is 2 * 10
-3pa, accelerating voltage 300V, magnetic field 50G, power density 1W/cm
2, adopt the mode of electron beam to prepare hole scattering layer at anode surface, the material of hole scattering layer be by titania additive in praseodymium sesquioxide, wherein, the mass percent that titanium dioxide accounts for titanium dioxide praseodymium is 20%, wherein, the particle diameter of titanium dioxide is 50nm, by titanium dioxide 4g, join 20ml ethanol and form titania solution, the solid-to-liquid ratio of titania solution is 20%, add again 0.2g polyethylene glycol as dispersant, stir and form suspension-turbid liquid, then calcining at 400 ℃, time is 60 minutes, obtain anatase titania, anatase titania is mixed according to mass ratio 1:9 with titanium dioxide praseodymium, adopting electron beam is 2 * 10 at pressure
-3pa, energy density be 100W/cm
2under condition, prepare hole scattering layer, the thickness that obtains hole scattering layer is 40nm, and evaporation is prepared hole transmission layer: selected materials is NPB, and the thickness of hole transmission layer is 40nm, and evaporation is prepared luminescent layer: selected materials is ADN, and thickness is 8nm, evaporation is prepared electron transfer layer, and material is Bphen, and thickness is 65nm, evaporation is prepared electron injecting layer, material is LiF, and thickness is 0.5nm, evaporation is prepared negative electrode, and material is Pt, and thickness is 80nm, finally obtain needed electroluminescent device.The operating pressure of preparation is 2 * 10
-3pa, the evaporation speed of organic material is 1nm/s, the evaporation speed of metal and metal oxide materials is 10nm/s.
Embodiment 3
The present embodiment is prepared structure
2o
3: TiO
2/ TAPC/DCJTB/TAZ/Cs
2cO
3the organic electroluminescence device of/Au.
Substrate of glass is N-LASF31A, distilled water for substrate of glass, alcohol flushing is clean after, be placed in isopropyl alcohol and soak an evening, adopt the mode of magnetron sputtering to prepare anode at glass basic surface, anode material is ITO, and the condition of magnetron sputtering is that pressure is 5 * 10
-5pa, accelerating voltage 800V, magnetic field 50G, power density 40W/cm
2, adopt the mode of electron beam to prepare hole scattering layer at anode surface, the material of hole scattering layer be by titania additive in three ytterbium oxides, wherein, the mass percent that titanium dioxide accounts for three ytterbium oxides is 30%, wherein, the particle diameter of titanium dioxide is 200nm, by titanium dioxide 6g, join 10ml ethanol and form titania solution, the solid-to-liquid ratio of titania solution is 60%, add again 0.5g acetone as dispersant, stir and form suspension-turbid liquid, then calcining at 600 ℃, time is 20 minutes, obtain anatase titania, anatase titania is mixed according to mass ratio 3:7 with titanium dioxide praseodymium, adopting electron beam is 5 * 10 at pressure
-5pa, energy density be 10W/cm
2under condition, prepare hole scattering layer, the thickness that obtains hole scattering layer is 10nm, and evaporation is prepared hole transmission layer: selected materials is TAPC, and the thickness of hole transmission layer is 80nm, and evaporation is prepared luminescent layer: selected materials is DCJTB, and thickness is 10nm, evaporation is prepared electron transfer layer, and material is TAZ, and thickness is 200nm, evaporation is prepared electron injecting layer, material is Cs
2cO
3, thickness is 10nm, evaporation is prepared negative electrode, and material is Au, and thickness is 100nm, finally obtain needed electroluminescent device.The operating pressure of preparation is 5 * 10
-5pa, the evaporation speed of organic material is 0.1nm/s, the evaporation speed of metal and metal oxide materials is 1nm/s.
Embodiment 4
It is substrate of glass/TiO that the present embodiment is prepared structure
2/ Sm
2o
3: TiO
2/ NPB/BCzVBi/TPBi/CsN
3the organic electroluminescence device of/Al.
Substrate of glass is N-LASF41A, distilled water for substrate of glass, alcohol flushing is clean after, be placed in isopropyl alcohol and soak an evening, adopt the mode of magnetron sputtering to prepare anode at glass basic surface, anode material is ITO, and the condition of magnetron sputtering is that pressure is 2 * 10
-4pa, accelerating voltage 550V, magnetic field 100G, power density 35W/cm
2, adopt the mode of electron beam to prepare hole scattering layer at anode surface, the material of hole scattering layer be by titania additive in samarium oxide, wherein, the mass percent that titanium dioxide accounts for samarium oxide is 20%, wherein, the particle diameter of titanium dioxide is 100nm, by titanium dioxide 9g, join 20ml ethanol and form titania solution, the solid-to-liquid ratio of titania solution is 45%, add again 6g polyethylene glycol as dispersant, stir the suspension-turbid liquid forming, then calcining at 450 ℃, time is 35 minutes, obtain anatase titania, anatase titania is mixed according to mass ratio 1:4 with samarium oxide, adopting electron beam is 2 * 10 at pressure
-4pa, energy density be 20W/cm
2under condition, prepare hole scattering layer, the thickness that obtains hole scattering layer is 25nm, and evaporation is prepared hole transmission layer: selected materials is NPB, and the thickness of hole transmission layer is 50nm, and evaporation is prepared luminescent layer: selected materials is BCzVBi, and thickness is 40nm, evaporation is prepared electron transfer layer, and material is TPBi, and thickness is 35nm, evaporation is prepared electron injecting layer, material is CsN
3, thickness is 3nm, evaporation is prepared negative electrode, and material is Al, and thickness is 250nm, finally obtain needed electroluminescent device.The operating pressure of preparation is 2 * 10
-4pa, the evaporation speed of organic material is 0.5nm/s, the evaporation speed of metal and metal oxide materials is 6nm/s.
The 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, it is characterized in that, comprise the substrate of glass, anode, hole scattering layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, the material of described hole scattering layer comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, and described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described hole scattering layer is 10nm ~ 40nm.
3. organic electroluminescence device according to claim 1, is characterized in that, the particle diameter of described titanium dioxide is 20nm～200nm.
4. organic electroluminescence device according to claim 1, it is characterized in that, the material of described luminescent layer is selected from 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'-, at least one in 1'-biphenyl and oxine aluminium.
5. organic electroluminescence device according to claim 1, is characterized in that, the material of described electron transfer layer is selected from 4,7-diphenyl-1,10-phenanthroline, 1,2, at least one in 4-triazole derivative and N-aryl benzimidazole.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
At the back side of substrate of glass, magnetron sputtering is prepared anode, the surface electronic bundle of described anode is prepared hole scattering layer, the material of described hole scattering layer comprises lanthanide oxide and is entrained in the titanium dioxide in described lanthanide oxide, the mass percent that described titanium dioxide accounts for described lanthanide oxide is 10%～30%, described lanthanide oxide is selected from least one in titanium dioxide praseodymium, praseodymium sesquioxide, three ytterbium oxides and samarium oxide, and
On the surface of described hole scattering layer, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively.
7. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: the thickness of described hole scattering layer is 10nm ~ 40nm, and the particle diameter of described titanium dioxide is 20nm～200nm.
8. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: the concrete steps of described preparation hole scattering layer are, described titanium dioxide is configured to solution, the solid-to-liquid ratio of described titania solution is 20%～60%, then add dispersant, the mass ratio of described dispersant and described titanium dioxide is 1:1.5～1:25, after stirring, calcining at 400 ℃～600 ℃, time is 20 minutes～60 minutes, obtain anatase titania, described anatase titania is mixed with lanthanide oxide, the preparation of employing electron beam, obtain hole scattering layer.
9. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: described hole scattering layer adopts electron beam preparation, and described electron beam preparation is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, energy density is 10W/cm
2～l00W/cm
2.
10. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: described magnetron sputtering is 5 * 10 at vacuum pressure
-5pa ~ 2 * 10
-3under Pa, carry out, acceleration pressure is 300V～800V, and magnetic field is 50G～200G, and power density is 1W/cm
2~ 40W/cm
2.
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