CN103928636A - Organic electroluminescence device and manufacturing method thereof - Google Patents
Organic electroluminescence device and manufacturing method thereof Download PDFInfo
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- CN103928636A CN103928636A CN201310015374.6A CN201310015374A CN103928636A CN 103928636 A CN103928636 A CN 103928636A CN 201310015374 A CN201310015374 A CN 201310015374A CN 103928636 A CN103928636 A CN 103928636A
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- organic electroluminescence
- electroluminescence device
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- metal oxide
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- 238000005401 electroluminescence Methods 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 83
- 239000002245 particle Substances 0.000 claims abstract description 48
- 239000011787 zinc oxide Substances 0.000 claims abstract description 42
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 33
- 238000001704 evaporation Methods 0.000 claims description 79
- 230000008020 evaporation Effects 0.000 claims description 75
- 239000000463 material Substances 0.000 claims description 47
- 150000004706 metal oxides Chemical class 0.000 claims description 32
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 24
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 19
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000004246 zinc acetate Substances 0.000 claims description 19
- ZVFQEOPUXVPSLB-UHFFFAOYSA-N 3-(4-tert-butylphenyl)-4-phenyl-5-(4-phenylphenyl)-1,2,4-triazole Chemical compound C1=CC(C(C)(C)C)=CC=C1C(N1C=2C=CC=CC=2)=NN=C1C1=CC=C(C=2C=CC=CC=2)C=C1 ZVFQEOPUXVPSLB-UHFFFAOYSA-N 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 11
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 9
- 238000001771 vacuum deposition Methods 0.000 claims description 8
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical group O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 238000011017 operating method Methods 0.000 claims description 6
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 3
- 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 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 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 2
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 2
- 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 2
- 239000000725 suspension Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 abstract description 11
- 239000007924 injection Substances 0.000 abstract description 11
- 230000005540 biological transmission Effects 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 15
- 239000010409 thin film Substances 0.000 description 15
- 239000010408 film Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000011521 glass Substances 0.000 description 10
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 9
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000001259 photo etching Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 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
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 230000005525 hole transport Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000075 oxide glass Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 description 1
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Natural products C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004776 molecular orbital Methods 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/15—Hole transporting layers
-
- 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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/15—Hole transporting layers
- H10K50/155—Hole transporting layers comprising dopants
-
- 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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/17—Carrier injection layers
-
- 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
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
-
- 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
-
- 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
- H10K2102/301—Details of OLEDs
- H10K2102/331—Nanoparticles used in non-emissive layers, e.g. in packaging layer
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention discloses an organic electroluminescence device which comprises a conductive anode, a hole doping layer, a light emitting layer, an electron transmission layer, an electron injection layer and a cathode which are stacked sequentially, wherein the hole doping layer is made of metallic oxide coated with zinc oxide particles. The invention further discloses a manufacturing method of the organic electroluminescence device. The hole doping layer has both the hole injection capacity and the hole transmission capacity, hole and electron composition probability can be effectively increased, and meanwhile, the light emitting efficiency of the organic electroluminescence device is improved.
Description
Technical field
The present invention relates to organic electroluminescent field, particularly 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 utilized ultrathin film technology to prepare high brightness, high efficiency double-deck organic electroluminescence device (OLED).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 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.Luminous efficiency is high, manufacture craft is simple because it has for OLED, and easily realizes the features such as panchromatic and flexible demonstration, has caused increasing concern in illumination and flat panel display field.
In traditional luminescent device, device inside luminescent material sends widely approximately only has 18% can be transmitted into outside, and the light that major part is sent can consume in device outside with other forms.Research discovery, oled light loss is large, has a big chunk reason to be the imperfection of hole injection layer.Because the material of existing hole injection layer is generally metal oxide, its absorptance in visible-range is higher, has caused light loss; In addition, metal oxide is inorganic matter, and larger with the organic material nature difference of hole transmission layer, both exist refringence between interface, easily cause total reflection, cause OLED entirety to go out optical property lower.Therefore be necessary very much the material of hole injection layer to improve.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of organic electroluminescence device, this device can effectively improve the recombination probability of hole and electronics, has improved light extraction efficiency and the luminous efficiency of organic electroluminescence device simultaneously.The present invention also provides the preparation method of this organic electroluminescence device.
First aspect, the invention provides a kind of organic electroluminescence device, comprise the conductive anode, hole doping layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, the material of described hole doping layer is the metal oxide that surface is coated with Zinc oxide particles, the particle diameter of described Zinc oxide particles is 10 ~ 50nm, and described metal oxide is molybdenum trioxide (MoO
3), tungstic acid (WO
3) or vanadic oxide (V
2o
5).
Preferably, the thickness of described hole doping layer is 80nm.
Described metal oxide is carried out after zinc acetate processing, metal oxide surface can cover last layer zinc oxide (ZnO) particle, thereby form a kind of p doped structure, this structure is conducive to the transmission in hole, and metal oxide is hole-injecting material, therefore described hole doping layer possesses the ability of hole injection and hole transport simultaneously, can effectively improve the recombination probability of hole and electronics; In addition, ZnO covers after metal oxide surface, can make the particle diameter of nano thin-film increase, and improves light scattering ability, and light extraction efficiency is enhanced.And intergranular connection is tightr, make film there is better compactness, effectively avoid the existence of film defects, and the particle diameter of nano thin-film increases, and also makes device hole transport performance be enhanced, and finally can effectively improve device luminous efficiency.
Preferably, described conductive anode substrate is indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO), and more preferably, described conductive anode substrate is ITO.
Preferably, described luminescent layer material is 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 described luminescent layer is 5～40nm.
More preferably, described luminescent layer material is Alq
3, thickness is 30nm.
Preferably, described electron transfer layer material is 4,7-diphenyl-1,10-phenanthroline (Bphen), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ) or N-aryl benzimidazole (TPBI), described electric transmission layer thickness is 40～200nm.
More preferably, described electron transfer layer material is TAZ, and thickness is 150nm.
Preferably, described electron injecting layer material is cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) or lithium fluoride (LiF), thickness is 0.5～10nm.
More preferably, described electron injecting layer material is CsF, and thickness is 1nm.
Preferably, described negative electrode is silver (Ag), aluminium (Al), platinum (Pt) or gold (Au), and thickness is 60～300nm.
More preferably, described negative electrode is Ag, and thickness is 100nm.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise following operating procedure:
The conductive anode of required size is provided, dry after cleaning;
Evaporation hole doping layer on conductive anode, the material of described hole doping layer is the metal oxide that surface is coated with Zinc oxide particles, the preparation method of described hole doping layer is: metal oxide is put into zinc acetate solution and soak 30～120min, obtain aaerosol solution, in described suspension, the mass ratio of zinc acetate and metal oxide is 0.02 ~ 0.6:1, after aaerosol solution is dried, in 300～500 DEG C of calcining 15～60min, obtain surface and be coated with the metal oxide of Zinc oxide particles; Then the metal oxide evaporation that by vacuum coating system, described surface is coated with to Zinc oxide particles, on conductive anode, obtains hole doping layer; The particle diameter of described Zinc oxide particles is 10 ~ 50nm, and described metal oxide is MoO
3, WO
3or V
2o
5;
On hole doping layer surface, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, obtains described organic electroluminescence device.
Preferably, the thickness of described hole doping layer is 20～100nm.
The mass percent concentration of described zinc acetate solution is 10%～60%, and the quality of described metal oxide is 1mg～5mg.
Preferably, described vacuum degree during by vacuum coating system evaporation hole doping layer is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 1～10nm/s.
Preferably, described calcining is carried out in Muffle furnace.
Preferably, described in the conductive anode of required size is provided, concrete operations are: conductive anode substrate is carried out to photoetching treatment, be then cut into needed size.
Preferably, after described cleaning, be dried as conductive anode is used to liquid detergent successively, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, the organic pollution of removal glass surface, cleans up rear air-dry.
Preferably, the evaporation condition of described luminescent layer, electron transfer layer and electron injecting layer is: vacuum degree is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 0.1～1nm/s.
Preferably, vacuum degree when described evaporation negative electrode is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 1～10nm/s.
Preferably, described conductive anode substrate is ITO, AZO or IZO, and more preferably, described conductive anode substrate is ITO.
Preferably, described luminescent layer material is DCJTB, ADN, BCzVBi or Alq
3, the thickness of described luminescent layer is 5～40nm.
More preferably, described luminescent layer material is Alq
3, thickness is 30nm.
Preferably, described electron transfer layer material is Bphen, TAZ or TPBI, and described electric transmission layer thickness is 40～200nm.
More preferably, described electron transfer layer material is TAZ, and thickness is 150nm.
Preferably, described electron injecting layer material is Cs
2cO
3, CsF, CsN
3or LiF, thickness is 0.5～10nm.
More preferably, described electron injecting layer material is CsF, and thickness is 1nm.
Preferably, described negative electrode is Ag, Al, Pt or Au, and thickness is 60～300nm.
More preferably, described negative electrode is Ag, and thickness is 100nm.
The present invention carries out described metal oxide after zinc acetate processing, metal oxide surface can cover last layer zinc oxide (ZnO) particle, thereby form a kind of p doped structure, this structure is conducive to the transmission in hole, and metal oxide is hole-injecting material, therefore described hole doping layer possesses the ability of hole injection and hole transport simultaneously, can effectively improve the recombination probability of hole and electronics; In addition, ZnO covers after metal oxide surface, the metal oxide that evaporation surface is coated with Zinc oxide particles on anode can form nano thin-film (particle diameter of nano thin-film is 15～80nm), using described nano thin-film as hole doping layer, ZnO can make the particle diameter of nano thin-film increase, improve light scattering ability, light extraction efficiency is enhanced.And intergranular connection is tightr, make film there is better compactness, effectively avoid the existence of film defects, and the particle diameter of nano thin-film increases, and also makes device hole transport performance be enhanced, and finally can effectively improve device luminous efficiency.
The existence of hole doping layer can instead of holes transport layer and hole injection layer, has reduced material cost and simplified film to form technique.Meanwhile, the preparation method of hole doping layer is simple, and cost of material is low, and processing ease is applicable to suitability for industrialized production.
The invention provides a kind of organic electroluminescence device and preparation method thereof, there is following beneficial effect:
(1) hole doping layer material is the metal oxide that surface is coated with Zinc oxide particles, metal oxide after treatment, its surface can cover last layer zinc oxide (ZnO) particle, this p-type structure is conducive to transmission and the hole in hole and injects, make hole doping layer possess hole injects and cavity transmission ability simultaneously, effectively improve the recombination probability of hole and electronics, improve light scattering ability, make film there is better compactness simultaneously, effectively avoid the existence of film defects, finally improve luminous efficiency;
(2) existence of the hole doping layer that prepared by the present invention can instead of holes transport layer and hole injection layer, has reduced material cost and simplified film to form technique, simultaneously, the preparation method of hole doping layer is simple, cost of material is low, and processing ease is applicable to suitability for industrialized production.
Brief description of the drawings
In order to be illustrated more clearly in technical scheme of the present invention, to the accompanying drawing of required use in execution mode be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of organic electroluminescence device of the present invention;
Fig. 2 is the embodiment of the present invention 1 and the brightness of comparative example's organic electroluminescence device and the graph of a relation of luminous efficiency.
Embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described.
Embodiment 1
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) conductive anode 1 is selected indium tin oxide glass (ITO), first conductive anode 1 is carried out to photoetching treatment, is then cut into 2 × 2cm
2square conductive anode, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry;
(2) by 20mg MoO
3be immersed in 10ml zinc acetate solution, the mass percent concentration of zinc acetate solution is 35%, soaks 60min, obtain aaerosol solution, after aaerosol solution is dried, be placed in Muffle furnace and calcine, calcining heat is 400 DEG C, and calcination time is 30min, obtains surface and be coated with the MoO of ZnO particle
3, then adopt vacuum coating system, with 5 × 10
-3the evaporation speed of the pressure of Pa and 1nm/s is coated with surface the MoO of ZnO particle
3evaporation is on conductive anode 1, and obtaining thickness is the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles of 80nm, and the particle diameter of film is 60nm, using the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles as hole doping layer 2;
(3) on hole doping layer 2, evaporation is prepared luminescent layer 3, electron transfer layer 4, electron injecting layer 5 and negative electrode 6 successively, obtains organic electroluminescence device, wherein,
Luminescent layer 3 materials are Alq
3, the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.1nm/s, evaporation thickness is 30nm;
The material of electron transfer layer 4 is TAZ, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.1nm/s, evaporation thickness is 150nm;
The material of electron injecting layer 5 is CsF, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.1nm/s, evaporation thickness is 1nm;
The material of negative electrode 6 is Ag, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 1nm/s, evaporation thickness is 100nm.
Fig. 1 is the structural representation of the organic electroluminescence device prepared of the present embodiment, and organic electroluminescence device prepared by the present embodiment, comprises the conductive anode 1, hole doping layer 2, luminescent layer 3, electron transfer layer 4, electron injecting layer 5 and the negative electrode 6 that stack gradually.Concrete structure is expressed as:
ITO/（MoO
3-ZnO）/Alq
3/TAZ/CsF/Ag。
Embodiment 2
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) conductive anode is selected the zinc oxide glass (AZO) of mixing aluminium, first conductive anode is carried out to photoetching treatment, is then cut into 2 × 2cm
2square conductive anode, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry;
(2) by 50mg WO
3be immersed in 10ml zinc acetate solution, the mass percent concentration of zinc acetate solution is 10%, soaks 30min, obtain aaerosol solution, after aaerosol solution is dried, be placed in Muffle furnace and calcine, calcining heat is 500 DEG C, and calcination time is 15min, obtains surface and be coated with the WO of ZnO particle
3, zinc acetate and tungsten oxide mass ratio are 0.02:1, then adopt vacuum coating system, with 2 × 10
-4the evaporation speed of the pressure of Pa and 10nm/s is coated with surface the WO of ZnO particle
3evaporation is on conductive anode, and obtaining thickness is the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles of 100nm, and the particle diameter of film is 80nm, using the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles as hole doping layer;
(3) on hole doping layer, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, obtains organic electroluminescence device, wherein,
Luminescent layer material is ADN, and the pressure adopting when evaporation is 2 × 10
-4pa, evaporation speed is 1nm/s, evaporation thickness is 5nm;
The material of electron transfer layer is Bphen, and the pressure adopting when evaporation is 2 × 10
-4pa, evaporation speed is 1nm/s, evaporation thickness is 75nm;
The material of electron injecting layer is Cs
2cO
3, the pressure adopting when evaporation is 2 × 10
-4pa, evaporation speed is 1nm/s, evaporation thickness is 0.5nm;
The material of negative electrode is Al, and the pressure adopting when evaporation is 2 × 10
-4pa, evaporation speed is 10nm/s, evaporation thickness is 300nm.
Organic electroluminescence device prepared by the present embodiment, comprises the conductive anode, hole doping layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Concrete structure is expressed as:
AZO/（WO
3-ZnO）/ADN/Bphen/Cs
2CO
3/Al。
Embodiment 3
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) conductive anode is selected the zinc oxide glass (IZO) of mixing indium, first conductive anode is carried out to photoetching treatment, is then cut into 2 × 2cm
2square conductive anode, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry;
(2) by 10mg V
2o
5be immersed in 10ml zinc acetate solution, the mass percent concentration of zinc acetate solution is 60%, soaks 60min, obtain aaerosol solution, after aaerosol solution is dried, be placed in Muffle furnace and calcine, calcining heat is 300 DEG C, and calcination time is 60min, obtains surface and be coated with the V of ZnO particle
2o
5, zinc acetate and vanadic oxide mass ratio are 0.6:1, then adopt vacuum coating system, with 1 × 10
-3the evaporation speed of the pressure of Pa and 5nm/s is coated with surface the V of ZnO particle
2o
5evaporation is on conductive anode, and obtaining thickness is the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles of 20nm, and the particle diameter of film is 15nm, using the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles as hole doping layer;
(3) on hole doping layer, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, obtains organic electroluminescence device, wherein,
Luminescent layer material is BCzVBi, and the pressure adopting when evaporation is 1 × 10
-3pa, evaporation speed is 0.6nm/s, evaporation thickness is 40nm;
The material of electron transfer layer is TPBI, and the pressure adopting when evaporation is 1 × 10
-3pa, evaporation speed is 0.5nm/s, evaporation thickness is 60nm;
The material of electron injecting layer is CsN
3, the pressure adopting when evaporation is 1 × 10
-3pa, evaporation speed is 0.7nm/s, evaporation thickness is 10nm;
The material of negative electrode is Au, and the pressure adopting when evaporation is 1 × 10
-3pa, evaporation speed is 6nm/s, evaporation thickness is 60nm.
Organic electroluminescence device prepared by the present embodiment, comprises the conductive anode, hole doping layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Concrete structure is expressed as:
IZO/（V
2O
5-ZnO）/BCzVBi/TPBI/CsN
3/Au。
Embodiment 4
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) conductive anode is selected the zinc oxide glass (IZO) of mixing indium, first conductive anode is carried out to photoetching treatment, is then cut into 2 × 2cm
2square conductive anode, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry;
(2) by 40mg MoO
3soak in 10ml zinc acetate solution, zinc acetate solution be 50% at mass percent concentration, soak 40min, obtain aaerosol solution, after aaerosol solution is dried, be placed in Muffle furnace and calcine, calcining heat is 350 DEG C, and calcination time is 30min, obtains surface and be coated with the MoO of ZnO particle
3, the mass ratio of zinc acetate and molybdenum oxide is 0.125:1, then adopts vacuum coating system, with 5 × 10
-3the evaporation speed of the pressure of Pa and 9nm/s is coated with surface the MoO of ZnO particle
3evaporation is on conductive anode, and obtaining thickness is the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles of 60nm, and the particle diameter of film is 50nm, using the Molybdenum Oxide Thin Films by Sol-Gel that contains Zinc oxide particles as hole doping layer;
(3) on hole doping layer, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, obtains organic electroluminescence device, wherein,
Luminescent layer material is DCJTB, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.9nm/s, evaporation thickness is 8nm;
The material of electron transfer layer is TAZ, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.9nm/s, evaporation thickness is 35nm;
The material of electron injecting layer is LiF, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 0.9nm/s, evaporation thickness is 0.5nm;
The material of negative electrode is Pt, and the pressure adopting when evaporation is 5 × 10
-3pa, evaporation speed is 9nm/s, evaporation thickness is 120nm.
Organic electroluminescence device prepared by the present embodiment, comprises the conductive anode, hole doping layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Concrete structure is expressed as:
IZO/（MoO
3-ZnO）/DCJTB/TAZ/LiF/Pt。
Comparative example
For being presented as creativeness of the present invention, the present invention is also provided with comparative example, comparative example comprises the conductive anode, hole injection layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, and the difference of comparative example and embodiment 1 is that the hole injection layer material in comparative example is MoO
3, the concrete structure of comparative example's organic electroluminescence device is: ITO/MoO
3/ Alq
3/ TAZ/CsF/Ag.
Effect embodiment
Adopt current-voltage tester (Keithly company of the U.S., 2400), colorimeter (Japanese Konica Minolta company model:, model: CS-100A) test organic electroluminescence device luminous efficiency with brightness change curve, to investigate the luminous efficiency of device, tested object is organic electroluminescence device prepared by embodiment 1 and comparative example.Test result as shown in Figure 2.
Fig. 2 is the brightness of organic electroluminescence device and the graph of a relation of luminous efficiency prepared by the embodiment of the present invention 1 and comparative example, as can be seen from Figure 2, the luminous efficiency of the embodiment of the present invention 1 organic electroluminescence device within the scope of institute's test brightness is all large than comparative example, wherein maximum luminous efficiency be 15.8lm/W(comparative example be only 8.8lm/W), and the luminous efficiency of comparative example along with the increase of brightness fast-descending.Illustrate that the present invention adopts metal oxide that surface is coated with Zinc oxide particles as hole doping layer material, make hole doping layer possess hole simultaneously and inject and cavity transmission ability, improve device light scattering ability, light extraction efficiency is enhanced.Effectively avoid the existence of film defects.Thereby improve device luminous efficiency.
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, it is characterized in that, comprise the conductive anode, hole doping layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually, the material of described hole doping layer is the metal oxide that surface is coated with Zinc oxide particles, the particle diameter of described Zinc oxide particles is 10 ~ 50nm, and described metal oxide is molybdenum trioxide, tungstic acid or vanadic oxide.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described hole doping layer is 20～100nm.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, described electron transfer layer material is 4,7-diphenyl-1,10-phenanthroline, 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole or N-aryl benzimidazole.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, described electron injecting layer material is cesium carbonate, cesium fluoride, nitrine caesium or lithium fluoride.
5. a preparation method for organic electroluminescence device, is characterized in that, comprises following operating procedure:
The conductive anode of required size is provided, dry after cleaning;
Evaporation hole doping layer on conductive anode, the material of described hole doping layer is the metal oxide that surface is coated with Zinc oxide particles, the preparation method of described hole doping layer is: metal oxide is put into zinc acetate solution, soak 30～120min, obtain aaerosol solution, in described suspension, the mass ratio of zinc acetate and metal oxide is 0.02 ~ 0.6:1, after aaerosol solution is dried, in 300～500 DEG C of calcining 15～60min, obtain surface and be coated with the metal oxide of Zinc oxide particles; Then the metal oxide evaporation that by vacuum coating system, described surface is coated with to Zinc oxide particles, on conductive anode, obtains hole doping layer; The particle diameter of described Zinc oxide particles is 10 ~ 50nm, and described metal oxide is molybdenum trioxide, tungstic acid or vanadic oxide;
On hole doping layer surface, evaporation is prepared luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively, obtains described organic electroluminescence device.
6. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described vacuum degree during by vacuum coating system evaporation hole doping layer is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 1～10nm/s.
7. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thickness of described hole doping layer is 20～100nm.
8. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the mass percent concentration of described zinc acetate solution is 10%～60%, and the quality of described metal oxide is 10mg～50mg.
9. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the evaporation condition of described luminescent layer, electron transfer layer and electron injecting layer is: vacuum degree is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 0.1～1nm/s.
10. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, vacuum degree when described evaporation negative electrode is 2 × 10
-4～5 × 10
-3pa, evaporation speed is 1～10nm/s.
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| US20030057828A1 (en) * | 2001-03-21 | 2003-03-27 | Roitman Daniel B. | Polymer organic light emitting device with improved color control |
| WO2009133907A1 (en) * | 2008-04-28 | 2009-11-05 | 大日本印刷株式会社 | Device having hole injection transport layer, method for production thereof, and ink for formation of hole injection transport layer |
| CN101587941A (en) * | 2009-06-25 | 2009-11-25 | 彩虹集团公司 | Organic electroluminescent display device |
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| US20030057828A1 (en) * | 2001-03-21 | 2003-03-27 | Roitman Daniel B. | Polymer organic light emitting device with improved color control |
| WO2009133907A1 (en) * | 2008-04-28 | 2009-11-05 | 大日本印刷株式会社 | Device having hole injection transport layer, method for production thereof, and ink for formation of hole injection transport layer |
| CN101587941A (en) * | 2009-06-25 | 2009-11-25 | 彩虹集团公司 | Organic electroluminescent display device |
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