CN103972411A - Organic light-emitting device and production method thereof - Google Patents
Organic light-emitting device and production method thereof Download PDFInfo
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- CN103972411A CN103972411A CN201310039175.9A CN201310039175A CN103972411A CN 103972411 A CN103972411 A CN 103972411A CN 201310039175 A CN201310039175 A CN 201310039175A CN 103972411 A CN103972411 A CN 103972411A
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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- H10K50/00—Organic light-emitting devices
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- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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- H10K50/17—Carrier injection layers
- H10K50/171—Electron injection layers
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Abstract
The invention provides an organic light-emitting device. The organic light-emitting device comprises an anode, a hole injection layer, a first hole transport layer, a first light-emitting layer, a first electron transport layer, a charge generation layer, a second hole transport layer, a second light-emitting layer, a second electron transport layer, an electron injection layer and a cathode which are laminated sequentially. The charge generation layer comprises a first doped layer laminated on the surface of the first electron transport layer, a second doped layer formed on the surface of the first doped layer and a third doped layer formed on the surface of the second doped layer, the first doped layer is made of materials including low work function metal and metal oxides doped in the low work function metal, the second doped layer is made of materials including low work function metal and high work function metal doped in the low work function metal, and the third doped layer is made of materials including high work function metal and metal oxides doped in the high work function metal. The organic light-emitting device is high in light emitting efficiency. The invention further provides a production method of the organic light-emitting 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.Yet the luminous efficiency of organic electroluminescence device is lower at present.
Summary of the invention
Based on this, be necessary to provide organic electroluminescence device that a kind of luminous efficiency is higher and preparation method thereof.
An organic electroluminescence device, comprises the anode stacking gradually, hole injection layer, the first hole transmission layer, the first luminescent layer, the first electron transfer layer, charge generation layer, the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode, described charge generation layer comprises the first doped layer that is laminated in described the first electron transfer layer surface, be formed at second doped layer on described the first doped layer surface and be formed at the 3rd doped layer on described the second doped layer surface, the material of described the first doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described in described the first doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:20 ~ 1:5, the material of described the second doped layer comprises low workfunction metal and is entrained in the high-work-function metal in described low workfunction metal, described in described the second doped layer, the mass ratio of high-work-function metal and described low workfunction metal is 1:10 ~ 3:10, the material of described the 3rd doped layer comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal, described in described the 3rd doped layer, the mass ratio of metal oxide and described high-work-function metal is 1:10 ~ 1:2, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described high work function is selected from silver, aluminium, at least one in platinum and gold, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide.
In an embodiment, the thickness of described the first doped layer is 5nm ~ 20nm therein, and the thickness of described the second doped layer is 2nm ~ 20nm, and the thickness of described the 3rd doped layer is 5nm ~ 30nm.
Therein in an embodiment, the material of described the first luminescent layer and described the second 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.
Therein in an embodiment, the material of described the first hole transmission layer and described the second hole transmission layer is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4 " tri-(carbazole-9-yl) triphenylamine and N, N '-(1-naphthyl)-N; N '-diphenyl-4, at least one in 4 '-benzidine.
In an embodiment, the material of described the first electron transfer layer and described the second 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 anode surface successively evaporation, prepare hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer;
At described the first electron transfer layer surface evaporation, prepare the first doped layer, the material of described the first doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described in described the first doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:20 ~ 1:5, described low workfunction metal is selected from least one in calcium, ytterbium, magnesium and barium, and described metal oxide is selected from least one in molybdenum trioxide, tungstic acid and vanadic oxide;
At described the first doped layer surface evaporation, prepare the second doped layer, the material of described the second doped layer comprises low workfunction metal and is entrained in the high-work-function metal in described low workfunction metal, described in described the second doped layer, the mass ratio of high-work-function metal and described low workfunction metal is 1:10 ~ 3:10, described low workfunction metal is selected from least one in calcium, ytterbium, magnesium and barium, and described high work function is selected from least one in silver, aluminium, platinum and gold;
At described the second doped layer surface evaporation, prepare the 3rd doped layer, the material of described the 3rd doped layer comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal, described in described the 3rd doped layer, the mass ratio of metal oxide and described high-work-function metal is 1:10 ~ 1:2, described high work function is selected from least one in silver, aluminium, platinum and gold, and described metal oxide is selected from least one in molybdenum trioxide, tungstic acid and vanadic oxide; And
On the 3rd doped layer surface successively evaporation, form the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode.
Therein in an embodiment, the material of described the first luminescent layer and described the second 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.
Therein in an embodiment, the material of described the first hole transmission layer and described the second hole transmission layer is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4 " tri-(carbazole-9-yl) triphenylamine and N, N '-(1-naphthyl)-N; N '-diphenyl-4, at least one in 4 '-benzidine.
In an embodiment, the thickness of described the first doped layer is 5nm ~ 20nm therein, and the thickness of described the second doped layer is 2nm ~ 20nm, and the thickness of described the 3rd doped layer is 5nm ~ 30nm.
Therein in an embodiment, before described anode surface forms hole injection layer, first antianode carries out pre-treatment, pre-treatment comprises: anode is carried out to photoetching treatment, be cut into needed size, adopt liquid detergent, deionized water, acetone, ethanol, each Ultrasonic Cleaning of isopropyl acetone 15min, to remove the organic pollution of anode surface.
Above-mentioned organic electroluminescence device and preparation method thereof, charge generation layer is by the first doped layer, the second doped layer and the 3rd doped layer form, the first doped layer uses bipolarity metal oxide as doping object, bipolarity metal oxide can improve the regeneration efficiency of electronics, and the existence of metal and metal oxide, can make interface compatibility better, reduce electron trap, the second doped layer adopts the metal of low work function and the metal of high work function to adulterate, low workfunction metal is conducive to reduce electronic injection potential barrier, but more active, and the metal of high work function can improve the stability of the second doped layer, simultaneously, also be conducive to the injection in hole, and the 3rd doped layer adopts high-work-function metal and bipolarity metal oxide to adulterate, high work function can make the potential barrier between the second doped layer and the 3rd doped layer reduce, reduce energy loss, be conducive to the generation in hole, and metal oxide can effectively reduce hole injection barrier, and three layers all used metal, can greatly improve conductivity and the photopermeability of charge generation layer, charge generation layer can effectively improve the luminous efficiency of organic electroluminescence device.
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 anode 10, hole injection layer 20, the first hole transmission layer 32, the first luminescent layer 34, the first electron transfer layer 36, charge generation layer 40, the second hole transmission layer 52, the second luminescent layer 54, the second electron transfer layer 56, electron injecting layer 60 and the negative electrode 70 stacking gradually.
Anode 10 is indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO), is preferably ITO.
Hole injection layer 20 is formed at anode 10 surfaces.The material of hole injection layer 20 is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one, be preferably V
2o
5.The thickness of hole injection layer 20 is 20nm ~ 80nm, is preferably 30nm.
The first hole transmission layer 32 is formed at the surface of hole injection layer 20.The material of the first hole transmission layer 32 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), is preferably NPB.The thickness of the first hole transmission layer 32 is 20nm ~ 60nm, is preferably 40nm.
The first luminescent layer 34 is formed at the surface of the first hole transmission layer 32.The material of the first luminescent layer 34 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 8-hydroxyquinoline aluminum (Alq
3) at least one, be preferably BCzVBi.The thickness of luminescent layer 40 is 5nm ~ 40nm, is preferably 30nm.
The first electron transfer layer 36 is formed at the surface of the first luminescent layer 34.The material of the first electron transfer layer 36 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 Bphen.The thickness of the first electron transfer layer 36 is 40nm ~ 200nm, is preferably 50nm.
Charge generation layer 40 is formed at the surface of the first electron transfer layer 36.Described charge generation layer 40 comprise be laminated in the first electron transfer layer 36 surfaces the first doped layer 42, be formed at second doped layer 44 on the first doped layer 42 surfaces and be formed at the 3rd doped layer on the second doped layer 44 surfaces.
The material of the first doped layer 42 comprises low workfunction metal and is entrained in the metal oxide in low workfunction metal.The work function of low workfunction metal is-2.0 ~-4.0eV, and preferred, low workfunction metal is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).Metal oxide is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one.In the first doped layer 42, the mass ratio of metal oxide and low workfunction metal is 1:20 ~ 1:5.The thickness of the first doped layer 42 is 5nm ~ 20nm.
The second doped layer 44 is formed at the first doped layer 42 surfaces.The material of the second doped layer 44 comprises low workfunction metal and is entrained in the high-work-function metal in low workfunction metal.Low workfunction metal is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).The work function of high-work-function metal is-4.0 ~-6.0eV, preferred, and high-work-function metal is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au).In the second doped layer 44, the mass ratio of high-work-function metal and low workfunction metal is 1:10 ~ 3:10.The thickness of the second doped layer 44 is 2nm ~ 20nm.
The 3rd doped layer 46 is formed at the surface of the second doped layer 44.The material of the 3rd doped layer 46 comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal.High-work-function metal is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au).Metal oxide is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one.In the 3rd doped layer, the mass ratio of metal oxide and high-work-function metal is 1: 10 ~ 1:2.The thickness of the 3rd doped layer 46 is 5nm ~ 30nm.
The second hole transmission layer 52 is formed at the surface of the 3rd doped layer 46.The material of the second hole transmission layer 52 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), is preferably TCTA.The thickness of the second hole transmission layer 52 is 20nm ~ 60nm, is preferably 30nm.
The second luminescent layer 54 is formed at the surface of the second hole transmission layer 52.The material of the second luminescent layer 54 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 8-hydroxyquinoline aluminum (Alq
3) at least one, be preferably BCzVBi.The thickness of luminescent layer 40 is 5nm ~ 40nm, is preferably 30nm.
The second electron transfer layer 56 is formed at the surface of the second luminescent layer 52.The material of the second electron transfer layer 56 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 TPBI.The thickness of the second electron transfer layer 56 is 40nm ~ 200nm, is preferably 150nm.
Electron injecting layer 60 is formed at the second electron transfer layer 56 surfaces.The material of electron injecting layer 60 is selected from cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) at least one, be preferably CsN
3.The thickness of electron injecting layer 60 is 0.5nm ~ 10nm, is preferably 2.5nm.
Negative electrode 70 is formed at electron injecting layer 60 surfaces.The material of negative electrode 70 is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au), is preferably Ag.The thickness of negative electrode 70 is 60nm ~ 300nm, is preferably 150nm.
Above-mentioned organic electroluminescence device 100, charge generation layer 40 is by the first doped layer 42, the second doped layer 44 and the 3rd doped layer 46 form, the first doped layer 42 use bipolarity metal oxides are as doping object, bipolarity metal oxide can improve the regeneration efficiency of electronics, and the existence of metal and metal oxide, can make interface compatibility better, reduce electron trap, the second doped layer 44 adopts the metal of low work function and the metal of high work function to adulterate, low workfunction metal is conducive to reduce electronic injection potential barrier, but more active, and the metal of high work function can improve the stability of the second doped layer 44, simultaneously, also be conducive to the injection in hole, and the 3rd doped layer 46 adopts high-work-function metal and bipolarity metal oxide to adulterate, high work function can make the potential barrier between the second doped layer 44 and the 3rd doped layer 46 reduce, reduce energy loss, be conducive to the generation in hole, and metal oxide can effectively reduce hole injection barrier, and three layers all used metal, can greatly improve conductivity and the photopermeability of charge generation layer 40, charge generation layer 40 can effectively improve the luminous efficiency of organic electroluminescence device.
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 anode surface successively evaporation, prepare hole injection layer 20, the first hole transmission layer 32, the first luminescent layer 34 and the first electron transfer layer 36.
Anode 10 is indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO), is preferably ITO.
In present embodiment, before anode 10 surfaces form hole injection layer 20, first antianode 10 carries out pre-treatment, pre-treatment comprises: anode 10 is carried out to photoetching treatment, be cut into needed size, adopt liquid detergent, deionized water, acetone, ethanol, each Ultrasonic Cleaning of isopropyl acetone 15min, to remove the organic pollution on anode 10 surfaces.
Hole injection layer 20 is formed at the surface of anode 10.Hole injection layer 20 is prepared by evaporation.The material of hole injection layer 20 is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one, be preferably V
2o
5.The thickness of hole injection layer 20 is 20nm ~ 80nm, is preferably 30nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
The first hole transmission layer 32 is formed at the surface of hole injection layer 20.The first hole transmission layer 32 is prepared by evaporation.The material of the first hole transmission layer 32 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), is preferably NPB.The thickness of the first hole transmission layer 32 is 20nm ~ 60nm, is preferably 40nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
The first luminescent layer 34 is formed at the surface of the first hole transmission layer 32.The first luminescent layer 34 is prepared by evaporation.The material of the first luminescent layer 34 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 8-hydroxyquinoline aluminum (Alq
3) at least one, be preferably BCzVBi.The thickness of luminescent layer 40 is 5nm ~ 40nm, is preferably 30nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
The first electron transfer layer 36 is formed at the surface of the first luminescent layer 34.The first electron transfer layer 36 is prepared by evaporation.The material of the first electron transfer layer 36 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 Bphen.The thickness of the first electron transfer layer 36 is 40nm ~ 200nm, is preferably 50nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Step S120, at the surperficial evaporation of the first electron transfer layer 36, prepare the first doped layer 42.
The material of the first doped layer 42 comprises low workfunction metal and is entrained in the metal oxide in low workfunction metal.The work function of low workfunction metal is-2.0 ~-4.0eV, and preferred, low workfunction metal is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).Metal oxide is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one.In the first doped layer 42, the mass ratio of metal oxide and low workfunction metal is 1:20 ~ 1:5.The thickness of the first doped layer 42 is 5nm ~ 20nm.
Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, low workfunction metal and metal oxide evaporate respectively in two evaporation boats, and the evaporation speed of metal oxide is 1nm/s ~ 10nm/s, and the evaporation speed of low workfunction metal is 1nm/s ~ 10nm/s.
Step S130, at the surperficial evaporation of the first doped layer 42, prepare the second doped layer 44.
The second doped layer 44 is formed at the first doped layer 42 surfaces.The material of the second doped layer 44 comprises low workfunction metal and is entrained in the high-work-function metal in low workfunction metal.Low workfunction metal is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).The work function of high-work-function metal is-4.0 ~-6.0eV, preferred, and high-work-function metal is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au).In the second doped layer 44, the mass ratio of high-work-function metal and low workfunction metal is 1:10 ~ 3:10.The thickness of the second doped layer 44 is 2nm ~ 20nm.
Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, low workfunction metal and high-work-function metal evaporate respectively in two evaporation boats, and the evaporation speed of high-work-function metal is 1nm/s ~ 10nm/s, and the evaporation speed of low workfunction metal is 1nm/s ~ 10nm/s.
Step S140, at the surperficial evaporation of the second doped layer 44, prepare the 3rd doped layer 46.
The 3rd doped layer 46 is formed at the surface of the second doped layer 44.The material of the 3rd doped layer 46 comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal.High-work-function metal is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au).Metal oxide is selected from molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) at least one.In the 3rd doped layer, the mass ratio of metal oxide and high-work-function metal is 1: 10 ~ 1:2.The thickness of the 3rd doped layer 46 is 5nm ~ 30nm.
Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, metal oxide and high-work-function metal evaporate respectively in two evaporation boats, and the evaporation speed of high-work-function metal is 1nm/s ~ 10nm/s, and the evaporation speed of metal oxide is 1nm/s ~ 10nm/s.
Step S150, on the 3rd doped layer 46 surfaces successively evaporation, prepare the second hole transmission layer 52, the second luminescent layer 54, the second electron transfer layer 56, electron injecting layer 60 and negative electrode 70.
The second hole transmission layer 52 is formed at the surface of the 3rd doped layer 46.The material of the second hole transmission layer 52 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), is preferably TCTA.The thickness of the second hole transmission layer 52 is 20nm ~ 60nm, is preferably 30nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
The second luminescent layer 54 is formed at the surface of the second hole transmission layer 52.The material of the second luminescent layer 54 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 8-hydroxyquinoline aluminum (Alq
3) at least one, be preferably BCzVBi.The thickness of luminescent layer 40 is 5nm ~ 40nm, is preferably 30nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
The second electron transfer layer 56 is formed at the surface of the second luminescent layer 52.The material of the second electron transfer layer 56 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 TPBI.The thickness of the second electron transfer layer 56 is 40nm ~ 200nm, is preferably 150nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Electron injecting layer 60 is formed at the second electron transfer layer 56 surfaces.The material of electron injecting layer 60 is selected from cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) at least one, be preferably CsN
3.The thickness of electron injecting layer 60 is 0.5nm ~ 10nm, is preferably 2.5nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Negative electrode 70 is formed at electron injecting layer 60 surfaces.The material of negative electrode 70 is selected from least one in silver (Ag), aluminium (Al), platinum (Pt) and gold (Au), is preferably Ag.The thickness of negative electrode 70 is 60nm ~ 300nm, is preferably 150nm.Evaporation is 5 * 10 at vacuum pressure
-3~ 2 * 10
-4under Pa, carry out, evaporation speed is 1nm/s ~ 10nm/s.
Above-mentioned organic electroluminescence device preparation method, technique is simple, and the luminous efficiency of the organic electroluminescence device of preparation is higher.
Below in conjunction with specific embodiment, the preparation method of organic electroluminescence device provided by the invention 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 test brightness and the colourity of Japanese Konica Minolta company.
Embodiment 1
Structure prepared by the present embodiment is ito glass/V
2o
5/ NPB/BCzVBi/Bphen/Ca:MoO
3/ Mg:Ag/MoO
3: Al/TCTA/BCzVBi/TPBi/CsN
3the organic electroluminescence device of/Ag.
First ITO is carried out to photoetching treatment, be cut into needed size, use successively liquid detergent, deionized water, acetone, ethanol, each ultrasonic 15min of isopropyl alcohol, the organic pollution of removal glass surface; Evaporation hole injection layer, material is V
2o
5, thickness is 30nm; Evaporation the first hole transmission layer, material is NPB, thickness is 40nm; Evaporation the first luminescent layer, material is BCzVBi, thickness is 30nm; Evaporation the first electron transfer layer, material is Bphen, thickness is 50nm; Prepare charge generation layer: by the first doped layer, the second doped layer and the 3rd doped layer, formed.Evaporation the first doped layer, material comprises Ca and is entrained in the MoO in Ca
3, MoO
3with the mass ratio of Ca be 1: 10, thickness is 7nm; Evaporation the second doped layer, material comprises Mg and is entrained in the Ag in Mg, the mass ratio 1:5 of Ag and Mg, thickness is 10nm; Evaporation the 3rd doped layer, material comprises Al and is entrained in the MoO in Al
3, MoO
3with the mass ratio of Al be 1; 4, thickness is 15nm; Evaporation the second hole transmission layer, material is TCTA, thickness is 30nm; Evaporation the second luminescent layer, material is BCzVBi, thickness is 30nm; Evaporation the second electron transfer layer, material is TPBI, thickness is 150nm; Evaporation electron injecting layer, material is CsN
3, thickness is 2.5nm; Evaporation negative electrode, material is Ag, thickness is 150nm.Finally obtain needed electroluminescent device.Evaporation is 8 * 10 at vacuum pressure
-4under Pa, carry out, organic material evaporation speed is 0.2nm/s, and the evaporation speed of metallic compound is 2nm/s, and the evaporation speed of metal is 5nm/s.
Refer to Fig. 3, the structure that is depicted as preparation in embodiment 1 is ito glass/V
2o
5/ NPB/BCzVBi/Bphen/Ca:MoO
3/ Mg:Ag/MoO
3: Al/TCTA/BCzVBi/TPBi/CsN
3the organic electroluminescence device of/Ag (curve 1) is ito glass/V with structure prepared by comparative example
2o
5/ NPB/BCzVBi/Bphen/CsN
3the current density of the organic electroluminescence device of/Ag (curve 2) and the relation of luminous efficiency.In the organic electroluminescence device that in organic electroluminescence device prepared by comparative example, each layer thickness is prepared with embodiment 1, each layer thickness is identical.
As seen from Figure 3, under different current densities, the luminous efficiency of embodiment 1 is large than comparative example all, the maximum lumen efficiency of the organic electroluminescence device of embodiment 1 preparation is 10.0lm/W, and the luminous efficiency of organic electroluminescence device prepared by comparative example is only 5.6lm/W, and the luminous efficiency of comparative example along with the increase of current density fast-descending, this explanation, charge generation layer is by the first doped layer, the second doped layer and the 3rd doped layer form, make interface compatibility better, reduce electron trap, the metal of high work function can improve the stability of doped layer, reduce energy loss, be conducive to the generation in hole, and metal oxide can effectively reduce hole injection barrier, and three layers all used metal, can greatly improve conductivity and the photopermeability of charge generation layer, this charge generation layer can effectively improve the luminous efficiency of organic electroluminescence device.
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
Structure prepared by the present embodiment is AZO/V
2o
5/ NPB/ADN/TPBi/Yb:WO
3/ Ca:Al/WO
3: Pt/NPB/ADN/TAZ/CsN
3the organic electroluminescence device of/Pt.
First AZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface, evaporation is prepared hole injection layer, and material is V
2o
5, thickness is 80nm; Evaporation the first hole transmission layer, material is NPB, thickness is 60nm; Evaporation the first luminescent layer, material is ADN, thickness is 5nm; Evaporation the first electron transfer layer, material is TPBi, thickness is 200nm; Prepare charge generation layer: by the first doped layer, the second doped layer and the 3rd doped layer, formed.Evaporation the first doped layer, material comprises Yb and is entrained in the WO in Yb
3, WO
3with the mass ratio of Yb be 1:20, thickness is 20nm; Evaporation the second doped layer, material comprises Ca and is entrained in the Al in Ca, and the mass ratio of Al and Ca is 3:10, and thickness is 2nm; Evaporation the 3rd doped layer is that material comprises Pt and is entrained in the WO in Pt
3, WO
3with the mass ratio of Pt be 1:2, thickness is 20nm; Evaporation the second hole transmission layer, material is NPB, thickness is 20nm; Evaporation the second luminescent layer, material is ADN, thickness is 7nm; Evaporation the second electron transfer layer, material is TAZ, thickness is 40nm; Evaporation electron injecting layer, material is CsN
3, thickness is 0.5nm; Evaporation negative electrode, material is Pt, thickness is 60nm, finally obtains needed electroluminescent device.Evaporation is 2 * 10 at vacuum pressure
-4under Pa, carry out, organic material evaporation speed is 0.1nm/s, and the evaporation speed of metallic compound is 10nm/s, and the evaporation speed of metal is 1nm/s.
Embodiment 3
Structure prepared by the present embodiment is IZO/MoO
3/ TAPC/Alq
3/ TAZ/Mg:V
2o
5/ Yb:Pt/V
2o
5: Ag/TCTA/Alq
3the organic electroluminescence device of/Bphen/CsF/Al.
First IZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface; Evaporation is prepared hole injection layer, and material is MoO
3, thickness is 20nm; Evaporation is prepared the first hole transmission layer, and material is TAPC, and thickness is 30nm; Evaporation is prepared the first luminescent layer, and material is Alq
3, thickness is 40nm; Evaporation is prepared the first electron transfer layer, and material is TAZ, and thickness is 200nm; Prepare charge generation layer: by the first doped layer, the second doped layer and the 3rd doped layer, formed.Evaporation the first doped layer, material comprises Mg and is entrained in the V in Mg
2o
5, V
2o
5with the mass ratio of Mg be 1:5, thickness is 5nm; Evaporation the second doped layer, material comprises Yb and is entrained in the Pt in Yb, and the mass ratio of Pt and Yb is 1:10, and thickness is 20nm; Evaporation the 3rd doped layer, material comprises Ag and is entrained in the V in Ag
2o
5, V
2o
5with the mass ratio of Ag be 1:10, thickness is 5nm; Evaporation is prepared the second hole transmission layer, and material is TCTA, and thickness is 60nm; Evaporation is prepared the second luminescent layer, and material is Alq
3, thickness is 30nm; Evaporation is prepared the second electron transfer layer, and material is Bphen, and thickness is 40nm; Evaporation is prepared electron injecting layer, and material is CsF, and thickness is 10nm; Evaporation is prepared negative electrode, and material is Al, and thickness is 300nm, finally obtains needed electroluminescent device.Evaporation is 5 * 10 at vacuum pressure
-3under Pa, carry out, organic material evaporation speed is 1nm/s, and the evaporation speed of metallic compound is 1nm/s, and the evaporation speed of metal is 10nm/s.
Embodiment 4
Structure prepared by the present embodiment is IZO/MoO
3/ TCTA/DCJTB/Bphen/Ba:MoO
3/ Ba:Au/MoO
3: Au/NPB/DCJTB/TAZ/Cs
2cO
3the organic electroluminescence device of/Au.
First IZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface; Evaporation is prepared hole injection layer, and material is MoO
3, thickness is 30nm; Evaporation is prepared the first hole transmission layer, and material is TCTA, and thickness is 50nm; Evaporation is prepared the first luminescent layer, and material is DCJTB, and thickness is 5nm; Evaporation is prepared the first electron transfer layer, and material is Bphen, and thickness is 40nm; Prepare charge generation layer: by the first doped layer, the second doped layer and the 3rd doped layer, formed.Evaporation the first doped layer, material comprises Ba and is entrained in the MoO in Ba
3, MoO
3with the mass ratio of Ba be 1: 10, thickness is 15nm; Evaporation the second doped layer, material comprises Ba and is entrained in the Au in Ba, and the mass ratio of Au and Ba is 1:4, and thickness is 3nm; Evaporation the 3rd doped layer, material comprise Au and be entrained in Au for MoO
3: Au, MoO
3with the mass ratio of Au be 2:5, thickness is 30nm; Evaporation is prepared the second hole transmission layer, and material is NPB, and thickness is 50nm; Evaporation is prepared the second luminescent layer, and material is DCJTB, and thickness is 5nm; Evaporation is prepared the second electron transfer layer, and material is TAZ, and thickness is 100nm; Evaporation is prepared electron injecting layer, and material is Cs
2cO
3, thickness is 2nm; Evaporation is prepared negative electrode, and material is Au, and thickness is 180nm, finally obtains needed electroluminescent device.Evaporation is 5 * 10 at vacuum pressure
-4under Pa, carry out, organic material evaporation speed is 0.6nm/s, and the evaporation speed of metal compound layer is 3nm/s, and the evaporation speed of metal is 2nm/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, is characterized in that, comprises the anode stacking gradually, hole injection layer, the first hole transmission layer, the first luminescent layer, the first electron transfer layer, charge generation layer, the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode, described charge generation layer comprises the first doped layer that is laminated in described the first electron transfer layer surface, be formed at second doped layer on described the first doped layer surface and be formed at the 3rd doped layer on described the second doped layer surface, the material of described the first doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described in described the first doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:20 ~ 1:5, the material of described the second doped layer comprises low workfunction metal and is entrained in the high-work-function metal in described low workfunction metal, described in described the second doped layer, the mass ratio of high-work-function metal and described low workfunction metal is 1:10 ~ 3:10, the material of described the 3rd doped layer comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal, described in described the 3rd doped layer, the mass ratio of metal oxide and described high-work-function metal is 1:10 ~ 1:2, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described high work function is selected from silver, aluminium, at least one in platinum and gold, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described the first doped layer is 5nm ~ 20nm, and the thickness of described the second doped layer is 2nm ~ 20nm, and the thickness of described the 3rd doped layer is 5nm ~ 30nm.
3. organic electroluminescence device according to claim 1, it is characterized in that, the material of described the first luminescent layer and described the second 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.
4. organic electroluminescence device according to claim 1, it is characterized in that, the material of described the first hole transmission layer and described the second hole transmission layer is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4 " tri-(carbazole-9-yl) triphenylamine and N; N '-(1-naphthyl)-N, N '-diphenyl-4, at least one in 4 '-benzidine.
5. organic electroluminescence device according to claim 1, is characterized in that, the material of described the first electron transfer layer and described the second 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 anode surface successively evaporation, prepare hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer;
At described the first electron transfer layer surface evaporation, prepare the first doped layer, the material of described the first doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described in described the first doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:20 ~ 1:5, described low workfunction metal is selected from least one in calcium, ytterbium, magnesium and barium, and described metal oxide is selected from least one in molybdenum trioxide, tungstic acid and vanadic oxide;
At described the first doped layer surface evaporation, prepare the second doped layer, the material of described the second doped layer comprises low workfunction metal and is entrained in the high-work-function metal in described low workfunction metal, described in described the second doped layer, the mass ratio of high-work-function metal and described low workfunction metal is 1:10 ~ 3:10, described low workfunction metal is selected from least one in calcium, ytterbium, magnesium and barium, and described high work function is selected from least one in silver, aluminium, platinum and gold;
At described the second doped layer surface evaporation, prepare the 3rd doped layer, the material of described the 3rd doped layer comprises high-work-function metal and is entrained in the metal oxide in described high-work-function metal, described in described the 3rd doped layer, the mass ratio of metal oxide and described high-work-function metal is 1:10 ~ 1:2, described high work function is selected from least one in silver, aluminium, platinum and gold, and described metal oxide is selected from least one in molybdenum trioxide, tungstic acid and vanadic oxide; And
On the 3rd doped layer surface successively evaporation, form the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode.
7. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: the material of described the first luminescent layer and described the second 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.
8. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: the material of described the first hole transmission layer and described the second hole transmission layer is selected from 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4 " tri-(carbazole-9-yl) triphenylamine and N, N '-(1-naphthyl)-N; N '-diphenyl-4, at least one in 4 '-benzidine.
9. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: the thickness of described the first doped layer is 5nm ~ 20nm, and the thickness of described the second doped layer is 2nm ~ 20nm, and the thickness of described the 3rd doped layer is 5nm ~ 30nm.
10. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: before described anode surface forms hole injection layer, first antianode carries out pre-treatment, pre-treatment comprises: anode is carried out to photoetching treatment, be cut into needed size, adopt liquid detergent, deionized water, acetone, ethanol, each Ultrasonic Cleaning of isopropyl acetone 15min, to remove the organic pollution of anode surface.
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