CN103972401A - Organic light-emitting device and production method thereof - Google Patents

Organic light-emitting device and production method thereof Download PDF

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CN103972401A
CN103972401A CN201310038848.9A CN201310038848A CN103972401A CN 103972401 A CN103972401 A CN 103972401A CN 201310038848 A CN201310038848 A CN 201310038848A CN 103972401 A CN103972401 A CN 103972401A
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layer
metal
evaporation
phthalocyanine
low workfunction
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周明杰
王平
黄辉
陈吉星
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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    • 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]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H10K50/125—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light
    • H10K50/13—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit
    • H10K50/131—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit with spacer layers between the electroluminescent 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
    • H10K50/16—Electron 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]
    • H10K50/17—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
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/17—Carrier injection layers
    • H10K50/171—Electron 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
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/311—Phthalocyanine

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  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Electroluminescent Light Sources (AREA)

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 low work function metal layer laminated on the surface of the first electron transport layer, a metal doped layer formed on the surface of the low work function metal layer and a phthalocyanine metal layer formed on the surface of the metal doped layer, the low work function metal layer is made of at least one of calcium, ytterbium, magnesium and barium, the metal doped layer is made of materials including low work function metal and metal oxides doped in the low work function metal, and the phthalocyanine metal layer is made of materials selected from at least one of copper phthalocyanine, magnesium phthalocyanine, zinc phthalocyanine and vanadium phthalocyanine. 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

Organic electroluminescence device and preparation method thereof
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.But 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.
A kind of 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 low workfunction metal layer that is laminated in described the first electron transfer layer surface, be formed at the metal-doped layer on described low workfunction metal layer surface and be formed at the surperficial phthalocyanine metal layer of described metal-doped layer, the material of described low workfunction metal layer is selected from calcium, ytterbium, at least one in magnesium and barium, the material of described metal-doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide, described in described metal-doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:5 ~ 3:5, the material of described phthalocyanine metal layer is selected from CuPc, magnesium phthalocyanine, at least one in Phthalocyanine Zinc and phthalocyanine vanadium.
In an embodiment, the thickness of described low workfunction metal layer is 1nm ~ 20nm therein, and the thickness of described metal-doped layer is 5nm ~ 20nm, and the thickness of described phthalocyanine metal layer is 1nm ~ 10nm.
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:
Prepare hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer at anode surface successively evaporation;
Prepare low workfunction metal layer at described the first electron transfer layer surface evaporation, the material of described low workfunction metal layer is selected from least one in calcium, ytterbium, magnesium and barium, and evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 1nm/s ~ 10nm/s;
On described low workfunction metal layer surface, evaporation is prepared metal-doped layer, the material of described metal-doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide, described in described metal-doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:5 ~ 3:5, described low workfunction metal and metal oxide evaporate respectively in two evaporation boats, evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, the evaporation speed of described low workfunction metal is 1nm/s ~ 10nm/s, and the evaporation speed of described metal oxide is 1nm/s ~ 10nm/s,
Prepare phthalocyanine metal layer at the surperficial evaporation of described metal-doped layer, the material of described phthalocyanine metal layer is selected from least one in CuPc, magnesium phthalocyanine, Phthalocyanine Zinc and phthalocyanine vanadium, and evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s; And
Form the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode on phthalocyanine metal layer surface successively evaporation.
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 low workfunction metal layer is 1nm ~ 20nm therein, and the thickness of described metal-doped layer is 5nm ~ 20nm, and the thickness of described phthalocyanine metal layer is 1nm ~ 10nm.
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, the each Ultrasonic Cleaning 15min of isopropyl acetone, to remove the organic pollution of anode surface.
Above-mentioned organic electroluminescence device and preparation method thereof, charge generation layer is by low workfunction metal layer, metal-doped layer and phthalocyanine metal layer composition, low workfunction metal layer can be used as the electron production layer of charge generation layer, reduce the injection barrier of electronics, be conducive to the injection of electronics, and metal-doped layer by metal oxide as doping object, low workfunction metal can provide electronics, improve conductivity and the photopermeability of charge generation layer, and can eliminate the energy level difference between metal-doped layer and low workfunction metal layer, the injection efficiency of electronics is got a promotion, reduce energy loss, metal oxide can provide electronics and hole, both generation efficiencies are improved significantly, and phthalocyanine metal layer can reduce hole injection barrier, improve the injection efficiency in hole, and the phthalocyanine metal of polycrystalline can form crystallization, after crystallization, crystal has obvious scattering process to light, improve light scattering ability, thereby raising light extraction efficiency, charge generation layer can effectively improve the luminous efficiency of organic electroluminescence device.
Brief description of the drawings
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is the preparation method's of the organic electroluminescence device of an execution mode flow chart;
Fig. 3 is brightness and the luminous efficiency graph of a relation of the organic electroluminescence device prepared of embodiment 1.
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 the 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 that stack 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 MoO 3.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 TAPC.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 low workfunction metal layer 42, be formed at the metal-doped layer 44 on low workfunction metal layer 42 surface and be formed at the phthalocyanine metal layer on metal-doped layer 44 surface.
The work function of the material of low workfunction metal layer 42 is-2.0 ~-4.0eV, and preferred, the material of low workfunction metal layer 42 is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).The thickness of low workfunction metal layer 42 is 1nm ~ 20nm.
Metal-doped layer 44 is formed at low workfunction metal layer 42 surface.The material of metal-doped layer 44 comprises low workfunction metal and is entrained in the metal oxide in low workfunction metal.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 metal-doped layer 44, the mass ratio of metal oxide and low workfunction metal is 1:5 ~ 3:5.The thickness of metal-doped layer 44 is 5nm ~ 20nm.
Phthalocyanine metal layer 46 is formed at the surface of metal-doped layer 44.The material of phthalocyanine metal layer 46 is selected from least one in CuPc (CuPc), magnesium phthalocyanine (MgPc), Phthalocyanine Zinc (ZnPc) and phthalocyanine vanadium (VPc).The thickness of phthalocyanine metal layer 46 is 1nm ~ 10nm.
The second hole transmission layer 52 is formed at the surface of phthalocyanine metal 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 low workfunction metal layer 42, metal-doped layer 44 and phthalocyanine metal layer 46 form, low workfunction metal layer 42 can be used as the electron production layer of charge generation layer 40, reduce the injection barrier of electronics, be conducive to the injection of electronics, and metal-doped layer 44 by metal oxide as doping object, low workfunction metal can provide electronics, improve conductivity and the photopermeability of charge generation layer 40, and can eliminate the energy level difference between metal-doped layer 44 and low workfunction metal layer 42, the injection efficiency of electronics is got a promotion, reduce energy loss, metal oxide can provide electronics and hole, both generation efficiencies are improved significantly, and phthalocyanine metal layer 46 can reduce hole injection barrier, improve the injection efficiency in hole, and the phthalocyanine metal of polycrystalline can form crystallization, after crystallization, crystal has obvious scattering process to light, improve light scattering ability, thereby raising light extraction efficiency, charge generation layer 40 can effectively improve the luminous efficiency of organic electroluminescence device.
Be appreciated that other functional layers also can be set in this organic electroluminescence device 100 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, prepare hole injection layer 20, the first hole transmission layer 32, the first luminescent layer 34 and the first electron transfer layer 36 at anode surface successively evaporation.
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, the each Ultrasonic Cleaning 15min of isopropyl acetone, 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 MoO 3.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 TAPC.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, prepare low workfunction metal layer 42 at the surperficial evaporation of the first electron transfer layer 36.
The work function of the material of low workfunction metal layer 42 is-2.0 ~-4.0eV, and preferred, the material of low workfunction metal layer 42 is selected from least one in calcium (Ca), ytterbium (Yb), magnesium (Mg) and barium (Ba).The thickness of low workfunction metal layer 42 is 1nm ~ 20nm.Evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 1nm/s ~ 10nm/s.
Step S130, prepare metal-doped layer 44 at the surperficial evaporation of low workfunction metal layer 42.
Metal-doped layer 44 is formed at low workfunction metal layer 42 surface.The material of metal-doped layer 44 comprises low workfunction metal and is entrained in the metal oxide in low workfunction metal.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 metal-doped layer 44, the mass ratio of metal oxide and low workfunction metal is 1:5 ~ 3:5.The thickness of metal-doped layer 44 is 5nm ~ 20nm.Low workfunction metal and metal oxide evaporate respectively in two evaporation boats, and evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, the evaporation speed of low workfunction metal is 1nm/s ~ 10nm/s, and the evaporation speed of metal oxide is 1nm/s～10nm/s.
Step S140, prepare phthalocyanine metal layer 46 at metal-doped layer 44 surperficial evaporation.
Phthalocyanine metal layer 46 is formed at the surface of metal-doped layer 44.The material of phthalocyanine metal layer 46 is selected from least one in CuPc (CuPc), magnesium phthalocyanine (MgPc), Phthalocyanine Zinc (ZnPc) and phthalocyanine vanadium (VPc).The thickness of phthalocyanine metal layer 46 is 1nm ~ 10nm.Evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s.
Step S150, 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 on phthalocyanine metal layer 46 surface successively evaporation.
The second hole transmission layer 52 is formed at the surface of phthalocyanine metal 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 Keithley company of the U.S., CS-100A colorimeter test brightness and the colourity of Japanese Konica Minolta company.
Embodiment 1
Structure prepared by the present embodiment is ITO/MoO 3/ TAPC/BCzVBi/Bphen/Ca/Mg:WO 3/ CuPc/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, the each ultrasonic 15min of isopropyl alcohol, the organic pollution of removal glass surface; Evaporation hole injection layer, material is MoO 3, thickness is 30nm; Evaporation the first hole transmission layer, material is TAPC, 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; Evaporation low workfunction metal layer, material is Ca, thickness is 2nm; Evaporation metal doped layer, material comprises Mg and is entrained in the WO in Mg 3, WO 3with the mass ratio 35:100 of Mg, thickness is 10nm; Evaporation phthalocyanine metal layer, material is CuPc, thickness is 2nm; 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 5 × 10 at vacuum pressure -4under Pa, carry out, organic material evaporation speed is 0.2nm/s, and the evaporation speed of metallic compound is 5nm/s, and the evaporation speed of metal is 3nm/s.
Refer to Fig. 3, the structure that is depicted as preparation in embodiment 1 is ITO/MoO 3/ TAPC/BCzVBi/Bphen/Ca/Mg:WO 3/ CuPc/TCTA/BCzVBi/TPBi/CsN 3the organic electroluminescence device (curve 1) of/Ag is ito glass/MoO with structure prepared by comparative example 3/ TAPC/BCzVBi/Bphen/CsN 3the brightness of the organic electroluminescence device (curve 2) of/Ag 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 brightness, all large than comparative example of the luminous efficiency of embodiment 1, the maximum lumen efficiency of organic electroluminescence device prepared by embodiment 1 is 7.9lm/W, and the luminous efficiency of organic electroluminescence device prepared by comparative example is only 4.8lm/W, and the luminous efficiency of comparative example along with the increase of brightness fast-descending, this explanation, can eliminate the energy level difference between doped layer and metal level, the injection efficiency of electronics is got a promotion, form crystallization, after crystallization, crystal has obvious scattering process to light, improve light scattering ability, thereby raising light extraction efficiency, 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/Ba/Ca:WO 3/ MgPc/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 is prepared the first hole transmission layer, and material is NPB, and thickness is 60nm; Evaporation is prepared the first luminescent layer, and material is ADN, and thickness is 5nm; Evaporation is prepared the first electron transfer layer, and material is TPBi, and thickness is 200nm; Prepare charge generation layer: be made up of low workfunction metal layer, metal-doped layer and phthalocyanine metal layer, low workfunction metal layer material is Ba, and thickness is 6nm; The material of metal-doped layer comprises Ca and is entrained in the WO in Ca 3, WO 3with the mass ratio of Ca be 2:5, thickness is 10nm; The material of phthalocyanine metal layer is MgPc, and thickness is 2nm; Evaporation is prepared the second hole transmission layer, and material is NPB, and thickness is 20nm; Evaporation is prepared the second luminescent layer, and material is ADN, and thickness is 7nm; Evaporation is prepared the second electron transfer layer, and material is TAZ, and thickness is 40nm; Evaporation is prepared electron injecting layer, and material is CsN 3, thickness is 0.5nm; Evaporation is prepared negative electrode, and material is Pt, and 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/Yb/Ba:V 2o 5/ ZnPc/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; Evaporation is prepared charge generation layer: be made up of low workfunction metal layer, metal-doped layer and phthalocyanine metal layer, the metal of low workfunction metal layer is Yb, and thickness is 1nm; The material of metal-doped layer comprises Ba and is entrained in the V in Ba 2o 5, V 2o 5with the mass ratio of Ba be 1:5, thickness is 20nm; The material of phthalocyanine metal layer is ZnPc, and thickness is 1nm; 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/Mg/Mg:WO 3/ VPc/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; Evaporation is prepared charge generation layer: be made up of low workfunction metal layer, metal-doped layer and phthalocyanine metal layer, low workfunction metal layer is Mg, and thickness is 20nm; The material of metal-doped layer comprises Mg and is entrained in the WO in Mg 3, WO 3with the mass ratio of Mg be 3:5, thickness is 5nm; The material of phthalocyanine metal layer is VPc, and thickness is 10nm; 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 8 × 10 at vacuum pressure -4under Pa, carry out, organic material evaporation speed is 0.3nm/s, and the evaporation speed of metal compound layer is 2nm/s, and the evaporation speed of metal is 5nm/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 low workfunction metal layer that is laminated in described the first electron transfer layer surface, be formed at the metal-doped layer on described low workfunction metal layer surface and be formed at the surperficial phthalocyanine metal layer of described metal-doped layer, the material of described low workfunction metal layer is selected from calcium, ytterbium, at least one in magnesium and barium, the material of described metal-doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide, described in described metal-doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:5 ~ 3:5, the material of described phthalocyanine metal layer is selected from CuPc, magnesium phthalocyanine, at least one in Phthalocyanine Zinc and phthalocyanine vanadium.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described low workfunction metal layer is 1nm ~ 20nm, and the thickness of described metal-doped layer is 5nm ~ 20nm, and the thickness of described phthalocyanine metal layer is 1nm ~ 10nm.
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:
Prepare hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer at anode surface successively evaporation;
Prepare low workfunction metal layer at described the first electron transfer layer surface evaporation, the material of described low workfunction metal layer is selected from least one in calcium, ytterbium, magnesium and barium, and evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 1nm/s ~ 10nm/s;
On described low workfunction metal layer surface, evaporation is prepared metal-doped layer, the material of described metal-doped layer comprises low workfunction metal and is entrained in the metal oxide in described low workfunction metal, described low workfunction metal is selected from calcium, ytterbium, at least one in magnesium and barium, described metal oxide is selected from molybdenum trioxide, at least one in tungstic acid and vanadic oxide, described in described metal-doped layer, the mass ratio of metal oxide and described low workfunction metal is 1:5 ~ 3:5, described low workfunction metal and metal oxide evaporate respectively in two evaporation boats, evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, the evaporation speed of described low workfunction metal is 1nm/s ~ 10nm/s, and the evaporation speed of described metal oxide is 1nm/s ~ 10nm/s,
Prepare phthalocyanine metal layer at the surperficial evaporation of described metal-doped layer, the material of described phthalocyanine metal layer is selected from least one in CuPc, magnesium phthalocyanine, Phthalocyanine Zinc and phthalocyanine vanadium, and evaporation is 5 × 10 at vacuum pressure -3~ 2 × 10 -4under Pa, carry out, evaporation speed is 0.1nm/s ~ 1nm/s; And
Form the second hole transmission layer, the second luminescent layer, the second electron transfer layer, electron injecting layer and negative electrode on phthalocyanine metal layer surface successively evaporation.
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 low workfunction metal layer is 1nm ~ 20nm, and the thickness of described metal-doped layer is 5nm ~ 20nm, and the thickness of described phthalocyanine metal layer is 1nm ~ 10nm.
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, the each Ultrasonic Cleaning 15min of isopropyl acetone, to remove the organic pollution of anode surface.
CN201310038848.9A 2013-01-31 2013-01-31 Organic light-emitting device and production method thereof Pending CN103972401A (en)

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Application publication date: 20140806