CN104051639A - Organic light-emitting device and preparation method thereof - Google Patents

Organic light-emitting device and preparation method thereof Download PDF

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Publication number
CN104051639A
CN104051639A CN201310077736.4A CN201310077736A CN104051639A CN 104051639 A CN104051639 A CN 104051639A CN 201310077736 A CN201310077736 A CN 201310077736A CN 104051639 A CN104051639 A CN 104051639A
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layer
aluminium
noble metal
light emitting
thickness
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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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Priority to CN201310077736.4A priority Critical patent/CN104051639A/en
Publication of CN104051639A publication Critical patent/CN104051639A/en
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/80—Constructional details
    • H10K30/865—Intermediate layers comprising a mixture of materials of the adjoining active 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
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Electromagnetism (AREA)
  • Optics & Photonics (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The invention provides an organic light-emitting device and a preparation method thereof. The organic light-emitting device comprises a conductive anode glass substrate, a first light emitting function layer, a charge generating layer, a second light emitting function layer and a cathode, wherein the units are successively laminated. The charge generating layer consists of a first n type layer, a second n type layer and a p type layer, wherein the layers are successively laminated; the lamination of the two n type layers enables the electron transport rate to be improved to the greatest extent; and the p type layer uses aluminum or precious metal and a metallic oxide to carry out doping, thereby improving the hole regeneration injection capability and improving the luminous efficiency of the device. According to the invention, the preparation method is simple and easy control and operation are realized; and the raw material is easy to access.

Description

A kind of organic electroluminescence device and preparation method thereof
Technical field
The invention belongs to organic electroluminescent field, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of taking organic material as luminescent material, the energy conversion device that can be luminous energy the electric energy conversion applying.It has the outstanding properties such as ultra-thin, self-luminous, response are fast, low-power consumption, has application prospect very widely in fields such as demonstration, illuminations.
The structure of organic electroluminescence device is sandwich structure, and containing in the device of sandwich construction, inner side, the two poles of the earth mainly comprises luminescent layer, implanted layer and transport layer.Organic electroluminescence device is carrier injection type luminescent device, add after operating voltage at the two poles of the earth, hole and electronics are injected into the organic material layer of device work from the two poles of the earth respectively, and it is luminous that two kinds of charge carriers form hole-duplet in luminous organic material, and then light sends from electrode.
At present, in order to improve luminosity and luminous efficiency, increasing research is taking laminated device as main, this structure normally uses charge generation layer as articulamentum, several light emitting functional layer (luminescence unit) to be together in series, compared with unit component, multilayer devices often has current efficiency and luminosity at double.In laminated device, conventionally utilize two or more material with hole injectability or electronic injection ability as charge generation layer (as Cs:BCP/V 2o 5), or utilize N-shaped and p-type doped layer as charge generation layer (as N-shaped (Alq 3: Li) and p-type (NPB:FeCl 3)) be linked in sequence multiple luminescence units and form, but adopt the luminous efficiency of this charge generation layer laminated organic electroluminescent device lower.
Summary of the invention
In order to address the above problem, the present invention aims to provide a kind of organic electroluminescence device having compared with high light-emitting efficiency.The present invention also provides a kind of preparation method of organic electroluminescence device.
First aspect, the invention provides a kind of organic electroluminescence device, comprises the conductive anode substrate of glass, the first light emitting functional layer, charge generation layer, the second light emitting functional layer and the negative electrode that stack gradually;
Described charge generation layer comprises the first N-shaped layer, the second N-shaped layer and the p-type layer that stack gradually; The material of described the first N-shaped layer is the mixture of lithium salts and aluminium or noble metal formation, and the mass fraction that described lithium salts accounts for described aluminium or noble metal is 10～60%; The material of described the second N-shaped layer is the mixture that lithium salts and electron transport material form, and the mass fraction that described lithium salts accounts for described electron transport material is 10～40%; The material of described p-type layer is the mixture of metal oxide and aluminium or noble metal formation, and the mass fraction that described metal oxide accounts for described aluminium or noble metal is 5～30%;
Described lithium salts is the one in lithium fluoride, lithium carbonate and lithium chloride; Described noble metal is the one in silver, platinum and gold; Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole; Described metal oxide is the one in molybdenum trioxide, tungstic acid and vanadic oxide.
Preferably, the material of conductive anode substrate of glass is indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).More preferably, the material of conductive anode substrate of glass is ITO.
The first light emitting functional layer is arranged in conductive anode substrate of glass.
The first light emitting functional layer comprises the first luminescent layer, also comprises at least one in the first hole injection layer, the first hole transmission layer and the first electron transfer layer.
Preferably, the first light emitting functional layer comprises the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually.
Preferably, the material of the first hole injection layer is molybdenum trioxide (MoO 3), tungstic acid (WO 3) or vanadic oxide (V 2o 5).More preferably, the material of the first hole injection layer is MoO 3.
Preferably, the thickness of the first hole injection layer is 20～80nm.More preferably, the thickness of the first hole injection layer is 40nm.
Preferably, the material of the first hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB).More preferably, the material of the first hole transmission layer is NPB.
Preferably, the thickness of the first hole transmission layer is 20～60nm.More preferably, the thickness of the first hole transmission layer is 40nm.
Preferably, the material of the first luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) or oxine aluminium (Alq 3).More preferably, the material of the first luminescent layer is Alq 3.
Preferably, the thickness of the first luminescent layer is 5～40nm.More preferably, the thickness of the first luminescent layer is 25nm.
Preferably, the material of the first electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of the first electron transfer layer is Bphen.
Preferably, the thickness of the first electron transfer layer is 40～200nm.More preferably, the thickness of the first electron transfer layer is 60nm.
In the first light emitting functional layer, set gradually the first N-shaped layer, the second N-shaped layer and p-type layer.
In the present invention, the first N-shaped layer, the second N-shaped layer and p-type layer are charge generation layer.
The material of the first N-shaped layer is lithium salt doping to the mixture forming in aluminium or noble metal, and wherein, lithium salts is guest materials, and aluminium or noble metal are material of main part.
In the material of the first N-shaped layer, the quality of guest materials is 10～60% of material of main part quality, and to account for the mass fraction of aluminium or noble metal be 10～60% to lithium salts.Preferably, in the material of the first N-shaped layer, the quality of guest materials is 40% of material of main part quality.
Lithium salts in the material of the first N-shaped layer is lithium fluoride (LiF), lithium carbonate (Li 2cO 3) and lithium chloride (LiCl) in one.Preferably, lithium salts is lithium fluoride.
Noble metal in the material of the first N-shaped layer is the one in silver (Ag), platinum (Pt) and gold (Au).
Preferably, the thickness of the first N-shaped layer is 2～20nm.More preferably, the thickness of the first N-shaped layer is 10nm.
The material of the second N-shaped layer is lithium salt doping to the mixture forming in electron transport material, and wherein, lithium salts is guest materials, and electron transport material is material of main part.
In the material of the second N-shaped layer, the quality of guest materials is 10～40% of material of main part quality, and to account for the mass fraction of electron transport material be 10～40% to lithium salts.Preferably, in the material of the second N-shaped layer, the quality of guest materials is 25% of material of main part quality.
Lithium salts in the material of the second N-shaped layer is lithium fluoride (LiF), lithium carbonate (Li 2cO 3) and lithium chloride (LiCl) in one.Preferably, lithium salts is lithium chloride.
Preferably, electron transport material is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole (PBD).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).
Preferably, the thickness of the second N-shaped layer is 1～10nm.More preferably, the thickness of the second N-shaped layer is 5nm.
The material of p-type layer is doped metallic oxide to the mixture forming in aluminium or noble metal, and wherein, metal oxide is guest materials, and aluminium or noble metal are material of main part.
In the material of p-type layer, the quality of guest materials is 5～30% of material of main part quality, and to account for the mass fraction of aluminium or noble metal be 5～30% to metal oxide.Preferably, in the material of p-type layer, the quality of guest materials is 20% of material of main part quality.
Preferably, metal oxide is molybdenum trioxide (MoO 3), tungstic acid (WO 3) and vanadic oxide (V 2o 5) in one.More preferably, metal oxide is molybdenum trioxide.
Noble metal in the material of p-type layer is the one in silver (Ag), platinum (Pt) and gold (Au).
Preferably, the thickness of p-type layer is 2～30nm.More preferably, the thickness of p-type layer is 20nm.
Charge generation layer is made up of the first N-shaped layer stacking gradually (aluminium or the noble metal of doping lithium salts), the second N-shaped layer (the crystallinity electron transport material of doping lithium salts) and p-type layer (aluminium of blended metal oxide or noble metal), the stacked speed that can farthest improve electric transmission of two N-shaped layers, use lithium salts to adulterate, in improving electric transmission speed, can improve conductivity; The existence of aluminium or noble metal can improve the light transmission rate of charge generation layer; The crystallinity electron transport material of the second N-shaped layer in the middle of being positioned at can form after crystallization arranges orderly structure, and light is carried out to scattering; P-type layer uses aluminium or noble metal and metal oxide to adulterate, the work function of metal oxide is lower, it is the bipolarity metal oxide with the generation of good hole and transmittability, can effectively carry out injection and the transmission in hole, improve hole regeneration injectability, effectively improve device luminous efficiency and brightness.
The second light emitting functional layer is arranged on p-type layer.
The second light emitting functional layer comprises the second luminescent layer, also comprises at least one in the second hole transmission layer, the second electron transfer layer and the second electron injecting layer.
Preferably, the second light emitting functional layer comprises the second hole transmission layer, the second luminescent layer, the second electron transfer layer and the second electron injecting layer that stack gradually.
Preferably, the material of the second hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB).More preferably, the material of the second hole transmission layer is NPB.
Preferably, the thickness of the second hole transmission layer is 20～60nm.More preferably, the thickness of the second hole transmission layer is 40nm.
Preferably, the material of the second luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) or oxine aluminium (Alq 3).More preferably, the material of the second luminescent layer is Alq 3.
Preferably, the thickness of the second luminescent layer is 5～40nm.More preferably, the thickness of the second luminescent layer is 25nm.
Preferably, the material of the second electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of the second electron transfer layer is TAZ.
Preferably, the thickness of the second electron transfer layer is 40～200nm.More preferably, the thickness of the second electron transfer layer is 80nm.
Preferably, the material of the second electron injecting layer is cesium carbonate (Cs 2cO 3), cesium fluoride (CsF), nitrine caesium (CsN 3) and lithium fluoride (LiF) in one.More preferably, the material of the second electron injecting layer is CsN 3.
Preferably, the thickness of the second electron injecting layer is 0.5～10nm.More preferably, the thickness of the second electron injecting layer is 1nm.
Negative electrode is arranged in the second light emitting functional layer.
Preferably, the material of negative electrode is the one in silver, aluminium, platinum and gold.More preferably, the material of negative electrode is aluminium.
Preferably, the thickness of negative electrode is 60～300nm.More preferably, the thickness of negative electrode is 100nm.
Second aspect, the invention provides a kind of preparation method of organic electroluminescence device, comprises the following steps:
Conductive anode substrate of glass is provided;
In described conductive anode substrate of glass, thermal resistance evaporation is prepared the first light emitting functional layer, charge generation layer, the second light emitting functional layer and negative electrode successively, obtains organic electroluminescence device;
Described charge generation layer comprises the first N-shaped layer, the second N-shaped layer and the p-type layer that stack gradually; The material of described the first N-shaped layer is the mixture of lithium salts and aluminium or noble metal formation, and the mass fraction that described lithium salts accounts for described aluminium or noble metal is 10～60%; The material of described the second N-shaped layer is the mixture that lithium salts and electron transport material form, and the mass fraction that described lithium salts accounts for described electron transport material is 10～40%; The material of described p-type layer is the mixture of metal oxide and aluminium or noble metal formation, and the mass fraction that described metal oxide accounts for described aluminium or noble metal is 5～30%;
Described lithium salts is the one in lithium fluoride, lithium carbonate and lithium chloride; Described noble metal is the one in silver, platinum and gold; Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole; Described metal oxide is the one in molybdenum trioxide, tungstic acid and vanadic oxide.
By the cleaning to conductive anode substrate of glass, remove the organic pollution of conductive anode glass basic surface.
Particularly, the clean operation of conductive anode substrate of glass is: conductive anode substrate of glass is used to distilled water, alcohol flushing successively, then be placed on soaked overnight in isopropyl alcohol, remove the organic pollution of conductive anode glass surface, obtain clean conductive anode substrate of glass.
Preferably, the material of conductive anode substrate of glass is indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).More preferably, the material of conductive anode substrate of glass is ITO.
The first light emitting functional layer is arranged in conductive anode substrate of glass by the method for thermal resistance evaporation.
Preferably, when thermal resistance evaporation is prepared the first light emitting functional layer, condition is pressure 5 × 10 -5～2 × 10 -3pa, speed 0.1～1nm/s.
The first light emitting functional layer comprises the first luminescent layer, also comprises at least one in the first hole injection layer, the first hole transmission layer and the first electron transfer layer.
Preferably, the first light emitting functional layer comprises the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually.
Preferably, the material of the first hole injection layer is molybdenum trioxide (MoO 3), tungstic acid (WO 3) or vanadic oxide (V 2o 5).More preferably, the material of the first hole injection layer is MoO 3.
Preferably, the thickness of the first hole injection layer is 20～80nm.More preferably, the thickness of the first hole injection layer is 40nm.
Preferably, the material of the first hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB).More preferably, the material of the first hole transmission layer is NPB.
Preferably, the thickness of the first hole transmission layer is 20～60nm.More preferably, the thickness of the first hole transmission layer is 40nm.
Preferably, the material of the first luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) or oxine aluminium (Alq 3).More preferably, the material of the first luminescent layer is Alq 3.
Preferably, the thickness of the first luminescent layer is 5～40nm.More preferably, the thickness of the first luminescent layer is 25nm.
Preferably, the material of the first electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of the first electron transfer layer is Bphen.
Preferably, the thickness of the first electron transfer layer is 40～200nm.More preferably, the thickness of the first electron transfer layer is 60nm.
In the first light emitting functional layer, thermal resistance evaporation arranges the first N-shaped layer, the second N-shaped layer and p-type layer successively.
In the present invention, the first N-shaped layer, the second N-shaped layer and p-type layer are charge generation layer.
Preferably, when thermal resistance evaporation is prepared charge generation layer, condition is pressure 5 × 10 -5～2 × 10 -3pa, speed 0.1～1nm/s.
The material of the first N-shaped layer is lithium salt doping to the mixture forming in aluminium or noble metal, and wherein, lithium salts is guest materials, and aluminium or noble metal are material of main part.
In the material of the first N-shaped layer, the quality of guest materials is 10～60% of material of main part quality, and to account for the mass fraction of aluminium or noble metal be 10～60% to lithium salts.Preferably, in the material of the first N-shaped layer, the quality of guest materials is 40% of material of main part quality.
Lithium salts in the material of the first N-shaped layer is lithium fluoride (LiF), lithium carbonate (Li 2cO 3) and lithium chloride (LiCl) in one.Preferably, lithium salts is lithium fluoride.
Noble metal in the material of the first N-shaped layer is the one in silver (Ag), platinum (Pt) and gold (Au).
Preferably, the thickness of the first N-shaped layer is 2～20nm.More preferably, the thickness of the first N-shaped layer is 10nm.
The material of the second N-shaped layer is lithium salt doping to the mixture forming in electron transport material, and wherein, lithium salts is guest materials, and electron transport material is material of main part.
In the material of the second N-shaped layer, the quality of guest materials is 10～40% of material of main part quality, and to account for the mass fraction of electron transport material be 10～40% to lithium salts.Preferably, in the material of the second N-shaped layer, the quality of guest materials is 25% of material of main part quality.
Lithium salts in the material of the second N-shaped layer is lithium fluoride (LiF), lithium carbonate (Li 2cO 3) and lithium chloride (LiCl) in one.Preferably, lithium salts is lithium chloride.
Preferably, electron transport material is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole (PBD).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).
Preferably, the thickness of the second N-shaped layer is 1～10nm.More preferably, the thickness of the second N-shaped layer is 5nm.
The material of p-type layer is doped metallic oxide to the mixture forming in aluminium or noble metal, and wherein, metal oxide is guest materials, and aluminium or noble metal are material of main part.
In the material of p-type layer, the quality of guest materials is 5～30% of material of main part quality, and to account for the mass fraction of aluminium or noble metal be 5～30% to metal oxide.Preferably, in the material of p-type layer, the quality of guest materials is 20% of material of main part quality.
Preferably, metal oxide is molybdenum trioxide (MoO 3), tungstic acid (WO 3) and vanadic oxide (V 2o 5) in one.More preferably, metal oxide is molybdenum trioxide.
Noble metal in the material of p-type layer is the one in silver (Ag), platinum (Pt) and gold (Au).
Preferably, the thickness of p-type layer is 2～30nm.More preferably, the thickness of p-type layer is 20nm.
Charge generation layer is made up of the first N-shaped layer stacking gradually (aluminium or the noble metal of doping lithium salts), the second N-shaped layer (the crystallinity electron transport material of doping lithium salts) and p-type layer (aluminium of blended metal oxide or noble metal), the stacked speed that can farthest improve electric transmission of two N-shaped layers, use lithium salts to adulterate, in improving electric transmission speed, can improve conductivity; The existence of aluminium or noble metal can improve the light transmission rate of charge generation layer; The crystallinity electron transport material of the second N-shaped layer in the middle of being positioned at can form after crystallization arranges orderly structure, and light is carried out to scattering; P-type layer uses aluminium or noble metal and metal oxide to adulterate, the work function of metal oxide is lower, it is the bipolarity metal oxide with the generation of good hole and transmittability, can effectively carry out injection and the transmission in hole, improve hole regeneration injectability, effectively improve device luminous efficiency and brightness.
The second light emitting functional layer is arranged on p-type layer by thermal resistance evaporation.
Preferably, when thermal resistance evaporation is prepared the second light emitting functional layer, condition is pressure 5 × 10 -5～2 × 10 -3pa, speed 0.1～1nm/s.
The second light emitting functional layer comprises the second luminescent layer, also comprises at least one in the second hole transmission layer, the second electron transfer layer and the second electron injecting layer.
Preferably, the second light emitting functional layer comprises the second hole transmission layer, the second luminescent layer, the second electron transfer layer and the second electron injecting layer that stack gradually.
Preferably, the material of the second hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB).More preferably, the material of the second hole transmission layer is NPB.
Preferably, the thickness of the second hole transmission layer is 20～60nm.More preferably, the thickness of the second hole transmission layer is 40nm.
Preferably, the material of the second luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) or oxine aluminium (Alq 3).More preferably, the material of the second luminescent layer is Alq 3.
Preferably, the thickness of the second luminescent layer is 5～40nm.More preferably, the thickness of the second luminescent layer is 25nm.
Preferably, the material of the second electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of the second electron transfer layer is TAZ.
Preferably, the thickness of the second electron transfer layer is 40～200nm.More preferably, the thickness of the second electron transfer layer is 80nm.
Preferably, the material of the second electron injecting layer is cesium carbonate (Cs 2cO 3), cesium fluoride (CsF), nitrine caesium (CsN 3) and lithium fluoride (LiF) in one.More preferably, the material of the second electron injecting layer is CsN 3.
Preferably, the thickness of the second electron injecting layer is 0.5～10nm.More preferably, the thickness of the second electron injecting layer is 1nm.
Negative electrode is arranged in the second light emitting functional layer by thermal resistance evaporation.
Preferably, when thermal resistance evaporation is prepared negative electrode, condition is pressure 5 × 10 -5～2 × 10 -3pa, speed 1～10nm/s.
Preferably, the material of negative electrode is the one in silver, aluminium, platinum and gold.More preferably, the material of negative electrode is aluminium.
Preferably, the thickness of negative electrode is 60～300nm.More preferably, the thickness of negative electrode is 100nm.
The present invention has following beneficial effect:
Charge generation layer prepared by the present invention is made up of the first N-shaped layer stacking gradually (aluminium or the noble metal of doping lithium salts), the second N-shaped layer (the crystallinity electron transport material of doping lithium salts) and p-type layer (aluminium of blended metal oxide or noble metal), the stacked speed that can farthest improve electric transmission of two N-shaped layers, use lithium salts to adulterate, in improving electric transmission speed, can improve conductivity; The existence of aluminium or noble metal can improve the light transmission rate of charge generation layer; The crystallinity electron transport material of the second N-shaped layer in the middle of being positioned at can form after crystallization arranges orderly structure, and light is carried out to scattering; P-type layer uses aluminium or noble metal and metal oxide to adulterate, the work function of metal oxide is lower, it is the bipolarity metal oxide with the generation of good hole and transmittability, can effectively carry out injection and the transmission in hole, improve hole regeneration injectability, effectively improve device luminous efficiency and brightness.
Meanwhile, preparation method of the present invention is simple, be easy to control and operation, and raw material easily obtains.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structure chart of the organic electroluminescence device that provides of the embodiment of the present invention 1;
Fig. 2 is organic electroluminescence device and the voltage of existing organic electroluminescence device and the graph of a relation of brightness that the embodiment of the present invention 1 provides.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) ito glass substrate is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 4 × 10 -4under the condition of Pa, prepare the first light emitting functional layer with evaporation speed thermal resistance evaporation in clean ito glass substrate of 0.6nm/s, comprise the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually;
Particularly, the material of the first hole injection layer is MoO 3, thickness is 40nm; The material of the first hole transmission layer is NPB, and thickness is 40nm; The material of the first luminescent layer is Alq 3, thickness is 25nm; The material of the first electron transfer layer is Bphen, and thickness is 60nm;
(3) be 4 × 10 at pressure -4under the condition of Pa, using the evaporation speed of 0.6nm/s on the first electron transfer layer successively thermal resistance evaporation prepare the first N-shaped layer, the second N-shaped layer and p-type layer as charge generation layer;
Particularly, the material of the first N-shaped layer is that LiF is doped to the composite material forming in Ag, and the quality of LiF is that the thickness of 40%, the first N-shaped layer of Ag quality is 10nm; The material of the second N-shaped layer is for thinking doped body, and LiCl is doped to the composite material forming in Bphen, and the quality of LiCl is that 25%, the second N-shaped layer thickness of Bphen quality is 5nm; The material of p-type layer is MoO 3be doped to the composite material forming in Ag, MoO 3quality be 20% of Ag quality, the thickness of p-type layer is 20nm;
(4) be 4 × 10 at pressure -4under the condition of Pa, evaporation speed thermal resistance evaporation on p-type layer with 0.6nm/s is prepared the second light emitting functional layer, comprise the second hole transmission layer, the second luminescent layer, the second electron transfer layer, the second electron injecting layer that stack gradually, evaporation speed evaporation on the second electron injecting layer with 6nm/s is prepared negative electrode, obtains needed electroluminescent device;
Particularly, the material of the second hole transmission layer is NPB, and thickness is 40nm; The material of the second luminescent layer is Alq 3, thickness is 25nm; The material of the second electron transfer layer is TAZ, and thickness is 80nm; The material of the second electron injecting layer is CsN 3, thickness is 1nm; The material of negative electrode is Al, and thickness is 100nm.
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: ito glass/MoO 3/ NPB/Alq 3/ Bphen/Ag:LiF/Bphen:LiCl/Ag:MoO 3/ NPB/Alq 3/ TAZ/CsN 3/ Al.
Fig. 1 is the structural representation of the organic electroluminescence device of the present embodiment.As shown in Figure 1, the structure of this organic electroluminescence device comprises that the conductive anode substrate of glass 10, the second light emitting functional layer 20(that stack gradually comprise the first hole injection layer 201, the first hole transport 202, the first luminescent layer 203 and the first electron transfer layer 204), charge generation layer 30(comprises the first N-shaped layer 301, the second N-shaped layer 302, p-type layer 303), the second light emitting functional layer 40(comprises the second hole transmission layer 401, the second luminescent layer 402, the second electron transfer layer 403 and the second electron injecting layer 404) and negative electrode 50.
Embodiment 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) AZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 5 × 10 -5under the condition of Pa, prepare the first light emitting functional layer with evaporation speed thermal resistance evaporation in clean AZO substrate of glass of 1nm/s, comprise the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually;
Particularly, the material of the first hole injection layer is V 2o 5, thickness is 80nm; The material of the first hole transmission layer is TAPC, and thickness is 20nm; The material of the first luminescent layer is DCJTB, and thickness is 5nm; The material of the first electron transfer layer is TAZ, and thickness is 40nm;
(3) be 5 × 10 at pressure -5under the condition of Pa, using the evaporation speed of 1nm/s on the first electron transfer layer successively thermal resistance evaporation prepare the first N-shaped layer, the second N-shaped layer and p-type layer as charge generation layer;
Particularly, the material of the first N-shaped layer is Li 2cO 3be doped to the composite material forming in Al, Li 2cO 3quality be that the thickness of 60%, the first N-shaped layer of Al quality is 20nm; The material of the second N-shaped layer is to be doped to LiF the composite material forming in PBD, and the quality of LiF is that 10%, the second N-shaped layer thickness of PBD quality is 1nm; The material of p-type layer is WO 3be doped to the composite material forming in Pt, WO 3quality be 30% of Pt quality, the thickness of p-type layer is 30nm;
(4) be 5 × 10 at pressure -5under the condition of Pa, evaporation speed thermal resistance evaporation on p-type layer with 1nm/s is prepared the second light emitting functional layer, comprise the second hole transmission layer, the second luminescent layer, the second electron transfer layer, the second electron injecting layer that stack gradually, evaporation speed evaporation on the second electron injecting layer with 10nm/s is prepared negative electrode, obtains needed electroluminescent device;
Particularly, the material of the second hole transmission layer is TAPC, and thickness is 20nm; The material of the second luminescent layer is BCzVBi, and thickness is 40nm; The material of the second electron transfer layer is TPBi, and thickness is 200nm; The material of the second electron injecting layer is LiF, and thickness is 0.5nm; The material of negative electrode is Pt, and thickness is 60nm.
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: AZO glass/V 2o 5/ TAPC/DCJTB/TAZ/Al:Li 2cO 3/ PBD:LiF/Pt:WO 3/ TAPC/BCzVBi/TPBi/LiF/Pt.
Embodiment 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) IZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 2 × 10 -3under the condition of Pa, prepare the first light emitting functional layer with evaporation speed thermal resistance evaporation in clean IZO substrate of glass of 0.1nm/s, comprise the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually;
Particularly, the material of the first hole injection layer is WO 3, thickness is 20nm; The material of the first hole transmission layer is TCTA, and thickness is 30nm; The material of the first luminescent layer is ADN, and thickness is 10nm; The material of the first electron transfer layer is Bphen, and thickness is 40nm;
(3) be 2 × 10 at pressure -3under the condition of Pa, using the evaporation speed of 0.1nm/s on the first electron transfer layer successively thermal resistance evaporation prepare the first N-shaped layer, the second N-shaped layer and p-type layer as charge generation layer;
Particularly, the material of the first N-shaped layer is that LiCl is doped to the composite material forming in Pt, and the quality of LiCl is that the thickness of 10%, the first N-shaped layer of Pt quality is 2nm; The material of the second N-shaped layer is that LiCl is doped to the composite material forming in TAZ, and the quality of LiCl is that 40%, the second N-shaped layer thickness of TAZ quality is 10nm; The material of p-type layer is V 2o 5be doped to the composite material forming in Au, V 2o 5quality be 5% of Au quality, the thickness of p-type layer is 2nm;
(4) be 2 × 10 at pressure -3under the condition of Pa, evaporation speed thermal resistance evaporation on p-type layer with 0.1nm/s is prepared the second light emitting functional layer, comprise the second hole transmission layer, the second luminescent layer, the second electron transfer layer, the second electron injecting layer that stack gradually, evaporation speed evaporation on the second electron injecting layer with 1nm/s is prepared negative electrode, obtains needed electroluminescent device;
Particularly, the material of the second hole transmission layer is TCTA, and thickness is 60nm; The material of the second luminescent layer is DCJTB, and thickness is 5nm; The material of the second electron transfer layer is Bphen, and thickness is 40nm; The material of the second electron injecting layer is Cs 2cO 3, thickness is 10nm; The material of negative electrode is Al, and thickness is 300nm.
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: IZO glass/WO 3/ TCTA/ADN/Bphen/Pt:LiCl/TAZ:LiCl/Au:V 2o 5/ TCTA/DCJTB/Bphen/Cs 2cO 3/ Al.
Embodiment 4
A preparation method for organic electroluminescence device, comprises the following steps:
(1) IZO substrate of glass is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 5 × 10 -4under the condition of Pa, prepare the first light emitting functional layer with evaporation speed thermal resistance evaporation in clean IZO substrate of glass of 0.5nm/s, comprise the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually;
Particularly, the material of the first hole injection layer is MoO 3, thickness is 30nm; The material of the first hole transmission layer is NPB, and thickness is 50nm; The material of the first luminescent layer is BCzVBi, and thickness is 40nm; The material of the first electron transfer layer is TPBi, and thickness is 200nm;
(3) be 5 × 10 at pressure -4under the condition of Pa, using the evaporation speed of 0.5nm/s on the first electron transfer layer successively thermal resistance evaporation prepare the first N-shaped layer, the second N-shaped layer and p-type layer as charge generation layer;
Particularly, the material of first N-shaped layer the first N-shaped layer is Li 2cO 3be doped to the composite material forming in Au, Li 2cO 3quality be that the thickness of 35%, the first N-shaped layer of Au quality is 15nm; The material of the second N-shaped layer is that LiF is doped to the composite material forming in Bphen, and the quality of LiF is that 15%, the second N-shaped layer thickness of Bphen quality is 8nm; The material of p-type layer is V 2o 5be doped to the composite material forming in Pt, V 2o 5quality be 18% of Pt quality, the thickness of p-type layer is 10nm;
(4) be 5 × 10 at pressure -4under the condition of Pa, evaporation speed thermal resistance evaporation on p-type layer with 0.5nm/s is prepared the second light emitting functional layer, comprise the second hole transmission layer, the second luminescent layer, the second electron transfer layer, the second electron injecting layer that stack gradually, evaporation speed evaporation on the second electron injecting layer with 5nm/s is prepared negative electrode, obtains needed electroluminescent device;
Particularly, the material of the second hole transmission layer is NPB, and thickness is 50nm; The material of the second luminescent layer is BCzVBi, and thickness is 35nm; The material of the second electron transfer layer is TPBi, and thickness is 100nm; The material of the second electron injecting layer is CsF, and thickness is 2nm; The material of negative electrode is Ag, and thickness is 100nm.
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: IZO glass/MoO 3/ NPB/BCzVBi/TPBi/Au:Li 2cO 3/ Bphen:LiF/Pt:V 2o 5/ NPB/BCzVBi/TPBi/CsF/Ag.
Comparative example
A preparation method for organic electroluminescence device, comprises the following steps:
(1) ito glass substrate is used to liquid detergent successively, deionized water, ultrasonic 15min, the organic pollution of removal glass surface;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 4 × 10 -4under the condition of Pa, with the evaporation speed of 0.6nm/s in clean ito glass substrate successively thermal resistance evaporation prepare hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, prepare negative electrode with evaporation speed thermal resistance evaporation on electron injecting layer of 6nm/s;
Particularly, the material of hole injection layer is MoO 3, thickness is 40nm; The material of hole transmission layer is NPB, and thickness is 40nm; The material of luminescent layer is Alq 3, thickness is 25nm; The material of electron transfer layer is TAZ, and thickness is 80nm; The material of electron injecting layer is CsN 3, thickness is 1nm; The material of negative electrode is Al, and thickness is 100nm.
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: ito glass/MoO 3/ NPB/Alq 3/ TAZ/CsN 3/ Al.
Utilize the Keithley2400 test electric property of Keithley company of the U.S., colorimeter (Japanese Konica Minolta company, model: CS-100A) test brightness and colourity.
Fig. 2 is the graph of a relation of the organic electroluminescence device of the present embodiment and the voltage of comparative example and brightness.Wherein, curve 1 is the present embodiment the voltage of organic electroluminescence device and the graph of a relation of brightness; For comparative example, (structure is specifically expressed as curve 2: ito glass/MoO 3/ NPB/Alq 3/ TAZ/CsN 3/ Al) voltage and the graph of a relation of brightness.
As can see from Figure 2, under different voltage, all large than comparative example of the brightness of embodiment 1, in the time of 8V, the brightness of embodiment 1 is 2421cd/m 2, and that comparative example is only 1341cd/m 2this explanation, the stacked speed that can farthest improve electric transmission of two N-shaped layers in charge generation layer, the existence of aluminium or noble metal can improve the light transmission rate of charge generation layer, and crystallinity electron transport material can form the orderly structure of arrangement after crystallization, light is carried out to scattering, and p-type layer can improve hole regeneration injectability, effectively improves device luminous efficiency and brightness.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

Claims (9)

1. an organic electroluminescence device, is characterized in that, comprises the conductive anode substrate of glass, the first light emitting functional layer, charge generation layer, the second light emitting functional layer and the negative electrode that stack gradually;
Described charge generation layer comprises the first N-shaped layer, the second N-shaped layer and the p-type layer that stack gradually; The material of described the first N-shaped layer is the mixture of lithium salts and aluminium or noble metal formation, and the mass fraction that described lithium salts accounts for described aluminium or noble metal is 10～60%; The material of described the second N-shaped layer is the mixture that lithium salts and electron transport material form, and the mass fraction that described lithium salts accounts for described electron transport material is 10～40%; The material of described p-type layer is the mixture of metal oxide and aluminium or noble metal formation, and the mass fraction that described metal oxide accounts for described aluminium or noble metal is 5～30%;
Described lithium salts is the one in lithium fluoride, lithium carbonate and lithium chloride; Described noble metal is the one in silver, platinum and gold; Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole; Described metal oxide is the one in molybdenum trioxide, tungstic acid and vanadic oxide.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, described the first light emitting functional layer comprises the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, described the second light emitting functional layer comprises the second hole injection layer, the second hole transmission layer, the second luminescent layer and the second electron transfer layer that stack gradually.
4. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
Conductive anode substrate of glass is provided;
In described conductive anode substrate of glass, thermal resistance evaporation is prepared the first light emitting functional layer, charge generation layer, the second light emitting functional layer and negative electrode successively, obtains organic electroluminescence device;
Described charge generation layer comprises the first N-shaped layer, the second N-shaped layer and the p-type layer that stack gradually; The material of described the first N-shaped layer is the mixture of lithium salts and aluminium or noble metal formation, and the mass fraction that described lithium salts accounts for described aluminium or noble metal is 10～60%; The material of described the second N-shaped layer is the mixture that lithium salts and electron transport material form, and the mass fraction that described lithium salts accounts for described electron transport material is 10～40%; The material of described p-type layer is the mixture of metal oxide and aluminium or noble metal formation, and the mass fraction that described metal oxide accounts for described aluminium or noble metal is 5～30%;
Described lithium salts is the one in lithium fluoride, lithium carbonate and lithium chloride; Described noble metal is the one in silver, platinum and gold; Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 1,2,4-triazole derivative or 2-(4-tert-butyl benzene)-5-(4-xenyl)-1,3,4-oxazole; Described metal oxide is the one in molybdenum trioxide, tungstic acid and vanadic oxide.
5. the preparation method of organic electroluminescence device as claimed in claim 4, is characterized in that, the condition of described thermal resistance evaporation is pressure 5 × 10 -5～2 × 10 -3pa.
6. the preparation method of organic electroluminescence device as claimed in claim 4, is characterized in that, described conductive anode substrate of glass is the one in indium tin oxide glass, aluminium zinc oxide glass and indium-zinc oxide glass.
7. the preparation method of organic electroluminescence device as claimed in claim 4, is characterized in that, the material of described negative electrode is the one in silver, aluminium, platinum and gold.
8. the preparation method of organic electroluminescence device as claimed in claim 4, is characterized in that, described the first light emitting functional layer comprises the first hole injection layer, the first hole transmission layer, the first luminescent layer and the first electron transfer layer that stack gradually.
9. the preparation method of organic electroluminescence device as claimed in claim 4, is characterized in that, described the second light emitting functional layer comprises the second hole injection layer, the second hole transmission layer, the second luminescent layer and the second electron transfer layer that stack gradually.
CN201310077736.4A 2013-03-12 2013-03-12 Organic light-emitting device and preparation method thereof Pending CN104051639A (en)

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Application publication date: 20140917