CN104218154A - Organic light emission diode device and fabrication method thereof - Google Patents
Organic light emission diode device and fabrication method thereof Download PDFInfo
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- CN104218154A CN104218154A CN201310208257.1A CN201310208257A CN104218154A CN 104218154 A CN104218154 A CN 104218154A CN 201310208257 A CN201310208257 A CN 201310208257A CN 104218154 A CN104218154 A CN 104218154A
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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
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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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
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- H10K50/85—Arrangements for extracting light from the devices
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- H—ELECTRICITY
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
- H10K71/611—Forming conductive regions or layers, e.g. electrodes using printing deposition, e.g. ink jet printing
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Abstract
The invention provides an organic light emission diode device which comprises a substrate, and an anode, a light emission functional layer and a cathode which are sequentially laminated on the substrate, a light extraction layer is arranged on a first surface and/or a second surface of the substrate, the material of the light extraction layer comprises nanoparticles with grain size of 50 to 1,500 nanometers and a polymer material, the nanoparticles are ceramic or high-polymer material particles, the polymer material is a heat cured polymer or photo cured polymer material, the thickness of the light extraction layer is 10 to 100 micrometers, the material of the anode is a conductive oxide membrane, the material of the cathode is an elementary substance of gold, silver, aluminum and magnesium or an alloy formed by any combination thereof, and the light emission functional layer at least comprises a hole transmission layer, a light emission layer and an electron transmission layer which are sequentially laminated. The light emergent efficiency of the cathode of the organic light emission diode device is high, so that the luminous efficiency of the device is improved. The invention also provides a fabrication method of the organic light emission diode device.
Description
Technical field
The present invention relates to organic electroluminescence device, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescent (Organic Light Emission Diode), hereinafter referred to as OLED, there is the characteristics such as brightness is high, material selection range is wide, driving voltage is low, all solidstate active illuminating, have high definition, wide viewing angle simultaneously, and the advantage such as fast response time, be a kind of Display Technique and light source of great potential, meet the development trend of information age mobile communication and information displaying, and the requirement of green lighting technique, be the focal point of current lot of domestic and foreign researcher.
In traditional OLED luminescent device, due to electrode material, refractive index between glass substrate and air is not mated, the light that OLED luminescence unit is launched transmits from electrode to glass substrate, when then entering in air, under the restriction of the cirtical angle of total reflection, generally only have the light of about 18% can outgoing, most light is then limited in OLED structure, dissipates with other forms.
Summary of the invention
For overcoming the defect of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and preparation method thereof.By arranging light-extraction layer between anode and substrate and/or between substrate and air, improve the luminous efficiency of organic electroluminescence device.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise substrate and the anode on substrate that is cascading, light emitting functional layer and negative electrode, described substrate comprises first surface and second surface, described first surface and/or second surface are provided with light-extraction layer, the material of described light-extraction layer comprises Nano microsphere and polymeric material that particle diameter is 50 ~ 1500nm, described Nano microsphere is pottery or macromolecule material particle, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, the thickness of described light-extraction layer is 10 ~ 100 μm, the material of described anode is conductive oxide film, the material of described negative electrode is the alloy that gold, silver, aluminium, magnesium simple substance or its combination in any are formed, and described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually.
Preferably, the polymeric material of described hot curing is heat-curable epoxy resin, and the polymeric material of described photocuring is light-cured acrylic resin.
Preferably, described ceramic particle is silicon dioxide or titanium dioxide, and described macromolecule material particle is polystyrene microsphere.
Preferably, the mass ratio of described Nano microsphere and polymeric material is 10 ~ 50:100.
The present invention arranges light-extraction layer between anode and substrate and/or between substrate and air, light-extraction layer includes the Nano microsphere of pottery or macromolecular material and the polymeric material of photocuring or hot curing, because Nano microsphere has light scattering effect, the reflection direction of incident light on its surface can be changed, thus change the cirtical angle of total reflection of overall light outgoing, increase light extraction efficiency; Therefore can organic electroluminescence device be made to have light extraction efficiency high, luminous efficiency is feature preferably.
The material of described anode is conductive oxide film.
Preferably, described conductive oxide film is indium and tin oxide film (ITO), aluminium zinc oxide film (AZO), indium-zinc oxide film (IZO) or gallium zinc oxide film (GZO).
Described substrate can be light transmissive material, as clear glass or transparent polymer film.
Described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that are cascading.In order to improve the luminous efficiency of device, can hole injection layer and electron injecting layer be set further.
The material of hole transmission layer, electron transfer layer and luminescent layer does not do concrete restriction, and this area current material is all applicable to the present invention.
Preferably, the material of hole transmission layer is 4,4', 4''-tri-(2-naphthylphenyl is amino) triphenylamine (2-TNATA), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA), N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1,1'-biphenyl-4,4'-diamines (TPD) or 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA), thickness is 20 ~ 60nm.
Preferably, the material of luminescent layer is the composite material that material of main part doping guest materials is formed, and described material of main part is 4,4'-bis-(9-carbazole) biphenyl (CBP), oxine aluminium (Alq
3), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB); Described guest materials is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), two (4,6-difluorophenyl pyridinato-N, C2) pyridinecarboxylic closes iridium (FIrpic), two (4,6-difluorophenyl pyridinato)-four (1-pyrazolyl) boric acid closes iridium (FIr6), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanediones) close iridium (Ir (MDQ)
2(acac)), three (1-phenyl-isoquinolin) close iridium (Ir (piq) 3) and three (2-phenylpyridines) close iridium (Ir (ppy)
3) in one or more, the mass ratio of guest materials and material of main part is 1 ~ 20:100.
Preferably, the material of described luminescent layer is fluorescent material, described fluorescent material is 4,4'-bis-(2,2-diphenylethyllene)-1,1'-biphenyl (DPVBi), 4,4'-two [4-(di-p-tolyl is amino) styryl] biphenyl (DPAVBi), 5,6,11,12-tetraphenyl naphthonaphthalene (Rubrene) or dimethylquinacridone (DMQA).
Preferably, the thickness of described luminescent layer is 10 ~ 30nm.
Preferably, the material of electron transfer layer is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1,3,4-oxadiazole (PBD), 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (as TAZ), N-aryl benzimidazole (TPBI) or 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP), thickness is 30 ~ 100nm.
Preferably, the material of hole injection layer is CuPc (CuPc), Phthalocyanine Zinc (ZnPc), ranadylic phthalocyanine (VOPc), and TiOPc (TiOPc) or phthalocyanine platinum (PtPc), thickness is 10 ~ 30nm.
Preferably, the material of electron injecting layer is cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) or lithium fluoride (LiF); Thickness is 0.5 ~ 10nm.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
On the substrate of cleaning, screen printing mode is adopted to prepare light-extraction layer at the first surface of described substrate and/or second surface, the material of described light-extraction layer comprises Nano microsphere and polymeric material that particle diameter is 50 ~ 1500nm, described Nano microsphere is pottery or macromolecule material particle, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described light-extraction layer is 10 ~ 100 μm;
Anode and light emitting functional layer is prepared successively again at the first surface of described substrate or second surface; The material of described anode is conductive oxide film; Described anode adopts the mode of vacuum sputtering to prepare, and vacuum degree is 1 × 10
-3~ 1 × 10
-5pa, sputter rate is 0.2 ~ 2nm/s, and described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually, and described hole transmission layer, luminescent layer and electron transfer layer all adopt the mode of vacuum evaporation to prepare;
Finally prepare negative electrode on described light emitting functional layer surface, obtain organic electroluminescence device; The material of described negative electrode is the alloy that gold, silver, aluminium, magnesium simple substance or its combination in any are formed, and described negative electrode adopts the mode of vacuum evaporation to prepare.
Preferably, the polymeric material of described hot curing is heat-curable epoxy resin, and the polymeric material of described photocuring is light-cured acrylic resin.
Preferably, described ceramic particle is silicon dioxide or titanium dioxide, and described macromolecule material particle is polystyrene microsphere.
Preferably, the mass ratio of described Nano microsphere and polymeric material is 10 ~ 50:100.
Preferably, the meshcount of described silk screen printing is 200 ~ 1000 orders.
The material of described anode is conductive oxide film.
Preferably, described conductive oxide film is indium and tin oxide film (ITO), aluminium zinc oxide film (AZO), indium-zinc oxide film (IZO) or gallium zinc oxide film (GZO).
Described substrate can be light transmissive material, as clear glass or transparent polymer film.
Described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that are cascading.In order to improve the luminous efficiency of device, can hole injection layer and electron injecting layer be set further.
The material of hole transmission layer, electron transfer layer and luminescent layer does not do concrete restriction, and this area current material is all applicable to the present invention.
Preferably, the material of hole transmission layer is 4,4', 4''-tri-(2-naphthylphenyl is amino) triphenylamine (2-TNATA), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA), N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1,1'-biphenyl-4,4'-diamines (TPD) or 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA), thickness is 20 ~ 60nm.
Preferably, the material of luminescent layer is the composite material that material of main part doping guest materials is formed, and described material of main part is 4,4'-bis-(9-carbazole) biphenyl (CBP), oxine aluminium (Alq
3), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi) or N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB); Described guest materials is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), two (4,6-difluorophenyl pyridinato-N, C2) pyridinecarboxylic closes iridium (FIrpic), two (4,6-difluorophenyl pyridinato)-four (1-pyrazolyl) boric acid closes iridium (FIr6), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanediones) close iridium (Ir (MDQ)
2(acac)), three (1-phenyl-isoquinolin) close iridium (Ir (piq) 3) and three (2-phenylpyridines) close iridium (Ir (ppy)
3) in one or more, the mass ratio of guest materials and material of main part is 1 ~ 20:100.
Preferably, the material of described luminescent layer is fluorescent material, described fluorescent material is 4,4'-bis-(2,2-diphenylethyllene)-1,1'-biphenyl (DPVBi), 4,4'-two [4-(di-p-tolyl is amino) styryl] biphenyl (DPAVBi), 5,6,11,12-tetraphenyl naphthonaphthalene (Rubrene) or dimethylquinacridone (DMQA).
Preferably, the thickness of described luminescent layer is 10 ~ 30nm.
Preferably, the material of electron transfer layer is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1,3,4-oxadiazole (PBD), 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2,4-triazole derivative (as TAZ), N-aryl benzimidazole (TPBI) or 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP), thickness is 30 ~ 100nm.
Preferably, the material of hole injection layer is CuPc (CuPc), Phthalocyanine Zinc (ZnPc), ranadylic phthalocyanine (VOPc), and TiOPc (TiOPc) or phthalocyanine platinum (PtPc), thickness is 10 ~ 30nm.
Preferably, the material of electron injecting layer is cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) or lithium fluoride (LiF); Thickness is 0.5 ~ 10nm.
The invention provides a kind of organic electroluminescence device and preparation method thereof and there is following beneficial effect:
(1) organic electroluminescence device provided by the invention, light-extraction layer is provided with between anode and substrate and/or between substrate and air, this light-extraction layer includes the Nano microsphere of pottery or macromolecular material and the polymeric material of photocuring or hot curing, the upper and lower surface of substrate is printed on by silk-screen printing technique, because Nano microsphere has light scattering effect, the reflection direction of incident light on its surface can be changed, thus change the cirtical angle of total reflection of overall light outgoing, increase light extraction efficiency; Therefore, it is high that organic electroluminescence device provided by the invention has light extraction efficiency, and luminous efficiency is feature preferably;
(2) preparation technology of organic electroluminescence device of the present invention is simple, and easy large area preparation, is suitable for industrialization and uses on a large scale.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains;
Fig. 2 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 6 obtains;
Fig. 3 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 11 obtains.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained 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) on clear glass, adopt silk-screen printing technique on the first surface of glass substrate, form the light-extraction layer that thickness is 100 μm, the material of light-extraction layer comprises titanium dioxide nanometer microballoons and light-cured acrylic resin that mass ratio is 50:100, the particle diameter of titanium dioxide nanometer microballoons is 50nm, and screen printing process adopts order number to be 400 object silk screen printing film forming;
(2) be 1 × 10 in vacuum degree again
-3in the coating chamber of Pa, adopt sputtering technology to prepare anode on the surface of described light-extraction layer, material is ito thin film, thickness is 100nm, sputter rate is 0.2nm/s, then on ito thin film, evaporation prepares light emitting functional layer, comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts CuPc, and thickness is 20nm; Hole transmission layer adopts NPB, and thickness is 30nm; Luminescent layer adopts Ir (ppy)
3be entrained in the composite material formed in CBP, Ir (ppy)
3be 10:100 with the mass ratio of CBP, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) finally on electron injecting layer, evaporation prepares negative electrode, and obtain organic electroluminescence device, the material of negative electrode is metal A g, and thickness is 100nm.
Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains.As shown in Figure 1, the present embodiment organic electroluminescence device, comprises transparent glass substrate 10, light-extraction layer 11, anode 12, light emitting functional layer 13 and negative electrode 14 successively.Light-extraction layer 11 is arranged between substrate 10 and anode 12.Titanium dioxide nanometer microballoons 110 is comprised in light-extraction layer 11.
Embodiment 2
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises titanium dioxide nanometer microballoons and light-cured acrylic resin that mass ratio is 20:100, the particle diameter of titanium dioxide nanometer microballoons is 100nm, screen printing process adopts order number to be 1000 object silk screen printing film forming, and the thickness of light-extraction layer is 80 μm.
Embodiment 3
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises titanium dioxide nanometer microballoons and light-cured acrylic resin that mass ratio is 20:100, the particle diameter of titanium dioxide nanometer microballoons is 250nm, screen printing process adopts order number to be 800 object silk screen printing film forming, and the thickness of light-extraction layer is 20 μm.
Embodiment 4
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises titanium dioxide nanometer microballoons and light-cured acrylic resin that mass ratio is 10:100, the particle diameter of titanium dioxide nanometer microballoons is 500nm, screen printing process adopts order number to be 800 object silk screen printing film forming, and the thickness of light-extraction layer is 10 μm.
Embodiment 5
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises titanium dioxide nanometer microballoons and light-cured acrylic resin that mass ratio is 10:100, the particle diameter of titanium dioxide nanometer microballoons is 1000nm, screen printing process adopts order number to be 1000 object silk screen printing film forming, and the thickness of light-extraction layer is 50 μm.
Embodiment 6
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on transparent glass substrate, adopt silk-screen printing technique on the first surface of glass substrate, form the light-extraction layer that thickness is 10 μm, the material of light-extraction layer comprises Properties of Polystyrene Nano Particles and light-cured acrylic resin that mass ratio is 50:100, the particle diameter of Properties of Polystyrene Nano Particles is 200nm, and screen printing process adopts order number to be 400 object silk screen printing film forming;
(2) be 1 × 10 in vacuum degree again
-5in the coating chamber of Pa, the second surface of described glass substrate adopt sputtering technology prepare anode, material is ito thin film, thickness is 100nm, sputter rate is 2nm/s, then on ito thin film, evaporation prepares light emitting functional layer, comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts CuPc, and thickness is 20nm; Hole transmission layer adopts NPB, and thickness is 30nm; Luminescent layer adopts Ir (ppy)
3be entrained in the composite material formed in CBP, Ir (ppy)
3be 10:100 with the mass ratio of CBP, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) finally on electron injecting layer, evaporation prepares negative electrode, and obtain organic electroluminescence device, the material of negative electrode is metal A g, and thickness is 100nm.
Fig. 2 is the structural representation of the organic electroluminescence device that the present embodiment obtains.As shown in Figure 2, the present embodiment organic electroluminescence device, comprises transparent glass substrate 20, light-extraction layer 21, anode 22, light emitting functional layer 23 and negative electrode 24.Light-extraction layer 21 is arranged between substrate 20 and air.
Embodiment 7
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises Properties of Polystyrene Nano Particles and light-cured acrylic resin that mass ratio is 20:100, the particle diameter of Properties of Polystyrene Nano Particles is 400nm, screen printing process adopts order number to be 1000 object silk screen printing film forming, and the thickness of light-extraction layer is 60 μm.
Embodiment 8
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises Properties of Polystyrene Nano Particles and light-cured acrylic resin that mass ratio is 20:100, the particle diameter of Properties of Polystyrene Nano Particles is 800nm, screen printing process adopts order number to be 600 object silk screen printing film forming, and the thickness of light-extraction layer is 15 μm.
Embodiment 9
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises Properties of Polystyrene Nano Particles and light-cured acrylic resin that mass ratio is 10:100, the particle diameter of Properties of Polystyrene Nano Particles is 1000nm, screen printing process adopts order number to be 800 object silk screen printing film forming, and the thickness of light-extraction layer is 20 μm.
Embodiment 10
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises Properties of Polystyrene Nano Particles and light-cured acrylic resin that mass ratio is 10:100, the particle diameter of Properties of Polystyrene Nano Particles is 1500nm, screen printing process adopts order number to be 1000 object silk screen printing film forming, and the thickness of light-extraction layer is 100 μm.
Embodiment 11
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on transparent glass substrate, adopt silk-screen printing technique to form the light-extraction layer that thickness is 100 μm respectively on the first surface and second surface of glass substrate, the material of light-extraction layer comprises silicon dioxide nanosphere and heat-curable epoxy resin that mass ratio is 50:100, the particle diameter of silicon dioxide nanosphere is 50nm, and screen printing process adopts order number to be 600 object silk screen printing film forming;
(2) be 1 × 10 in vacuum degree again
-4in the coating chamber of Pa, the first surface of described glass substrate or the light-extraction layer of second surface adopt sputtering technology to prepare anode, material is ito thin film, thickness is 100nm, sputter rate is 1nm/s, then on ito thin film, evaporation prepares light emitting functional layer, comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts CuPc, and thickness is 20nm; Hole transmission layer adopts NPB, and thickness is 30nm; Luminescent layer adopts Ir (ppy)
3be entrained in the composite material formed in CBP, Ir (ppy)
3be 10:100 with the mass ratio of CBP, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) finally on electron injecting layer, evaporation prepares negative electrode, and obtain organic electroluminescence device, the material of negative electrode is metal A g, and thickness is 100nm.
Fig. 3 is the structural representation of the organic electroluminescence device that the present embodiment obtains.As shown in Figure 3, the present embodiment organic electroluminescence device, comprises transparent glass substrate 30, light-extraction layer 31 and 31 ', anode 32, light emitting functional layer 33 and negative electrode 34.Light-extraction layer 31 and 31 ' is separately positioned between substrate 30 and air, and between substrate 30 and anode 32.
Embodiment 12
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises silicon dioxide nanosphere and heat-curable epoxy resin that mass ratio is 50:100, the particle diameter of silicon dioxide nanosphere is 100nm, screen printing process adopts order number to be 400 object silk screen printing film forming, and the thickness of light-extraction layer is 60 μm.
Embodiment 13
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises silicon dioxide nanosphere and heat-curable epoxy resin that mass ratio is 15:100, the particle diameter of silicon dioxide nanosphere is 250nm, screen printing process adopts order number to be 200 object silk screen printing film forming, and the thickness of light-extraction layer is 20 μm.
Embodiment 14
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises silicon dioxide nanosphere and heat-curable epoxy resin that mass ratio is 10:100, the particle diameter of silicon dioxide nanosphere is 400nm, screen printing process adopts order number to be 200 object silk screen printing film forming, and the thickness of light-extraction layer is 60 μm.
Comparative example
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopt sputtering technology to prepare anode, material is ito thin film, and thickness is 100nm, then on ito thin film, evaporation prepares light emitting functional layer, comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts CuPc, and thickness is 20nm; Hole transmission layer adopts NPB, and thickness is 30nm; Luminescent layer adopts Ir (ppy)
3be entrained in the composite material formed in CBP, Ir (ppy)
3be 10:100 with the mass ratio of CBP, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(2) finally on electron injecting layer, evaporation prepares negative electrode, and obtain organic electroluminescence device, the material of negative electrode is metal A g, and thickness is 100nm.
Effect example
Test of the present invention and Preparation equipment 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 of Keithley company of the U.S. tests electric property, the CS-100A colorimeter test brightness of Japanese Konica Minolta company and colourity.
Organic electroluminescence device obtained by the embodiment of the present invention 1 ~ 5 and comparative example is carried out luminous efficiency test under 6V driving voltage, and test result is as shown in table 1:
Table 1
As can be seen from the data of table 1, the organic electroluminescence device provided of the present invention, by arranging light-extraction layer between substrate and anode, luminous efficiency has brought up to more than 30.6lm/W from the 16.3lm/W of comparative example, at least improves more than 88%.This is because light-extraction layer includes the Nano microsphere of pottery or macromolecular material, and Nano microsphere has light scattering effect, the reflection direction of incident light on its surface can be changed, thus change the cirtical angle of total reflection of overall light outgoing, thus increase light extraction efficiency, the final luminous efficiency improving device.
Organic electroluminescence device obtained by the embodiment of the present invention 6 ~ 10 is carried out luminous efficiency test under 6V driving voltage, and test result is as shown in table 2:
Table 2
As can be seen from the data of table 2, the organic electroluminescence device provided of the present invention, by arranging light-extraction layer between substrate and extraneous air interface, luminous efficiency has brought up to more than 29.1lm/W from the 16.3lm/W of comparative example, at least improves more than 79%.This is because light-extraction layer includes the Nano microsphere of pottery or macromolecular material, and Nano microsphere has light scattering effect, the reflection direction of incident light on its surface can be changed, thus change the cirtical angle of total reflection of overall light in substrate and Air Interface outgoing, thus increase light extraction efficiency, the final luminous efficiency improving device.
Organic electroluminescence device obtained by the embodiment of the present invention 11 ~ 14 is carried out luminous efficiency test under 6V driving voltage, and test result is as shown in table 3:
Table 3
As can be seen from the data of table 3, the organic electroluminescence device provided of the present invention, by between substrate and extraneous air, all arranges light-extraction layer between substrate and anode, luminous efficiency has brought up to more than 36.9lm/W from the 16.3lm/W of comparative example, at least improves more than 126%.This is because light-extraction layer includes the Nano microsphere of pottery or macromolecular material, and Nano microsphere has light scattering effect, the reflection direction of incident light on its surface can be changed, thus change overall light at anode and substrate, the cirtical angle of total reflection of the outgoing of substrate and Air Interface, thus increase light extraction efficiency, the final luminous efficiency improving device.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. an organic electroluminescence device, comprise substrate and the anode on substrate that is cascading, light emitting functional layer and negative electrode, it is characterized in that, described substrate comprises first surface and second surface, described first surface and/or second surface are provided with light-extraction layer, the material of described light-extraction layer comprises Nano microsphere and polymeric material that particle diameter is 50 ~ 1500nm, described Nano microsphere is pottery or macromolecule material particle, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, the thickness of described light-extraction layer is 10 ~ 100 μm, the material of described anode is conductive oxide film, the material of described negative electrode is the alloy that gold, silver, aluminium, magnesium simple substance or its combination in any are formed, and described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually.
2. organic electroluminescence device as claimed in claim 1, it is characterized in that, the polymeric material of described hot curing is heat-curable epoxy resin, and the polymeric material of described photocuring is light-cured acrylic resin.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, described ceramic particle is silicon dioxide or titanium dioxide, and described macromolecule material particle is polystyrene microsphere.
4. organic electroluminescence device as claimed in claim 1, it is characterized in that, the mass ratio of described Nano microsphere and polymeric material is 10 ~ 50:100.
5. organic electroluminescence device as claimed in claim 1, it is characterized in that, described conductive oxide film is indium and tin oxide film, aluminium zinc oxide film, indium-zinc oxide film or gallium zinc oxide film.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
On the substrate of cleaning, screen printing mode is adopted to prepare light-extraction layer at the first surface of described substrate and/or second surface, the material of described light-extraction layer comprises Nano microsphere and polymeric material that particle diameter is 50 ~ 1500nm, described Nano microsphere is pottery or macromolecule material particle, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described light-extraction layer is 10 ~ 100 μm;
Anode and light emitting functional layer is prepared successively again at the first surface of described substrate or second surface; The material of described anode is conductive oxide film; Described anode adopts the mode of vacuum sputtering to prepare, and vacuum degree is 1 × 10
-3~ 1 × 10
-5pa, sputter rate is 0.2 ~ 2nm/s, and described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually, and described hole transmission layer, luminescent layer and electron transfer layer all adopt the mode of vacuum evaporation to prepare;
Finally prepare negative electrode on described light emitting functional layer surface, obtain organic electroluminescence device; The material of described negative electrode is the alloy that gold, silver, aluminium, magnesium simple substance or its combination in any are formed, and described negative electrode adopts the mode of vacuum evaporation to prepare.
7. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the polymeric material of described hot curing is heat-curable epoxy resin, and the polymeric material of described photocuring is light-cured acrylic resin.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, described ceramic particle is silicon dioxide or titanium dioxide, and described macromolecule material particle is polystyrene microsphere.
9. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the mass ratio of described Nano microsphere and polymeric material is 10 ~ 50:100.
10. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the meshcount of described silk screen printing is 200 ~ 1000 orders.
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