CN104218180A - 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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- CN104218180A CN104218180A CN201310210324.3A CN201310210324A CN104218180A CN 104218180 A CN104218180 A CN 104218180A CN 201310210324 A CN201310210324 A CN 201310210324A CN 104218180 A CN104218180 A CN 104218180A
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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- H10K50/856—Arrangements for extracting light from the devices comprising reflective means
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Abstract
The invention provides an organic light emission diode device. The organic light emission diode device comprises a substrate and a reflection layer, a light scattering layer, a first transmitting electrode, a light emission functional layer and a second transmitting electrode which are sequentially laminated on the substrate, the material of the light scattering layer comprises nanoparticles and a polymer material, the nanoparticles are ceramic or high-polymer material particles with grain size of 50 to 1,500 nanometers, the polymer material is a heat cured polymer or photo cured polymer material, the thickness of the light scattering layer is 10 to 100 micrometers, the material of the reflection electrode is a metal membrane, and the metal membrane comprises metal elemental gold, silver, aluminum, copper, nickel, platinum and magnesium or an alloy formed by any combination thereof. In the organic light emission diode device, through the arrangement of the light scattering layer on the surface of the reflection electrode, the reflectivity of the device is greatly reduced, so that the contrast 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 the OLED luminescent device of existing top emitting, the general reflective electrodes reflects light by bottom, then from the transmission electrode emergent ray at top.Because the reflecting electrode of bottom generally adopts metal electrode, there is higher reflectivity, cause the reflection that outside ambient light also can be strong at bottom electrode, OLED is made to have lower contrast and display resolution like this, and top emitting device adopts semitransparent electrode, and emitting brightness is generally lower.And although existing light polarizing film can offset these ambient lights, light polarizing film is easily by impact that is moist and ambient temperature, and manufacturing cost is higher.
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 preparing light scattering layer at reflective electrode surface, improve the contrast of organic electroluminescence device.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise substrate and the reflecting electrode on substrate that is cascading, light scattering layer, first transmission electrode, light emitting functional layer and the second transmission electrode, the material of described light scattering layer comprises Nano microsphere and polymeric material, pottery or the macromolecule material particle of described Nano microsphere to be particle diameter be 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, the thickness of described light scattering layer is 10 ~ 100 μm, the material of described reflecting electrode is metallic film, described metallic film comprises metallic gold, silver, aluminium, copper, nickel, platinum, the alloy that magnesium simple substance or its combination in any are formed, the material of described first transmission electrode is conductive oxide film or metallic gold, silver, aluminium, platinum film, the material of described second transmission electrode is gold, silver, aluminium, the alloy firm that magnesium or its combination in any are formed, described light emitting functional layer at least comprises the hole transmission layer stacked gradually, luminescent layer and electron transfer layer.
Preferably, described second transmission electrode surface comprises the second light scattering layer further, the material of described second light scattering layer comprises Nano microsphere and polymeric material, pottery or the macromolecule material particle of described Nano microsphere to be particle diameter be 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described second light scattering layer is 10 ~ 100 μm.
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 thickness of the metallic film of described reflecting electrode is 70 ~ 500nm.
The material of the first transmission electrode is conductive oxide film or metal gold, silver, aluminium, platinum film.
Preferably, conductive oxide film is indium tin oxide (ITO), aluminium zinc oxide (AZO), indium-zinc oxide (IZO) or gallium zinc oxide (GZO), and thickness is 100 ~ 500nm.
Preferably, the thickness of metal gold, silver, aluminium, platinum film is 18 ~ 30nm.
The alloy firm that the material of the second transmission electrode is gold (Au), silver (Ag), aluminium (Al), magnesium (Mg) or its combination in any are formed, thickness is preferably 18 ~ 30nm.
Described substrate can be light transmissive material, as clear glass or transparent polymer film, also can be light-proof material, as sheet metal or silicon chip.
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 (Alq3), 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:
The substrate of cleaning being placed in vacuum degree is 1 × 10
-3~ 1 × 10
-5in the vacuum film coating chamber of Pa, the mode of vacuum thermal resistance evaporation is adopted to prepare reflecting electrode on the substrate, evaporation rate is 0.2 ~ 2nm/s, and the material of described reflecting electrode is metallic film, and described metallic film comprises metallic gold, silver, aluminium, copper, nickel, platinum, the alloy that magnesium simple substance or its combination in any are formed;
The mode of silk screen printing is adopted to prepare light scattering layer at described reflective electrode surface, the material of described light scattering layer comprises Nano microsphere and polymeric material, described Nano microsphere is pottery or macromolecule material particle, particle diameter is 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described light scattering layer is 10 ~ 100 μm;
Prepare the first transmission electrode, light emitting functional layer and the second transmission electrode successively on described light scattering layer surface, obtain organic electroluminescence device; The material of described first transmission electrode is conductive oxide film or metal gold, silver, aluminium, platinum film, the material of described second transmission electrode is the alloy firm that gold, silver, aluminium, magnesium or its combination in any are formed, described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually, described first transmission electrode adopts the mode of vacuum evaporation or magnetron sputtering to prepare, and described light emitting functional layer and the second transmission electrode adopt the mode of vacuum evaporation to prepare.
Preferably, preparation method comprises further, adopt the mode of silk screen printing at described second transmission electrode surface preparation the second light scattering layer, the material of described second light scattering layer comprises Nano microsphere and polymeric material, described Nano microsphere is pottery or macromolecule material particle, particle diameter is 50 ~ 1500nm, and described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described second light scattering layer is 10 ~ 100 μm.
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.
Preferably, the thickness of the metallic film of described reflecting electrode is 70 ~ 500nm.
The material of the first transmission electrode is conductive oxide film or metal gold, silver, aluminium, platinum film.
Preferably, conductive oxide film is indium tin oxide (ITO), aluminium zinc oxide (AZO), indium-zinc oxide (IZO) or gallium zinc oxide (GZO), and thickness is 100 ~ 500nm.
Described conductive oxide film adopts the mode of magnetron sputtering to prepare.Preferably, sputtering rate is 0.2 ~ 2nm/s.
Preferably, the thickness of metal gold, silver, aluminium, platinum film is 18 ~ 30nm.
Described metallic film adopts the mode of vacuum evaporation to prepare.Preferably, evaporation rate is 0.2 ~ 2nm/s.
The alloy firm that the material of the second transmission electrode is gold (Au), silver (Ag), aluminium (Al), magnesium (Mg) or its combination in any are formed, thickness is preferably 18 ~ 30nm.
The evaporation rate of described second transmission electrode is 0.1 ~ 1nm/s.
Described substrate can be light transmissive material, as clear glass or transparent polymer film, also can be light-proof material, as sheet metal or silicon chip.
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 (Alq3), 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 scattering layer is provided with at reflective electrode surface, described light scattering layer is the thin polymer film of the Nano microsphere adding pottery or macromolecular material, because Nano microsphere has light scattering effect, light scattering layer can make outside ambient light form scattering on bottom reflection electrode, and directly can not be reflected back the transmission electrode at top, thus reduce the reflection of ambient light in OLED inside, improve device contrast;
(3) second light scattering layer on transmission electrode surface, top second is positioned at, also outside ambient light can be made directly directly to carry out scattering on the transmission electrode surface at top, avoid entering OLED inside to reflect, thus improve light extraction efficiency and the contrast of device further, in addition, the second light scattering layer can also play the effect improving luminosity;
(3) 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.
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) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the metal A g film of 500nm is as reflecting electrode;
(2) adopt silk-screen printing technique on the surface of reflecting electrode, form the light scattering layer that thickness is 100 μm, the material of light scattering 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 200 object silk screen printing film forming;
(3) adopt magnetron sputtering mode light scattering layer surface sputtering prepare a layer thickness be the ito thin film of 200nm as the first transmission electrode, sputtering rate is 0.2nm/s; Adopt the mode of vacuum evaporation in ito thin film surface preparation light emitting functional layer again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(4) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal A g, and evaporation rate is 0.5nm/s, and thickness is 18nm, obtains organic electroluminescence device.
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 glass substrate 10, reflecting electrode 11, light scattering layer 12, first transmission electrode 13, light emitting functional layer 14 and the second transmission electrode 15 successively.Titanium dioxide nanometer microballoons 120 is comprised in light scattering layer 12.
Embodiment 2
The difference of the present embodiment and embodiment 1 is, the material of light scattering 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 scattering layer is 80 μm.
Embodiment 3
The difference of the present embodiment and embodiment 1 is, the material of light scattering 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 400 object silk screen printing film forming, and the thickness of light scattering layer is 20 μm.
Embodiment 4
The difference of the present embodiment and embodiment 1 is, the material of light scattering 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 500 object silk screen printing film forming, and the thickness of light scattering layer is 10 μm.
Embodiment 5
The difference of the present embodiment and embodiment 1 is, the material of light scattering 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 600 object silk screen printing film forming, and the thickness of light scattering layer is 50 μm.
Embodiment 6
A preparation method for organic electroluminescence device, comprises the following steps:
(1) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the Pt metal film of 70nm is as reflecting electrode;
(2) adopt silk-screen printing technique on the surface of reflecting electrode, form the light scattering layer that thickness is 10 μm, the material of light scattering 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;
(3) adopt magnetron sputtering mode light scattering layer surface sputtering prepare a layer thickness be the AZO film of 100nm as the first transmission electrode, sputtering rate is 2nm/s; Adopt the mode of vacuum evaporation to prepare light emitting functional layer at AZO film surface again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(4) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal A g-Mg alloy, and evaporation rate is 0.1nm/s, and thickness is 30nm;
(5) finally adopt silk-screen printing technique on the surface of the second transmission electrode, form the second light scattering layer that thickness is 10 μm, obtain organic electroluminescence device; The material of the second light scattering layer is identical with the light scattering layer of preparation technology and reflective electrode surface.
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 glass substrate 20, reflecting electrode 21, light scattering layer 22, first transmission electrode 23, light emitting functional layer 24, second transmission electrode 25 and the second light scattering layer 26 successively.
Embodiment 7
The difference of the present embodiment and embodiment 6 is, the material of light scattering 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 scattering layer is 60 μm.
Embodiment 8
The difference of the present embodiment and embodiment 6 is, the material of light scattering 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 scattering layer is 15 μm.
Embodiment 9
The difference of the present embodiment and embodiment 6 is, the material of light scattering 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 scattering layer is 20 μm.
Embodiment 10
The difference of the present embodiment and embodiment 6 is, the material of light scattering 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 scattering layer is 100 μm.
Embodiment 11
A preparation method for organic electroluminescence device, comprises the following steps:
(1) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the W metal film of 500nm is as reflecting electrode;
(2) adopt silk-screen printing technique on the surface of reflecting electrode, form the light scattering layer that thickness is 100 μm, the material of light scattering layer comprises silicon dioxide nanosphere and heat-curable epoxy resin that mass ratio is 20:100, 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;
(3) adopt vacuum evaporation mode light scattering layer surface preparation a layer thickness be the metal A u film of 20nm as the first transmission electrode, evaporation rate is 1nm/s; Adopt the mode of vacuum evaporation to prepare light emitting functional layer at metal A u film surface again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(4) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal M g-Al alloy, and evaporation rate is 1nm/s, and thickness is 20nm, obtains organic electroluminescence device.
Embodiment 12
The difference of the present embodiment and embodiment 11 is, the material of light scattering 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 scattering layer is 10 μm.
Embodiment 13
The difference of the present embodiment and embodiment 11 is, the material of light scattering 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 scattering layer is 20 μm.
Embodiment 14
The difference of the present embodiment and embodiment 11 is, the material of light scattering 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 scattering layer is 50 μm.
Comparative example 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the metal A g film of 500nm is as reflecting electrode;
(2) mode adopting magnetron sputtering is that the ito thin film of 200nm is as the first transmission electrode in reflective electrode surface Slag coating a layer thickness, adopt the mode of vacuum evaporation in ito thin film surface preparation light emitting functional layer again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal A g, and thickness is 18nm, obtains organic electroluminescence device.
Comparative example 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the Pt metal film of 70nm is as reflecting electrode;
(2) mode adopting magnetron sputtering is that the AZO film of 100nm is as the first transmission electrode in reflective electrode surface Slag coating a layer thickness, adopt the mode of vacuum evaporation to prepare light emitting functional layer at AZO film surface again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal A g-Mg alloy, and thickness is 30nm, obtains organic electroluminescence device.
Comparative example 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) glass substrate is placed in 1 × 10
-4in the vacuum film coating chamber of Pa, adopting the mode of vacuum evaporation to prepare a layer thickness at substrate surface is that the W metal film of 500nm is as reflecting electrode;
(2) adopting the mode of vacuum evaporation to prepare a layer thickness at reflective electrode surface is that the metal A u film of 20nm is as the first transmission electrode, adopt the mode of vacuum evaporation to prepare light emitting functional layer at metal A u film surface again, comprise hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively;
Wherein, hole injection layer layer adopts ZnPc, and thickness is 20nm; Hole transmission layer adopts TPD, and thickness is 20nm; 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 Bphen, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation at electron injecting layer surface preparation the second transmission electrode, material is metal M g-Al alloy, and thickness is 20nm, obtains organic electroluminescence device.
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, Japan's CS-100A colorimeter test brightness of Konica Minolta company and colourity, U.S. Filmetrics(US business phenanthrene is happy) the F10-RT type reflectance test instrument test reflectivity of company.
Organic electroluminescence device obtained by the embodiment of the present invention 1 ~ 5 and comparative example 1 is carried out under 6V driving voltage the test of luminosity, and the reflectivity of test component between wavelength 380 ~ 780nm, 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 scattering layer at reflective electrode surface, the reflectivity of device have decreased to less than 32% from 86% of comparative example 1, illustrates that ambient light reflectivity in the devices greatly reduces.This is because light scattering layer includes Nano microsphere, and Nano microsphere has light scattering effect, light scattering layer can make outside ambient light form scattering on bottom reflection electrode, and directly can not be reflected back the transmission electrode at top, thus reduce the reflection of ambient light in OLED inside, improve device light extraction efficiency and contrast; From luminosity, although reflectivity reduces greatly, it is not very large that the luminous efficiency of device reduces amplitude.
Organic electroluminescence device obtained by the embodiment of the present invention 6 ~ 10 and comparative example 2 is carried out under 6V driving voltage the test of luminosity, and the reflectivity of test component between wavelength 380 ~ 780nm, 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 scattering layer at reflective electrode surface, and at second transmission electrode surface preparation the second light scattering layer, the reflectivity of device have decreased to less than 25% from 88% of comparative example 2, illustrates that ambient light reflectivity in the devices greatly reduces.From luminosity, although reflectivity reduces greatly, the luminosity of device but can keep higher, this is due to the second light scattering layer on the second transmission electrode, except reducing the ambient light reflects of outside, can also play the effect that light extracts, therefore brightness is higher.
Organic electroluminescence device obtained by the embodiment of the present invention 11 ~ 14 and comparative example 3 is carried out under 6V driving voltage the test of luminosity, and the reflectivity of test component between wavelength 380 ~ 780nm, 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 arranging light scattering layer at reflective electrode surface, the reflectivity of device have decreased to less than 29% from 87% of comparative example 3, illustrates that ambient light reflectivity in the devices greatly reduces.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. an organic electroluminescence device, it is characterized in that, comprise substrate and the reflecting electrode on substrate that is cascading, light scattering layer, first transmission electrode, light emitting functional layer and the second transmission electrode, the material of described light scattering layer comprises Nano microsphere and polymeric material, pottery or the macromolecule material particle of described Nano microsphere to be particle diameter be 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, the thickness of described light scattering layer is 10 ~ 100 μm, the material of described reflecting electrode is metallic film, described metallic film comprises metallic gold, silver, aluminium, copper, nickel, platinum, the alloy that magnesium simple substance or its combination in any are formed, the material of described first transmission electrode is conductive oxide film or metallic gold, silver, aluminium, platinum film, the material of described second transmission electrode is gold, silver, aluminium, the alloy firm that magnesium or its combination in any are formed, described light emitting functional layer at least comprises the hole transmission layer stacked gradually, luminescent layer and electron transfer layer.
2. organic electroluminescence device as claimed in claim 1, it is characterized in that, described second transmission electrode surface comprises the second light scattering layer further, the material of described second light scattering layer comprises Nano microsphere and polymeric material, pottery or the macromolecule material particle of described Nano microsphere to be particle diameter be 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described second light scattering layer is 10 ~ 100 μm.
3. organic electroluminescence device as claimed in claim 1 or 2, 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.
4. organic electroluminescence device as claimed in claim 1 or 2, it is characterized in that, described ceramic particle is silicon dioxide or titanium dioxide, and described macromolecule material particle is polystyrene microsphere.
5. organic electroluminescence device as claimed in claim 1 or 2, it is characterized in that, the mass ratio of described Nano microsphere and polymeric material is 10 ~ 50:100.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
The substrate of cleaning being placed in vacuum degree is 1 × 10
-3~ 1 × 10
-5in the vacuum film coating chamber of Pa, the mode of vacuum thermal resistance evaporation is adopted to prepare reflecting electrode on the substrate, evaporation rate is 0.2 ~ 2nm/s, and the material of described reflecting electrode is metallic film, and described metallic film comprises metallic gold, silver, aluminium, copper, nickel, platinum, the alloy that magnesium simple substance or its combination in any are formed;
The mode of silk screen printing is adopted to prepare light scattering layer at described reflective electrode surface, the material of described light scattering layer comprises Nano microsphere and polymeric material, described Nano microsphere is pottery or macromolecule material particle, particle diameter is 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described light scattering layer is 10 ~ 100 μm;
Prepare the first transmission electrode, light emitting functional layer and the second transmission electrode successively on described light scattering layer surface, obtain organic electroluminescence device; The material of described first transmission electrode is conductive oxide film or metal gold, silver, aluminium, platinum film, the material of described second transmission electrode is the alloy firm that gold, silver, aluminium, magnesium or its combination in any are formed, described light emitting functional layer at least comprises the hole transmission layer, luminescent layer and the electron transfer layer that stack gradually, described first transmission electrode adopts the mode of vacuum evaporation or magnetron sputtering to prepare, and described light emitting functional layer and the second transmission electrode adopt 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, comprise further, adopt the mode of silk screen printing at described second transmission electrode surface preparation the second light scattering layer, the material of described second light scattering layer comprises Nano microsphere and polymeric material, described Nano microsphere is pottery or macromolecule material particle, particle diameter is 50 ~ 1500nm, described polymeric material is the polymer of hot curing or the polymeric material of photocuring, and the thickness of described second light scattering layer is 10 ~ 100 μm.
8. the preparation method of organic electroluminescence device as claimed in claims 6 or 7, 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; 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 claims 6 or 7, 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 claims 6 or 7, it is characterized in that, the meshcount of described silk screen printing is 200 ~ 1000 orders.
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