CN104218173A - 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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- CN104218173A CN104218173A CN201310209538.9A CN201310209538A CN104218173A CN 104218173 A CN104218173 A CN 104218173A CN 201310209538 A CN201310209538 A CN 201310209538A CN 104218173 A CN104218173 A CN 104218173A
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- CECAIMUJVYQLKA-UHFFFAOYSA-N iridium 1-phenylisoquinoline Chemical compound [Ir].C1=CC=CC=C1C1=NC=CC2=CC=CC=C12.C1=CC=CC=C1C1=NC=CC2=CC=CC=C12.C1=CC=CC=C1C1=NC=CC2=CC=CC=C12 CECAIMUJVYQLKA-UHFFFAOYSA-N 0.000 description 2
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- MQCHTHJRANYSEJ-UHFFFAOYSA-N n-[(2-chlorophenyl)methyl]-1-(3-methylphenyl)benzimidazole-5-carboxamide Chemical compound CC1=CC=CC(N2C3=CC=C(C=C3N=C2)C(=O)NCC=2C(=CC=CC=2)Cl)=C1 MQCHTHJRANYSEJ-UHFFFAOYSA-N 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- YRZZLAGRKZIJJI-UHFFFAOYSA-N oxyvanadium phthalocyanine Chemical compound [V+2]=O.C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 YRZZLAGRKZIJJI-UHFFFAOYSA-N 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 description 2
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- 125000005504 styryl group Chemical group 0.000 description 2
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Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention provides an organic light emission diode device. The organic light emission diode device comprises a substrate and an anode, a light emission functional layer and a cathode which are sequentially laminated on the substrate, a light matching layer and a light extraction layer are sequentially arranged on the surface of the cathode, the material of the light extraction layer comprises nanoparticles and a polymer material, the nanoparticles are ceramic or high-polymer material particles with the 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 extraction layer is 10 to 100 micrometers, the material of the light matching layer is a mixed material formed by metal and an organic material, the metal is silver, aluminum or magnesium, and the organic material is N,N'-diphenyl-N,N'-bis(1-naphthyl)-1,1'-biphenyl-4,4'-diamine, copper phthalocyanine or 8- hydroxyquinoline aluminum. The luminous 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 to be referred as OLED, have that brightness is high, material range of choice is wide, driving voltage is low, entirely solidify the characteristics such as 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 that has potentiality, meet the development trend that information age mobile communication and information show, and the requirement of green lighting technique, be current lot of domestic and foreign researcher's focal point.
In the OLED luminescent device of traditional top transmitting, conventionally adopted semi-transparent metallic film as euphotic electrode, because the light transmission of metal electrode own is poor, make the rate variance that sees through of light, and when the optical fiber that also has quite a few enters the interface of air from negative electrode, due to other reason of refringence, the optical fiber of a large portion is limited in ray structure, can not shine outside, therefore make the luminous efficiency of top ballistic device lower.
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 prepare light matching layer and light-extraction layer at cathode surface, improved 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, light emitting functional layer and the negative electrode that are cascading on substrate, described cathode surface be cascading light matching layer and light-extraction layer, the material of described smooth matching layer is the composite material that metal and organic material form, the mass ratio of described metal and organic material is 10～50:100, described metal is silver, aluminium or magnesium, described organic material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, CuPc or oxine aluminium; The material of described light-extraction layer comprises Nano microsphere and polymeric material, described Nano microsphere is that particle diameter is pottery or the macromolecule material particle of 50～1500nm, 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 μ m; The material of described anode is conductive metal film; The material of described negative electrode is the alloy that silver, aluminium, magnesium simple substance or its combination in any form, and described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer stacking 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.
Preferably, the thickness of described smooth matching layer is 5～20nm.
Between light-extraction layer and metal electrode, because the refractive index difference of light-extraction layer and metal electrode is larger, if light directly transmits to light-extraction layer from metal electrode, not because seriously not mating of refractive index, cause light that serious scattering occurs between light-extraction layer and metal electrode, swash source ripple, the phenomenons such as dissipation, therefore a light matching layer need to be set at this interface, it is index matching layer, guarantee light is more smooth to the transfer ratio between light-extraction layer from metal electrode like this, thereby realize light and see through metal electrode, then arrive light-extraction layer, finally shine outside OLED structure.
The material of described anode is conductive metal film.
Preferably, described conductive metal film is metallic gold (Au), silver (Ag), aluminium (Al) or platinum (Pt) film, and thickness is 70～200nm.
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.
The material of negative electrode is the alloy that silver (Ag), aluminium (Al), magnesium (Mg) simple substance or its combination in any form, and thickness is 18～30nm.
Described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer being cascading.In order to improve the luminous efficiency of device, hole injection layer and electron injecting layer can be further set.
The material of hole transmission layer, electron transfer layer and luminescent layer is not done 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-naphthyl phenyl 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-aminomethyl phenyl-N-phenyl amino) triphenylamines (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-yl) triphenylamine (TCTA), thickness is 20～60nm.
Preferably, the material of luminescent layer is the composite material that material of main part doping guest materials forms, 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-yl) 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 pyridine-N, C2) pyridine formyl closes iridium (FIrpic), two (4,6-difluorophenyl pyridines)-tetra-(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-diphenylethyllenes)-1,1 '-biphenyl (DPVBi), 4,4 '-bis-[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), and ranadylic phthalocyanine (VOPc), 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:
It is 1 * 10 that clean substrate is placed in to vacuum degree
-3～1 * 10
-5in the vacuum film coating chamber of Pa, prepare successively anode, light emitting functional layer and negative electrode; The material of described anode is conductive metal film; Described anode adopts the mode of the evaporation of vacuum thermal resistance or electron beam evaporation to prepare, and evaporation rate is 0.2～2nm/s; Described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer stacking gradually; The material of described negative electrode is the alloy that silver, aluminium, magnesium simple substance or its combination in any form; Described hole transmission layer, luminescent layer, electron transfer layer and negative electrode all adopt the mode of vacuum thermal resistance evaporation to prepare;
Adopt the mode of vacuum coevaporation on described negative electrode, to prepare light matching layer, the material of described smooth matching layer is the composite material that metal and organic material form, the mass ratio of described metal and organic material is 10～50:100, described metal is silver, aluminium or magnesium, and described organic material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, CuPc or oxine aluminium; The material evaporation rate of described smooth matching layer is 0.1～2nm/s, and described metal is 10～50:100 with the evaporation rate ratio of organic material;
Finally adopt the mode of silk screen printing to prepare light-extraction layer on described smooth matching layer, obtain organic electroluminescence device; The material of described light-extraction 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-extraction layer is 10～100 μ m.
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 described smooth matching layer is 5～20nm.
The material of described anode is conductive metal film.
Preferably, described conductive metal film is metal gold, silver, aluminium or platinum film, and thickness is 70～200nm.
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.
The material of negative electrode is the alloy that silver (Ag), aluminium (Al), magnesium (Mg) simple substance or its combination in any form, and thickness is 18～30nm.
Described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer being cascading.In order to improve the luminous efficiency of device, hole injection layer and electron injecting layer can be further set.
The material of hole transmission layer, electron transfer layer and luminescent layer is not done 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-naphthyl phenyl 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-aminomethyl phenyl-N-phenyl amino) triphenylamines (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-yl) triphenylamine (TCTA), thickness is 20～60nm.
Preferably, the material of luminescent layer is the composite material that material of main part doping guest materials forms, 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-yl) 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 pyridine-N, C2) pyridine formyl closes iridium (FIrpic), two (4,6-difluorophenyl pyridines)-tetra-(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-diphenylethyllenes)-1,1 '-biphenyl (DPVBi), 4,4 '-bis-[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), and ranadylic phthalocyanine (VOPc), 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, going out optical position, be that cathode surface is provided with light matching layer and light-extraction layer, described light-extraction layer is the thin polymer film that has added the Nano microsphere of pottery or macromolecular material, because Nano microsphere has light scattering effect, can make the refractive index comparison match between air and light matching layer, and can change the exit direction of incident light, increase the refractive index of extract layer, thereby increase the critical angle of emergent light, increase light extraction efficiency; Light matching layer is set between light-extraction layer and metallic cathode, and guarantee light is more smooth to the transfer ratio between light-extraction layer from metal electrode like this, thereby realize light, sees through metal electrode, then arrives light-extraction layer, finally shines outside OLED structure; 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 easily large area preparation is suitable for large-scale industrialization and uses.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device that makes of the embodiment of the present invention 1.
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, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, 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) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the metal A g film of 100nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, the material of negative electrode is metal A g, and thickness is 18nm;
(4) adopt the mode of vacuum coevaporation to prepare at cathode surface the light matching layer that a layer thickness is 20nm, light matching layer is by metal A g and Alq
3coevaporation preparation, metal A g and Alq
3mass ratio be 10:100, the evaporation rate of metal A g is 0.1nm/s, Alq
3evaporation rate be 1nm/s;
(5) adopt silk-screen printing technique on the surface of light matching layer, to form the light-extraction layer that thickness is 100 μ m, obtain organic electroluminescence device; The material of light-extraction layer comprises that mass ratio is titanium dioxide nanometer microballoons and the light-cured acrylic resin of 50:100, and the particle diameter of titanium dioxide nanometer microballoons is 50nm, and it is 400 object silk screen printing film forming that screen printing process adopts order number.
Fig. 1 is the structural representation of the organic electroluminescence device that makes of the embodiment of the present invention 1.As shown in Figure 1, the present embodiment organic electroluminescence device, comprises transparent glass substrate 10, anode 11, light emitting functional layer 12, negative electrode 13, light matching layer 14 and light-extraction layer 15 successively.In light-extraction layer 15, comprise titanium dioxide nanometer microballoons 150.
Embodiment 2
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises that mass ratio is titanium dioxide nanometer microballoons and the light-cured acrylic resin of 20:100, the particle diameter of titanium dioxide nanometer microballoons is 100nm, it is 1000 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 80 μ m.
Embodiment 3
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises that mass ratio is titanium dioxide nanometer microballoons and the light-cured acrylic resin of 20:100, the particle diameter of titanium dioxide nanometer microballoons is 250nm, it is 800 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 20 μ m.
Embodiment 4
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises that mass ratio is titanium dioxide nanometer microballoons and the light-cured acrylic resin of 10:100, the particle diameter of titanium dioxide nanometer microballoons is 500nm, it is 800 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 10 μ m.
Embodiment 5
The difference of the present embodiment and embodiment 1 is, the material of light-extraction layer comprises that mass ratio is titanium dioxide nanometer microballoons and the light-cured acrylic resin of 10:100, the particle diameter of titanium dioxide nanometer microballoons is 1000nm, it is 1000 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 50 μ m.
Embodiment 6
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the metal A u film of 200nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, the material of negative electrode is metal A l-Mg alloy, and thickness is 30nm;
(4) adopt the mode of vacuum coevaporation to prepare at cathode surface the light matching layer that a layer thickness is 5nm, light matching layer is prepared by metal M g and NPB coevaporation, and the mass ratio of metal M g and NPB is 50:100; The evaporation rate of metal M g is 0.5nm/s, and the evaporation rate of NPB is 1nm/s;
(5) adopt silk-screen printing technique on the surface of light matching layer, to form the light-extraction layer that thickness is 10 μ m, obtain organic electroluminescence device; The material of light-extraction layer comprises that mass ratio is Properties of Polystyrene Nano Particles and the light-cured acrylic resin of 50:100, and the particle diameter of Properties of Polystyrene Nano Particles is 200nm, and it is 400 object silk screen printing film forming that screen printing process adopts order number.
Embodiment 7
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises that mass ratio is Properties of Polystyrene Nano Particles and the light-cured acrylic resin of 20:100, the particle diameter of Properties of Polystyrene Nano Particles is 400nm, it is 1000 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 60 μ m.
Embodiment 8
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises that mass ratio is Properties of Polystyrene Nano Particles and the light-cured acrylic resin of 20:100, the particle diameter of Properties of Polystyrene Nano Particles is 800nm, it is 600 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 15 μ m.
Embodiment 9
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises that mass ratio is Properties of Polystyrene Nano Particles and the light-cured acrylic resin of 10:100, the particle diameter of Properties of Polystyrene Nano Particles is 1000nm, it is 800 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 20 μ m.
Embodiment 10
The difference of the present embodiment and embodiment 6 is, the material of light-extraction layer comprises that mass ratio is Properties of Polystyrene Nano Particles and the light-cured acrylic resin of 10:100, the particle diameter of Properties of Polystyrene Nano Particles is 1500nm, it is 1000 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 100 μ m.
Embodiment 11
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the Pt metal film of 100nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, the material of negative electrode is metal A g-Mg alloy, and thickness is 25nm;
(4) adopt the mode of vacuum coevaporation to prepare at cathode surface the light matching layer that a layer thickness is 15nm, light matching layer is prepared by metal M g and CuPc coevaporation, and the mass ratio of metal M g and CuPc is 20:100; The evaporation rate of metal M g is 0.4nm/s, and the evaporation rate of NPB is 2nm/s;
(5) adopt silk-screen printing technique on the surface of light matching layer, to form the light-extraction layer that thickness is 100 μ m, obtain organic electroluminescence device; The material of light-extraction layer comprises that mass ratio is silicon dioxide nanosphere and the heat-curable epoxy resin of 20:100, and the particle diameter of silicon dioxide nanosphere is 50nm, and it is 600 object silk screen printing film forming that screen printing process adopts order number.
Embodiment 12
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises that mass ratio is silicon dioxide nanosphere and the heat-curable epoxy resin of 50:100, the particle diameter of silicon dioxide nanosphere is 100nm, it is 400 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 60 μ m.
Embodiment 13
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises that mass ratio is silicon dioxide nanosphere and the heat-curable epoxy resin of 15:100, the particle diameter of silicon dioxide nanosphere is 250nm, it is 200 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 20 μ m.
Embodiment 14
The difference of the present embodiment and embodiment 11 is, the material of light-extraction layer comprises that mass ratio is silicon dioxide nanosphere and the heat-curable epoxy resin of 10:100, the particle diameter of silicon dioxide nanosphere is 400nm, it is 200 object silk screen printing film forming that screen printing process adopts order number, and the thickness of light-extraction layer is 60 μ m.
Comparative example 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the metal A g film of 100nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, obtain organic electroluminescence device, the material of negative electrode is metal A g, and thickness is 18nm.
Comparative example 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the metal A u film of 200nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, obtain organic electroluminescence device, the material of negative electrode is metal A l-Mg alloy, and thickness is 30nm.
Comparative example 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) transparent glass substrate is placed in to 1 * 10
-4in the vacuum film coating chamber of Pa, it is that the Pt metal film of 100nm is as anode that the mode that adopts vacuum evaporation is prepared a layer thickness at substrate surface;
(2) adopt the mode of vacuum evaporation to prepare light emitting functional layer at anode surface, comprise successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
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 forming in CBP, wherein Ir (ppy)
3with the mass ratio of CBP be 10:100, thickness is 15nm; Electron transfer layer adopts TPBi, and thickness is 30nm; Electron injecting layer adopts LiF, and thickness is 1nm;
(3) adopt the mode of vacuum evaporation to prepare negative electrode on electron injecting layer surface, obtain organic electroluminescence device, the material of negative electrode is metal A g-Mg alloy, and thickness is 25nm.
Effect embodiment
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 test electric property of U.S. Keithley company, CS-100A colorimeter test brightness and the colourity of Japanese Konica Minolta company.
The embodiment of the present invention 1～5 and the prepared organic electroluminescence device of comparative example 1 are carried out to luminous efficiency test under 6V driving voltage, and test result is as shown in table 1:
Table 1
Data by table 1 can be found out, the organic electroluminescence device providing of the present invention, by light matching layer and light-extraction layer are set at cathode surface, more than luminous efficiency has been brought up to 20.9lm/W from the 11.2lm/W of comparative example.This is because light-extraction layer includes Nano microsphere, and Nano microsphere has light scattering effect, can make the refractive index comparison match between air and light matching layer, and can change the exit direction of incident light, thereby increase the critical angle of emergent light, thereby increase light extraction efficiency, finally improves the luminous efficiency of device.
The embodiment of the present invention 6～10 and the prepared organic electroluminescence device of comparative example 2 are carried out to luminous efficiency test under 6V driving voltage, and test result is as shown in table 2:
Table 2
From the data of table 2, can find out, the organic electroluminescence device providing of the present invention, by light matching layer and light-extraction layer are set at cathode surface, more than luminous efficiency has been brought up to 19.1lm/W from the 10.2lm/W of comparative example 2.
The embodiment of the present invention 11～14 and the prepared organic electroluminescence device of comparative example 3 are carried out to luminous efficiency test under 6V driving voltage, and test result is as shown in table 3:
Table 3
From the data of table 3, can find out, the organic electroluminescence device providing of the present invention, by light matching layer and light-extraction layer are set at cathode surface, more than luminous efficiency has been brought up to 21.4lm/W from the 12.1lm/W of comparative example 3.
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, light emitting functional layer and the negative electrode that are cascading on substrate, it is characterized in that, described cathode surface be cascading light matching layer and light-extraction layer, the material of described smooth matching layer is the composite material that metal and organic material form, the mass ratio of described metal and organic material is 10～50:100, described metal is silver, aluminium or magnesium, described organic material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, CuPc or oxine aluminium; The material of described light-extraction layer comprises Nano microsphere and polymeric material, described Nano microsphere is that particle diameter is pottery or the macromolecule material particle of 50～1500nm, 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 μ m; The material of described anode is conductive metal film; The material of described negative electrode is the alloy that silver, aluminium, magnesium simple substance or its combination in any form, and described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer stacking gradually.
2. organic electroluminescence device as claimed in claim 1, 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, 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, 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, is characterized in that, the thickness of described smooth matching layer is 5～20nm.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
It is 1 * 10 that clean substrate is placed in to vacuum degree
-3～1 * 10
-5in the vacuum film coating chamber of Pa, prepare successively anode, light emitting functional layer and negative electrode; The material of described anode is conductive metal film; Described anode adopts the mode of the evaporation of vacuum thermal resistance or electron beam evaporation to prepare, and evaporation rate is 0.2～2nm/s; Described light emitting functional layer at least comprises hole transmission layer, luminescent layer and the electron transfer layer stacking gradually; The material of described negative electrode is the alloy that silver, aluminium, magnesium simple substance or its combination in any form; Described hole transmission layer, luminescent layer, electron transfer layer and negative electrode all adopt the mode of vacuum thermal resistance evaporation to prepare;
Adopt the mode of vacuum coevaporation on described negative electrode, to prepare light matching layer, the material of described smooth matching layer is the composite material that metal and organic material form, the mass ratio of described metal and organic material is 10～50:100, described metal is silver, aluminium or magnesium, and described organic material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, CuPc or oxine aluminium; The material evaporation rate of described smooth matching layer is 0.1～2nm/s, and described metal is 10～50:100 with the evaporation rate ratio of organic material;
Finally adopt the mode of silk screen printing to prepare light-extraction layer on described smooth matching layer, obtain organic electroluminescence device; The material of described light-extraction 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-extraction layer is 10～100 μ m.
7. the preparation method of organic electroluminescence device as claimed in claim 6, 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.
8. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, the mass ratio of described Nano microsphere and polymeric material is 10～50:100.
9. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, the meshcount of described silk screen printing is 200～1000 orders.
10. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, the thickness of described smooth matching layer is 5～20nm.
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Application publication date: 20141217 |