CN104183759A - Organic light-emitting device and preparation method thereof - Google Patents
Organic light-emitting device and preparation method thereof Download PDFInfo
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- CN104183759A CN104183759A CN201310192569.8A CN201310192569A CN104183759A CN 104183759 A CN104183759 A CN 104183759A CN 201310192569 A CN201310192569 A CN 201310192569A CN 104183759 A CN104183759 A CN 104183759A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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- 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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
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Abstract
Disclosed is an organic light-emitting device which includes a conductive substrate provided with anode patterns, a light-emitting layer, a cathode, a protective layer and a package cover, which are sequentially laminated. The material of the protective layer is copper phthalocyanine, silicon monoxide, magnesium fluoride or zinc sulfide. The package cover packages the light-emitting layer, the cathode and the protective layer on the conductive substrate. The package cover includes a barrier layer and a package layer laminated on the surface of the barrier layer. The material of the barrier layer is organic silicon. The material of the package layer is polyethylene glycol terephthalate. The service life of the organic light-emitting device is comparatively long. The invention also provides a preparation method for the organic light-emitting device.
Description
Technical field
The present invention relates to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is that the luminous organic material of making one deck tens nanometer thickness on ito glass is made luminescent layer, and there is the metal electrode of one deck low work function luminescent layer top.While being added with voltage on electrode, luminescent layer just produces light radiation.
Organic electroluminescence device is subject to after moisture and moisture erosion, can cause that the material of organic electroluminescence device inner member occurs aging and then lost efficacy, thereby the life-span of described organic electroluminescence device is shorter.
Summary of the invention
Based on this, be necessary to provide longer organic electroluminescence device of a kind of life-span and preparation method thereof.
An organic electroluminescence device, comprises the conductive substrates with anode pattern, luminescent layer, negative electrode and the protective layer that stack gradually, and the material of described protective layer is CuPc, silicon monoxide, magnesium fluoride or zinc sulphide;
Described organic electroluminescence device also comprises cap; described cap is packaged in described luminescent layer, negative electrode and protective layer in described conductive substrates; described cap comprises barrier layer and is laminated in the surperficial encapsulated layer on described barrier layer; the material on described barrier layer is organic germanium; the material of described encapsulated layer is PETG, and the structural formula of described organic germanium is:
or
In an embodiment, described cap coordinates and is formed with host cavity with described conductive substrates therein, and described luminescent layer, negative electrode and protective layer are all contained in described host cavity.
In an embodiment, the thickness on described barrier layer is 4 μ m～6 μ m therein; The thickness of described encapsulated layer is 100 μ m～200 μ m.
In an embodiment, the edge of described cap is tightly connected by packaging plastic and described conductive substrates therein.
In an embodiment, the thickness of described protective layer is 100nm～150nm therein; The thickness on described barrier layer is 4 μ m～6 μ m; The thickness of described encapsulated layer is 100 μ m～200 μ m.
A preparation method for organic electroluminescence device, comprises the following steps:
Form luminescent layer having in the conductive substrates of anode pattern;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer, the material of described protective layer is for being CuPc, silicon monoxide, magnesium fluoride or zinc sulphide; And
Use cap that described luminescent layer, negative electrode and protective layer are packaged in described conductive substrates; described cap comprises barrier layer and is laminated in the surperficial encapsulated layer on described barrier layer; the material on described barrier layer is organic germanium; the material of described encapsulated layer is PETG, and the structural formula of described organic germanium is:
or
In an embodiment, by coating packaging plastic, make described cap and described conductive substrates be tightly connected that described luminescent layer, negative electrode and protective layer are packaged in described conductive substrates therein.
In an embodiment, the thickness on described barrier layer is 4 μ m～6 μ m therein; The thickness of described encapsulated layer is 100 μ m～200 μ m.
In an embodiment, described cap coordinates and is formed with host cavity with described conductive substrates therein, and described luminescent layer, negative electrode and protective layer are all contained in described host cavity.。
In an embodiment, described barrier layer by solidifying preparation after the inner surface spin coating organic germanium of described encapsulated layer therein.
Above-mentioned organic electroluminescence device and preparation method thereof, protective layer can be protected negative electrode, avoid negative electrode to be damaged in follow-up preparation technology, the material on barrier layer is organic germanium, not only contain organic group but also contain germanium, can effectively stop the corrosion of aqueous vapor, simultaneously characteristic and the one of the organic characteristic of organic germanium collection and inorganic matter, can improve the barrier properties on barrier layer and the effective stress between slowly-releasing rete; Encapsulated layer adopts PET can effectively improve waterproof oxygen ability, thereby the life-span of organic electroluminescence device is longer.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of an embodiment;
Fig. 2 is preparation method's the flow chart of the organic electroluminescent of an embodiment.
Embodiment
Below in conjunction with the drawings and specific embodiments, organic electroluminescence device and preparation method thereof is further illustrated.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode comprises the conductive substrates with anode pattern 10, functional layer 20, negative electrode 30, protective layer 40 and the cap 70 stacking gradually.
Conductive substrates 10 is glass conductive substrates or organic PETG (PET) film substrate that conducts electricity.The ITO layer in conductive substrates 10 with the anode pattern of being prepared with.The thickness of ITO layer is 100nm～150nm.
Functional layer 20 is formed at substrate 10 surfaces.Functional layer 20 comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer stacking gradually.Be appreciated that hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, now functional layer 20 only comprises luminescent layer.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3).CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.
Negative electrode 30 is formed at functional layer 20 surfaces.Negative electrode 30 is single layer structure.The thickness of negative electrode is 100nm.The material of negative electrode 30 is aluminium (Al), silver (Ag) or gold (Au).
Protective layer 40 is formed at negative electrode 30 surfaces.The material of protective layer 40 is CuPc (CuPc), silicon monoxide (SiO), magnesium fluoride (MgF
2) or zinc sulphide (ZnS).The thickness of protective layer 40 is 100nm～150nm.
Cap 70 is covered on protective layer 40.Cap 70 is formed with host cavity.Host cavity is the groove from the surface of cap 70 depression.Cap 70 is covered on 50 surfaces, barrier layer and functional layer 20, negative electrode 30, protective layer 40 and barrier layer 50 is contained in to host cavity.Cap 70 comprises barrier layer 72 and is laminated in the surperficial encapsulated layer 74 on barrier layer 72.
The material on barrier layer 72 is organic germanium.Preferably, the structural formula of organic germanium is:
or
The material of encapsulated layer 74 is PETG (PET).The thickness on barrier layer 72 is 4 μ m～6 μ m.The thickness of encapsulated layer 74 is 100 μ m～200 μ m.
The edge of cap 70 is tightly connected by packaging plastic (not shown) and conductive substrates 10, thereby cap 70 is encapsulated in functional layer 20, negative electrode 30 and protective layer 40 in conductive substrates 10.Preferably, the thickness of packaging plastic is 1 μ m～1.5 μ m.
The protective layer 40 of above-mentioned organic electroluminescence device 100 can be protected negative electrode 30, avoid negative electrode 30 to be damaged in follow-up preparation technology, the material on barrier layer 72 is organic germanium, not only contain organic group but also contain germanium, can effectively stop the corrosion of aqueous vapor, simultaneously characteristic and the one of the organic characteristic of organic germanium collection and inorganic matter, can improve the barrier properties on barrier layer 72 and the effective stress between slowly-releasing rete; Encapsulated layer 74 adopts PET can effectively improve waterproof oxygen ability, thereby the life-span of organic electroluminescence device 100 is longer.
The host cavity that is appreciated that cap 70 can omit, and now directly makes cap 70 coated functional layer 20, negative electrode 30 and protective layer 40 or in conductive substrates 10, host cavity is set.
Please refer to Fig. 2, the preparation method of the organic electroluminescence device 100 of an execution mode, it comprises the following steps:
Step S110, in conductive substrates 10, form functional layer 20.
Functional layer 20 comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer stacking gradually.
Conductive substrates 10 can be glass conductive substrates or organic PETG (PET) film substrate that conducts electricity.Conductive substrates 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm～150nm.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.Hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, and now functional layer 20 only comprises luminescent layer.
Step S120, on functional layer 20 surface, form negative electrodes 30.
Negative electrode 30 is single layer structure.The thickness of negative electrode 30 is 100nm.The material of negative electrode 30 is aluminium (Al), silver (Ag) or gold (Au), and negative electrode 30 is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
Step S130, on negative electrode 30 surface, form protective layers 40.
The material of protective layer 40 is CuPc (CuPc), silicon monoxide (SiO), magnesium fluoride (MgF
2) or zinc sulphide (ZnS).The thickness of protective layer 40 is 100nm～150nm.Protective layer 40 is formed by vacuum evaporation, and vacuum degree is 8 * 10
-5pa～3 * 10
-5pa, evaporation rate is
Step S140, use cap 70 are packaged in functional layer 20, negative electrode 30 and protective layer 40 in conductive substrates 10.
Cap 70 is covered on protective layer 40.Cap 70 is formed with host cavity.Host cavity is the groove from the surface of cap 70 depression.Cap 70 is covered on 50 surfaces, barrier layer and functional layer 20, negative electrode 30, protective layer 40 and barrier layer 50 is contained in to host cavity.Cap 70 comprises barrier layer 72 and is laminated in the surperficial encapsulated layer 74 on barrier layer 72.
The material on barrier layer 72 is organic germanium.Preferably, the structural formula of organic germanium is:
or
The material of encapsulated layer 74 is PETG (PET).The thickness on barrier layer 72 is 4 μ m～6 μ m.The thickness of encapsulated layer 74 is 100 μ m～200 μ m.
In present embodiment, barrier layer 72 by solidifying preparation after the inner surface spin coating of encapsulated layer 74.The rotating speed of spin coating is 2000rpm～6000rpm, and the time of spin coating is 10s～60s.Preferably, ozone treatment is carried out in barrier layer 72 after solidifying.
The edge of cap 70 is tightly connected by packaging plastic (not shown) and conductive substrates 10, thereby cap 70 is encapsulated in functional layer 20, negative electrode 30 and protective layer 40 in conductive substrates 10.Preferably, the thickness of packaging plastic is 1 μ m～1.5 μ m.
In present embodiment, packaging plastic is epoxy encapsulation glue, with UV light (λ=200～400nm), is cured, and light intensity is 10～15mW/cm
2, the time for exposure is 300～400s.
The preparation method of above-mentioned organic electroluminescence device, preparation technology is simple, easily preparation in enormous quantities; The life-span of the organic electroluminescence device 100 of preparation is longer.
Below in conjunction with specific embodiment, organic electroluminescence device preparation method provided by the invention is elaborated.
Embodiment 1
The present embodiment is prepared structure: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3the organic electroluminescence device of/Al/CuPc/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface evaporation protective layer.
The material of protective layer is CuPc (CuPc).The thickness of protective layer 40 is 150nm.Protective layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
4, use cap that functional layer, negative electrode and protective layer are packaged in conductive substrates.
On the inner surface of PET film, adopt the mode of spin coating to prepare barrier layer, after spin coating, by UV, solidify, after having solidified, carry out ozone treatment.The rotating speed of spin coating is 6000rpm, and the time of spin coating is 60s.PET film and barrier layer form cap.The thickness on barrier layer is 6 μ m.The thickness of encapsulated layer is 200 μ m.
The material on barrier layer is
Cap edge-coating epoxy encapsulation glue (thickness 1.5 μ m), is cured light intensity 11mW/cm with UV light (λ=200～400nm)
2, time for exposure 300s.
Embodiment 2
The present embodiment is prepared structure: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3the organic electroluminescence device of/Al/SiO/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface evaporation protective layer.
The material of protective layer is SiO.The thickness of protective layer is 100nm.Protective layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
4, use cap that functional layer, negative electrode and protective layer are packaged in conductive substrates.
On the inner surface of PET film, adopt the mode of spin coating to prepare barrier layer, after spin coating, by UV, solidify, after having solidified, carry out ozone treatment.The rotating speed of spin coating is 2000rpm, and the time of spin coating is 10s.PET film and barrier layer form cap.The thickness on barrier layer is 4 μ m.The thickness of encapsulated layer is 100 μ m.
The material on barrier layer is
Cap edge-coating epoxy encapsulation glue (thickness 1 μ m), is cured light intensity 11mW/cm with UV light (λ=200～400nm)
2, time for exposure 300s.
Embodiment 3
The present embodiment is prepared structure: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/MgF
2the organic electroluminescence device of/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface evaporation protective layer.
The material of protective layer is MgF
2.The thickness of protective layer is 150nm.Protective layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
4, use cap that functional layer, negative electrode and protective layer are packaged in conductive substrates.
On the inner surface of PET film, adopt the mode of spin coating to prepare barrier layer, after spin coating, by UV, solidify, after having solidified, carry out ozone treatment.The rotating speed of spin coating is 4000rpm, and the time of spin coating is 40s.PET film and barrier layer form cap.The thickness on barrier layer is 5 μ m.The thickness of encapsulated layer is 150 μ m.
The material on barrier layer is
Cap edge-coating epoxy encapsulation glue (thickness 1.5 μ m), is cured light intensity 11mW/cm with UV light (λ=200～400nm)
2, time for exposure 400s.
Comparative example
The present embodiment is prepared structure: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/MgF
2the organic electroluminescence device of/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 25%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA).The thickness of hole transmission layer is 40nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 30nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 25%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface evaporation protective layer.
The material of protective layer is MgF
2.The thickness of protective layer is 150nm.Protective layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
4, use cap that functional layer, negative electrode and protective layer are packaged in conductive substrates.
The thickness of encapsulated layer is 150 μ m.
Cap edge-coating epoxy encapsulation glue (thickness 1.5 μ m), is cured light intensity 11mW/cm with UV light (λ=200～400nm)
2, time for exposure 400s.
The preparation used of the embodiment of the present invention and comparative example and tester are: high vacuum coating equipment (scientific instrument development center, Shenyang Co., Ltd, pressure <1 * 10-3Pa), magnetron sputtering apparatus (scientific instrument development center, Shenyang Co., Ltd), current-voltage tester (U.S. Keithly company, 2400), chroma-luminance meter (Konica Minolta, model: CS-100A), IEI point gum machine system, DYMAX photocuring system model:.
Refer to table 1, table 1 is depicted as the test result of the aqueous vapor penetrance (Water Vapor Transmission Rate) of organic electroluminescence device prepared by embodiment 1～embodiment 3 and comparative example.The aqueous vapor penetrance of the organic electroluminescence device that the aqueous vapor penetrance of the organic electroluminescence device of embodiment 1～embodiment 3 preparations is all prepared much smaller than comparative example as can be seen from Table 1, waterproof effect is better, can effectively reduce the erosion of outside aqueous vapor to organic electroluminescence device, thereby improve the life-span of organic electroluminescence device.
Table 1
| ? | WVTR(g/m 2/day) |
| Embodiment 1 | 4.5×10 -4 |
| Embodiment 2 | 3.2×10 -4 |
| Embodiment 3 | 5.6×10 -4 |
| Comparative example | 8.9×10 -2 |
Refer to table 2, it is 1000cd/m at original intensity that table 2 is depicted as organic electroluminescence device prepared by embodiment 1～embodiment 3 and comparative example
2condition under life-span (brightness be reduced to original intensity 70% time time used).
Table 2
As can be seen from Table 2, the initial brightness of the organic electroluminescence device of embodiment 1～embodiment 3 preparations is 1000cd/m
2time, the life-span reaches more than 8500 hours, and the life-span is longer.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an organic electroluminescence device, comprise the conductive substrates with anode pattern, luminescent layer and the negative electrode that stack gradually, it is characterized in that, described organic electroluminescence device also comprises the protective layer being laminated on described negative electrode, and the material of described protective layer is CuPc, silicon monoxide, magnesium fluoride or zinc sulphide;
Described organic electroluminescence device also comprises cap; described cap is packaged in described luminescent layer, negative electrode and protective layer in described conductive substrates; described cap comprises barrier layer and is laminated in the surperficial encapsulated layer on described barrier layer; the material on described barrier layer is organic germanium; the material of described encapsulated layer is PETG, and the structural formula of described organic germanium is:
or
2. organic electroluminescence device according to claim 1, is characterized in that, described cap coordinates and is formed with host cavity with described conductive substrates, and described luminescent layer, negative electrode and protective layer are all contained in described host cavity.
3. organic electroluminescence device according to claim 1, is characterized in that, the thickness on described barrier layer is 4 μ m～6 μ m; The thickness of described encapsulated layer is 100 μ m～200 μ m.
4. organic electroluminescence device according to claim 1, is characterized in that, the edge of described cap is tightly connected by packaging plastic and described conductive substrates.
5. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described protective layer is 100nm～150nm.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
Form luminescent layer having in the conductive substrates of anode pattern;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer, the material of described protective layer is for being CuPc, silicon monoxide, magnesium fluoride or zinc sulphide; And
Use cap that described luminescent layer, negative electrode and protective layer are packaged in described conductive substrates; described cap comprises barrier layer and is laminated in the surperficial encapsulated layer on described barrier layer; the material on described barrier layer is organic germanium; the material of described encapsulated layer is PETG, and the structural formula of described organic germanium is:
or
7. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: by coating packaging plastic, make described cap and described conductive substrates be tightly connected that described luminescent layer, negative electrode and protective layer are packaged in described conductive substrates.
8. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: the thickness on described barrier layer is 4 μ m～6 μ m; The thickness of described encapsulated layer is 100 μ m～200 μ m.
9. the preparation method of organic electroluminescence device according to claim 6, described cap coordinates and is formed with host cavity with described conductive substrates, and described luminescent layer, negative electrode and protective layer are all contained in described host cavity.
10. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: prepared by the solution that organic germanium is contained by the inner surface spin coating at described encapsulated layer in described barrier layer.
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| CN101359722A (en) * | 2008-09-23 | 2009-02-04 | 吉林大学 | A method for encapsulating a top-emitting organic electroluminescent device |
| JP2011233912A (en) * | 2004-11-17 | 2011-11-17 | Ube Ind Ltd | Organic electroluminescent element |
| CN102856503A (en) * | 2011-06-28 | 2013-01-02 | 海洋王照明科技股份有限公司 | Organic electroluminescent device and preparation method thereof |
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2013
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| JP2011233912A (en) * | 2004-11-17 | 2011-11-17 | Ube Ind Ltd | Organic electroluminescent element |
| CN101080121A (en) * | 2007-07-06 | 2007-11-28 | 清华大学 | An organic EL part and its making method |
| CN101359722A (en) * | 2008-09-23 | 2009-02-04 | 吉林大学 | A method for encapsulating a top-emitting organic electroluminescent device |
| CN102856503A (en) * | 2011-06-28 | 2013-01-02 | 海洋王照明科技股份有限公司 | Organic electroluminescent device and preparation method thereof |
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Application publication date: 20141203 |