CN103594648A - Organic electroluminescent device and preparation method thereof - Google Patents
Organic electroluminescent device and preparation method thereof Download PDFInfo
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- CN103594648A CN103594648A CN201210290604.5A CN201210290604A CN103594648A CN 103594648 A CN103594648 A CN 103594648A CN 201210290604 A CN201210290604 A CN 201210290604A CN 103594648 A CN103594648 A CN 103594648A
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Abstract
The invention provides an organic electroluminescent device and a preparation method thereof. The organic electroluminescent device comprises an anode substrate, a luminescent layer, a protective layer, a metal barrier layer, an organic barrier layer, an insulating layer and an external protective layer which are sequentially laminated, wherein the metal barrier layer is made of at least one of Ag, Al, Au, Cu, Ni and Mg; the organic barrier layer is made of at least one of polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin; and the insulating layer is made of at least one of WO3, V2O5, MoO3 and In2O3. The organic electroluminescent device has the advantages of long service life, strong water oxygen resistant ability, cost reduction and the like, and is suitable for mass production.
Description
Technical field
The present invention relates to technical field of organic electroluminescence, particularly relate 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 to make luminescent layer at the luminous organic material of ITO (tin indium oxide) making one deck tens nanometer thickness on glass, 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.
OLED device have active illuminating, luminous efficiency high, low in energy consumption, light, thin, without advantages such as angle limitations, by insider, thought to be most likely at the device of new generation that occupies dominance on following illumination and display device market.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, has obtained huge achievement.Because the whole world is increasing, throw light on and show that producer drops into research and development one after another, having promoted greatly the industrialization process of OLED, making the growth rate of OLED industry surprising, having arrived the prospect of scale of mass production at present.
Flexible OLED device products is the development trend of organic electroluminescence device, but short shortcoming of ubiquity life-span at present, has greatly limited the process of OLED device.Life-span is short is due to the unstable of organic material or OLED device package effect is bad, react and cause with the gas such as water vapour, oxygen, therefore, make OLED device reach the hot fields that be current domestic and international research enough useful life by steady operation.
Summary of the invention
Based on this, be necessary to provide organic electroluminescence device that a kind of life-span is long, waterproof oxygen ability is strong and preparation method thereof.
, comprise the anode substrate, luminescent layer, negative electrode, protective layer, metal barrier, organic barrier layer, insulating barrier and the outer protective layer that stack gradually; Wherein,
The material of described metal barrier is at least one in Ag, Al, Au, Cu, Ni and Mg;
The material on described organic barrier layer is at least one in polytetrafluoroethylene, methacrylic resin and cyclic aliphatic epoxy resin;
The material of described insulating barrier is WO
3, V
2o
5, MoO
3and In
2o
3in at least one.
In an embodiment, the material of described protective layer is CuPc, NPB, Alq3, SiO, MgF therein
2and at least one in ZnS.
Therein in an embodiment, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, and the material of described metal level is at least one in aluminium, silver and gold, and the material of described dielectric layer is zinc sulphide or tin indium oxide.
In an embodiment, the material of described outer protective layer is SiO therein.
In an embodiment, described metal barrier, organic barrier layer, insulating barrier form barrier layer therein, and the number of plies on described barrier layer is three layers.
A preparation method for organic electroluminescence device, comprises the following steps:
On anode substrate, form luminescent layer;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer;
Adopt the method for vacuum evaporation to form metal barrier on described protective layer, wherein, the material of described metal barrier is at least one in Ag, Al, Au, Cu, Ni and Mg, and vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 200nm;
Adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer, under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cyclic aliphatic epoxy resin is spin-coated on described carbide lamella, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200s ~ 300s;
Adopt the method for vacuum evaporation to form insulating barrier on described organic barrier layer, the material of described insulating barrier is WO
3, V
2o
5, MoO
3and In
2o
3in at least one, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 50nm ~ 100nm; And
On described insulating barrier, form outer protection layer.
In an embodiment, adopt the method for vacuum evaporation to form described protective layer therein, the material of wherein said protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
In an embodiment, adopt the method for vacuum evaporation to form described outer protective layer therein, the material of described outer protective layer is SiO, and vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 150nm.
Therein in an embodiment, adopt vapour deposition method to form described negative electrode, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, and the material of described metal level is at least one in aluminium, silver and gold, and the material of described dielectric layer is zinc sulphide or tin indium oxide.
In an embodiment, described metal barrier, organic barrier layer, insulating barrier form barrier layer therein, and the number of plies on described barrier layer is three layers.
Above-mentioned organic electroluminescence device is prepared protective layer and is prevented that negative electrode is damaged; Adopt metal barrier and insulating barrier as inorganic barrier layer, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, improve waterproof oxygen ability; Increase outer protective layer, form fine and close diaphragm, further improve waterproof oxygen ability, improve the useful life of organic electroluminescence device.
Accompanying drawing explanation
Fig. 1 is the organic electroluminescence device structure chart of an execution mode;
Fig. 2 is preparation method's the flow chart of the organic electroluminescence device of an execution mode.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, so the present invention is not subject to the restriction of following public concrete enforcement.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode, comprises the anode substrate 110, functional layer 120, negative electrode 130, protective layer 140, metal barrier 150, organic barrier layer 160, insulating barrier 170 and the outer protective layer 180 that stack gradually.
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 30%.The thickness of hole injection layer is 10nm.
The material of hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.
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 10nm.
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3).CsN
3quality percentage composition be 30%.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.
Insulating barrier 170 is formed at the surface on organic barrier layer 160.The material of described insulating barrier 170 is WO
3, V
2o
5, MoO
3and In
2o
3at least one in rete.Insulating barrier 170 thickness are 50 ~ 100nm.Insulating barrier has good insulation property, improves the anti-blocking capability of organic electroluminescence device packaging film.
Described metal barrier 150, organic barrier layer 160,170 3 layers of formation barrier layer of insulating barrier, preferred, repeat barrier layer at least three times, form multilayer barrier layer.Form block water, the erosion of oxygen isoreactivity material to organic electroluminescence device better of acting as of multilayer barrier layer, the life-span of improving organic electroluminescence device.
Outer protective layer 180 is formed at the surface of insulating barrier 170.The material of described outer protective layer 180 is SiO.Acting as of outer protective layer forms fine and close diaphragm, can further improve the packaging effect of organic electroluminescence device.
Above-mentioned organic electroluminescence device 100, adopts metal barrier 150, organic barrier layer 160 and insulating barrier 170 as barrier layer, block water, the erosion of oxygen isoreactivity material to organic electroluminescence device, the life-span of improving organic electroluminescence device.
Refer to Fig. 2, the preparation method of above-mentioned organic electroluminescence device 100 comprises the steps:
Step S110, on anode substrate 110, form functional layer 120.
Preliminary treatment was first carried out to remove the pollutant on anode substrate 110 surfaces in anode substrate 110 surfaces before forming functional layer 120, and the oxygen content of carrying out surface active increase anode substrate 110 surfaces is to improve the work function on anode substrate 110 surfaces.Be specially, anode substrate 110 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 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 120 only comprises luminescent layer.
Step S120, in described functional layer 120, form negative electrode 130.
When negative electrode 130 is single layer structure, the thickness of negative electrode 130 is 100nm, and the material of negative electrode 130 is aluminium (Al), silver (Ag) or gold (Au), and negative electrode 130 is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
When negative electrode 130 is sandwich construction, negative electrode 130 comprises two layer medium layer and is located at the metal level between two layer medium layer.The thickness of dielectric layer is 30nm, and the thickness of metal level is 10nm.The material of dielectric layer is zinc sulphide (ZnS) or tin indium oxide (ITO), and the material of metal level is silver (Ag).Wherein, tin indium oxide (ITO) is made by sputter, base vacuum degree 2 * 10
-4pa; ZnS or Ag are formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
Step S130, on described negative electrode 130, form protective layer 140.
The material of protective layer 140 is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS.During vacuum evaporation, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
The method of step S140, employing vacuum evaporation forms metal barrier 150 on described protective layer 140.
The material of metal barrier 150 is at least one in Ag, Al, Au, Cu, Ni and Mg.During vacuum evaporation, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100 ~ 200nm;
Step S150, adopt the method for first spin coating post-exposure on described metal barrier 150, to form organic barrier layer 160.
The method of first spin coating post-exposure is specially: under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cyclic aliphatic epoxy resin is spin-coated on described carbide lamella, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200 ~ 300s.
The method of step S160, employing evaporation forms insulating barrier 170 on described organic barrier layer 160.
The material of insulating barrier 170 is WO
3, V
2o
5, MoO
3and In
2o
3in at least one.During evaporation, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 50 ~ 100nm.
Preferably, metal barrier 150, organic barrier layer 160,170 3 layers of formation barrier layer of insulating barrier, repeating step S140, S150, S160 are at least three times successively, form multilayer barrier layer.
Step S170, on described insulating barrier 170, form outer protection layer 180.
The material of outer protective layer 180 is SiO.Adopt the method for vacuum evaporation to form outer protective layer 180, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100 ~ 150nm.
The preparation method of above-mentioned organic electroluminescence device, preparation technology is simple, easily preparation in enormous quantities; Adopt the method for evaporation to prepare protective layer 140, avoid negative electrode to be damaged; Adopt metal barrier 150, organic barrier layer 160 and insulating barrier 170 as barrier layer, block water, the erosion of oxygen isoreactivity material to organic electroluminescence device, the life-span of improving organic electroluminescence device.
Below in conjunction with embodiment, the invention will be further elaborated.
Embodiment 1
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/CuPc/ (Ag/ polytetrafluoroethylene/WO
3)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck CuPc, vacuum degree is 3 * 10
-5pa, evaporation rate is
thickness is 200nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.
The material of metal barrier is Ag.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is polytetrafluoroethylene, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier 180 is WO
3.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 80nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
Embodiment 2
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/NPB/ (Al/ methacrylic resin/V
2o
5)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck NPB, vacuum degree is 3 * 10
-5pa, evaporation rate is
thickness is 300nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.The material of metal barrier is Al.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 200nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is polytetrafluoroethylene, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier is V
2o
5.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 60nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 150nm.
Embodiment 3
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/Alq3/ (Au/ cyclic aliphatic epoxy resin/MoO
3)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck Alq3, vacuum degree is 3 * 10
-5pa, evaporation rate is
thickness is 250nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.
The material of metal barrier is Au.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 150nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is cyclic aliphatic epoxy resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.2 μ m, are then cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 230s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier is MoO
3.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 80nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 120nm.
Embodiment 4
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/SiO/ (Cu/ polytetrafluoroethylene/In
2o
3)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 200nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.
The material of metal barrier is Cu.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is polytetrafluoroethylene, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier is In
2o
3.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 70nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
Embodiment 5
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/MgF
2/ (Ni/ methacrylic resin/WO
3)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck MgF
2, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 300nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.
The material of metal barrier is Ni.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 200nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is methacrylic resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier is WO
3.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 50nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 150nm.
Embodiment 6
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/ZnS/ (Mg/ cyclic aliphatic epoxy resin/V
2o
5)
3the organic electroluminescence device of/SiO.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode substrate, form functional layer.
Anode substrate is glass electrically-conductive backing plate.Anode substrate 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 anode substrate surface in anode substrate surface before forming functional layer, and the oxygen content of carrying out surface active increase anode substrate surface is to improve the work function on anode substrate surface.Be specially, anode substrate is adopted to each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min successively, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises NPB and is entrained in the MoO in NPB
3.MoO
3quality percentage composition be 30%.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) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.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 10nm.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 30%.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 described function and luminescent layer, 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, on described negative electrode, form protective layer.
Adopt the method for vacuum evaporation on negative electrode, to prepare one deck ZnS, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 250nm.
4, adopt the method for vacuum evaporation to form metal barrier on described protective layer.
The material of metal barrier is Mg.During vacuum evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 150nm.
5, adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer.
The material on organic barrier layer is cyclic aliphatic epoxy resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.2 μ m, are then cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 230s.
6, adopt the method for evaporation to form insulating barrier on described organic barrier layer.
The material of insulating barrier is V
2o
5.During evaporation, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
7, twice of repeating step 4 ~ 6 again, form multilayer barrier layer.
8, on described insulating barrier, form outer protection layer.
Adopt the method for vacuum evaporation to form outer protective layer SiO, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 130nm.
Performance test
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
-32400), chroma-luminance meter (Konica Minolta, model: CS-100A), IEI point gum machine system, DYMAX photocuring system Pa), current-voltage tester (U.S. Keithly company, model:.
Organic electroluminescence device in above-described embodiment is carried out to performance test, test its water resistance (WVTR) and useful life, be to be 1000cd/m at original intensity useful life
2condition under test, its test result is as shown in table 1.
The performance test results of table 1 organic electroluminescence device
As seen from the above table, the water resistance of organic electroluminescence device reaches 10
-5g/m
2/ day, has improved waterproof oxygen performance, and meanwhile, reached more than 10000 hours the useful life of organic electroluminescence device, increased the useful life of organic electroluminescence device, is more conducive to the market application of organic electroluminescence device.
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, is characterized in that, comprises the anode substrate, luminescent layer, negative electrode, protective layer, metal barrier, organic barrier layer, insulating barrier and the outer protective layer that stack gradually; Wherein,
The material of described metal barrier is at least one in Ag, Al, Au, Cu, Ni and Mg;
The material on described organic barrier layer is at least one in polytetrafluoroethylene, methacrylic resin and cyclic aliphatic epoxy resin;
The material of described insulating barrier is WO
3, V
2o
5, MoO
3and In
2o
3in at least one.
2. organic electroluminescence device according to claim 1, is characterized in that, the material of described protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS.
3. organic electroluminescence device according to claim 1, it is characterized in that, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, the material of described metal level is at least one in aluminium, silver and gold, and the material of described dielectric layer is zinc sulphide or tin indium oxide.
4. organic electroluminescence device according to claim 1, is characterized in that, the material of described outer protective layer is SiO.
5. organic electroluminescence device according to claim 1, is characterized in that, described metal barrier, organic barrier layer, insulating barrier form barrier layer, and the number of plies on described barrier layer is three layers.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
On anode substrate, form luminescent layer;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer;
Adopt the method for vacuum evaporation to form metal barrier on described protective layer, wherein, the material of described metal barrier is at least one in Ag, Al, Au, Cu, Ni and Mg, and vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 200nm;
Adopt the method for first spin coating post-exposure on described metal barrier, to form organic barrier layer, under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cyclic aliphatic epoxy resin is spin-coated on described carbide lamella, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200s ~ 300s;
Adopt the method for vacuum evaporation to form insulating barrier on described organic barrier layer, the material of described insulating barrier is WO
3, V
2o
5, MoO
3and In
2o
3in at least one, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 50nm ~ 100nm; And
On described insulating barrier, form outer protection layer.
7. the preparation method of organic electroluminescence device according to claim 6, is characterized in that, adopts the method for vacuum evaporation to form described protective layer, and the material of wherein said protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
8. the preparation method of organic electroluminescence device according to claim 6, is characterized in that, adopts the method for vacuum evaporation to form described outer protective layer, and the material of described outer protective layer is SiO, and vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 150nm.
9. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that, adopt vapour deposition method to form described negative electrode, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, the material of described metal level is at least one in aluminium, silver and gold, and the material of described dielectric layer is zinc sulphide or tin indium oxide.
10. the preparation method of organic electroluminescence device according to claim 6, is characterized in that, described metal barrier, organic barrier layer, insulating barrier form barrier layer, and the number of plies on described barrier layer is three layers.
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