CN103427040B - Organic electroluminescence device and preparation method thereof - Google Patents
Organic electroluminescence device and preparation method thereof Download PDFInfo
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Abstract
A kind of organic electroluminescence device, including the conductive substrates with anode pattern stacked gradually, luminescent layer, negative electrode, intermediate layer, protecting film and cap, the material in intermediate layer is titanium cyanines copper, N, N ' two (1 naphthyl) N, N ' diphenyl 1, 1 ' biphenyl 44 ' diamidogen, 8 hydroxyquinoline aluminums, silicon oxide, Afluon (Asta) or zinc sulfide, protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer, the material of inorganic protective layer is silver, aluminum, barium, gold or calcium, the material of organic protection layer is fluorocarbon polymer, the chemical formula of fluorocarbon polymer is as follows:Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2；Luminescent layer, negative electrode, intermediate layer and protecting film are packaged in conductive substrates by cap, and the material of cap is the polyethylene terephthalate film of aluminum.Lasting a long time of above-mentioned organic electroluminescence device.The present invention also provides for the preparation method of a kind of organic electroluminescence 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 case
Structure is that the luminous organic material making one layer of tens nanometer thickness on ito glass makees luminescent layer, has one layer low above luminescent layer
The metal electrode of work function.When on electrode added with voltage, luminescent layer just produces light radiation.
After organic electroluminescence device is corroded by dampness and moisture, organic electroluminescence device inner member can be caused
Material occurs aging and then lost efficacy, thus the life-span of described organic electroluminescence device is shorter.
Summary of the invention
Based on this, it is necessary to provide a kind of organic electroluminescence device lasted a long time and preparation method thereof.
A kind of organic electroluminescence device, has the conductive substrates of anode pattern, luminescent layer, the moon including stack gradually
Pole, intermediate layer, protecting film and cap, the material in intermediate layer is titanium cyanines copper, N, N '-two (1-naphthyl)-N, N '-diphenyl-1,
1 '-biphenyl-4-4 '-diamidogen, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, protecting film includes inorganic protective layer and layer
The organic protection layer being laminated on inorganic protective layer, the material of inorganic protective layer is silver, aluminum, barium, gold or calcium, the material of organic protection layer
Material is fluorocarbon polymer, and the chemical formula of fluorocarbon polymer is as follows:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2；Luminescent layer, negative electrode, intermediate layer and protecting film are packaged in by cap
In conductive substrates, the material of cap is the polyethylene terephthalate film of aluminum.
Wherein in an embodiment, described cap is formed with host cavity, described luminescent layer, negative electrode, intermediate layer and guarantor
Cuticula is all contained in described host cavity.
Wherein in an embodiment, described conductive substrates is formed with host cavity, described luminescent layer, negative electrode, intermediate layer and
Protecting film is all contained in described host cavity.
Wherein in an embodiment, described inorganic protective layer and described organic protection layer are 3 layers～6 layers, described nothing
Machine protective layer replaces with described organic protection layer and superposes.
Wherein in an embodiment, the edge of described cap is tightly connected with described electrically-conductive backing plate by packaging plastic.
Wherein in an embodiment, described negative electrode includes two layer medium layer and is located at the gold between described two layer medium layer
Belonging to layer, the material of described dielectric layer is zinc sulfide, tin indium oxide or zinc oxide aluminum, and the material of described metal level is silver.
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
Step one, in conductive substrates formed luminescent layer；
Step 2, form negative electrode on the light-emitting layer；
Step 3, forming intermediate layer on the cathode, the material in described intermediate layer is titanium cyanines copper, N, N '-two (1-naphthalene
Base)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide；
Step 4, forming protecting film on described intermediate layer, described protecting film includes inorganic protective layer and is laminated in described
Organic protection layer on inorganic protective layer, the material of described inorganic protective layer is silver, aluminum, barium, gold or calcium, described organic protection layer
Material be fluorocarbon polymer, the chemical formula of described fluorocarbon polymer is as follows:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2；And
Step 5, the use the most described luminescent layer of cap, negative electrode, intermediate layer and protecting film are packaged in described conductive substrates
On, the material of described cap is the polyethylene terephthalate film of aluminum.
Wherein in an embodiment, in step 5, make described cap and described conductive substrates by coating packaging plastic
It is tightly connected.
Wherein in an embodiment, described cap is formed with host cavity, described luminescent layer, negative electrode, intermediate layer and guarantor
Cuticula is contained in described host cavity.
Wherein in an embodiment, described inorganic protective layer and described organic protection layer are 3 layers～6 layers, described nothing
Machine protective layer replaces with described organic protection layer and superposes.
Above-mentioned organic electroluminescence device and preparation method thereof, intermediate layer and protecting film can effectively reduce external water,
Oxygen isoreactivity material is to luminescent layer and the erosion of negative electrode；Use fluorocarbon polymer as organic protection layer, inorganic guarantor can be alleviated
The stress of sheath, increases the corrosion resistance of protecting film simultaneously；Cap uses the polyethylene terephthalate film of aluminum to have
The raising water oxygen resistant ability of effect, thus the lasting a long time of organic electroluminescence device.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of an embodiment；
Fig. 2 is the flow chart of the preparation method of the organic electroluminescent of an embodiment；
Fig. 3 is the life curve figure that embodiment 1～embodiment 10 prepare organic electroluminescence device.
Detailed description of the invention
With specific embodiment, organic electroluminescence device and preparation method thereof is further elucidated with below in conjunction with the accompanying drawings.
Referring to Fig. 1, what the organic electroluminescence device 100 of an embodiment included stacking gradually has anode pattern
Conductive substrates 10, functional layer 20, negative electrode 30, intermediate layer 40, protecting film 50 and cap 70.
Conductive substrates 10 is glass conductive substrates or organic polyethylene terephthalate (PET) film substrate that conducts electricity.
There is in conductive substrates 10 preparation and have the ITO layer of anode pattern.The thickness of ITO layer is 100nm～150nm.
Functional layer 20 is formed at substrate 10 surface.Hole injection layer that functional layer 20 includes stacking gradually, hole transmission layer,
Luminescent layer, electron transfer layer, electron injecting layer.It is appreciated that hole injection layer, hole transmission layer, electron transfer layer, electronics are noted
Entering layer can omit, now functional layer 20 only includes luminescent layer.
In present embodiment, the material of hole injection layer is molybdenum oxide (MoO3).The thickness of hole injection layer is 10nm.
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material 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 is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.
It should be noted that hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer can also
Use other materials as required.
Negative electrode 30 is formed at functional layer 20 surface.The thickness of negative electrode is 100nm.Negative electrode 30 can be single layer structure or multilamellar
Structure.When negative electrode 30 is single layer structure, the material of negative electrode 30 is aluminum (Al), silver (Ag) or gold (Au)；When negative electrode 30 is multilamellar
During structure, negative electrode 30 includes two layer medium layer and is located at the metal level between two layer medium layer, and the material of dielectric layer is zinc sulfide
(ZnS), tin indium oxide (ITO) or zinc oxide aluminum (AZO), the material of metal level is silver (Ag).
Intermediate layer 40 is formed at negative electrode 30 surface.The material in intermediate layer 40 is titanium cyanines copper (CuPc), N, N '-two (1-naphthalene
Base)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen (NPB), 8-hydroxyquinoline aluminum (Alq3), silicon oxide (SiO), fluorination
Magnesium (MgF2) or zinc sulfide (ZnS).The thickness in intermediate layer 40 is 100nm～150nm.
Protecting film 50 is formed at surface, intermediate layer 40.Protecting film 50 includes inorganic protective layer and is laminated on inorganic protective layer
Organic protection layer.
The material of inorganic protective layer is silver (Ag), aluminum (Al), barium (Ba), gold (Au) or calcium (Ca).The thickness of inorganic protective layer
Degree is 100nm～150nm.
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1 μm～1.5 μm.Organic protection
The material of layer is the fluorocarbon polymer that structural formula is following:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2.
Fluorocarbon polymer is from Bellex International Corporation (agency of China: Mei Bang world trade
Easily (Shanghai) Co., Ltd.) company's purchase.
In present embodiment, inorganic protective layer and organic protection layer are 3 layers～6 layers, inorganic protective layer and organic protection
Layer alternately superposition.
Cap 70 is covered on protective layer 50.The material of cap 70 is the polyethylene terephthalate film of aluminum.Envelope
Capping 70 is formed with host cavity.Host cavity is the groove of the surface indentation from cap 70.Cap 70 is covered on protecting film 50
Surface and functional layer 20, negative electrode 30, intermediate layer 40 and protecting film 50 are contained in host cavity, the edge of cap 70 is by encapsulation
Glue (not shown) is tightly connected with conductive substrates 10, thus cap 70 is by functional layer 20, negative electrode 30, intermediate layer 40 and protecting film
50 are encapsulated in conductive substrates 10.
The intermediate layer 40 of above-mentioned organic electroluminescence device 100 and protecting film 50 can effectively reduce external water, oxygen etc.
Active substance is to functional layer 20, the erosion of negative electrode 30；Use fluorocarbon polymer as organic protection layer 52, inorganic guarantor can be alleviated
The stress of sheath, increases the corrosion resistance of protecting film 50 simultaneously；Cap 70 uses the polyethylene terephthalate film of aluminum
Can effectively improve water oxygen resistant ability, thus the lasting a long time of organic electroluminescence device 100.
It is appreciated that the host cavity of cap 70 can omit, the most directly makes cap 70 be coated with functional layer 20, negative electrode
30, intermediate layer 40 and protecting film 50 or host cavity is set in conductive substrates 10.
Please refer to Fig. 2, the preparation method of the organic electroluminescence device 100 of an embodiment, it includes following step
Rapid:
Step S110, in conductive substrates 10 formed functional layer 20.
Functional layer 20 includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics are noted
Enter layer.
Conductive substrates 10 can be glass conductive substrates or organic polyethylene terephthalate (PET) the thin film base that conducts electricity
Plate.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.The thickness of ITO layer is 100nm～150nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
In present embodiment, the material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole is injected
Layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum 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 can also
Use other materials as required.Hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, now
Functional layer 20 only includes luminescent layer.
Step S120, functional layer 20 surface formed negative electrode 30.
Negative electrode 30 can be single layer structure or multiple structure.
When negative electrode 30 is single layer structure, the thickness of negative electrode 30 is 100nm, and the material of negative electrode 30 is aluminum (Al), silver (Ag)
Or gold (Au), negative electrode 30 is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate is
When negative electrode 30 is multiple structure, negative electrode 30 includes two layer medium layer and is located at the metal between two layer medium layer
Layer.The thickness of dielectric layer is 30nm, and the thickness of metal level is 10nm.The material of dielectric layer is zinc sulfide (ZnS), tin indium oxide
(ITO) or zinc oxide aluminum (AZO), the material of metal level is silver (Ag).Wherein, tin indium oxide (ITO) or zinc oxide aluminum (AZO) by
Vacuum sputtering makes, background vacuum 2 × 10-4Pa；ZnS or Ag is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation
Speed is
Step S130, in formation intermediate layer, negative electrode 30 surface 40.
The material in intermediate layer 40 is titanium cyanines copper (CuPc), N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-
4 '-diamidogen (NPB), 8-hydroxyquinoline aluminum (Alq3), silicon oxide (SiO), Afluon (Asta) (MgF2) or zinc sulfide (ZnS).Intermediate layer
The thickness of 40 is 100nm～150nm.Intermediate layer 40 is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa～3 × 10-4Pa, steams
Sending out speed is
Step S140, surface, intermediate layer 40 formed protecting film 50.
Protecting film 50 includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is silver (Ag), aluminum (Al), barium (Ba), gold (Au) or calcium (Ca).The thickness of inorganic protective layer
Degree is 100nm～150nm.Inorganic protective layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa～3 × 10-4Pa, evaporation speed
Degree is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1 μm～1.5 μm.Organic protection
The material of layer is the fluorocarbon polymer that structural formula is following:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2.
Organic protection layer is prepared by spin coating, and rotating speed is 500rpm～1500rpm, and spin coating post-exposure solidifies.
In present embodiment, inorganic protective layer and organic protection layer are 3 layers～6 layers, inorganic protective layer and organic protection
Layer alternately superposition.
Functional layer 20, negative electrode 30, intermediate layer 40 and protecting film 50 are packaged in conductive substrates by step S150, use cap
On 10.
The material of cap 70 is the polyethylene terephthalate film of aluminum.Cap 70 is formed with host cavity.House
Chamber is the groove of the surface indentation from cap 70.Cap 70 be covered on protecting film 50 surface and by functional layer 20, negative electrode 30,
Intermediate layer 40 and protecting film 50 are contained in host cavity.
The edge of cap 70 supports conductive substrates 10, and the edge-coating packaging plastic at cap 70 is cap 70 and lead
Electricity substrate 10 is tightly connected, thus functional layer 20, negative electrode 30, intermediate layer 40 and protecting film 50 are encapsulated in conductive base by cap 70
At at the end 10.In present embodiment, packaging plastic is epoxy encapsulation glue, and the thickness of packaging plastic is 15 μm～20 μm, with UV light (λ
=365nm) solidify, light intensity is 10～15mW/cm2, time of exposure is 300～400s.
The preparation method of above-mentioned organic electroluminescence device, preparation technology is simple, is easily prepared on a large scale；Intermediate layer 40 and
Protecting film 50 can effectively reduce external water, oxygen isoreactivity material to functional layer 20, the erosion of negative electrode 30；Use the polymerization of carbon fluorine
Thing, as organic protection layer 52, can be alleviated the stress of inorganic protective layer, increase the corrosion resistance of protecting film 50 simultaneously；Cap
70 use the polyethylene terephthalate film of aluminum can effectively improve water oxygen resistant ability, thus organic electroluminescence device
100 last a long time.
The organic electroluminescence device preparation method provided the present invention below in conjunction with specific embodiment is described in detail.
Embodiment 1
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/Al/CuPc/Al/
The organic electroluminescence device of fluorocarbon polymer/Al/ fluorocarbon polymer/Al/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is titanium cyanines copper (CuPc).Intermediate layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation
Speed isThe thickness in intermediate layer is 100nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is silver (Ag).The thickness of inorganic protective layer is 100nm.Inorganic protective layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1 μm.The material of organic protection layer
For the fluorocarbon polymer that structural formula is following:
Wherein, x=1, y=1, z=1.
Organic protection layer is prepared by spin coating, and rotating speed is 500rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 6 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 15 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 10mW/cm2, time of exposure 400s.
Embodiment 2
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/ Al/NPB/Ag/ carbon
The organic electroluminescence device of fluoropolymer/Ag/ fluorocarbon polymer/Ag/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is NPB.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 150nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Al.The thickness of inorganic protective layer is 150nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.5 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=2, y=2, z=2.
Organic protection layer is prepared by spin coating, and rotating speed is 1500rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 5 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 20 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 15mW/cm2, time of exposure 300s.
Embodiment 3
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/Al/Alq3/Ba/
The organic electroluminescence device of fluorocarbon polymer/Ba/ fluorocarbon polymer/Ba/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is Alq3.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Ba.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.5 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=1, y=2, z=1.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 3 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 350s.
Embodiment 4
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/ Al/SiO/Mg/ carbon
The organic electroluminescence device of fluoropolymer/Mg/ fluorocarbon polymer/Mg/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is SiO.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Mg.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.2 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=2, y=1, z=2.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 3 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 17 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 330s.
Embodiment 5
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/Al/MgF2/Au/
The organic electroluminescence device of fluorocarbon polymer/Au/ fluorocarbon polymer/Au/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is MgF2.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Au.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.2 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=1, y=1, z=2.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 3 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 350s.
Embodiment 6
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/ Al/ZnS/Ca/ carbon
The organic electroluminescence device of fluoropolymer/Ca/ fluorocarbon polymer/Ca/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is ZnS.Intermediate layer is formed by vacuum evaporation, and vacuum is 3 × 10-4Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Ca.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 3 × 10-4Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.2 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=2, y=2, z=1.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 3 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 18mW/cm2, time of exposure 350s.
Embodiment 7
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/ZnS:Ag:ZnS/
The organic electroluminescence device of Alq3/Ba/ fluorocarbon polymer/Ba/ fluorocarbon polymer/Ba/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is ZnS (30nm)/Ag (10nm)/ZnS (30nm).Negative electrode is formed by vacuum evaporation, and vacuum is 5
×10-5Pa, evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is Alq3.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Ba.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.5 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=1, y=2, z=1.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 3 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 350s.
Embodiment 8
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/ITO:Ag:ITO/
The organic electroluminescence device of SiO/Mg/ fluorocarbon polymer/Mg/ fluorocarbon polymer/Mg/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 120nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is ITO (30nm)/Ag (10nm)/ITO (30nm).AZO by sputtering making, background vacuum 2 ×
10-4Pa；Ag is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is SiO.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Mg.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.2 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=2, y=1, z=2.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 5 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 17 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 330s.
Embodiment 9
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/AZO:Ag:AZO/
MgF2The organic electroluminescence device of/Au/ fluorocarbon polymer/Au/ fluorocarbon polymer/Au/ fluorocarbon polymer/cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 150nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is AZO (30nm)/Ag (10nm)/AZO (30nm).AZO by sputtering making, background vacuum 2 ×
10-4Pa；Ag is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is MgF2.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film includes inorganic protective layer and the organic protection layer being laminated on inorganic protective layer.
The material of inorganic protective layer is Au.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Organic protection layer is formed at inorganic protective layer surface.The thickness of organic protection layer is 1.2 μm.The material of organic protection layer
Material is the fluorocarbon polymer that structural formula is following:
Wherein, x=1, y=1, z=2.
Organic protection layer is prepared by spin coating, and rotating speed is 1000rpm, and spin coating post-exposure solidifies.
Inorganic protective layer and organic protection layer are 4 layers, and inorganic protective layer replaces with organic protection layer and superposes.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 350s.
Embodiment 10
The present embodiment prepares structure: ITO/MoO3/TCTA/TPBI:Ir(ppy)3/Bphen/CsN3/Al/MgF2/Ca/
The organic electroluminescence device of Ca/Ca/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, functional layer is formed.
Conductive substrates 10 is glass conductive substrates.Conductive substrates 10 has preparation and has the ITO layer of anode pattern.ITO layer
Thickness is 100nm.
Conductive substrates 10 surface first carried out the pretreatment pollutant with removal substrate 10 surface before forming functional layer 20,
And carry out the oxygen content on surface active increase conductive substrates 10 surface to improve the work function on conductive substrates 10 surface.Specifically,
Conductive substrates 10 is used successively and goes each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up with nitrogen afterwards,
Baking box is dried.
Functional layer includes that the hole injection layer stacked gradually, hole transmission layer, luminescent layer, electron transfer layer, electronics inject
Layer.
The material of hole injection layer is (MoO3).The thickness of hole injection layer is 10nm.Hole injection layer is by vacuum evaporation
Being formed, vacuum is 3 × 10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is 1,3,5-
Three (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes iridium (Ir (ppy)3).Visitor
The weight/mass percentage composition of body material is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum 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 is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer is nitrine caesium (CsN3).The thickness of electron injecting layer is 5nm.Electron injecting layer is by vacuum
Evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminum.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa,
Evaporation rate is
3, it is deposited with intermediate layer at cathode surface.
The material in intermediate layer is MgF2.Intermediate layer is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isThe thickness in intermediate layer is 120nm.
4, protecting film is formed in interlayer surfaces.
Protecting film is inorganic protective layer.
The material of inorganic protective layer is Ca.The thickness of inorganic protective layer is 120nm.Inorganic protective layer is by vacuum evaporation shape
Becoming, vacuum is 5 × 10-5Pa, evaporation rate is
Inorganic protective layer is 3 layers.
5, cap is used functional layer, negative electrode, intermediate layer and protecting film to be packaged in conductive substrates.
PET film edge-coating epoxy encapsulation glue (thickness 18 μm) containing Al, enters with UV light (λ=365nm) overleaf
Row solidification, light intensity 11mW/cm2, time of exposure 350s.
Preparation used in the embodiment of the present invention and comparative example with test instrunment is: high vacuum coating equipment (Shenyang science
Instrument development centered finite company, pressure < 1 × 10-3Pa), current-voltage tester (Keithly company of the U.S., model:
2400), color luminance meter (Konica Minolta, model: CS-100A), IEI point gum machine system, DYMAX photocuring system.
Referring to table 1, the aqueous vapor of the organic electroluminescence device that table 1 show embodiment 1～embodiment 10 preparation penetrates
The test result of rate (Water Vapor Transmission Rate).Embodiment 1～embodiment 9 are made as can be seen from Table 1
The aqueous vapor penetrance of standby organic electroluminescence device is respectively less than 8.1 × 10-4g/m2/ day, much smaller than having of embodiment 10 preparation
The aqueous vapor penetrance (6.1 × 10 of organic electroluminescence devices-3g/m2/ day) waterproof effect is preferable, can effectively reduce outside aqueous vapor
Erosion to organic electroluminescence device, thus improve the life-span of organic electroluminescence device.
Table 1
| WVTR(g/m2/day) | |
| Embodiment 1 | 1.7×10-4 |
| Embodiment 2 | 2.6×10-4 |
| Embodiment 3 | 3.2×10-4 |
| Embodiment 4 | 4.3×10-4 |
| Embodiment 5 | 4.8×10-4 |
| Embodiment 6 | 5.5×10-4 |
| Embodiment 7 | 7.2×10-4 |
| Embodiment 8 | 7.7×10-4 |
| Embodiment 9 | 8.1×10-4 |
| Embodiment 10 | 6.1×10-3 |
Please refer to Fig. 3 and table 2, Fig. 3 show the organic electroluminescence device of embodiment 1～embodiment 10 preparation
Life curve, table 2 show the use time of the organic electroluminescence device of embodiment 1～embodiment 10 preparation and the survey of brightness
Test result.
Table 2
From Fig. 3 and table 2 it can be seen that the starting brightness of the organic electroluminescence device of embodiment 1～embodiment 9 preparation is
1000cd/m2Time, the life-span reaches more than 7000 hours, lasts a long time；Embodiment 1～the organic electroluminescent of embodiment 9 preparation
After device uses 7620h, the organic electroluminescence device of brightness ratio embodiment 10 preparation is much higher.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an organic electroluminescence device, has the conductive substrates of anode pattern, luminescent layer and negative electrode including stack gradually,
It is characterized in that: described organic electroluminescence device also includes stacking gradually the intermediate layer on described negative electrode and protecting film, institute
The material stating intermediate layer is titanium cyanines copper, N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen, 8-hydroxyl
Quinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, described protecting film includes inorganic protective layer and is laminated on described inorganic protective layer
Organic protection layer, the material of described inorganic protective layer is silver, aluminum, barium, gold or calcium, and the material of described organic protection layer is carbon fluorine
Polymer, the chemical formula of described fluorocarbon polymer is as follows:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2；
Described organic electroluminescence device also includes cap, and described cap is by described luminescent layer, negative electrode, intermediate layer and protection
Film is packaged in described conductive substrates, and the material of described cap is the polyethylene terephthalate film of aluminum.
Organic electroluminescence device the most according to claim 1, it is characterised in that: described cap is formed with host cavity,
Described luminescent layer, negative electrode, intermediate layer and protecting film are all contained in described host cavity.
Organic electroluminescence device the most according to claim 1, it is characterised in that: described conductive substrates is formed with collecting
Chamber, described luminescent layer, negative electrode, intermediate layer and protecting film are all contained in described host cavity.
Organic electroluminescence device the most according to claim 1, it is characterised in that: described inorganic protective layer and described organic
Protective layer is 3 layers ~ 6 layers, and described inorganic protective layer replaces with described organic protection layer and superposes.
Organic electroluminescence device the most according to claim 1, it is characterised in that: the edge of described cap is by encapsulation
Glue is tightly connected with described electrically-conductive backing plate.
Organic electroluminescence device the most according to claim 1, it is characterised in that: described negative electrode include two layer medium layer and
Being located at the metal level between described two layer medium layer, the material of described dielectric layer is zinc sulfide, tin indium oxide or zinc oxide aluminum, institute
The material stating metal level is silver.
7. the preparation method of an organic electroluminescence device, it is characterised in that comprise the following steps:
Step one, in conductive substrates formed luminescent layer；
Step 2, form negative electrode on the light-emitting layer；
Step 3, forming intermediate layer on the cathode, the material in described intermediate layer is titanium cyanines copper, N, N '-two (1-naphthyl)-N,
N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide；
Step 4, on described intermediate layer formed protecting film, described protecting film includes inorganic protective layer and is laminated in described inorganic
Organic protection layer on protective layer, the material of described inorganic protective layer is silver, aluminum, barium, gold or calcium, the material of described organic protection layer
Material is fluorocarbon polymer, and the chemical formula of described fluorocarbon polymer is as follows:
Wherein, x is 1 or 2, and y is 1 or 2, and z is 1 or 2；And
Step 5, the use the most described luminescent layer of cap, negative electrode, intermediate layer and protecting film are packaged in described conductive substrates,
The material of described cap is the polyethylene terephthalate film of aluminum.
The preparation method of organic electroluminescence device the most according to claim 7, it is characterised in that: in step 5, pass through
Coating packaging plastic makes described cap be tightly connected with described conductive substrates.
The preparation method of organic electroluminescence device the most according to claim 7, it is characterised in that: described cap is formed
Host cavity, described luminescent layer, negative electrode, intermediate layer and protecting film is had to be contained in described host cavity.
The preparation method of organic electroluminescence device the most according to claim 7, it is characterised in that: described inorganic protection
Layer and described organic protection layer are 3 layers ~ 6 layers, and described inorganic protective layer replaces with described organic protection layer and superposes.
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| CN101359722A (en) * | 2008-09-23 | 2009-02-04 | 吉林大学 | Encapsulation method for top radiation organic EL part |
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