CN103367647A - Organic electroluminescent device and preparation method thereof - Google Patents
Organic electroluminescent device and preparation method thereof Download PDFInfo
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- CN103367647A CN103367647A CN2012100876740A CN201210087674A CN103367647A CN 103367647 A CN103367647 A CN 103367647A CN 2012100876740 A CN2012100876740 A CN 2012100876740A CN 201210087674 A CN201210087674 A CN 201210087674A CN 103367647 A CN103367647 A CN 103367647A
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- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The invention provides an organic electroluminescent device comprising a transparent anode substrate, a function layer, a luminescent layer, a transparent cathode and an encapsulation layer. A closed space is formed by the transparent anode substrate and the encapsulation layer. The function layer, the luminescent layer and the transparent cathode are accommodated in the closed space. The encapsulation layer comprises an undoped film layer, a doped film layer and a polyethylene terephthalate film layer in order. The undoped film layer is a MgF2, phenyl morpholine, 8-Hydroxyquinoline aluminum, ZnS or ZnSe film, and the doped layer is a film formed by doping MgF2, ZnS or ZnSe film with the metal elements, wherein the metal elements comprise Ca, Ba, Sr or Mg. The invention also provides the preparation method of the organic electroluminescent device, the erosion on the organic electroluminescent device by vapor can be effectively reduced, the service life of the organic electroluminescent device is prolonged significantly, and the light transmission rate is higher than 80%. The method is especially suitable for the packaging of a flexible organic electroluminescent device.
Description
Technical field
The invention belongs to organic electroluminescence device, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is based on a kind of current mode light emitting semiconductor device of organic material.Its typical structure is to accompany multilayer organic material film (hole injection layer, hole transmission layer, luminescent layer, electron supplying layer and electron injecting layer) between transparent anode and metallic cathode, and after applying certain voltage between electrode, luminescent layer will be luminous.In recent years, organic electroluminescence device has been because the characteristics such as cost of manufacture own is low, the response time is short, luminosity is high, wide visual angle, low driving voltage and energy-conserving and environment-protective have been subject to extensive concern in fields such as panchromatic demonstration, backlight and illuminations, and is considered to be most likely at the device of new generation that occupies the dominance on following illumination and the display device market.
At present, the problem that the organic electroluminescence device average life is short, this mainly is because organic material film is very loose, occurs rapidly aging after easily being infiltrated by compositions such as airborne steam and oxygen.Therefore, organic electroluminescence device must encapsulate before entering actual use, and the quality of encapsulation is directly connected to the life-span of organic electroluminescence device.
Adopt glass cover or crown cap to encapsulate in the conventional art, its edge is resin-sealed with ultraviolet polymerization, but the glass cover that uses in this method or crown cap volume are often larger, have increased the weight of device, and the method can not be applied to the give out light encapsulation of device of flexible organic electroluminescence.And existing organic electroluminescence device can not provide good light transmittance usually.
Summary of the invention
For overcoming the defective of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and preparation method thereof.This preparation method can reduce steam effectively to the erosion of organic electroluminescence device, improves significantly the life-span of organic electroluminescence device; Light transmittance reaches more than 80%, can be used for transparent organic light emission product; Be particularly useful for encapsulating flexible organic electroluminescent device.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise transparent anode substrate, functional layer, luminescent layer, transparent cathode and encapsulated layer, transparent anode substrate and encapsulated layer form enclosure space, described functional layer, luminescent layer and transparent cathode are contained in the described enclosure space, encapsulated layer comprises non-doping rete, doping rete and PETG rete successively, and non-doping rete is MgF
2, phenyl beautiful jade, oxine aluminium, ZnS or ZnSe film, the doping rete is MgF
2, ZnS or ZnSe film and the metallic element film that mixes mutually and form, wherein, metallic element comprises Ca, Ba, Sr or Mg.
Preferably, the transparent anode substrate is conducting glass substrate or conduction PETG film substrate.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and the electron transfer layer.Preferably, functional layer and luminescent layer are by the method for vacuum evaporation or the method setting of solution coating.
Transparent cathode is dielectric layer/metal level of forming of dielectric layer tramp metal layer/dielectric layer structure.
Encapsulated layer comprises non-doping rete, doping rete and PETG rete successively.
Non-doping rete is MgF
2, phenyl beautiful jade (NPB), oxine aluminium (Alq
3), ZnS or ZnSe film, play the effect of the organic and cathode layer of protection, the water of prolongation oxygen permeation pathway is also arranged.
The doping rete is MgF
2, ZnS or ZnSe film and the metallic element film that mixes mutually and form, wherein, metallic element comprises Ca, Ba, Sr or Mg.Ca, Ba, Sr and Mg are the high-hydroscopicity material, can effectively reduce steam to the erosion of organic electroluminescence device, improve significantly the life-span of organic electroluminescence device.One or more of mixing in the doping rete among Ca, Ba, Sr and the Mg can strengthen water and oxygen barrier property.Preferably, the mass percent that metallic element accounts for the doping rete in the doping rete is 5%～15%.
Preferably, the thickness of non-doping rete is 30nm～50nm, and the thickness of doping rete is 30nm～50nm.
The number of plies of non-doping rete is not limit, and can be individual layer, can be two-layer or multilayer yet.The number of plies of doping rete is not limit, and can be individual layer, can be two-layer or multilayer yet.Preferably, non-doping rete and described doping rete alternative stacked arrange.At this moment, non-doping rete is multilayer with the doping rete and the number of plies is identical.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, may further comprise the steps:
Prepare functional layer, luminescent layer and transparent cathode at the transparent anode substrate;
Mode by vacuum evaporation is non-doping rete and doping rete on transparent cathode surface successively evaporation, last vacuum evaporation PETG rete forms encapsulated layer, at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, are formed with organic electroluminescence devices;
Vacuum degree in the vacuum evaporation process is 7 * 10
-5～3 * 10
-5Pa, evaporation rate is
Non-doping rete is MgF
2, phenyl beautiful jade, oxine aluminium, ZnS or ZnSe;
The doping rete is MgF
2, ZnS or ZnSe film and the metallic element film that mixes mutually and form, wherein, metallic element comprises Ca, Ba, Sr or Mg.
Preferably, the transparent anode substrate is conducting glass substrate or conduction PETG film substrate.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and the electron transfer layer.Preferably, functional layer and luminescent layer are by the method for vacuum evaporation or the method setting of solution coating.
Transparent cathode is dielectric layer/metal level of forming of dielectric layer tramp metal layer/dielectric layer structure.
Preferably, the mass percent that metallic element accounts for the doping rete in the doping rete is 5%～15%.
Preferably, the thickness of non-doping rete is 30nm～50nm, and the thickness of doping rete is 30nm～50nm.
Preferably, the step of the non-doping rete of evaporation and doping rete is two-layer or two-layer above non-doping rete and doping rete of evaporation successively, wherein, and non-doping rete and the setting of doping rete alternative stacked.At this moment, non-doping rete is multilayer with the doping rete and the number of plies is identical.The packaging effect of multi-layer doping rete and doping rete is more good.
Preferably, UV glue is epoxy resin, and thickness is 20～40 μ m, time for exposure 300～400s.
A kind of organic electroluminescence device provided by the invention and preparation method thereof has following beneficial effect:
(1) preparation method of organic electroluminescence device of the present invention can reduce steam effectively to the erosion of organic electroluminescence device, improves significantly the life-span of organic electroluminescence device;
(2) organic electroluminescence device light transmittance of the present invention reaches more than 80%, can be used for transparent organic light emission product;
(3) the inventive method is applicable to encapsulate take electro-conductive glass as the transparent anode substrate organic electroluminescence device of preparation, also is applicable to the flexible organic electroluminescent device of encapsulation take plastics (for example phthalic acid glycol ester film) or metal as the anode substrate preparation.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device;
(4) organic electroluminescence device material of the present invention is cheap, and preparation method's technique is simple, and easily large tracts of land preparation is suitable for large-scale industrialization and uses.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention 1 organic electroluminescence device;
Fig. 2 is the life curve figure of the embodiment of the invention 1～6 organic electroluminescence device.
Embodiment
The following stated is preferred implementation of the present invention.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvement and adjustment, these improvement and adjustment also are considered as in protection scope of the present invention.
Embodiment 1:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, the ito glass substrate after cleaning is carried out surface activation process, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on ito glass substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is MgF
2: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 50nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is for being doped with the MgF of Ca
2Film is about to Ca and MgF
2A skim is made in common evaporation, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Ca accounts for 15% of doping rete gross mass, and the doping layer thickness is 40nm;
According to above-mentioned preparation method, the more successively two-layer non-doping rete of evaporation and two-layer doping rete, wherein, non-doping rete and doping rete alternative stacked arrange.
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 3.4E
-3
Fig. 1 is the structural representation of the transparent organic electroluminescence device of present embodiment.As shown in Figure 1, transparent organic electroluminescence device comprises transparent anode substrate 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, transparent cathode 7 and encapsulated layer 8 successively.Transparent anode substrate 1 and encapsulated layer 8 form an enclosure space by epoxy sealing, and hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6 and transparent cathode 7 are contained in this enclosure space.Encapsulated layer 8 comprises that successively non-doping rete 811, doping rete 821, non-doping rete 812, doping rete 822, non-doping rete 813, doping rete 823 and load have the phthalic acid glycol ester film 83 of metallic aluminium.
The material of transparent anode substrate 1 is ito glass substrate; The material of hole injection layer 2 is phenyl beautiful jade doping MoO
3The composite material that forms; The material of hole transmission layer 3 is 4,4 ', 4 " three (carbazole-9-yl) triphenylamines; The material of luminescent layer 4 is that (1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene doping three (2-phenylpyridines) close the composite material that iridium forms to 1,3,5-three; The material of electron transfer layer 5 is 4,7-diphenyl-1, the 10-phenanthroline; The material of electron injecting layer 6 is phenyl beautiful jade doping CsN
3The composite material that forms; Transparent cathode 7 is dielectric layer/metal level of forming of dielectric layer tramp metal layer/dielectric layer structure, dielectric layer in this structure is the thick ZnS of 30nm, metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm); The material of non-doping rete 811, non-doping rete 812 and non-doping rete 813 is MgF
2, the material of doping rete 821, doping rete 822 and doping rete 823 is the MgF that is doped with Ca
2Film.
Embodiment 2:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, the ito glass substrate after cleaning is carried out surface activation process, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on ito glass substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is the phenyl beautiful jade: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 30nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is about to Ba and ZnS and jointly evaporates a making skim for being doped with the ZnS film of Ba, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Ba accounts for 10% of doping rete gross mass, and the doping layer thickness is 50nm;
According to above-mentioned preparation method, the more successively two-layer non-doping rete of evaporation and two-layer doping rete, wherein, non-doping rete and doping rete alternative stacked arrange.
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 4.5E
-3
Embodiment 3:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, the ito glass substrate after cleaning is carried out surface activation process, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on ito glass substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is Alq
3: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 30nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is about to Sr and ZnSe and jointly evaporates a making skim for being doped with the ZnSe film of Sr, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Sr accounts for 5% of doping rete gross mass, and the doping layer thickness is 30nm;
According to above-mentioned preparation method, the more successively two-layer non-doping rete of evaporation and two-layer doping rete, wherein, non-doping rete and doping rete alternative stacked arrange.
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 5.1E
-3
Embodiment 4:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, the ito glass substrate after cleaning is carried out surface activation process, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on ito glass substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is ZnS: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 40nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is about to Sr and ZnSe and jointly evaporates a making skim for being doped with the ZnSe film of Sr, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Sr accounts for 15% of doping rete gross mass, and the doping layer thickness is 40nm;
According to above-mentioned preparation method, the more successively two-layer non-doping rete of evaporation and two-layer doping rete, wherein, non-doping rete and doping rete alternative stacked arrange.
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 5.8E
-3
Embodiment 5:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. conduct electricity the pre-treatment of PETG film substrate
Get conduction PETG film substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, conduction PETG film substrate after cleaning is carried out surface activation process, to increase the oxygen content of conduction PETG film substrate surface layer, improve the work function of conduction PETG film substrate surface; Conduction PETG film substrate thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on conduction PETG film substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is ZnS: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 30nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is about to Ba and ZnS and jointly evaporates a making skim for being doped with the ZnS film of Ba, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Ba accounts for 5% of doping rete gross mass, and the doping layer thickness is 30nm;
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 6.7E
-3
Embodiment 6:
The preparation method of organic electroluminescence device may further comprise the steps:
(1) prepares functional layer, luminescent layer and negative electrode at the transparent anode substrate
A. the pre-treatment of conducting glass substrate
Get ito glass substrate, carrying out liquid detergent cleaning, ethanol cleaning, pure water cleaning and acetone with supersonic wave cleaning machine successively cleans, each washing is adopted and was cleaned 5 minutes, stop 5 minutes, repeat respectively 3 times, and then stand-by with oven for drying, the ito glass substrate after cleaning is carried out surface activation process, to increase the oxygen content of ito glass substrate superficial layer, improve the work function on ito glass substrate surface; ITO thickness 100nm;
B. the preparation of functional layer, luminescent layer and negative electrode
Adopt the method for the method of vacuum evaporation on ito glass substrate, to form successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Adopt evaporation to make transparent cathode;
Hole injection layer: with MoO
3Be doped in the phenyl beautiful jade doping content 25wt%, thickness 10nm, vacuum degree 3 * 10
-5Pa, evaporation rate
Hole transmission layer: adopt 4,4 ', 4 " three (carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 40nm;
Luminescent layer: material of main part adopts 1,3,5-three, and (benzene (TPBI) of 1-phenyl-1H-benzimidazolyl-2 radicals-yl), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) be as electron transport material, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 30nm;
The preparation of electron injecting layer: with CsN
3Mix in the phenyl beautiful jade doping content 25wt%, vacuum degree 3 * 10
-5Pa, evaporation rate
Evaporation thickness 20nm;
The preparation of transparent cathode: adopt evaporation to make transparent cathode layer, vacuum degree 3 * 10
-5Pa, evaporation rate
Make dielectric layer/metal level that dielectric layer tramp metal layer forms/dielectric layer structure, the dielectric layer in this structure is the thick ZnS of 30nm, and metal level is the thick Ag of 10nm, and concrete structure is ZnS (30nm)+Ag (10nm)+ZnS (30nm).
(2) prepare encapsulated layer at negative electrode
Mode by vacuum evaporation is at the non-doping rete of transparent cathode surface evaporation, and this layer material is ZnSe: the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, evaporation rate is
Non-doping layer thickness is 50nm;
Mode by vacuum evaporation is at non-doping film surface evaporation doping rete, and this layer is about to Mg and ZnSe and jointly evaporates a making skim for being doped with the ZnSe film of Mg, and the vacuum degree in the vacuum evaporation process is 5 * 10
-5Pa, doping rete gross mass is 0.8g, and the quality of Mg accounts for 15% of doping rete gross mass, and the doping layer thickness is 40nm;
According to above-mentioned preparation method, the more successively two-layer non-doping rete of evaporation and two-layer doping rete, wherein, non-doping rete and doping rete alternative stacked arrange.
Vacuum evaporation PETG rete forms encapsulated layer on the doping rete at last.
(3) at PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, time for exposure 300s, sealing forms enclosure space, functional layer, luminescent layer and transparent cathode are contained in the enclosure space, be formed with organic electroluminescence devices, this UV glue is epoxy resin, and the thickness of coating is 20 μ m.
The water oxygen permeability of the organic electroluminescence device behind the present embodiment composite package (WVTR, g/m
2Day) be 8.3E
-3
Effect embodiment
Be the beneficial effect of valid certificates organic electroluminescence device of the present invention and preparation method thereof, provide the related experiment data as follows.
Table 1. embodiment 1～6 organic electro-luminescence device lifetime information slip
Table 1 is embodiment 1～6 organic electro-luminescence device lifetime information slip.Fig. 2 is embodiment 1～6 organic electro-luminescence device lifetime curve chart.Can find out that from table 1 and Fig. 2 the initial brightness of the organic electroluminescence device behind the composite package of the present invention is 5,000cd/m
2Lower, the life-span reached more than 700 hours.
Table 2. embodiment 1～6 organic electroluminescence device light transmittance test result
| Embodiment 1 | Embodiment 2 | |
|
|
|
|
| Light transmittance (%) | 85.6 | 84.0 | 83.1 | 82.2 | 81.5 | 80.3 |
Table 2 is embodiment 1～6 organic electroluminescence device light transmittance test case tables.As can be seen from Table 2, organic electroluminescence device light transmittance of the present invention reaches more than 80%, can be used for transparent organic light emission product.
To sum up, the preparation method of organic electroluminescence device provided by the invention can reduce steam effectively to the erosion of organic electroluminescence device, improve significantly the life-span of organic electroluminescence device, organic electroluminescence device light transmittance of the present invention reaches more than 80% simultaneously.
Claims (9)
1. organic electroluminescence device, comprise transparent anode substrate, functional layer, luminescent layer, transparent cathode and encapsulated layer, transparent anode substrate and encapsulated layer form enclosure space, described functional layer, luminescent layer and transparent cathode are contained in the described enclosure space, it is characterized in that, described encapsulated layer comprises non-doping rete, doping rete and PETG rete successively, and described non-doping rete is MgF
2, phenyl beautiful jade, oxine aluminium, ZnS or ZnSe film, described doping rete is MgF
2, ZnS or ZnSe film and the metallic element film that mixes mutually and form, wherein, described metallic element comprises Ca, Ba, Sr or Mg.
2. organic electroluminescence device as claimed in claim 1 is characterized in that, it is 5%～15% that metallic element described in the described doping rete accounts for the mass percent of doping rete.
3. organic electroluminescence device as claimed in claim 1 is characterized in that, the thickness of described non-doping rete is 30nm～50nm, and the thickness of described doping rete is 30nm～50nm.
4. organic electroluminescence device as claimed in claim 1 is characterized in that, described non-doping rete and described doping rete alternative stacked arrange.
5. the preparation method of an organic electroluminescence device is characterized in that, may further comprise the steps:
Prepare functional layer, luminescent layer and transparent cathode at the transparent anode substrate;
Mode by vacuum evaporation is at the non-doping rete in described transparent cathode surface successively evaporation and doping rete, last vacuum evaporation PETG rete forms encapsulated layer, at described PETG rete edge-coating UV glue, by the described UV glue of the dry sclerosis of the mode of ultraviolet curing, sealing forms enclosure space, described functional layer, luminescent layer and transparent cathode are contained in the described enclosure space, are formed with organic electroluminescence devices;
Vacuum degree in the described vacuum evaporation process is 7 * 10
-5～3 * 10
-5Pa, evaporation rate is
Described non-doping rete is MgF
2, phenyl beautiful jade, oxine aluminium, ZnS or ZnSe;
Described doping rete is MgF
2, ZnS or ZnSe film and the metallic element film that mixes mutually and form, wherein, described metallic element comprises Ca, Ba, Sr or Mg.
6. preparation method as claimed in claim 5 is characterized in that, it is 5%～15% that metallic element described in the described doping rete accounts for the mass percent of doping rete.
7. preparation method as claimed in claim 5 is characterized in that, the thickness of described non-doping rete is 30nm～50nm, and the thickness of described doping rete is 30nm～50nm.
8. preparation method as claimed in claim 5, it is characterized in that, the step of the non-doping rete of described evaporation and doping rete is two-layer or two-layer above non-doping rete and doping rete of evaporation successively, wherein, and described non-doping rete and the setting of described doping rete alternative stacked.
9. preparation method as claimed in claim 5 is characterized in that, described UV glue is epoxy resin, and thickness is 20～40 μ m, time for exposure 300～400s.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1383182A2 (en) * | 2002-07-17 | 2004-01-21 | SAES GETTERS S.p.A. | System for applying a gas sorbing device on a surface and processes for the production thereof |
| CN101080121A (en) * | 2007-07-06 | 2007-11-28 | 清华大学 | An organic EL part and its making method |
| CN101128074A (en) * | 2007-09-20 | 2008-02-20 | 清华大学 | A kind of organic electroluminescence device and preparation method thereof |
-
2012
- 2012-03-29 CN CN2012100876740A patent/CN103367647A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1383182A2 (en) * | 2002-07-17 | 2004-01-21 | SAES GETTERS S.p.A. | System for applying a gas sorbing device on a surface and processes for the production thereof |
| CN101080121A (en) * | 2007-07-06 | 2007-11-28 | 清华大学 | An organic EL part and its making method |
| CN101128074A (en) * | 2007-09-20 | 2008-02-20 | 清华大学 | A kind of organic electroluminescence device and preparation method thereof |
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Application publication date: 20131023 |