CN104078595A - Organic light-emitting diode and preparation method thereof - Google Patents
Organic light-emitting diode and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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Abstract
The invention provides an organic light-emitting diode which comprises an anode conductive substrate, a light-emitting function layer, a cathode layer and a packaging layer which are laminated sequentially, wherein the packaging layer is in a composite structure formed by overlapping a packaging layer unit; and the packaging layer unit comprises a first organic barrier layer, a second organic barrier layer, a first inorganic barrier layer, a third organic barrier layer, a fourth organic barrier layer and a second inorganic barrier layer which are laminated sequentially. The invention further provides a preparation method of the organic light-emitting diode. The method can effectively reduce corrosion of water vapor and oxygen to the organic light-emitting diode, so that an organic function material and an electrode of the organic light-emitting diode are effectively protected, the light transmittance of the organic light-emitting diode is improved, and the service life of the organic light-emitting diode can be prolonged significantly. The method is particularly suitable for packaging a flexible organic light-emitting diode.
Description
Technical field
The present invention relates to electronic device association area, relate in particular to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is that the luminous organic material of preparing tens nanometer thickness on ito glass is made luminescent layer, and there is the metal electrode of low work function luminescent layer top.While being added with voltage on electrode, luminescent layer just produces light radiation.
OLED device have active illuminating, luminous efficiency high, low in energy consumption, light, thin, without advantages such as angle limitations, by insider, thought to be most likely at the device of new generation that occupies dominance on following illumination and display device market.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, has obtained huge achievement.Because the whole world is increasing, throw light on and show that producer drops into research and development one after another, having promoted greatly the industrialization process of OLED, making the growth rate of OLED industry surprising, having arrived the eve of scale of mass production at present.
Flexible product is the development trend of organic electroluminescence device, but current short problem of ubiquity life-span, therefore the quality of encapsulation directly affects the life-span of device.In conventional art, adopt glass cover or crown cap to encapsulate, its edge is resin-sealed by ultraviolet polymerization, but the glass cover using in this method or crown cap volume are often larger, 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 conventionally.
Summary of the invention
For overcoming the defect of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and preparation method thereof.Organic electroluminescence device of the present invention can reduce steam, the erosion of oxygen to organic electroluminescence device effectively; organic functional material and the electrode of protection organic electroluminescence device exempt from destruction; meet the sealing requirements of encapsulation; can improve significantly the life-span of OLED device; preparation method of the present invention is simple; easily large area preparation, is suitable for large-scale industrialization and uses.The inventive method is applicable to the organic electroluminescence device prepared with conducting glass substrate of encapsulation, is also applicable to encapsulation and take the flexible organic electroluminescent device that plastics or metal prepared as substrate.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise the anode conducting substrate, light emitting functional layer, cathode layer and the encapsulated layer that stack gradually, the composite construction of described encapsulated layer for being formed by encapsulated layer cells overlap; Described encapsulated layer unit comprises first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer stacking gradually;
The material on described first organic barrier layer and the 3rd organic barrier layer is all selected from 1,1-bis-((4-N, N '-bis-(p-methylphenyl) amine) phenyl) cyclohexane, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 2,9-dimethyl-4,7-diphenyl-1, a kind of in 10-phenanthroline and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The material on described second organic barrier layer and the 4th organic barrier layer is all selected from 4,7-diphenyl Phen, 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, oxine aluminium, two (2-methyl-8-quinoline)-(4-phenylphenol) aluminium and 3-(4-xenyl)-4 phenyl-5-tert-butyl benzene-1, a kind of in 2,4-triazole;
Described the first inorganic barrier layer material is titanium dioxide, magnesium oxide, silicon dioxide, zirconium dioxide, zinc oxide or alundum (Al2O3);
Described the second inorganic barrier layer material is the composite material that metal fluoride and metal oxide form, described metal fluoride is magnesium fluoride, aluminum fluoride, hexafluoro sodium aluminate, lanthanum fluoride, neodymium fluoride or gadolinium fluoride, and described metal oxide is molybdenum trioxide, vanadic oxide, tungstic acid, cesium oxide, nickel oxide or manganese dioxide.
Preferably, described encapsulated layer is the composite construction that 2～4 encapsulated layer cells overlaps form.
Preferably, the thickness on described first organic barrier layer, second organic barrier layer, the 3rd organic barrier layer and the 4th organic barrier layer is 200nm～300nm, described the first inorganic barrier layer thickness is 50nm～100nm, and described the second inorganic barrier layer thickness is 100nm～200nm.
Preferably, in described the second inorganic barrier layer, the mass fraction of described metal fluoride in composite material is 10%～30%.
Preferably, described light emitting functional layer comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer stacking gradually.
Preferably, described anode conducting substrate is conducting glass substrate or conduction organic film substrate.
More preferably, described anode conducting substrate is tin indium oxide (ITO) conducting glass substrate.
Preferably, described cathode layer can be non-transparent metals negative electrode (aluminium, silver, gold etc.) layer or transparent cathode layer (dielectric layer/metal level/dielectric layer etc., as ITO/Ag/ITO, ZnS/Ag/ZnS etc.).
More preferably, described cathode layer is aluminium.
The existence on organic barrier layer can stop outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device on the one hand, can increase the flexibility of encapsulated layer on the other hand, prevent the appearance crackle of encapsulated layer, simultaneously organic barrier layer have quality light, prepare the advantages such as easy.The pliability of encapsulated layer has been strengthened in the preparation that repeats on organic barrier layer.
Inorganic barrier layer good insulating, has good water, oxygen obstructing capacity, improves packaging effect, extends the encapsulation life-span.Described the second inorganic barrier layer material is the composite material that metal fluoride and metal oxide form, and can further improve the water oxygen obstructing capacity of device, can reduce the reflection to light simultaneously, improves the light transmittance of device.
The impact of the defect that encapsulated layer of the present invention can reduce single organic barrier layer, single inorganic barrier layer on packaging effect, extend water, oxygen permeation pathway, make water, oxygen enter the path of organic electroluminescence device more complicated, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, the pliability that can improve encapsulated layer simultaneously, reaches encapsulation requirement.Can improve the light transmittance of organic electroluminescence device light, reduce the impact of encapsulation on light efficiency, improve energy efficiency simultaneously.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) on clean electrically-conductive backing plate, be prepared with the anode pattern formation anode conducting substrate of organic electroluminescence devices; Adopt the method for vacuum evaporation on anode conducting substrate, to prepare light emitting functional layer and cathode layer;
(2) on cathode layer, prepare encapsulated layer, preparation method is as follows:
(a) the organic barrier layer of vacuum evaporation first on cathode layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(b) the organic barrier layer of vacuum evaporation second on first organic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(c) on second organic barrier layer, adopt the method for magnetron sputtering to prepare the first inorganic barrier layer, during sputter, base vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, passing into gas is argon gas and methane, and the flow of argon gas is 5～15sccm, and the flow of methane is 10～20sccm;
(d) vacuum evaporation the 3rd organic barrier layer on the first inorganic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(e) vacuum evaporation the 4th organic barrier layer on the 3rd organic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(f) vacuum evaporation the second inorganic barrier layer on the 4th organic barrier layer, evaporation rate is
vacuum degree is 1 * 10
-5～1 * 10
-3pa;
(a)～after (f) step completes, make an encapsulated layer unit;
(g) repeating step (a)～(f), make the encapsulated layer with composite construction, finally obtains described organic electroluminescence device;
The material on described first organic barrier layer and the 3rd organic barrier layer is all selected from 1,1-bis-((4-N, N '-bis-(p-methylphenyl) amine) phenyl) cyclohexane (TAPC), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq3), 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine (m-MTDATA), 2,9-dimethyl-4,7-diphenyl-1, a kind of in 10-phenanthroline (BCP) and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi);
Described second organic barrier layer and the 4th organic barrier layer material are all selected from 4,7-diphenyl Phen (Bphen), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi), oxine aluminium (Alq3), two (2-methyl-8-quinoline)-(4-phenylphenol) aluminium (Balq) and 3-(4-xenyl)-4 phenyl-5-tert-butyl benzene-1, a kind of in 2,4-triazole (TAZ);
The material of described the first inorganic barrier layer is titanium dioxide (TiO
2), magnesium oxide (MgO), silicon dioxide (SiO
2), zirconium dioxide (ZrO
2), zinc oxide (ZnO) or alundum (Al2O3) (Al
2o
3);
Described the second inorganic barrier layer material is the composite material that metal fluoride and metal oxide form, and described metal fluoride is magnesium fluoride (MgF
2), aluminum fluoride (AlF
3), hexafluoro sodium aluminate (Na
3alF
6), lanthanum fluoride (LaF
3), neodymium fluoride (NdF
3) or gadolinium fluoride (GdF
3), described metal oxide is molybdenum trioxide (MoO
3), vanadic oxide (V
2o
5), tungstic acid (WO
3), cesium oxide (Cs
2o), nickel oxide (NiO) or manganese dioxide (MnO
2).
Preferably, described encapsulated layer is the composite construction that 2～4 encapsulated layer cells overlaps form.
Preferably, the thickness on described first organic barrier layer, second organic barrier layer, the 3rd organic barrier layer and the 4th organic barrier layer is 200nm～300nm, described the first inorganic barrier layer thickness is 50nm～100nm, and described the second inorganic barrier layer thickness is 100nm～200nm.
Preferably, the mass fraction of described metal fluoride in composite material is 10%～30%.
Preferably, described light emitting functional layer comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer stacking gradually, and all adopts the method preparation of vacuum evaporation.
Preferably, described anode conducting substrate is conducting glass substrate or conduction organic film substrate.
More preferably, described anode conducting substrate is tin indium oxide (ITO) conducting glass substrate.
Preferably, described cathode layer can be non-transparent metals negative electrode (aluminium, silver, gold etc.) layer or transparent cathode layer (dielectric layer/metal level/dielectric layer etc., as ITO/Ag/ITO, ZnS/Ag/ZnS etc.).
More preferably, described cathode layer is aluminium.
Described encapsulated layer is that a plurality of basic structure repeats to form, water, oxygen permeation pathway have been extended, can reach good packaging effect, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, make up the shortcoming on single oxide layer and single organic substance barrier layer, extended device lifetime.Can improve the light transmittance of organic electroluminescence device light, reduce the impact of encapsulation on light efficiency, improve energy efficiency simultaneously.
The invention provides a kind of organic electroluminescence device and preparation method thereof and there is following beneficial effect:
(1) organic electroluminescence device of the present invention can reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device effectively, thereby device light emitting functional layer and electrode are formed to effective protection, improve significantly the life-span of organic electroluminescence device;
(2) water resistance of organic electroluminescence device encapsulated layer of the present invention (WVTR) reaches 10
-4g/m
2day, the life-span reaches 3,791 hours above (T701000cd/m
2), light transmittance reaches more than 52%;
(3) organic electroluminescence device preparation method of the present invention is simple, and easily large area preparation is suitable for large-scale industrialization and uses.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of the embodiment of the present invention 1 preparation.
Embodiment
The following stated is the preferred embodiment of the present invention.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvement and adjustment, these improvement and adjustment are also considered as in protection scope of the present invention.
Embodiment 1:
A preparation method for organic electroluminescence device, comprises the following steps:
(1) ito glass substrate 1 pre-treatment: ITO conducting glass substrate 1 is put into acetone, ethanol, deionized water, ethanol successively, and ultrasonic cleaning is 5 minutes respectively, then dries up with nitrogen, and stove-drying is stand-by; Ito glass substrate 1 after cleaning is carried out to surface activation process, to increase the oxygen content of conductive surface layer, improve the work function of conductive layer surface; Ito glass substrate 1 thickness is 100nm;
(2) preparation of light emitting functional layer 2:
Hole injection layer 21: evaporation MoO on ito glass substrate 1
3the composite material that doping NPB obtains, MoO
3doping mass fraction be 30%, evaporation all adopts high vacuum coating equipment to carry out, during evaporation, vacuum degree is 1 * 10
-5pa, evaporation rate is
obtain hole injection layer 21, thickness is 10nm;
Hole transmission layer 22: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, evaporation TCTA on hole injection layer 21, vacuum degree is 1 * 10
-5pa, evaporation rate is
evaporation thickness is 30nm;
Luminescent layer 23: evaporation luminescent layer 23 on hole transmission layer 22, luminescent layer 23 material of main parts adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), guest materials quality accounts for 5% of material of main part, and evaporation vacuum degree is 1 * 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
The preparation of electron transfer layer 24: evaporation 4 on luminescent layer 23,7-diphenyl-1,10-phenanthroline (Bphen) is as electron transport material, and vacuum degree is 1 * 10
-5pa, evaporation rate is
evaporation thickness is 10nm;
The preparation of electron injecting layer 25: evaporation electron injection material forms electron injecting layer 25 on electron transfer layer 24, and electron injecting layer 25 materials are CsN
3the composite material that doping Bphen forms, doping mass fraction is 30%, vacuum degree is 1 * 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
(3) preparation of cathode layer 3: evaporation metal negative electrode 3 on electron injecting layer 25, metallic cathode 3 adopts aluminium (Al), and thickness is 100nm, and evaporation vacuum degree is 1 * 10
-5pa, evaporation rate is
(4) preparation of encapsulated layer 4:
(a) preparation on first organic barrier layer 401: vacuum evaporation TPBi on cathode layer 3, obtaining thickness is first organic barrier layer 401 of 200nm, vacuum degree is 1 * 10
-3pa, evaporation rate is
(b) preparation on second organic barrier layer 402: vacuum evaporation TAZ on first organic barrier layer 401, obtaining thickness is second organic barrier layer 802 of 220nm, vacuum degree is 1 * 10
-3pa, evaporation rate is
(c) preparation of the first inorganic barrier layer 403: adopting magnetron sputtering to prepare thickness on second organic barrier layer 402 is that the material of the first inorganic barrier layer 403, the first inorganic barrier layers 403 of 70nm is Al
2o
3, base vacuum degree is 1 * 10
-3pa, passes into Ar and CH
4, Ar flow is 7sccm, CH
4flow is 13sccm;
(d) preparation on the 3rd organic barrier layer 404: prepare material, thickness and the preparation method on 404, the three organic barrier layers 404, the 3rd organic barrier layer with first organic barrier layer 401 on the first inorganic barrier layer 403;
(e) preparation on the 4th organic barrier layer 405: prepare material, thickness and the preparation method on 405, the four organic barrier layers 405, the 4th organic barrier layer with second organic barrier layer 402 on the 3rd organic barrier layer 404;
(f) preparation of the second inorganic barrier layer 406: evaporation GdF on the 4th organic barrier layer 405
3and MnO
2the composite material forming, obtaining thickness is the second inorganic barrier layer 406 of 120nm, GdF
3the mass fraction that accounts for composite material is 10%, evaporation rate
vacuum degree 1 * 10
-3pa;
(g) first organic barrier layer 407, second organic barrier layer 408, the first inorganic barrier layer 409, the 3rd organic barrier layer 410, the 4th organic barrier layer 411, second inorganicly stops 412 preparation: after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer 406, to prepare first organic barrier layer 407, on first organic barrier layer 407, adopt again method and the material that step (b) is identical to prepare second organic barrier layer 408, on second organic barrier layer 408, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer 409, on the first inorganic barrier layer 409, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer 410, on the 3rd organic barrier layer 410, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer 411, on the 4th organic barrier layer 411, adopt method that step (f) is identical and material to prepare second and inorganicly stop 412, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, finally obtain the encapsulated layer that contains 2 encapsulated layer unit.
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 9.5 * 10
-4, the life-span of organic electroluminescence device is 3,791h(T701000cd/m
2), light transmittance is 58%.
Fig. 1 is the structural representation of the organic electroluminescence device that makes of the embodiment of the present invention 1.As shown in Figure 1, the present embodiment organic electroluminescence device, comprise the ito glass substrate 1, light emitting functional layer 2, cathode layer 3 and the encapsulated layer 4 that stack gradually, light emitting functional layer 2 comprises hole injection layer 21, hole transmission layer 22, luminescent layer 23, electron transfer layer 24, the electron injecting layer 25 stacking gradually, encapsulated layer 4 comprises first organic barrier layer 401,407, second organic barrier layer 402,408, the first inorganic barrier layer 403,409, the 3rd organic barrier layer 405,411, organic barrier layer 404,410, the four and the second inorganic barrier layer 406,412.
Embodiment 2:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
(a) preparation on first organic barrier layer: vacuum evaporation TAPC on cathode layer, obtaining thickness is first organic barrier layer of 200nm, vacuum degree is 1 * 10
-5pa, evaporation rate is
(b) preparation on second organic barrier layer: vacuum evaporation Bphen on first organic barrier layer, obtaining thickness is second organic barrier layer of 200nm, vacuum degree is 1 * 10
-5pa, evaporation rate is
(c) preparation of the first inorganic barrier layer: adopt magnetron sputtering to prepare the first inorganic barrier layer that thickness is 100nm on second organic barrier layer, the material of the first inorganic barrier layer is TiO
2, base vacuum degree is 1 * 10
-5pa, passes into Ar and CH
4, Ar flow is 10sccm, CH
4flow is 20sccm;
(d) preparation on the 3rd organic barrier layer: prepare the 3rd organic barrier layer on the first inorganic barrier layer, the material on the 3rd organic barrier layer, thickness and preparation method are with first organic barrier layer;
(e) preparation on the 4th organic barrier layer: prepare the 4th organic barrier layer on the 3rd organic barrier layer, the material on the 4th organic barrier layer, thickness and preparation method are with second organic barrier layer;
(f) preparation of the second inorganic barrier layer: evaporation MgF on the 4th organic barrier layer
2and MoO
3the composite material forming, obtaining thickness is the second inorganic barrier layer of 200nm, MgF
2the mass fraction that accounts for composite material is 30%, evaporation rate
vacuum degree is 1 * 10
-5pa;
(g) after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer, to prepare first organic barrier layer, on first organic barrier layer, adopt again method and the material that step (b) is identical to prepare second organic barrier layer, on second organic barrier layer, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer, on the first inorganic barrier layer, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer, on the 3rd organic barrier layer, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer, on the 4th organic barrier layer, adopt method and the material that step (f) is identical to prepare the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, prepare a plurality of encapsulated layers unit, finally obtain the encapsulated layer that contains 4 encapsulated layer unit.
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 8.1 * 10
-4, the life-span of organic electroluminescence device is 3,910h(T701000cd/m
2), light transmittance is 52%.
The present embodiment organic electroluminescence device, comprise the ito glass substrate stacking gradually, light emitting functional layer, cathode layer and encapsulated layer, encapsulated layer comprises the first organic barrier layer stacking gradually, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer.
Embodiment 3:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
(a) preparation on first organic barrier layer: vacuum evaporation NPB on cathode layer, obtaining thickness is first organic barrier layer of 300nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(b) preparation on second organic barrier layer: vacuum evaporation BCP on first organic barrier layer, obtaining thickness is second organic barrier layer of 300nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(c) preparation of the first inorganic barrier layer: adopt magnetron sputtering to prepare the first inorganic barrier layer that thickness is 50nm on second organic barrier layer, the material of the first inorganic barrier layer is MgO, and base vacuum degree is 1 * 10
-5pa, passes into Ar and CH
4, Ar flow is 5sccm, CH
4flow is 15sccm;
(d) preparation on the 3rd organic barrier layer: prepare the 3rd organic barrier layer on the first inorganic barrier layer, the material on the 3rd organic barrier layer, thickness and preparation method are with first organic barrier layer;
(e) preparation on the 4th organic barrier layer: prepare the 4th organic barrier layer on the 3rd organic barrier layer, the material on the 4th organic barrier layer, thickness and preparation method are with second organic barrier layer;
(f) preparation of the second inorganic barrier layer: evaporating Al F on the 4th organic barrier layer
3and V
2o
5the composite material forming, obtaining thickness is the second inorganic barrier layer of 150nm, AlF
3the mass fraction that accounts for composite material is 20%, evaporation rate
vacuum degree is 1 * 10
-4pa;
(g) after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer, to prepare first organic barrier layer, on first organic barrier layer, adopt again method and the material that step (b) is identical to prepare second organic barrier layer, on second organic barrier layer, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer, on the first inorganic barrier layer, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer, on the 3rd organic barrier layer, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer, on the 4th organic barrier layer, adopt method and the material that step (f) is identical to prepare the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, prepare a plurality of encapsulated layers unit, finally obtain the encapsulated layer that contains 3 encapsulated layer unit.
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 8.6 * 10
-4, the life-span of organic electroluminescence device is 3,817h(T701000cd/m
2), light transmittance is 55%.
The present embodiment organic electroluminescence device, comprise the ito glass substrate stacking gradually, light emitting functional layer, cathode layer and encapsulated layer, encapsulated layer comprises the first organic barrier layer stacking gradually, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer.
Embodiment 4:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
(a) preparation on first organic barrier layer: vacuum evaporation Alq3 on cathode layer, obtaining thickness is first organic barrier layer of 250nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(b) preparation on second organic barrier layer: vacuum evaporation TPBi on first organic barrier layer, obtaining thickness is second organic barrier layer of 250nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(c) preparation of the first inorganic barrier layer: adopt magnetron sputtering to prepare the first inorganic barrier layer that thickness is 70nm on second organic barrier layer, the material of the first inorganic barrier layer is SiO
2, base vacuum degree is 1 * 10
-5pa, passes into Ar and CH
4, Ar flow is 7sccm, CH
4flow is 10sccm;
(d) preparation on the 3rd organic barrier layer: prepare the 3rd organic barrier layer on the first inorganic barrier layer, the material on the 3rd organic barrier layer, thickness and preparation method are with first organic barrier layer;
(e) preparation on the 4th organic barrier layer: prepare the 4th organic barrier layer on the 3rd organic barrier layer, the material on the 4th organic barrier layer, thickness and preparation method are with second organic barrier layer;
(f) preparation of the second inorganic barrier layer: evaporation Na on the 4th organic barrier layer
3alF
6and WO
3the composite material forming, obtaining thickness is the second inorganic barrier layer of 140nm, Na
3alF
6the mass fraction that accounts for composite material is 10%, and evaporation rate is
vacuum degree is 1 * 10
-4pa;
(g) after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer, to prepare first organic barrier layer, on first organic barrier layer, adopt again method and the material that step (b) is identical to prepare second organic barrier layer, on second organic barrier layer, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer, on the first inorganic barrier layer, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer, on the 3rd organic barrier layer, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer, on the 4th organic barrier layer, adopt method and the material that step (f) is identical to prepare the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, prepare a plurality of encapsulated layers unit, finally obtain the encapsulated layer that contains 3 encapsulated layer unit.
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 8.7 * 10
-4, the life-span of organic electroluminescence device is 3,848h(T701000cd/m
2), light transmittance is 57%.
The present embodiment organic electroluminescence device, comprise successively ito glass substrate, light emitting functional layer, cathode layer and encapsulated layer, encapsulated layer comprises first organic barrier layer successively, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer.
Embodiment 5:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
(a) preparation on first organic barrier layer: vacuum evaporation m-MTDATA on cathode layer, obtaining thickness is first organic barrier layer of 220nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(b) preparation on second organic barrier layer: vacuum evaporation Alq3 on first organic barrier layer, obtaining thickness is second organic barrier layer of 240nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(c) preparation of the first inorganic barrier layer: adopt magnetron sputtering to prepare the first inorganic barrier layer that thickness is 100nm on second organic barrier layer, the material of the first inorganic barrier layer is ZrO
2, base vacuum degree is 5 * 10
-5pa, passes into Ar and CH
4, Ar flow is 15sccm, CH
4flow is 15sccm;
(d) preparation on the 3rd organic barrier layer: prepare the 3rd organic barrier layer on the first inorganic barrier layer, the material on the 3rd organic barrier layer, thickness and preparation method are with first organic barrier layer;
(e) preparation on the 4th organic barrier layer: prepare the 4th organic barrier layer on the 3rd organic barrier layer, the material on the 4th organic barrier layer, thickness and preparation method are with second organic barrier layer;
(f) preparation of the second inorganic barrier layer: evaporation LaF on the 4th organic barrier layer
3and Cs
2the composite material that O forms, obtaining thickness is the second inorganic barrier layer of 120nm, LaF
3the mass fraction that accounts for composite material is 10%, and evaporation rate is
vacuum degree is 1 * 10
-4pa;
(g) after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer, to prepare first organic barrier layer, on first organic barrier layer, adopt again method and the material that step (b) is identical to prepare second organic barrier layer, on second organic barrier layer, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer, on the first inorganic barrier layer, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer, on the 3rd organic barrier layer, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer, on the 4th organic barrier layer, adopt method and the material that step (f) is identical to prepare the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, prepare a plurality of encapsulated layers unit, finally obtain the encapsulated layer that contains 2 encapsulated layer unit,
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 8.9 * 10
-4, the life-span of organic electroluminescence device is 3,829h(T701000cd/m
2), light transmittance is 54%.
The present embodiment organic electroluminescence device, comprise the ito glass substrate, light emitting functional layer, cathode layer and the encapsulated layer that stack gradually, encapsulated layer comprises first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer stacking gradually.
Embodiment 6:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
(a) preparation on first organic barrier layer: vacuum evaporation BCP on cathode layer, obtaining thickness is first organic barrier layer of 260nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(b) preparation on second organic barrier layer: vacuum evaporation Balq on first organic barrier layer, obtaining thickness is second organic barrier layer of 200nm, vacuum degree is 1 * 10
-4pa, evaporation rate is
(c) preparation of the first inorganic barrier layer: adopt magnetron sputtering to prepare the first inorganic barrier layer that thickness is 80nm on second organic barrier layer, the material of the first inorganic barrier layer is ZnO, and base vacuum degree is 5 * 10
-5pa, passes into Ar and CH
4, Ar flow is 5sccm, CH
4flow is 20sccm;
(d) preparation on the 3rd organic barrier layer: prepare the 3rd organic barrier layer on the first inorganic barrier layer, the material on the 3rd organic barrier layer, thickness and preparation method are with first organic barrier layer;
(e) preparation on the 4th organic barrier layer: prepare the 4th organic barrier layer on the 3rd organic barrier layer, the material on the 4th organic barrier layer, thickness and preparation method are with second organic barrier layer;
(f) preparation of the second inorganic barrier layer: evaporation NdF on the 4th organic barrier layer
3with the composite material that NiO forms, obtaining thickness is the second inorganic barrier layer of 100nm, NdF
3the mass fraction that accounts for composite material is 15%, evaporation rate
vacuum degree is 1 * 10
-4pa;
(g) after step (f), adopt method and the material identical with step (a) on the second inorganic barrier layer, to prepare first organic barrier layer, on first organic barrier layer, adopt again method and the material that step (b) is identical to prepare second organic barrier layer, on second organic barrier layer, adopt method and the material that step (c) is identical to prepare the first inorganic barrier layer, on the first inorganic barrier layer, adopt method and the material that step (d) is identical to prepare the 3rd organic barrier layer, on the 3rd organic barrier layer, adopt again method and the material identical with step (e) to prepare the 4th organic barrier layer, on the 4th organic barrier layer, adopt method and the material that step (f) is identical to prepare the second inorganic barrier layer, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer form an encapsulated layer unit, prepare a plurality of encapsulated layers unit, finally obtain the encapsulated layer that contains 2 encapsulated layer unit.
The water oxygen permeability of the present embodiment organic electroluminescence device (WVTR, g/m
2day) be 9.2 * 10
-4, the life-span of organic electroluminescence device is 3,814h(T701000cd/m
2), light transmittance is 56%.
The present embodiment organic electroluminescence device, comprise the ito glass substrate, light emitting functional layer, cathode layer and the encapsulated layer that stack gradually, encapsulated layer comprises the first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer that stack gradually, first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic
Barrier layer and the second inorganic barrier layer.
Effect embodiment
For the beneficial effect of valid certificates organic electroluminescence device of the present invention and preparation method thereof, provide related experiment data as follows.
Table 1. embodiment 1～6 organic electroluminescence device water oxygen permeability
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| WVTR(g/m 2/day) | 9.5×10 -4 | 8.1×10 -4 | 8.6×10 -4 | 8.7×10 -4 | 8.9×10 -4 | 9.2×10 -4 |
Table 2. embodiment 1～6 organic electro-luminescence device lifetime situation
Table 3. embodiment 1～6 organic electroluminescence device light transmittance
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Light transmittance | 58% | 52% | 55% | 57% | 54% | 56% |
As can be seen from Table 1, the water oxygen permeability of organic electroluminescence device of the present invention (WVTR) reaches 8.1 * 10
-4g/m
2day, as can be seen from Table 2, the life-span of organic electroluminescence device of the present invention reaches 3,791 hours above (T701000cd/m
2), the light transmittance of organic electroluminescence device reaches 52% as can be seen from Table 3.
To sum up; organic electroluminescence device provided by the invention can reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device effectively; thereby device organic functional material and electrode are formed to effective protection; meet the requirement of the sealing of encapsulation; and improve the light transmittance of device; meet the sealing requirements of encapsulation, the life-span that can improve significantly OLED device.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. an organic electroluminescence device, comprises the anode conducting substrate, light emitting functional layer, cathode layer and the encapsulated layer that stack gradually, it is characterized in that the composite construction of described encapsulated layer for being formed by encapsulated layer cells overlap; Described encapsulated layer unit comprises first organic barrier layer, second organic barrier layer, the first inorganic barrier layer, the 3rd organic barrier layer, the 4th organic barrier layer and the second inorganic barrier layer stacking gradually;
The material on described first organic barrier layer and the 3rd organic barrier layer is all selected from 1,1-bis-((4-N, N '-bis-(p-methylphenyl) amine) phenyl) cyclohexane, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 2,9-dimethyl-4,7-diphenyl-1, a kind of in 10-phenanthroline and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The material on described second organic barrier layer and the 4th organic barrier layer is all selected from 4,7-diphenyl Phen, 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, oxine aluminium, two (2-methyl-8-quinoline)-(4-phenylphenol) aluminium and 3-(4-xenyl)-4 phenyl-5-tert-butyl benzene-1, a kind of in 2,4-triazole;
Described the first inorganic barrier layer material is titanium dioxide, magnesium oxide, silicon dioxide, zirconium dioxide, zinc oxide or alundum (Al2O3);
Described the second inorganic barrier layer material is the composite material that metal fluoride and metal oxide form, described metal fluoride is magnesium fluoride, aluminum fluoride, hexafluoro sodium aluminate, lanthanum fluoride, neodymium fluoride or gadolinium fluoride, and described metal oxide is molybdenum trioxide, vanadic oxide, tungstic acid, cesium oxide, nickel oxide or manganese dioxide.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, described encapsulated layer is the composite construction that 2～4 encapsulated layer cells overlaps form.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness on described first organic barrier layer, second organic barrier layer, the 3rd organic barrier layer and the 4th organic barrier layer is 200nm～300nm, described the first inorganic barrier layer thickness is 50nm～100nm, and described the second inorganic barrier layer thickness is 100nm～200nm.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, in described the second inorganic barrier layer, the mass fraction of described metal fluoride in composite material is 10%～30%.
5. organic electroluminescence device as claimed in claim 1, is characterized in that, described light emitting functional layer comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer stacking gradually.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
(1) on clean electrically-conductive backing plate, be prepared with the anode pattern formation anode conducting substrate of organic electroluminescence devices; Adopt the method for vacuum evaporation on anode conducting substrate, to prepare light emitting functional layer and cathode layer;
(2) on cathode layer, prepare encapsulated layer, encapsulated layer preparation method is as follows:
(a) the organic barrier layer of vacuum evaporation first on cathode layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(b) the organic barrier layer of vacuum evaporation second on first organic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(c) on second organic barrier layer, adopt the method for magnetron sputtering to prepare the first inorganic barrier layer, during sputter, base vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, passing into gas is argon gas and methane, and the flow of argon gas is 5～15sccm, and the flow of methane is 10～20sccm;
(d) vacuum evaporation the 3rd organic barrier layer on the first inorganic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(e) vacuum evaporation the 4th organic barrier layer on the 3rd organic barrier layer, evaporation condition is: vacuum degree is 1 * 10
-5pa～1 * 10
-3pa, evaporation rate is
(f) vacuum evaporation the second inorganic barrier layer on the 4th organic barrier layer, evaporation rate is
vacuum degree is 1 * 10
-5～1 * 10
-3pa;
(a)～after (f) step completes, make an encapsulated layer unit;
(g) repeating step (a)～(f), make the encapsulated layer with composite construction, finally obtains described organic electroluminescence device;
The material on described first organic barrier layer and the 3rd organic barrier layer is all selected from 1,1-bis-((4-N, N '-bis-(p-methylphenyl) amine) phenyl) cyclohexane, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 2,9-dimethyl-4,7-diphenyl-1, a kind of in 10-phenanthroline and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The material on described second organic barrier layer and the 4th organic barrier layer is all selected from 4,7-diphenyl Phen, 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, oxine aluminium, two (2-methyl-8-quinoline)-(4-phenylphenol) aluminium and 3-(4-xenyl)-4 phenyl-5-tert-butyl benzene-1, a kind of in 2,4-triazole;
Described the first inorganic barrier layer material is titanium dioxide, magnesium oxide, silicon dioxide, zirconium dioxide, zinc oxide or alundum (Al2O3);
Described the second inorganic barrier layer material is the composite material that metal fluoride and metal oxide form, described metal fluoride is magnesium fluoride, aluminum fluoride, hexafluoro sodium aluminate, lanthanum fluoride, neodymium fluoride or gadolinium fluoride, and described metal oxide is molybdenum trioxide, vanadic oxide, tungstic acid, cesium oxide, nickel oxide or manganese dioxide.
7. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, described encapsulated layer is the composite construction that 2～4 encapsulated layer cells overlaps form.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the thickness on described first organic barrier layer, second organic barrier layer, the 3rd organic barrier layer and the 4th organic barrier layer is 200nm～300nm, described the first inorganic barrier layer thickness is 50nm～100nm, and described the second inorganic barrier layer thickness is 100nm～200nm.
9. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, the mass fraction of described metal fluoride in composite material is 10%～30%.
10. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, described light emitting functional layer comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer stacking gradually, and all adopts the method preparation of vacuum evaporation.
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