CN104518101A - Organic electroluminescent device and preparation method thereof - Google Patents
Organic electroluminescent device and preparation method thereof Download PDFInfo
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Abstract
The invention provides an organic electroluminescent device. The organic electroluminescent device comprises an anode conductive substrate, a luminescence function layer, a cathode layer and a packaging layer which are successively stacked. The packaging layer comprises an organic barrier layer and a mixed barrier layer which are successively arranged in a laminated mode. The material of the organic barrier layer is CuPc, NPB, Alq3, m-MTDATA or BCP, the material of the mixed barrier layer is a mixed material formed by doping dialkyl beryllium into a metal fluoride, the metal fluoride is AlF3, HfF4, ZrF4, LiF, CeF2 and YF3, and the structural formula of the dialkyl beryllium is shown in the descriptions, k being a natural number from 1 to 4. The organic electroluminescent device is alternatively packed by use of multi-layer material layers, is high in compactness, can effectively reduce corrosion caused by oxygen and steam to the organic electroluminescent device, and substantially improves the life of the organic electroluminescent device. The invention further provides a preparation method of the organic electroluminescent device.
Description
Technical field
The present invention relates 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 a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is between transparent anode and cathode layer, accompany multilayer organic material film (hole injection layer, hole transmission layer, luminescent layer, electron supplying layer and electron injecting layer), and apply certain voltage when between electrode after, luminescent layer will be luminous.In recent years, organic electroluminescence device because cost of manufacture own is low, the response time is short, luminosity is high, the feature such as wide viewing angle, low driving voltage and energy-conserving and environment-protective received extensive concern in fields such as total colouring, backlight and illuminations, and has been considered to be most likely at the device of new generation following illumination and display device market occupying dominance.
At present, there is life-span shorter problem in organic electroluminescence device, and this occurs rapidly aging mainly because organic material film is very loose after easily being infiltrated by compositions such as the steam in air and oxygen.When real work, cathode layer is corroded 10% work that will have a strong impact on device.Therefore, be necessary to provide a kind of method for packing that effectively can intercept the organic electroluminescence device of water Oxygen permeation.
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.The encapsulated layer of this organic electroluminescence device adopts multilayer inorganic barrier layer and mixes barrier layer and alternately encapsulate, and compactness is high, effectively can reduce oxygen and steam to the erosion of organic electroluminescence device, thus improve the life-span of organic electroluminescence device significantly.The inventive method is applicable to take electro-conductive glass as organic electroluminescence device prepared by substrate, is also applicable to the flexible organic electroluminescent device prepared for substrate with plastics or metal.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, described encapsulated layer comprises inorganic barrier layer and the mixing barrier layer of lamination setting successively, the material of described inorganic barrier layer is CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq
3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA) or 4,7-diphenyl-1,10-Phen (BCP), the material on described mixing barrier layer is the composite material that glucinum alkyl BeR2 doping metals fluoride is formed, and described metal fluoride is aluminum fluoride (AlF
3), tetrafluoride hafnium (HfF
4), zirconium fluoride (ZrF
4), lithium fluoride (LiF), bifluoride cerium (CeF
2) or yttrium fluoride (YF
3), the structural formula of described glucinum alkyl BeR2 is as shown in P:
In formula, k is the natural number of 1 ~ 4.
Preferably, in the composite material that described glucinum alkyl BeR2 doping metals fluoride is formed, the doping molar fraction of described metal fluoride is 20 ~ 40%.
Preferably, the thickness of described inorganic barrier layer is 200nm ~ 300nm, and the thickness on described mixing barrier layer is 200nm ~ 300nm.
Preferably, described inorganic barrier layer and mixing barrier layer alternately repeat to arrange 4 ~ 6 times successively.
Preferably, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
Preferably, described anode substrate is conducting glass substrate or conductive plastics or metallic film substrate.
Hole injection layer adopts common used material in industry, be preferably N, N'-diphenyl-N, N'-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB) to adulterate molybdenum trioxide (MoO
3).
Hole transmission layer adopts common used material in industry, is preferably 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA).
Luminescent layer adopts common used material in industry, is preferably 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), three (the 2-phenylpyridines) that adulterate and closes iridium (Ir (ppy) 3).
Electron transfer layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen).
Electron injecting layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen) and adulterates cesium azide (CsN
3).
Cathode layer can be non-transparent metals cathode layer (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed).
Preferably, the material of cathode layer is aluminium, silver or golden.
Preferably, cathode layer is the sandwich of tin indium oxide (ITO)/Ag/ tin indium oxide (ITO), ZnS/Ag/ZnS formation.
Described encapsulated layer adopts inorganic barrier layer to be deposited on cathode layer surface with mixing barrier layer successively alternative stacked set-up mode, and light emitting functional layer and cathode layer can be protected in subsequent operation process to exempt from destruction.Described mixing barrier layer structure is fine and close, effectively can intercept water Oxygen permeation and enter device inside, the material on described mixing barrier layer is the composite material that glucinum alkyl BeR2 doping metals fluoride is formed, wherein, described metal fluoride has good heat conductivility, can effectively prevent device over-heat inside and cause the situation of service life reduction, described glucinum alkyl BeR2 has the pliability of organic compound, can reduce stress; Described inorganic barrier layer can make up the fragility shortcoming of inorganic material in encapsulated layer effectively, improves the pliability of device, can reduce stress in thin film simultaneously, prevents be full of cracks, also can extend water, Oxygen permeation path; Encapsulated layer provided by the invention effectively can stop that extraneous steam and oxygen are to the erosion of organic electroluminescence device, thus extends device lifetime.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) anode pattern preparing organic electroluminescence device on the electrically-conductive backing plate of cleaning forms anode conducting substrate; The method of vacuum evaporation is adopted to prepare light emitting functional layer and cathode layer on anode conducting substrate;
(2) on cathode layer, prepare encapsulated layer, preparation method is as follows:
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, the material of described inorganic barrier layer is CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq
3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl amino) triphenylamine (m-MTDATA) or 4,7-diphenyl-1,10-Phens (BCP), the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
The making on (b) mixing barrier layer:
On described inorganic barrier layer, prepare mixing barrier layer by the method for magnetron sputtering, the material on described mixing barrier layer is the composite material that glucinum alkyl BeR2 doping metals fluoride is formed, and described metal fluoride is aluminum fluoride (AlF
3), tetrafluoride hafnium (HfF
4), zirconium fluoride (ZrF
4), lithium fluoride (LiF), bifluoride cerium (CeF
2) or yttrium fluoride (YF
3), the structural formula of described glucinum alkyl BeR2 is as shown in P:
In formula, k is the natural number of 1 ~ 4, and the background vacuum in described magnetron sputtering process is 1 × 10
-5pa ~ 1 × 10
-3pa.
Preferably, in the composite material that described glucinum alkyl BeR2 doping metals fluoride is formed, the doping molar fraction of described metal fluoride is 20 ~ 40%.
Preferably, the thickness of described inorganic barrier layer is 200nm ~ 300nm, and the thickness on described mixing barrier layer is 200nm ~ 300nm.
Preferably, described inorganic barrier layer and mixing barrier layer alternately repeat to arrange 4 ~ 6 times successively.
Preferably, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
Preferably, described anode substrate is conducting glass substrate or conductive plastics or metallic film substrate.
Hole injection layer adopts common used material in industry, be preferably N, N'-diphenyl-N, N'-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB) to adulterate MoO
3(molybdenum trioxide).
Hole transmission layer adopts common used material in industry, is preferably 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA).
Luminescent layer adopts common used material in industry, is preferably 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), three (the 2-phenylpyridines) that adulterate and closes iridium (Ir (ppy) 3).
Electron transfer layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen).
Electron injecting layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen) and adulterates cesium azide (CsN
3).
Cathode layer can be non-transparent metals cathode layer (aluminium, silver, gold etc.), also can be transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed).
Preferably, the material of cathode layer is aluminium, silver or golden.
Preferably, cathode layer is the sandwich that tin indium oxide (ITO)/Ag/ITO, ZnS/Ag/ZnS is formed.
Obtain described organic electroluminescence device by above-mentioned steps, comprise the anode conducting substrate, light emitting functional layer, cathode layer and the encapsulated layer that are cascading.
Organic electroluminescence device provided by the invention adopts the alternately encapsulation of multilayer material layer, and preparation method is easy, and the encapsulating material of employing is less expensive, is easy to large area preparation, and the method is particularly useful for encapsulating flexible organic electroluminescent device.
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 adopts inorganic barrier layer and mixing barrier layer alternative stacked to arrange, compactness is high, effectively can reduce oxygen and steam to the erosion of organic electroluminescence device, and rapid thermal conduction can be realized and evacuate heat, improve the life-span of organic electroluminescence device significantly;
(2) water resistance (WVTR) of organic electroluminescence device of the present invention reaches 8.0 × 10
-4g/m
2day, the life-span reaches 2, more than 500 hours (T70@1000cd/m
2: namely starting brightness is 1000cd/m
2, brightness decay is to 70% time used);
(3) the inventive method is applicable to encapsulation is organic electroluminescence device prepared by anode substrate with electro-conductive glass, is also applicable to encapsulate the flexible organic electroluminescent device prepared for anode substrate with plastics or metal.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device;
(4) organic electroluminescence device material of the present invention is cheap, and method for packing technique is simple, and easy large area preparation, is suitable for industrialization and uses on a large scale.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In conjunction with the structural representation of organic electroluminescence device as shown in Figure 1, present embodiments provide a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) on anode substrate, prepare light emitting functional layer 20 and cathode layer 30
A. the pre-treatment of conducting glass substrate
Get ito glass substrate 10, carry out acetone cleaning → ethanol purge → washed with de-ionized water → ethanol purge successively, all clean with supersonic wave cleaning machine, individual event washing cleaning 5 minutes, then dry up with nitrogen, stove-drying is stand-by; Also need to carry out surface activation process to the ito glass after cleaning, to increase the oxygen content of conductive surface layer, improve the work function of conductive layer surface; ITO thickness is 100nm;
B. the preparation of light emitting functional layer 20 and cathode layer 30
The method of vacuum evaporation is adopted to form hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively on ito glass substrate 10, described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer form light emitting functional layer 20, and method is as follows:
The preparation of hole injection layer: evaporation to be adulterated MoO by NPB on ito glass substrate 10
3the composite material formed, MoO
3the mass fraction accounting for NPB is 30wt%, and this layer thickness is 10nm, vacuum degree 3 × 10
-5pa, evaporation rate
The preparation of hole transmission layer: evaporation hole transmission layer on hole injection layer, adopts 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA) as hole mobile material, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
The preparation of luminescent layer: evaporation luminescent layer on hole transmission layer, the material of main part of luminescent layer adopts 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), Ir (ppy)
3the mass fraction accounting for TPBI is 5wt%, 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) is as electron transport material on luminescent layer, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
The preparation of electron injecting layer: evaporation electron injecting layer on the electron transport layer, mixes CsN3 in Bphen, and the mass fraction that CsN3 accounts for Bphen is 30wt%, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
On electron injecting layer, evaporation prepares cathode layer 30 again, and metal cathode layer 30 adopts aluminium (Al), and thickness is 100nm, vacuum degree 3 × 10
-5pa, evaporation rate
(2) on cathode layer 30, encapsulated layer 40 is prepared
The making of (a) inorganic barrier layer 401:
By the mode of vacuum evaporation at the surperficial evaporation inorganic barrier layer 401 of described cathode layer 30, the thickness of described inorganic barrier layer 401 is 250nm, and the material of described inorganic barrier layer 401 is CuPc, and the vacuum degree in described vacuum evaporation process is 1 × 10
-3pa, evaporation rate is
The making on (b) mixing barrier layer 402:
Adopt the mode of magnetron sputtering on described inorganic barrier layer 401, prepare mixing barrier layer 402, the material on described mixing barrier layer 402 is two (3,7-dimethyl octyl group) beryllium doping YF
3, the structural formula of described two (3,7-dimethyl octyl group) beryllium is as shown in P1:
Described YF
3doping molar fraction be 25%, the thickness on described mixing barrier layer 402 is 210nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-3pa;
Alternately repeat to prepare inorganic barrier layer 401 and mix barrier layer 402 4 times respectively, form encapsulated layer 40, obtain organic electroluminescence device, the concrete structure of organic electroluminescence device provided by the invention can be expressed as ITO (100nm)/NPB:30wt%MoO
3(10nm)/TCTA (30nm)/TPBI:5wt% (Ir (ppy)
3) (20nm)/Bphen (10nm)/Bphen:30wt%CsN3/Al (100nm)/CuPc (250nm)/P1:30mol%YF
3(210nm)/CuPc (250nm)/P1:30mol%YF
3(210nm)/CuPc (250nm)/P1:30mol%YF
3(210nm)/CuPc (250nm)/P1:30mol%YF
3(210nm); Wherein, slash "/" represents layer structure, colon ": " represents doping, " wt% " represents mass percent, " mol% " represents mole percent, " NPB:30wt%MoO3 " represents that the mass fraction that MoO3 accounts for NPB is 30wt%, the mass fraction that " TPBI:5wt% (Ir (ppy) 3) " expression (Ir (ppy) 3) accounts for TPBI is 5wt%, " Bphen:30wt%CsN3 " represents that the mass fraction that CsN3 accounts for Bphen is 30wt%, P1 is two (3,7-dimethyl octyl group) beryllium that the embodiment of the present invention 1 adopts.Fig. 1 is the structural representation of the organic electroluminescence device that the embodiment of the present invention 1 obtains.Organic electroluminescence device as shown in Figure 1, comprise ito glass substrate 10, light emitting functional layer 20, cathode layer 30, encapsulated layer 40 successively, described encapsulated layer is that the stack combinations on inorganic barrier layer 401 and mixing barrier layer 402 repeats 4 times and forms, wherein, the thickness of described inorganic barrier layer 401 is 250nm, and the thickness on described mixing barrier layer 402 is 210nm.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 9.4 × 10
-4g/m
2day, the life-span is 2,500 hours.
Embodiment 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on anode substrate, light emitting functional layer and cathode layer is prepared
With embodiment one;
(2) on cathode layer, encapsulated layer is prepared
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, described in described inorganic barrier layer, the thickness of inorganic barrier layer is 250nm, and material is NPB, and the vacuum degree in described vacuum evaporation process is 5 × 10
-5pa, evaporation rate is
The making on (b) mixing barrier layer:
Adopt the mode of magnetron sputtering on described inorganic barrier layer, prepare mixing barrier layer, the material on described mixing barrier layer is two (3,7-dimethyl octyl group) beryllium doping YF
3, the structural formula of described two (3,7-dimethyl octyl group) beryllium as shown in the P1 in embodiment 1, described YF
3doping molar fraction be 25%, the thickness on described mixing barrier layer is 250nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-5pa;
Alternately repeat prepare inorganic barrier layer and mix barrier layer 6 times, form encapsulated layer, obtain organic electroluminescence device.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 8.4 × 10
-4g/m
2day, the life-span is 2,570 hours.
Embodiment 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on anode substrate, light emitting functional layer and cathode layer is prepared
With embodiment one;
(2) on cathode layer, encapsulated layer is prepared
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, described in described inorganic barrier layer, the thickness of inorganic barrier layer is 200nm, and material is Alq
3, the vacuum degree in described vacuum evaporation process is 5 × 10
-5pa, evaporation rate is
The making on (b) mixing barrier layer:
Adopt the mode of magnetron sputtering on described inorganic barrier layer, prepare mixing barrier layer, the material on described mixing barrier layer is two (3,7,11-trimethyldodecane base) beryllium doping ZrF
4, the structural formula of described two (3,7,11-trimethyldodecane base) beryllium is as shown in P3:
Described ZrF
4doping molar fraction be 20%, the thickness on described mixing barrier layer is 200nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-4pa;
Alternately repeat prepare inorganic barrier layer and mix barrier layer 6 times, form encapsulated layer, obtain organic electroluminescence device.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 8.9 × 10
-4g/m
2day, the life-span is 2,551 hours.
Embodiment 4
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on anode substrate, light emitting functional layer and cathode layer is prepared
With embodiment one;
(2) on cathode layer, encapsulated layer is prepared
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, described in described inorganic barrier layer, the thickness of inorganic barrier layer is 250nm, and material is m-MTDATA, and the vacuum degree in described vacuum evaporation process is 5 × 10
-5pa, evaporation rate is
The making on (b) mixing barrier layer:
Adopt the mode of magnetron sputtering on described inorganic barrier layer, prepare mixing barrier layer, the material on described mixing barrier layer is two (3,7,11,15-tetramethyl cetyl) beryllium Doped LiF, described two (3,7,11,15-tetramethyl cetyl) structural formula of beryllium is as shown in P4:
The doping molar fraction of described LiF is 25%, and the thickness on described mixing barrier layer is 250nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-4pa;
Alternately repeat prepare inorganic barrier layer and mix barrier layer 5 times, form encapsulated layer, obtain organic electroluminescence device.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 9.1 × 10
-4g/m
2day, the life-span is 2,526 hours.
Embodiment 5
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on anode substrate, light emitting functional layer and cathode layer is prepared
With embodiment one;
(2) on cathode layer, encapsulated layer is prepared
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, described in described inorganic barrier layer, the thickness of inorganic barrier layer is 250nm, and material is BCP, and the vacuum degree in described vacuum evaporation process is 5 × 10
-5pa, evaporation rate is
The making on (b) mixing barrier layer:
Adopt the mode of magnetron sputtering on described inorganic barrier layer, prepare mixing barrier layer, the material on described mixing barrier layer is two (3-methyl butyl) beryllium doped Ce F
2, the structural formula of described two (3-methyl butyl) beryllium is as shown in P4:
Described CeF
2doping molar fraction be 20%, the thickness on described mixing barrier layer is 220nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-4pa;
Alternately repeat prepare inorganic barrier layer and mix barrier layer 5 times, form encapsulated layer, obtain organic electroluminescence device.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 9.2 × 10
-4g/m
2day, the life-span is 2,515 hours.
Embodiment 6
A preparation method for organic electroluminescence device, comprises the following steps:
(1) on anode substrate, light emitting functional layer and cathode layer is prepared
With embodiment one;
(2) on cathode layer, encapsulated layer is prepared
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, described in described inorganic barrier layer, the thickness of inorganic barrier layer is 300nm, and material is CuPc, and the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa, evaporation rate is
The making on (b) mixing barrier layer:
Adopt the mode of magnetron sputtering on described inorganic barrier layer, prepare mixing barrier layer, the material on described mixing barrier layer is two (3-methyl butyl) beryllium doped with Al F
3, the structural formula of described two (3-methyl butyl) beryllium as shown in P5 in embodiment 5, described AlF
3doping molar fraction be 40%, the thickness on described mixing barrier layer is 300nm, and the background vacuum in described magnetron sputtering process is 1 × 10
-5pa;
Alternately repeat prepare inorganic barrier layer and mix barrier layer 6 times, form encapsulated layer, obtain organic electroluminescence device.
Be full of N
2in glove box, temperature is 20 ~ 25 DEG C, and water content and oxygen content be less than the condition of 1ppm under test the water resistance (WVTR) of the organic electroluminescence device after the present embodiment encapsulation, the water resistance of the organic electroluminescence device that result shows after the present embodiment encapsulation is 8.0 × 10
-4g/m
2day, the life-span is 2,587 hours.
To sum up, the preparation method of organic electroluminescence device provided by the invention can reduce steam and oxygen effectively to the erosion of organic electroluminescence device, improves the life-span of organic electroluminescence device significantly, and cathode layer can be protected to exempt from destruction.
Encapsulation rete compactness is most important, can select suitable process conditions according to device detection result.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, comprise the anode conducting substrate stacked gradually, light emitting functional layer, cathode layer and encapsulated layer, it is characterized in that, described encapsulated layer comprises inorganic barrier layer and the mixing barrier layer of lamination setting successively, the material of described inorganic barrier layer is CuPc, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, 4'-diamines, oxine aluminium, 4, 4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine or 4, 7-diphenyl-1, 10-Phen, the material on described mixing barrier layer is the composite material that glucinum alkyl BeR2 doping metals fluoride is formed, described metal fluoride is aluminum fluoride, tetrafluoride hafnium, zirconium fluoride, lithium fluoride, bifluoride cerium or yttrium fluoride, the structural formula of described glucinum alkyl BeR2 is as shown in P:
In formula, k is the natural number of 1 ~ 4.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, in the composite material that described glucinum alkyl BeR2 doping metals fluoride is formed, the doping molar fraction of described metal fluoride is 20 ~ 40%.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness of described inorganic barrier layer is 200nm ~ 300nm, and the thickness on described mixing barrier layer is 200nm ~ 300nm.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, described inorganic barrier layer and mixing barrier layer alternately repeat to arrange 4 ~ 6 times successively.
5. organic electroluminescence device as claimed in claim 1, it is characterized in that, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
(1) anode pattern preparing organic electroluminescence device on the electrically-conductive backing plate of cleaning forms anode conducting substrate; The method of vacuum evaporation is adopted to prepare light emitting functional layer and cathode layer on anode conducting substrate;
(2) on cathode layer, prepare encapsulated layer, preparation method is as follows:
The making of (a) inorganic barrier layer:
By the mode of vacuum evaporation at described cathode layer surface evaporation inorganic barrier layer, the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
The making on (b) mixing barrier layer:
On described inorganic barrier layer, mixing barrier layer is prepared by the method for magnetron sputtering, the material on described mixing barrier layer is the composite material that glucinum alkyl BeR2 doping metals fluoride is formed, described metal fluoride is aluminum fluoride, tetrafluoride hafnium, zirconium fluoride, lithium fluoride, bifluoride cerium or yttrium fluoride, and the structural formula of described glucinum alkyl BeR2 is as shown in P:
In formula, k is the natural number of 1 ~ 4, and the background vacuum in described magnetron sputtering process is 1 × 10
-5pa ~ 1 × 10
-3pa.
7. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, in the composite material that described glucinum alkyl BeR2 doping metals fluoride is formed, the doping molar fraction of described metal fluoride is 20 ~ 40%.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the thickness of described inorganic barrier layer is 200nm ~ 300nm, and the thickness on described mixing barrier layer is 200nm ~ 300nm.
9. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, described inorganic barrier layer and mixing barrier layer alternately repeat to arrange 4 ~ 6 times successively.
10. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
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Application publication date: 20150415 |