CN103904230A - Organic light-emitting device and preparation method - Google Patents
Organic light-emitting device and preparation method Download PDFInfo
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- CN103904230A CN103904230A CN201210570666.1A CN201210570666A CN103904230A CN 103904230 A CN103904230 A CN 103904230A CN 201210570666 A CN201210570666 A CN 201210570666A CN 103904230 A CN103904230 A CN 103904230A
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H—ELECTRICITY
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Abstract
The invention provides an organic light-emitting device which comprises an anode conductive substrate, a hole injection layer, a hole transporting layer, a luminescent layer, an electron transporting layer, an electron injection layer and a cathode which are successively stacked. The organic light-emitting device also contains a protective layer arranged on the surface of the cathode. The protective layer successively comprises an organic barrier layer, an inorganic barrier layer and a moisture absorption layer. The material of the inorganic barrier layer is metallic telluride which is one or more of Sb2Te3, Bi2Te, CdTe, In2Te3, SnTe and PbTe. The material of the moisture absorption layer is calcium oxide, barium oxide, strontium oxide or magnesium oxide. The invention also provides a preparation method of the organic light-emitting device. By the method, erosion of active materials such as steam, oxygen and the like to the organic light-emitting device can be effectively reduced, and service life of the organic light-emitting device is prolonged.
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 metallic cathode, to accompany multilayer organic material film (hole injection layer, hole transmission layer, luminescent layer, electron supplying layer and electron injecting layer), and when applying between electrode after certain voltage, 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 visual angle, low driving voltage and energy-conserving and environment-protective has been subject to extensive concern in fields such as panchromatic demonstration, backlight and illuminations, and has been considered to be most likely at the device of new generation that occupies dominance on following illumination and display device market.
At present, the problem that organic electroluminescence device average life is shorter, this is mainly 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.
In conventional art, adopt glass cover or crown cap to encapsulate, ultraviolet polymerization resin sealing for its edge, 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.
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.This organic electroluminescence device is provided with protective layer at cathode surface, can effectively reduce water, the erosion of oxygen isoreactivity material to device, thus the life-span of improving significantly organic electroluminescence device.Its preparation method technique is simple, and material is cheap and easy to get, is suitable for suitability for industrialized production.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise the anode conducting substrate stacking gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, also comprise the protective layer that is arranged on described cathode surface, described protective layer comprises organic barrier layer successively, inorganic barrier layer and moisture absorption layer, the material on described organic barrier layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4, 4 '-benzidine, 8-hydroxyquinoline aluminum, 4, 4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4, 7-diphenyl-1, 10-Phen, the material of described inorganic barrier layer is metal telluride, and described metal telluride is Sb
2te
3, Bi
2te, CdTe, In
2te
3, one or more in SnTe and PbTe, the material of described moisture absorption layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide.
The effect of each functional layer is respectively anode conducting substrate (substrate and anode conducting effect), hole injection layer (injected hole, being conducive to hole is injected into transferring material from anode), hole transmission layer (transporting holes, be conducive to hole transport in luminescent material), (electronics and hole are compound in this layer for luminescent layer, then energy is transferred to light emitting molecule luminous), electron transfer layer (transmission electronic, be conducive to electric transmission in luminescent material), electron injecting layer (injects electronics, being conducive to electronics is injected into transferring material from anode), negative electrode (power supply electronics is provided for device), the protective layer (protection negative electrode and organic layer) of cathode surface.
Preferably, the thickness on described organic barrier layer is 200 ~ 300nm.
Organic barrier layer material CuPc (CuPc), N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine (NPB), 8-hydroxyquinoline aluminum (Alq
3), 4, " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine (m-MTDATA) or 4,7-diphenyl-1,10-Phen (BCP) can be deposited on metallic cathode surface by the mode of vacuum evaporation for 4', 4.The existence on organic barrier layer can protect each functional layer and negative electrode to exempt from destruction in subsequent operation process.
The material of described inorganic barrier layer is metal telluride, and described metal telluride is Sb
2te
3, Bi
2te, CdTe, In
2te
3, one or more in SnTe and PbTe.The inorganic barrier layer compactness being prepared into tellurides is high, and the ability of the anti-oxygen of waterproof is strong, can effectively stop outside steam, the erosion of oxygen to device inside, extends the useful life of device.
Preferably, the thickness of inorganic barrier layer is 100 ~ 200nm.
Preferably, the material of described moisture absorption layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide.Preferably, the thickness of described moisture absorption layer is 100 ~ 200nm.Calcium oxide (CaO), barium monoxide (BaO), strontium oxide strontia (SrO) and magnesium oxide (MgO) are high-hydroscopicity material, thereby can effectively absorb the steam of invasion device, reduce the destruction that steam produces device.
Preferably, anode conducting substrate comprises anode conductive layer and substrate, its substrate can be glass substrate or organic film substrate, the material of anode conductive layer can be conductive oxide, as, tin indium oxide (ITO), Al-Doped ZnO (AZO), mix indium zinc oxide (IZO) or mix fluorine zinc oxide (FTO), these conductive oxides are prepared on glass substrate, are called for short ito glass, AZO glass, IZO glass, FTO glass.Anode conducting substrate can be made by oneself, also can commercially obtain.In actual applications, can select as required other suitable materials as anode conducting substrate.In actual applications, can on anode conducting substrate, prepare the anode pattern of required organic electroluminescence device.Anode conducting substrate is prior art, does not repeat them here.
Preferably, the material of described hole injection layer is MoO
3the adulterate N of 30% mass fraction, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the composite material that 4'-diamines (NPB) forms; The material of described hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA); The material of described luminescent layer is that three (2-phenylpyridines) of 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) doping, 5% mass fraction close iridium (Ir (ppy)
3) form composite material; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen); The material of described electron injecting layer is 4,7-diphenyl-1, the CsN of 10-phenanthroline (Bphen) doping 30% mass fraction
3the composite material forming.
Negative electrode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), can be also transparent cathode (dielectric layer/metal level/dielectric layer structure that dielectric layer tramp metal layer forms etc.).
Preferably; described organic electroluminescence device also comprises the heat dissipating layer and the cap that are arranged on described protective layer; described cap and described anode conducting substrate form enclosure space, and described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode, protective layer and heat dissipating layer are contained in described enclosure space.
Preferably, the material of described heat dissipating layer is one or more combinations in metallic aluminium, silver and copper.Preferably, the thickness of described heat dissipating layer is 200 ~ 500nm.Because device is accompanied by the generation of amount of heat in the course of the work, heat dissipating layer metal has good heat conductivility, the heat that can rapidly device be produced in luminescence process from device inside conduction in time out, thereby effectively prevent device over-heat inside and cause the situation that the life-span reduces, improve useful life of device.
Cap is set, forms enclosure space with anode conducting substrate, can form protection to organic electroluminescence device better.Wherein, described cap is tinsel or contains aluminium high temperature resistance polyester film (being abbreviated as the film containing aluminium PET).Preferably, described cap is tinsel.Using tinsel as cap, can improve the heat-sinking capability of organic electroluminescence device, encapsulation is dropped to minimum on the impact of light efficiency.
Anode conducting substrate and cap can form enclosure space under the adhesive effect of UV glue.Preferably, UV glue is epoxy resin.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) provide clean anode electrically-conductive backing plate, on anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared in vacuum evaporation successively;
(2) on described negative electrode, prepare protective layer, obtain organic electroluminescence device; Wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, concrete preparation method is as follows: the mode by vacuum evaporation is prepared organic barrier layer at described cathode surface evaporation, then adopts magnetron sputtering method to prepare successively inorganic barrier layer and moisture absorption layer at described organic barrier layer surface;
The material on described organic barrier layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, 4,4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4; 7-diphenyl-1,10-Phen; The material of described inorganic barrier layer is metal telluride, and described metal telluride is Sb
2te
3, Bi
2te, CdTe, In
2te
3, one or more in SnTe and PbTe; The material of described moisture absorption layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide.
Described organic barrier layer adopts the mode of vacuum evaporation to prepare at cathode surface.Preferably, the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa~1 × 10
-3pa, evaporation rate is
Preferably, the thickness on described organic barrier layer is 200 ~ 300nm.The existence on organic barrier layer can protect each functional layer and negative electrode to exempt from destruction in subsequent operation process.
Described inorganic barrier layer adopts magnetron sputtering method to prepare at organic barrier layer surface.Preferably, the base vacuum degree in described magnetron sputtering process is 1 × 10
-4pa~1 × 10
-3pa.Preferably, the thickness of inorganic barrier layer is 100 ~ 200nm.The inorganic barrier layer compactness being prepared into tellurides is high, and the ability of the anti-oxygen of waterproof is strong, can effectively stop outside steam, the erosion of oxygen to device inside, extends the useful life of device.
Described moisture absorption layer adopts magnetron sputtering method to prepare on inorganic barrier layer surface.Preferably, the base vacuum degree in described magnetron sputtering process is 1 × 10
-4pa~1 × 10
-3pa.Preferably, the thickness of described moisture absorption layer is 100 ~ 200nm.Calcium oxide, barium monoxide, strontium oxide strontia and magnesium oxide are high-hydroscopicity material, thereby can effectively absorb the steam of invasion device, reduce the destruction that steam produces device.
Preferably, anode conducting substrate comprises anode conductive layer and substrate, its substrate can be glass substrate or organic film substrate, the material of anode conductive layer can be conductive oxide, as, tin indium oxide (ITO), Al-Doped ZnO (AZO), mix indium zinc oxide (IZO) or mix fluorine zinc oxide (FTO), these conductive oxides are prepared on glass substrate, are called for short ito glass, AZO glass, IZO glass, FTO glass.Anode conducting substrate can be made by oneself, also can commercially obtain.In actual applications, can select as required other suitable materials as anode conducting substrate.In actual applications, can on anode conducting substrate, prepare the anode pattern of required organic electroluminescence device.Anode conducting substrate is prior art, does not repeat them here.
Described anode substrate carries out following clean operation conventionally: carry out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol and clean, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dries up with nitrogen, and stove-drying is stand-by; Again the substrate 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.
Preferably, the material of described hole injection layer is MoO
3the adulterate N of 30% mass fraction, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the composite material that 4'-diamines (NPB) forms; The material of described hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA); The material of described luminescent layer is that three (2-phenylpyridines) of 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) doping, 5% mass fraction close iridium (Ir (ppy)
3) form composite material; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen); The material of described electron injecting layer is 4,7-diphenyl-1, the CsN of 10-phenanthroline (Bphen) doping 30% mass fraction
3the composite material forming.
Negative electrode can be non-transparent metals negative electrode (aluminium, silver, gold etc.), can be also transparent cathode (dielectric layer/metal level/dielectric layer structure that dielectric layer tramp metal layer forms etc.).
Described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared by vacuum evaporation.Preferably, the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa~1 × 10
-3pa, evaporation rate is
Preferably, described preparation method further comprises: prepare heat dissipating layer at described moisture absorption layer surface vacuum evaporation; At described heat dissipating layer surface coverage cap; at described cap edge-coating UV glue; by the described UV glue of the dry sclerosis of mode of ultraviolet curing; sealing forms enclosure space; described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode, protective layer and heat dissipating layer are contained in described enclosure space, obtain the organic electroluminescence device of sealing.
Described heat dissipating layer adopts the mode of vacuum evaporation to prepare on moisture absorption layer surface.Preferably, the vacuum degree in described vacuum evaporation process is 1 × 10
-5pa~1 × 10
-3pa, evaporation rate is
preferably, the material of described heat dissipating layer is one or more combinations in metallic aluminium, silver and copper.Preferably, the thickness of described heat dissipating layer is 200 ~ 500nm.Because device is accompanied by the generation of amount of heat in the course of the work, heat dissipating layer metal has good heat conductivility, the heat that can rapidly device be produced in luminescence process from device inside conduction in time out, thereby effectively prevent device over-heat inside and cause the situation that the life-span reduces, improve useful life of device.
Wherein, described cap is tinsel or contains aluminium high temperature resistance polyester film (being abbreviated as the film containing aluminium PET).Preferably, described cap is tinsel.Using tinsel as cap, can improve the heat-sinking capability of organic electroluminescence device, encapsulation is dropped to minimum on the impact of light efficiency.
Anode conducting substrate and cap can form enclosure space under the adhesive effect of UV glue.Preferably, UV glue is epoxy resin.
Preferably, the light intensity of UV light is 15~25mW/cm
2, the time for exposure is 300~400s.
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, by protective layer being set at cathode surface, has greatly reduced steam, the erosion of oxygen to organic electroluminescence device, improves the life-span of organic electroluminescence device;
(2) preparation method of the present invention is applicable to the organic electroluminescence device of preparation take electro-conductive glass as anode substrate, is also applicable to the flexible organic electroluminescent device of preparation take plastics or metal as anode substrate; And preparation method's technique is simple, 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 that makes of the embodiment of the present invention 1.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on the embodiment in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein:
The material of hole injection layer is MoO
3adulterate 30% mass fraction NPB form composite material (be expressed as MoO
3-NPB), vacuum degree when evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 10nm;
The material of hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamine (TCTA), the vacuum degrees 3 × 10 when evaporation
-5pa, evaporation rate is
evaporation thickness is 30nm;
The material of luminescent layer comprises material of main part and guest materials.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (being expressed as TPBI), and guest materials is that three (2-phenylpyridines) close iridium and (are expressed as Ir (ppy)
3), and the doping mass fraction of guest materials is 5%; Vacuum degree when vacuum evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), the vacuum degree 3 × 10 when vacuum evaporation
-5pa, evaporation rate is
evaporation thickness is 10nm;
The material of electron injecting layer is 4,7-diphenyl-1, the CsN of 10-phenanthroline (Bphen) doping 30% mass fraction
3the composite material forming, vacuum degree when vacuum evaporation is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
The material of metallic cathode is metallic aluminium (Al), and evaporation thickness is 100nm, and vacuum degree when vacuum evaporation is 3 × 10
-5pa, evaporation rate is
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the CuPc film of 300nm as organic barrier layer, vacuum degree control is 1 × 10
-5pa, evaporation rate is
On CuPc film surface, adopt magnetron sputtering method to prepare the Sb that a layer thickness is 100nm
2te
3layer is as inorganic barrier layer, and base vacuum degree is 1 × 10
-4pa;
Adopt again magnetron sputtering method at Sb
2te
3the CaO layer that preparation a layer thickness in layer surface is 100nm is as moisture absorption layer, and base vacuum degree is 1 × 10
-4pa.
For better protection device construction, improve the anti-oxygen performance of waterproof, carry out following further operation:
(4) CaO layer surface evaporation prepare a layer thickness be the metal aluminium lamination of 200nm as heat dissipating layer, vacuum degree control is 1 × 10
-5pa, evaporation rate is
(5) on metal aluminium lamination, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 20mW/cm with UV light (λ=365nm)
2, time for exposure 350s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
Adopt water vapour permeability tester to measure the water vapour permeability of this organic electroluminescence device, record water vapour permeability (WVTR, the g/m of this organic electroluminescence device
2day) be 3.6 × 10
-4, at T70@1000cd/m
2luminescent condition under test this organic electroluminescence device life-span be 9001 hours.
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, comprises ito glass substrate 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, metallic cathode 7, protective layer 8, heat dissipating layer 9 and cap 10 successively.Ito glass substrate 1 and cap 10 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, metallic cathode 7, protective layer 8 and heat dissipating layer 9 are contained in this enclosure space.Described protective layer 8 comprises that a layer thickness is organic barrier layer CuPc film 81 of 300nm successively, the Sb that a layer thickness is 100nm
2te
3the CaO moisture absorption layer 83 that organic barrier layer 82 and a layer thickness are 100nm.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/CuPc/Sb
2te
3/ CaO/Al/ tinsel.
Embodiment 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the NPB film of 250nm as organic barrier layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
On NPB film surface, adopt magnetron sputtering method to prepare the Bi that a layer thickness is 120nm
2te layer is as inorganic barrier layer, and base vacuum degree is 5 × 10
-4pa;
Adopt again magnetron sputtering method at Bi
2the BaO layer that preparation a layer thickness in Te layer surface is 200nm is as moisture absorption layer, and base vacuum degree is 5 × 10
-4pa;
(4) BaO layer surface evaporation prepare a layer thickness be the metallic silver layer of 500nm as heat dissipating layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
(5) in metallic silver layer, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 25mW/cm with UV light (λ=365nm)
2, time for exposure 400s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/NPB/Bi
2te/BaO/Ag/ tinsel.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 1.9 × 10
-4, at T70@1000cd/m
2luminescent condition under life-span of testing be 9112 hours.
Embodiment 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation prepares at cathode surface the Alq that a layer thickness is 200nm
3film is as organic barrier layer, and vacuum degree control is 5 × 10
-5pa, evaporation rate is
At Alq
3on film surface, adopt magnetron sputtering method prepare a layer thickness be the CdTe layer of 200nm as inorganic barrier layer, base vacuum degree is 5 × 10
-4pa;
Adopt SrO layer that magnetron sputtering method is 150nm in CdTe layer surface preparation a layer thickness as moisture absorption layer, base vacuum degree is 5 × 10 again
-4pa;
(3) SrO layer surface evaporation prepare a layer thickness be the metal copper layer of 300nm as heat dissipating layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
(5) in metal copper layer, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 300s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/Alq
3/ CdTe/SrO/Cu tinsel.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 1.2 × 10
-4, at T70@1000cd/m
2luminescent condition under life-span of testing be 9338 hours.
Embodiment 4
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the m-MTDATA film of 250nm as organic barrier layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
On m-MTDATA film surface, adopt magnetron sputtering method to prepare the In that a layer thickness is 100nm
2te
3layer is as inorganic barrier layer, and base vacuum degree is 2 × 10
-4pa;
Adopt again magnetron sputtering method at In
2te
3the MgO layer that preparation a layer thickness in layer surface is 100nm is as moisture absorption layer, and base vacuum degree is 5 × 10
-4pa;
(4) prepare metallic copper that a layer thickness is 500nm, aluminium alloy layer as heat dissipating layer at MgO layer surface evaporation, the mass ratio of copper and aluminium is 3:1, and vacuum degree control is 5 × 10
-5pa, evaporation rate is
(5) on metallic copper, aluminium alloy layer, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 20mW/cm with UV light (λ=365nm)
2, time for exposure 350s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/m-MTDATA/In
2te
3/ MgO/Cu-Al/ tinsel.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 2.2 × 10
-4, at T70@1000cd/m
2luminescent condition under life-span of testing be 9093 hours.
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the BCP film of 250nm as organic barrier layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
On BCP film surface, adopt magnetron sputtering method prepare a layer thickness be the SnTe layer of 150nm as inorganic barrier layer, base vacuum degree is 2 × 10
-4pa;
Adopt CaO layer that magnetron sputtering method is 200nm in SnTe layer surface preparation a layer thickness as moisture absorption layer, base vacuum degree is 5 × 10 again
-4pa;
(4) CaO layer surface evaporation prepare a layer thickness be the metal aluminium lamination of 300nm as heat dissipating layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
(5) on metal aluminium lamination, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 20mW/cm with UV light (λ=365nm)
2, time for exposure 340s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/BCP/SnTe/CaO/Al/ tinsel.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 3.1 × 10
-4, at T70@1000cd/m
2luminescent condition under life-span of testing be 9022 hours.
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the CuPc film of 250nm as organic barrier layer, vacuum degree control is 1 × 10
-3pa, evaporation rate is
On CuPc film surface, adopt magnetron sputtering method prepare a layer thickness be the PbTe layer of 120nm as inorganic barrier layer, base vacuum degree is 1 × 10
-3pa;
Adopt BaO layer that magnetron sputtering method is 150nm in PbTe layer surface preparation a layer thickness as moisture absorption layer, base vacuum degree is 1 × 10 again
-3pa;
(4) BaO layer surface evaporation prepare a layer thickness be the metallic silver layer of 300nm as heat dissipating layer, vacuum degree control is 5 × 10
-5pa, evaporation rate is
(5) in metallic silver layer, cover a tinsel as cap, at tinsel edge-coating UV glue, UV glue is epoxy resin, and coating thickness is 10 μ m, is cured light intensity 18mW/cm with UV light (λ=365nm)
2, time for exposure 360s, sealing forms enclosure space, and hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, aluminium negative electrode, protective layer and heat dissipating layer are contained in this enclosure space, forms and is sealed with organic electroluminescence devices.
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/CuPc/PbTe/BaO/Ag/ tinsel.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 1.5 × 10
-4, at T70@1000cd/m
2luminescent condition under life-span of testing be 9203 hours.
A preparation method for organic electroluminescence device, comprises the following steps:
(1) get ito glass substrate, carrying out successively acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all clean with supersonic wave cleaning machine, individual event washing is cleaned 5 minutes, then dry up with nitrogen, stove-drying is stand-by, then the ito glass substrate after cleaning is carried out to 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;
(2) mode that adopts vacuum evaporation is prepared successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode on clean dry and ito glass substrate after surface activation process, wherein, specifically prepare with embodiment 1;
(3) on described negative electrode, prepare protective layer, obtain organic electroluminescence device, wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, and concrete preparation method is as follows:
Mode by vacuum evaporation cathode surface prepare a layer thickness be the CuPc film of 250nm as organic barrier layer, vacuum degree control is 1 × 10
-3pa, evaporation rate is
On CuPc film surface, adopt magnetron sputtering method prepare a layer thickness be the PbTe layer of 120nm as inorganic barrier layer, base vacuum degree is 1 × 10
-3pa;
Adopt BaO layer that magnetron sputtering method is 150nm in PbTe layer surface preparation a layer thickness as moisture absorption layer, base vacuum degree is 1 × 10 again
-3pa;
The structure of organic electroluminescence device prepared by the present embodiment is:
Ito glass substrate/(MoO
3-NPB)/TCTA/ (TPBI-Ir (ppy)
3)/Bphen/ (Bphen-CsN
3)/Al/CuPc/PbTe/BaO.
Water vapour permeability (WVTR, the g/m of organic electroluminescence device prepared by the present embodiment
2day) be 2.1 × 10
-1, at T70@1000cd/m
2luminescent condition under life-span of testing be 1546 hours.
To sum up; the preparation method of the organic electroluminescence device that the embodiment of the present invention provides, can reduce steam and the erosion of oxygen to organic electroluminescence device effectively, and heat is evacuated in heat conduction in time; improve significantly the life-span of organic electroluminescence device, and can protect negative electrode to exempt from destruction.
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 stacking gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, it is characterized in that, also comprise the protective layer that is arranged on described cathode surface, described protective layer comprises organic barrier layer successively, inorganic barrier layer and moisture absorption layer, the material on described organic barrier layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4, 4 '-benzidine, 8-hydroxyquinoline aluminum, 4, 4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4, 7-diphenyl-1, 10-Phen, the material of described inorganic barrier layer is metal telluride, and described metal telluride is Sb
2te
3, Bi
2te, CdTe, In
2te
3, one or more in SnTe and PbTe, the material of described moisture absorption layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide.
2. organic electroluminescence device as claimed in claim 1; it is characterized in that; also comprise the heat dissipating layer and the cap that are arranged on described protective layer; described cap and described anode conducting substrate form enclosure space, and described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode, protective layer and heat dissipating layer are contained in described enclosure space.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness on described organic barrier layer is 200 ~ 300nm; The thickness of described inorganic barrier layer is 100 ~ 200nm; The thickness of described moisture absorption layer is 100 ~ 200nm.
4. organic electroluminescence device as claimed in claim 2, is characterized in that, the material of described heat dissipating layer is one or more combinations in metallic aluminium, silver and copper, and the thickness of described heat dissipating layer is 200 ~ 500nm.
5. organic electroluminescence device as claimed in claim 1 or 2, is characterized in that, the material of described hole injection layer is MoO
3the adulterate N of 30% mass fraction, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the composite material that 4'-diamines forms; The material of described hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines; The material of described luminescent layer is that adulterate three (2-phenylpyridines) of 5% mass fraction of 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene close the composite material that iridium forms; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline; The material of described electron injecting layer is 4,7-diphenyl-1, the CsN of 10-phenanthroline (Bphen) doping 30% mass fraction
3the composite material forming.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
(1) provide clean anode electrically-conductive backing plate, on anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode are prepared in vacuum evaporation successively;
(2) on described negative electrode, prepare protective layer, obtain organic electroluminescence device; Wherein, described protective layer comprises organic barrier layer, inorganic barrier layer and moisture absorption layer, concrete preparation method is as follows: the mode by vacuum evaporation is prepared organic barrier layer at described cathode surface evaporation, then adopts magnetron sputtering method to prepare successively inorganic barrier layer and moisture absorption layer at described organic barrier layer surface;
The material on described organic barrier layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, 4,4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4; 7-diphenyl-1,10-Phen; The material of described inorganic barrier layer is metal telluride, and described metal telluride is Sb
2te
3, Bi
2te, CdTe, In
2te
3, one or more in SnTe and PbTe; The material of described moisture absorption layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide.
7. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, described preparation method further comprises: prepare heat dissipating layer at described moisture absorption layer surface vacuum evaporation; At described heat dissipating layer surface coverage cap; at described cap edge-coating UV glue; by the described UV glue of the dry sclerosis of mode of ultraviolet curing; sealing forms enclosure space; described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, negative electrode, protective layer and heat dissipating layer are contained in described enclosure space, obtain the organic electroluminescence device of sealing.
8. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, the thickness on described organic barrier layer is 200 ~ 300nm; The thickness of described inorganic barrier layer is 100 ~ 200nm; The thickness of described moisture absorption layer is 100 ~ 200nm.
9. the preparation method of organic electroluminescence device as claimed in claim 7, is characterized in that, the material of described heat dissipating layer is one or more combinations in metallic aluminium, silver and copper, and the thickness of described heat dissipating layer is 200 ~ 500nm.
10. the preparation method of the organic electroluminescence device as described in claim 6 or 7, is characterized in that, the material of described hole injection layer is MoO
3the adulterate N of 30% mass fraction, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the composite material that 4'-diamines forms; The material of described hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines; The material of described luminescent layer is that adulterate three (2-phenylpyridines) of 5% mass fraction of 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene close the composite material that iridium forms; The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline; The material of described electron injecting layer is 4,7-diphenyl-1, the CsN of 10-phenanthroline (Bphen) doping 30% mass fraction
3the composite material forming.
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