CN103855308B - A kind of organic electroluminescence device and preparation method thereof - Google Patents
A kind of organic electroluminescence device and preparation method thereof Download PDFInfo
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- CN103855308B CN103855308B CN201210501432.1A CN201210501432A CN103855308B CN 103855308 B CN103855308 B CN 103855308B CN 201210501432 A CN201210501432 A CN 201210501432A CN 103855308 B CN103855308 B CN 103855308B
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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
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/841—Self-supporting sealing arrangements
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
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- H—ELECTRICITY
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- H10K50/00—Organic light-emitting devices
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- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K50/00—Organic light-emitting devices
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- H—ELECTRICITY
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- H—ELECTRICITY
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Abstract
The invention provides a kind of organic electroluminescence device, comprise the substrate, anode, functional layer, negative electrode, encapsulated layer and the cap that stack gradually, substrate and cap form enclosure space, anode, functional layer, negative electrode and encapsulated layer are contained in this enclosure space, and described encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer successively; Described sulfur-nitrogen compound film is the nitride film doped with sulfide; present invention also offers the preparation method of this organic electroluminescence device; the method can reduce steam, oxygen effectively to the erosion of organic electroluminescence device; thus effective protection is formed to device organic functional material and electrode, the life-span of organic electroluminescence device can be improved significantly.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device.
Description
Technical field
The present invention relates to electronic device association area, particularly relate 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 preparing tens nanometer thickness on ito glass makes luminescent layer, has the metal electrode of low work function above luminescent layer.When electrode being added with voltage, luminescent layer just produces light radiation.
OLED have active illuminating, luminous efficiency high, low in energy consumption, light, thin, without advantages such as angle limitations, thought by insider to be most likely at the device of new generation following illumination and display device market occupying dominance.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, achieves huge achievement.More and more throw light on due to the whole world and show producer and drop into research and development one after another, promoted the industrialization process of OLED greatly, make the growth rate of OLED industry surprising, reached the eve of scale of mass production at present.
Glass cover or crown cap is adopted to encapsulate in conventional art, its edge ultraviolet polymerization resin seal, but the glass cover used in this method or crown cap volume are often comparatively large, add the weight of device, and the method can not be applied to flexible organic electroluminescence gives out light the encapsulation of device.
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 can reduce steam, oxygen isoreactivity material effectively to the erosion of organic electroluminescence device, and organic functional material and the electrode of protection organic electroluminescence device exempt from destruction, increase significantly to the life-span of device.The inventive method is applicable to encapsulate the organic electroluminescence device prepared with conducting glass 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 substrate, anode, functional layer, negative electrode, encapsulated layer and the cap that stack gradually, substrate and cap form enclosure space, anode, functional layer, negative electrode, encapsulated layer are contained in this enclosure space, and described encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer successively;
Described sulfur-nitrogen compound film is the nitride film doped with sulfide, wherein, described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment, described nitride material is silicon nitride, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, and the mass ratio of described sulfide and described nitride is 1:5 ~ 15:19.
Preferably, the thickness of described sulfur-nitrogen compound film is 100nm ~ 150nm.
Preferably, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm;
The material of described inorganic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin, and the thickness of described inorganic barrier layer is 1 μm ~ 1.5 μm.
Preferably, the material of described moist absorbing layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and the thickness of described moist absorbing layer is 100nm ~ 200nm;
The material of described heat dissipating layer is aluminium, silver, copper or their composition, and thickness is 200nm ~ 500nm; And
Described cap is sheet metal, and the material of sheet metal is silver, aluminium or copper.
Preferably, described sulfur-nitrogen compound film and the alternately laminated setting of described inorganic barrier layer, the stacked number of plies is more than or equal to three layers.
The present invention provides a kind of preparation method of organic electroluminescence device on the other hand, comprises the following steps:
The glass substrate or organic film substrate of cleaning are prepared the anode of organic electroluminescence device; Adopt the method for vacuum evaporation to prepare functional layer, negative electrode and encapsulated layer successively on anode conducting substrate, adopt ultraviolet light polymerization mode to be encapsulated by cap, make described substrate and described cap form enclosure space;
The preparation of described encapsulated layer comprises on negative electrode, first adopts the mode of vacuum evaporation to prepare described protective layer;
Described protective layer adopt magnetron sputtering spatter the described sulfur-nitrogen compound film of preparation altogether; wherein; described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; described nitride material is silicon nitride, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride; described magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 1 × 10
-5pa ~ 1 × 10
-3pa, thicknesses of layers is set to 100nm ~ 150nm, using the mass ratio of described sulfide and described nitride be 1:5 ~ 15:19 as target, under sputter rate be 5nm/min ~ 40nm/min condition, carry out magnetron sputtering obtain sulfur-nitrogen compound film;
Then on described sulfur-nitrogen compound film, adopt the technique of first spin coating post-exposure to prepare described inorganic barrier layer, the technical process of described first spin coating post-exposure is, by the spin coating of described Organic barrier layer material, be then 200nm ~ 400nm ultraviolet light polymerization with wavelength, light intensity is 10mW/cm
2~ 15mW/cm
2, time for exposure 200s ~ 300s;
Then on described inorganic barrier layer, sputtering mode is adopted to prepare described moist absorbing layer, fin described in vacuum evaporation on described moist absorbing layer;
Finally adopt packaging plastic that sheet metal encapsulation is formed cap, make described substrate and described cap form confined space, described anode, functional layer, negative electrode and encapsulated layer are contained in this enclosure space.
Preferably, the thickness of described sulfur-nitrogen compound film is 100nm ~ 150nm.
Preferably, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm;
The material of described organic barrier is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin, and the thickness of described organic barrier is 1 μm ~ 1.5 μm.
Preferably, the material of described moist absorbing layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and the thickness of described moist absorbing layer is 100nm ~ 200nm.
Preferably, the material of described heat dissipating layer is aluminium, silver, copper or their composition, and the thickness of described heat dissipating layer is 200nm ~ 500nm.
Preferably, described cap is sheet metal, and the material of sheet metal is silver, aluminium or copper.
Preferably, repeat the preparation technology preparing described sulfur-nitrogen compound film and inorganic barrier layer, make described sulfur-nitrogen compound film and the stacked setting of inorganic barrier layer, the alternately laminated number of plies is for being more than or equal to three layers.
The invention provides a kind of organic electroluminescence device and preparation method thereof and there is following beneficial effect:
Organic electroluminescence device of the present invention can reduce outside water effectively, oxygen isoreactivity material to the erosion of organic electroluminescence device, thus forms effective protection to device organic functional material and electrode, improves the life-span of organic electroluminescence device significantly; Water resistance (WVTR) is made to reach 6.3E
-5g/m
2day, the life-span reaches 10, more than 013 hour, and organic electroluminescence device material of the present invention is cheap, and method for packing 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 organic electroluminescence device of the present invention;
Fig. 2 is the preparation flow figure of organic electroluminescence device of the present invention;
Fig. 3 is the preparation flow figure of the encapsulated layer of organic electroluminescence device of the present invention.
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 improve and adjustment is also considered as in protection scope of the present invention.
A kind of organic electroluminescence device 100 is the invention provides according to Fig. 1, comprise the substrate 10, anode 20, functional layer 30, negative electrode 40, encapsulated layer 50 and the cap 60 that stack gradually, substrate 10 and cap 60 form enclosure space, anode 20, functional layer 30, negative electrode 40 and encapsulated layer 50 are encapsulated in this space.
In the present embodiment, substrate 10 is glass substrate or organic film, and this organic film is specially: polyethylene terephthalate;
In the present embodiment, arrange anode 20 on the substrate 10, anode 20 is indium tin oxide;
In the present embodiment, functional layer 30 is formed at anode 20 surface.Functional layer 30 comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer that stack gradually.Be appreciated that hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, now functional layer 30 only comprises luminescent layer;
Molybdenum oxide (the MoO that hole injection layer is N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and is entrained in NPB
3).MoO
3mass percentage be 30%.The thickness of hole injection layer is 10nm;
Hole transmission layer is 4,4', 4 "-three (carbazole-9-base) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.
Emitting layer material comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3).CsN
3mass percentage be 30%.The thickness of electron injecting layer is 20nm.
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.
In the present embodiment, functional layer 30 arranges negative electrode 40, negative electrode 40 can be single metal layer, and this single-layer metal is aluminium, silver and golden; Also can be laminating transparent negative electrode, this transparent cathode be ITO/Ag/ITO or ZnS/Ag/ZnS.
In the present embodiment, negative electrode 40 arranges encapsulated layer 50, this encapsulated layer 50 comprises protective layer 501, sulfur-nitrogen compound film 502, inorganic barrier layer 503, moist absorbing layer 504 and heat dissipating layer 505.
Protective layer 501, the material of protective layer 501 is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm.
In the present embodiment; protective layer 501 arranges sulfur-nitrogen compound film 502; sulfur-nitrogen compound film 502 is the nitride film doped with sulfide; wherein; described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; described nitride material is silicon nitride, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, and the mass ratio of described sulfide and described nitride is 1:5 ~ 15:19;
In the present embodiment, the thickness of sulfur-nitrogen compound film 502 is 100nm ~ 150nm.
In the present embodiment, arrange inorganic barrier layer 503 on sulfur-nitrogen compound film 502 surface, the material of inorganic barrier layer 503 is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin, and thickness is 1 ~ 1.5 μm.
In the present embodiment, described sulfur-nitrogen compound film 502 and the alternately laminated setting of inorganic barrier layer 503, the alternately laminated number of plies is for being more than or equal to 3 layers.
Sulfur-nitrogen compound film and the alternately laminated setting of inorganic barrier layer can be extended water Oxygen permeation path, be arranged alternately and can make up hole, organic substance and inorganic matter be combined thus can relieve stresses.
In the present embodiment, arrange moist absorbing layer 504 on inorganic barrier layer 503 surface, the material of moist absorbing layer 504 is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and thickness is 100nm ~ 200nm.
In the present embodiment, arrange heat dissipating layer 505 on moist absorbing layer 504 surface, the material of heat dissipating layer 505 is aluminium, silver, copper or their composition, and thickness is 200nm ~ 500nm.
In the present embodiment, adopt cap 60 to encapsulate with substrate 10 for boundary, make to form confined space between substrate 10 and cap 60, above-mentioned each layer is arranged in this confined space, described cap 60 is sheet metal, and sheet metal comprises silver, aluminium or copper foil.
According to the preparation method of the known organic electroluminescence device 100 provided by the invention of Fig. 2, concrete steps comprise:
S101 prepares anode 20 on the substrate 10, and forms functional layer 30 on anode 20.
Functional layer 30 comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer that stack gradually.
Substrate 10 can be substrate of glass or organic PETG (PET) film substrate.Substrate 10 has preparation and has anode 20, and anode 20 is ITO layer.The thickness of ITO layer is 100nm ~ 150nm.
Substrate 10 surface formation anode 20 and functional layer 30 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase substrate 10 surface oxygen content to improve the work function on substrate 10 surface.Be specially, substrate 10 adopted successively and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB
3).MoO
3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 "-three (carbazole-9-base) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.Hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, and now functional layer 20 only comprises luminescent layer.
Step S120, functional layer 30 surface formed negative electrode 40.
Negative electrode 30 can be single layer structure.The thickness of negative electrode 30 is 100nm.The material of negative electrode 30 is aluminium (Al), silver (Ag) or gold (Au), and negative electrode 30 is formed by vacuum evaporation, and vacuum degree is 5 × 10
-5pa, evaporation rate is
also can be laminating transparent negative electrode, this transparent cathode be ITO/Ag/ITO or ZnS/Ag/ZnS.
Step S130, on negative electrode 40 evaporation formed encapsulated layer.
According to Fig. 3, the preparation process of encapsulated layer is as follows:
Encapsulated layer comprises protective layer 501, sulfur-nitrogen compound film 502, inorganic barrier layer 503, moist absorbing layer 504 and heat dissipating layer 505 successively.
Step S1301, on negative electrode 40 evaporation formed protective layer 501; the material of protective layer 501 is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4; 4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm.Evaporation condition is, vacuum degree is 8 × 10
-5pa ~ 3 × 10
-5pa, evaporation rate is
Step S1302, on protective layer 502, magnetron sputtering is adopted to make sulfur-nitrogen compound film 502; sulfur-nitrogen compound film 502 is the nitride film doped with sulfide; wherein; described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; described nitride material is silicon nitride, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, and the mass ratio of described sulfide and described nitride is 1:5 ~ 15:19.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 1 × 10
-5pa ~ 1 × 10
-3pa, thicknesses of layers is set to 100nm ~ 150nm, using the mass ratio of sulfide and nitride be 1:5 ~ 15:19 as target, be that 5nm/min ~ 40nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film 502 at sputter rate.
Step S1303, at sulfur-nitrogen compound film 502 spin coating inorganic barrier layer 503, then adopt ultraviolet light polymerization under an inert atmosphere, ultraviolet light polymerization condition is wavelength 200nm ~ 400nm, light intensity 10mW/cm
2~ 15mW/cm
2, time for exposure 200s ~ 300s, inorganic barrier layer 503 thickness is 1 μm ~ 1.5 μm;
Step S1304, on inorganic barrier layer 503, adopt sputtering mode to prepare moist absorbing layer 504, the material of moist absorbing layer 504 is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and thickness is 100nm ~ 200nm.Sputtering condition is that described sputtering mode is specially vacuum degree 1 × 10
-5pa ~ 1 × 10
-3pa, steams firing rate degree
Step S1305, on moist absorbing layer 504, adopt evaporation mode to prepare heat dissipating layer 505, the material of heat dissipating layer 505 is aluminium, silver, copper or their composition, and thickness is 200nm ~ 500nm.Evaporation condition is, vacuum degree is 8 × 10
-5pa ~ 3 × 10
-5pa, evaporation rate
In a preferred embodiment, by alternately repeating sulfur-nitrogen compound film 502 and inorganic barrier layer 503 that step S1303 and step S1304 prepares stacked setting, the alternately laminated number of plies is for being more than or equal to 3 layers;
Encapsulated layer is formed by step S1302 to step S1305;
Step S140, encapsulated layer 50 surface formed cap 60.
At cap edge coating cloth packaging plastic, adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 200nm ~ 400nm, and light intensity is 10mW/cm
2~ 15mW/cm
2, time for exposure 300s ~ 400s, makes to form confined space between cap 60 and substrate 10.
Embodiment 1:
A preparation method for organic electroluminescence device, comprises the following steps:
1, the preparation of substrate pre-treatment and anode: adopt acetone, ethanol, deionized water and ethanol to adopt supersonic wave cleaning machine to clean successively, each washing scavenging period is 5 minutes, then dries up with nitrogen, stand-by after using stove-drying; Substrate arranges ito glass, has the substrate of ito glass to carry out surface activation process to load, to increase the oxygen content of superficial layer, improve the work function of anode surface; Ito glass thickness is 100nm;
2, the preparation of functional layer:
Evaporation hole injection layer on anode;
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB
3).MoO
3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
Evaporation hole transmission layer on hole injection layer;
The material of hole transmission layer is 4,4', 4 "-three (carbazole-9-base) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
Evaporation luminescent layer on hole transmission layer;
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
Evaporation electron transfer layer on luminescent layer;
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
Evaporation electron injecting layer on the electron transport layer;
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN3) in Bphen, and the mass percentage of CsN3 is 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10
-5pa, evaporation rate is
3, evaporation negative electrode on electron injecting layer:
Metallic cathode adopts aluminium (Al), and thickness is 100nm, and evaporation vacuum degree is 5 × 10
-5pa, evaporation rate is
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is CuPc, and the thickness of protective layer is 200nm.Evaporation condition is, vacuum degree is 3 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is tungsten disulfide, and nitride material is silicon nitride, and the mass ratio of sulfide and described nitride is 3:17.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 1 × 10
-4pa, thicknesses of layers is set to 120nm, is that 5nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is polytetrafluoroethylene, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 10mW/cm
2, time for exposure 200s, Organic barrier layer thickness is 1 μm;
Sulfur-nitrogen compound film and inorganic barrier layer replace preparation three times;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is calcium oxide, and thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is aluminium, and thickness is 200nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 11mW/cm
2, time for exposure 350s, makes to form confined space between cap and substrate.
Embodiment 2:
A preparation method for organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1;
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, the thickness of protective layer is 300nm.Evaporation condition is, vacuum degree is 3 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is molybdenum bisuphide, and nitride material is aluminium nitride, and the mass ratio of sulfide and described nitride is 1:19.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 2 × 10
-4pa, thicknesses of layers is set to 100nm, is that 1nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is methacrylic resin, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 15mW/cm
2, time for exposure 200s, Organic barrier layer thickness is 1.5 μm;
Sulfur-nitrogen compound film and inorganic barrier layer replace preparation three times;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is barium monoxide, and thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is silver, and thickness is 500nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is aluminum slice, and adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 10mW/cm
2, time for exposure 400s, makes to form confined space between cap and substrate.
Embodiment 3:
A preparation method for organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1;
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is 8-hydroxyquinoline aluminum, and the thickness of protective layer is 250nm.Evaporation condition is, vacuum degree is 3 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is tantalum disulfide, and nitride material is boron nitride, and the mass ratio of sulfide and described nitride is 1:3.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 2 × 10
-4pa, thicknesses of layers is set to 150nm, is that 40nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is cycloaliphatic epoxy resin, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 11mW/cm
2, time for exposure 230s, Organic barrier layer thickness is 1.2 μm;
Sulfur-nitrogen compound film and inorganic barrier layer replace preparation four times;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is strontium oxide strontia, and thickness is 150nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is copper, and thickness is 300nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, and adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 15mW/cm
2, time for exposure 300s, makes to form confined space between cap and substrate.
Embodiment 4:
A preparation method for organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1;
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is silica, and the thickness of protective layer is 200nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is curing niobium, and nitride material is silicon nitride, and the mass ratio of sulfide and described nitride is 1:9.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 2 × 10
-4pa, thicknesses of layers is set to 110nm, is that 20nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is polytetrafluoroethylene, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 10mW/cm
2, time for exposure 200s, Organic barrier layer thickness is 1 μm;
Sulfur-nitrogen compound film and inorganic barrier layer replace preparation five times;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is magnesium oxide, and thickness is 100nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is albronze, and the mass ratio of copper and aluminium is 3:1, and thickness is 500nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, and adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 11mW/cm
2, time for exposure 350s, makes to form confined space between cap and substrate.
Embodiment 5:
A preparation method for organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1;
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is magnesium fluoride, and the thickness of protective layer is 300nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is antimonous sulfide, and nitride material is tantalum nitride, and the mass ratio of sulfide and described nitride is 3:17.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 2 × 10
-4pa, thicknesses of layers is set to 130nm, is that 1nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is methacrylic resin, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 15mW/cm
2, time for exposure 200s, Organic barrier layer thickness is 1.5 μm;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is calcium oxide, and thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is albronze, and the mass ratio of copper and aluminium is 3:1, and thickness is 500nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, and adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 15mW/cm
2, time for exposure 400s, makes to form confined space between cap and substrate.
Embodiment 6:
A preparation method for organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1;
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, and encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer;
On negative electrode, evaporation forms protective layer, and the material of protective layer is zinc sulphide, and the thickness of protective layer is 250nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate is
Adopt magnetron sputtering to make sulfur-nitrogen compound film on the protection layer, sulfur-nitrogen compound film is the nitride film doped with sulfide, and wherein, sulfide material is orpiment, and nitride material is titanium nitride, and the mass ratio of sulfide and described nitride is 1:4.Wherein, magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 2 × 10
-4pa, thicknesses of layers is set to 140nm, is that 5nm/min carries out magnetron sputtering and obtains sulfur-nitrogen compound film at sputter rate.
At sulfur-nitrogen compound film spin coating inorganic barrier layer, Organic barrier layer material is cycloaliphatic epoxy resin, then adopts ultraviolet light polymerization under an inert atmosphere, and ultraviolet light polymerization condition is wavelength 365nm, light intensity 11mW/cm
2, time for exposure 230s, Organic barrier layer thickness is 1.2 μm;
Inorganic barrier layer adopts sputtering mode prepare moist absorbing layer, the material of moist absorbing layer is barium monoxide, and thickness is 150nm.Sputtering condition is that described sputtering mode is specially vacuum degree 2 × 10
-4pa, steams firing rate degree
Moist absorbing layer adopts evaporation mode prepare heat dissipating layer, the material of heat dissipating layer is silver, and thickness is 300nm.Evaporation condition is, vacuum degree is 5 × 10
-5pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, and adopt the mode of ultraviolet curing to harden packaging plastic, ultraviolet wavelength is 365nm, and light intensity is 11mW/cm
2, time for exposure 350s, makes to form confined space between cap and substrate.
Effect example
For the beneficial effect of valid certificates organic electroluminescence device of the present invention and preparation method thereof, provide relevant experimental data as follows.
The test condition of organic electroluminescence device water oxygen permeability is: equipment: the Keithley2400 of Keithley company, specimen holder; Method: the change of test Ca film resistance; Condition: temperature 20 DEG C ~ 25 DEG C, humidity 40% ~ 60%.Result is 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) | 5.4E -5 | 4.1E -5 | 6.3E -5 | 5.0E -5 | 3.5E -5 | 4.7E -5 |
Table 1 is embodiment 1 ~ 6 organic electroluminescence device water oxygen permeability, makes water resistance (WVTR) reach 6.3E
-5g/m
2day.
Organic electro-luminescence device lifetime test condition: equipment: the Keithley2400 of Keithley company, the CS-100A colorimeter of Konica Minolta company; Method: test brightness is from 1000cd/m
2drop to 700cd/m
2time used; Condition: temperature 20 DEG C ~ 25 DEG C, humidity 40% ~ 60%.
Table 2. embodiment 1 ~ 6 organic electro-luminescence device lifetime situation
Table 2 is that embodiment 1 ~ 6 organic electro-luminescence device lifetime situation can be found out, the life-span of organic electroluminescence device of the present invention reaches more than 1.0013 ten thousand hours (T701000cd/m
2).
To sum up; organic electroluminescence device provided by the invention can reduce outside water, oxygen isoreactivity material effectively to the erosion of organic electroluminescence device; thus effective protection is formed to device organic functional material and electrode; meet the sealing requirements of encapsulation, the life-span of OLED can be improved significantly.
Claims (9)
1. an organic electroluminescence device, comprise the substrate, anode, functional layer, negative electrode, encapsulated layer and the cap that stack gradually, substrate and cap form enclosure space, anode, functional layer, negative electrode, encapsulated layer are contained in this enclosure space, it is characterized in that, described encapsulated layer comprises protective layer, sulfur-nitrogen compound film, inorganic barrier layer, moist absorbing layer and heat dissipating layer successively;
Described sulfur-nitrogen compound film is the nitride film doped with sulfide, wherein, described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment, described nitride material is silicon nitride, aluminium nitride, boron nitride, tantalum nitride or titanium nitride, and the mass ratio of described sulfide and described nitride is 1:5 ~ 15:19.
2. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness of described sulfur-nitrogen compound film is 100nm ~ 150nm.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm;
The material of described inorganic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin, and the thickness of described inorganic barrier layer is 1 μm ~ 1.5 μm.
4. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described moist absorbing layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and described moist absorbing layer thickness is 100nm ~ 200nm;
The material of described heat dissipating layer is aluminium, silver, copper or their composition, and the thickness of described heat dissipating layer is 200nm ~ 500nm; And
Described cap is sheet metal, and the material of sheet metal is silver, aluminium or copper.
5. organic electroluminescence device as claimed in claim 1, it is characterized in that, described sulfur-nitrogen compound film and the alternately laminated setting of described inorganic barrier layer, the stacked number of plies is more than or equal to three layers.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
The glass substrate or organic film substrate of cleaning are prepared the anode of organic electroluminescence device; Adopt the method for vacuum evaporation to prepare functional layer, negative electrode and encapsulated layer successively on anode conducting substrate, adopt ultraviolet light polymerization mode to be encapsulated by cap, make described substrate and described cap form enclosure space;
The preparation of described encapsulated layer comprises on negative electrode, first adopts the mode of vacuum evaporation to prepare protective layer;
Described protective layer adopts magnetron sputtering spatter altogether and prepare sulfur-nitrogen compound film; wherein; described sulfur-nitrogen compound film is the nitride film doped with sulfide; described sulfide material is tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; described nitride material is silicon nitride, aluminium nitride, boron nitride, tantalum nitride or titanium nitride; described magnetron sputtering condition is: adopt three target magnetic control sputtering depositing systems, and arranging background vacuum is 1 × 10
-5pa ~ 1 × 10
-3pa, thicknesses of layers is set to 100nm ~ 150nm, using the mass ratio of described sulfide and described nitride be 1:5 ~ 15:19 as target, under sputter rate be 5nm/min ~ 40nm/min condition, carry out magnetron sputtering obtain sulfur-nitrogen compound film;
Then on described sulfur-nitrogen compound film, adopt the technique of first spin coating post-exposure to prepare inorganic barrier layer, the technical process of described first spin coating post-exposure is, by the material spin coating of described inorganic barrier layer, be then 200nm ~ 400nm ultraviolet light polymerization with wavelength, light intensity is 10mW/cm
2~ 15mW/cm
2, time for exposure 200s ~ 300s;
Then on described inorganic barrier layer, adopt sputtering mode to prepare moist absorbing layer, vacuum evaporation heat dissipating layer on described moist absorbing layer;
Finally adopt packaging plastic that sheet metal encapsulation is formed cap, make described substrate and described cap form confined space, described anode, functional layer, negative electrode and encapsulated layer are contained in this enclosure space.
7. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silica, magnesium fluoride or zinc sulphide, the thickness of protective layer is 200nm ~ 300nm;
The material of described inorganic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin, and the thickness of described inorganic barrier layer is 1 μm ~ 1.5 μm.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, the material of described moist absorbing layer is calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, the thickness of described moist absorbing layer is 100nm ~ 200nm, the material of described heat dissipating layer is aluminium, silver, copper or their composition, the thickness of described heat dissipating layer is 200nm ~ 500nm, and described cap is sheet metal, and the material of sheet metal is silver, aluminium or copper.
9. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterized in that, repeat the preparation technology preparing described sulfur-nitrogen compound film and inorganic barrier layer, make described sulfur-nitrogen compound film and the stacked setting of inorganic barrier layer, the alternately laminated number of plies is for being more than or equal to 3 layers.
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