CN103730595A - Organic light-emitting device and preparation method thereof - Google Patents

Organic light-emitting device and preparation method thereof Download PDF

Info

Publication number
CN103730595A
CN103730595A CN201210388951.1A CN201210388951A CN103730595A CN 103730595 A CN103730595 A CN 103730595A CN 201210388951 A CN201210388951 A CN 201210388951A CN 103730595 A CN103730595 A CN 103730595A
Authority
CN
China
Prior art keywords
layer
organic electroluminescence
electroluminescence device
organic
barrier
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201210388951.1A
Other languages
Chinese (zh)
Inventor
周明杰
王平
钟铁涛
黄辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
Original Assignee
Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Oceans King Lighting Science and Technology Co Ltd, Shenzhen Oceans King Lighting Engineering Co Ltd filed Critical Oceans King Lighting Science and Technology Co Ltd
Priority to CN201210388951.1A priority Critical patent/CN103730595A/en
Publication of CN103730595A publication Critical patent/CN103730595A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • H10K50/844Encapsulations
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • H10K50/844Encapsulations
    • H10K50/8445Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00Manufacture or treatment specially adapted for the organic devices covered by this subclass

Abstract

The invention provides an organic light-emitting device which comprises an anode conductive substrate, a functional layer, a light-emitting layer, a cathode layer and an encapsulation layer, wherein the anode conductive substrate, the functional layer, the light-emitting layer, the cathode layer and the encapsulation layer are stacked in sequence. Enclosed space is formed by the anode conductive substrate and the encapsulation layer, and the functional layer, the light-emitting layer and the cathode layer are arranged in the enclosed space. The encapsulation layer sequentially comprises a protective layer, a barrier layer and a polyethylene terephthalate film, wherein the barrier layer is of a multilayer stacked structure and made of mixed materials formed by an organic blocking material and an inorganic blocking material. The invention further provides a preparation method of the organic light-emitting device. The method can effectively reduce erosion of moisture and oxygen on the organic light-emitting device, and therefore organic functional materials and electrodes of the organic light-emitting device are effectively protected, light transmittance of the organic light-emitting device is improved, and the service life of the organic light-emitting device can be remarkably prolonged. The method is particularly suitable for encapsulation of flexible organic light-emitting devices.

Description

A kind of organic electroluminescence device and preparation method thereof
Technical field
The present invention relates to electronic device association area, relate in particular to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is that the luminous organic material of preparing tens nanometer thickness on ito glass is made luminescent layer, and there is the metal electrode of low work function luminescent layer top.When being added with voltage on electrode, luminescent layer just produces light radiation.
OLED device have active illuminating, luminous efficiency high, low in energy consumption, light, thin, without advantages such as angle limitations, by insider, thought to be most likely at the device of new generation that occupies dominance on following illumination and display device market.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, has obtained huge achievement.Because the whole world is increasing, throw light on and show that producer drops into research and development one after another, having promoted greatly the industrialization process of OLED, making the growth rate of OLED industry surprising, having arrived the eve of scale of mass production at present.
Flexible product is the development trend of organic electroluminescence device, but the current ubiquity life-span is short, and therefore the quality of encapsulation directly affects the life-span of 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.And existing organic electroluminescence device can not provide good light transmittance conventionally.
Summary of the invention
For overcoming the defect of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and preparation method thereof.This organic electroluminescence device can reduce steam, the erosion of oxygen to organic electroluminescence device effectively; organic functional material and the electrode of protection organic electroluminescence device exempt from destruction; and improve the light transmittance of device, the life-span of OLED device is increased significantly.The inventive method is applicable to the organic electroluminescence device prepared with conducting glass substrate of encapsulation, is also applicable to the flexible organic electroluminescent device that encapsulation is prepared as substrate take plastics or metal.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device.
On the one hand, the invention provides a kind of organic electroluminescence device, comprise anode conducting substrate, functional layer, luminescent layer, cathode layer and encapsulated layer, anode conducting substrate and encapsulated layer form enclosure space, functional layer, luminescent layer and cathode layer are contained in this enclosure space, it is characterized in that, described encapsulated layer comprises protective layer successively, barrier layer and polyethylene terephthalate (PET) film, described barrier layer is multilayer laminated structure, the material on described barrier layer is the composite material that organic barrier material and inorganic barrier material form, wherein, organic barrier material is polytetrafluoroethylene, methacrylic resin or methyl cyclopentenyl ketone, inorganic barrier material is titanium dioxide (TiO 2), zirconium dioxide (ZrO 2) or hafnium oxide (HfO 2), the mass fraction of described inorganic barrier material in barrier layer is 15~30%.
Barrier layer is multilayer laminated structure, can extend water, oxygen permeation pathway, effectively reduces outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, reaches good packaging effect.
Preferably, described barrier layer is the stepped construction of 4~6 layers.
The material on barrier layer is the composite material that organic barrier material and inorganic barrier material form.
Organic barrier material and inorganic barrier material are mixed to form barrier layer material, can improve the light transmittance of organic electroluminescence device light, reduce the impact of encapsulation on light efficiency, improve energy efficiency, make encapsulated layer have advantages of that quality is light, intercept water, oxygen ability is strong.
Preferably, inorganic barrier material diameier 20~40nm.
Mode by vacuum evaporation is prepared protective layer on cathode layer, and the existence of protective layer can protect negative electrode to exempt from destruction in subsequent operation process.
Protective layer material is selected from the one in organic small molecule material, inorganic material or metal material, preferably from CuPc (CuPc), N, and N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine (NPB), 8-hydroxyquinoline aluminum (Alq 3), silica (SiO), magnesium fluoride (MgF 2) or zinc sulphide (ZnS).Preferably, the thickness of protective layer is 200nm~300nm.
At the PET film edge coating packaging plastic with barrier layer, be cured with UV light, described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Preferably, anode conducting substrate is conducting glass substrate or conduction organic film substrate.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and electron transfer layer.Preferably, functional layer and luminescent layer are the method setting by vacuum evaporation.
Preferably, cathode layer is transparent cathode layer.
More preferably, cathode layer is ZnS/Ag/ZnS.
On the other hand, the invention provides a kind of preparation method of organic electroluminescence device, comprise the following steps:
(1) on clean conducting glass substrate or conduction organic film substrate, be prepared with the anode pattern of organic electroluminescence devices; Adopt the method for vacuum evaporation on substrate, to prepare successively functional layer, luminescent layer and cathode layer;
(2) adopt the mode of vacuum evaporation on cathode layer, to prepare protective layer;
(3) adopt the mode of first spin coating post-exposure to prepare barrier layer on PET film, the material on described barrier layer is the composite material that organic barrier material and inorganic barrier material form, wherein, organic barrier material is polytetrafluoroethylene, methacrylic resin or methyl cyclopentenyl ketone, and inorganic barrier material is TiO 2, ZrO 2or HfO 2, the mass fraction of inorganic barrier material in barrier layer is 15~30%;
(4) repeating step (3), obtains having the barrier layer of multilayer laminated structure.
(5) at the PET film edge coating packaging plastic with barrier layer, be cured with UV light, described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Step (3) adopts the mode of first spin coating post-exposure to prepare barrier layer on PET film, and the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form.
Organic barrier material and inorganic barrier material are mixed to form barrier layer material, can improve on the one hand the light transmittance of organic electroluminescence device light, reduce the impact of encapsulation on light efficiency, improve energy efficiency; On the other hand, the mixed membranous layer that organic barrier material and inorganic barrier material form has made up the shortcoming of single inorganic layer and single organic matter layer, makes encapsulated layer have advantages of that quality is light, intercept water, oxygen ability is strong.
Preferably, step (3), under inert atmosphere, is carried out spin coating and exposure, and gluing thickness 1~1.5 μ m, is then cured light intensity 10~15mW/cm with UV light 2, time for exposure 300~400s.
Organic barrier material is polytetrafluoroethylene, methacrylic resin or methyl cyclopentenyl ketone, and inorganic barrier material is TiO 2, ZrO 2or HfO 2.
Preferably, inorganic barrier material diameier 20~40nm.
Barrier layer is multilayer laminated structure, can extend water, oxygen permeation pathway, effectively reduces outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, reaches good packaging effect.
Preferably, described barrier layer is the stepped construction of 4~6 layers.
Step (2) is for to prepare protective layer by the mode of vacuum evaporation on cathode layer, the existence of protective layer can defencive function layer and metallic cathode in subsequent operation process, exempt from destruction.
Protective layer material is selected from the one in organic small molecule material, inorganic material or metal material, preferably from CuPc, NPB, Alq 3, SiO, MgF 2or ZnS.Preferably, the thickness of protective layer is 200nm~300nm.
Preferably, the vacuum degree 1 × 10 of step (2) vacuum evaporation process -5pa~1 × 10 -3pa, evaporation rate
Figure BDA00002255189800041
Preferably, anode conducting substrate is conducting glass substrate or conduction organic film substrate.
Adopt the method for vacuum evaporation on anode conducting substrate, to prepare functional layer, luminescent layer and cathode layer.
Functional layer generally includes hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer.Luminescent layer is arranged between hole transmission layer and electron transfer layer.
Adopt evaporation mode to prepare cathode layer.
Preferably, cathode layer is transparent cathode layer.
More preferably, cathode layer is ZnS/Ag/ZnS.
Step (5) is at the PET film edge coating packaging plastic with barrier layer, is cured with UV light, and described organic electroluminescence device is encapsulated in described PET film and electrically-conductive backing plate.
Preferably, the light intensity 15~25mW/cm of UV light 2, time for exposure 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 can reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device effectively, thereby device organic functional material and electrode are formed to effective protection, improve device light transmittance, the life-span that can improve significantly organic electroluminescence device;
(2) light transmittance of organic electroluminescence device encapsulated layer of the present invention reaches more than 69%, and water resistance (WVTR) reaches 3.1 × 10 -4g/m 2day, the life-span reaches 4,600 hours above (T701000cd/m 2);
(3) the inventive method is applicable to the organic electroluminescence device prepared take electro-conductive glass as anode substrate of encapsulation, is also applicable to the flexible organic electroluminescent device that encapsulation is prepared as anode substrate take plastics or metal.The inventive method is particularly useful for encapsulating flexible organic electroluminescent device;
(4) organic electroluminescence device material cheapness of the present invention, method for packing is simple to operate, and easily large area preparation is suitable for large-scale industrialization and uses.
Accompanying drawing explanation
Fig. 1 is the structural representation 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 improvement and adjustment are also considered as in protection scope of the present invention.
Embodiment 1:
A preparation method for organic electroluminescence device, comprises the following steps:
(1) ito glass substrate 1 pre-treatment: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, all cleans with supersonic wave cleaning machine, and individual event washing is cleaned 5 minutes, then with nitrogen, dries up, and stove-drying is stand-by; Ito glass substrate 1 after cleaning is carried out to surface activation process, to increase the oxygen content of conductive surface layer, improve the work function of conductive layer surface; ITO thickness is 100nm;
(2) preparation of functional layer and luminescent layer: hole injection layer 2: evaporation MoO on ito glass substrate 1 3the composite material that doping NPB obtains, MoO 3doping mass fraction be 30%, evaporation all adopts high vacuum coating equipment to carry out, during evaporation, vacuum degree is 1 × 10 -5pa, evaporation rate is
Figure BDA00002255189800051
obtain hole injection layer 2, thickness is 10nm;
Hole transmission layer 3: " tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, evaporation TCTA on hole injection layer 2, evaporation vacuum degree 1 × 10 to adopt 4,4', 4 -5pa, evaporation rate
Figure BDA00002255189800052
evaporation thickness 30nm;
Luminescent layer 4: evaporation luminescent layer 4 on hole transmission layer 3, luminescent layer 4 material of main parts adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy) 3), guest materials quality accounts for 5% of material of main part, evaporation vacuum degree 1 × 10 -5pa, evaporation rate
Figure BDA00002255189800061
evaporation thickness 20nm;
The preparation of electron transfer layer 5: evaporation 4 on luminescent layer 4,7-diphenyl-1,10-phenanthroline (Bphen) is as electron transport material, evaporation vacuum degree 1 × 10 -5pa, evaporation rate
Figure BDA00002255189800062
evaporation thickness 10nm;
The preparation of electron injecting layer 6: evaporation electron injection material forms electron injecting layer 6 on electron transfer layer 5, and electron injecting layer 6 materials are CsN 3doping Bphen, doping mass fraction 30%, evaporation vacuum degree 1 × 10 -5pa, evaporation rate
Figure BDA00002255189800063
evaporation thickness 20nm;
(3) preparation of cathode layer 7: evaporation ZnS, Ag and ZnS form cathode layer ZnS/Ag/ZnS, ZnS thickness 30nm, Ag thickness 10nm, evaporation vacuum degree 1 × 10 successively on electron injecting layer 6 -5pa, evaporation rate
Figure BDA00002255189800064
(4) preparation of protective layer 81: adopt mode evaporation CuPc on cathode layer 7 of vacuum evaporation, vacuum degree 1 × 10 -5pa, evaporation rate
Figure BDA00002255189800065
thickness 200nm;
(5) preparation on barrier layer 87: preparation on PET film 88, the material on barrier layer 87 is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is polytetrafluoroethylene, and inorganic barrier material is TiO 2, inorganic barrier material diameier 30nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 22%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm) 2, time for exposure 400s;
(6) preparation on barrier layer 86,85,84,83 and 82: adopt method and the material identical with step (5) to prepare barrier layer 86 after step (5) on barrier layer 87, on barrier layer 86, adopt again method and the material identical with step (5) to prepare barrier layer 85, on barrier layer 85, adopt method and the material identical with step (5) to prepare barrier layer 84, on barrier layer 84, adopt method and the material identical with step (5) to prepare barrier layer 83, on barrier layer 83, adopt method and the material identical with step (5) to prepare barrier layer 82;
(7) covering of PET film 88: at the PET film edge coating packaging plastic with barrier layer, be cured light intensity 20mW/cm with UV light (λ=365nm) 2, time for exposure 350s; Described organic electroluminescence device is encapsulated in described PET film 88 and anode conducting substrate 1.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 3.1 × 10 -4, the life-span of organic electroluminescence device is 5,398h(T701000cd/m 2), light transmittance is 71.5%.
Fig. 1 is the structural representation of the organic electroluminescence device that makes of the embodiment of the present invention 1.As shown in Figure 1; the present embodiment organic electroluminescence device; comprise successively ito glass substrate 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, cathode layer 7 and encapsulated layer 8; encapsulated layer 8 comprises protective layer 81 successively; 6 layers of barrier layer 82,83,84,85,86 and 87, and PET film 88.Ito glass substrate 1 and PET film 88 are sealed and are formed enclosure space, hole injection layer 2, hole transmission layer 3 by packaging plastic; luminescent layer 4, electron transfer layer 5, electron injecting layer 6; cathode layer 7, protective layer 81 and barrier layer 82,83,84,85,86 and 87 are contained in this enclosure space.
Embodiment 2:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of protective layer: adopt mode evaporation NPB on cathode layer of vacuum evaporation, vacuum degree 5 × 10 -5pa, evaporation rate
Figure BDA00002255189800071
thickness 300nm;
(5) preparation on barrier layer: prepare on PET film, the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is methyl cyclopentenyl ketone, and inorganic barrier material is ZrO 2, inorganic barrier material diameier 20nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 30%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1.2 μ m, are then cured light intensity 12mW/cm with UV light (λ=365nm) 2, time for exposure 350s;
(6) on the barrier layer of preparing in step (5), adopt method and the material identical with step (5) to repeat to prepare barrier layer 4 times;
(7) covering of PET film: at the PET film edge coating packaging plastic with barrier layer, be cured light intensity 25mW/cm with UV light (λ=365nm) 2, time for exposure 400s; Described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 4.3 × 10 -4, the life-span of organic electroluminescence device is 5,265h(T701000cd/m 2), light transmittance is 72.3%.
Embodiment 3:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of protective layer: the mode evaporating Al q on cathode layer that adopts vacuum evaporation 3, vacuum degree 5 × 10 -5pa, evaporation rate
Figure BDA00002255189800081
thickness 250nm;
(5) preparation on barrier layer: prepare on PET film, the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is methacrylic resin, and inorganic barrier material is HfO 2, inorganic barrier material diameier 40nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 15%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm) 2, time for exposure 300s;
(6) on the barrier layer of preparing in step (5), adopt method and the material identical with step (5) to repeat to prepare barrier layer 3 times;
(7) covering of PET film: at the PET film edge coating packaging plastic with barrier layer, be cured light intensity 15mW/cm with UV light (λ=365nm) 2, time for exposure 300s; Described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 5.2 × 10 -4, the life-span of organic electroluminescence device is 5,187h(T701000cd/m 2), light transmittance is 73.2%.
Embodiment 4:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of protective layer: adopt mode evaporation SiO on cathode layer of vacuum evaporation, vacuum degree 1 × 10 -5pa, evaporation rate
Figure BDA00002255189800082
thickness 200nm;
(5) preparation on barrier layer: prepare on PET film, the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is polytetrafluoroethylene, and inorganic barrier material is TiO 2, inorganic barrier material diameier 30nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 20%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm) 2, time for exposure 400s;
(6) on the barrier layer of preparing in step (5), adopt method and the material identical with step (5) to repeat to prepare barrier layer 3 times;
(7) covering of PET film: at the PET film edge coating packaging plastic with barrier layer, be cured light intensity 20mW/cm with UV light (λ=365nm) 2, time for exposure 350s; Described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 6.0 × 10 -4, the life-span of organic electroluminescence device is 5,013h(T701000cd/m 2), light transmittance is 74.4%.
Embodiment 5:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of protective layer: the mode evaporation MgF on cathode layer that adopts vacuum evaporation 2, vacuum degree 5 × 10 -5pa, evaporation rate thickness 300nm;
(5) preparation on barrier layer: prepare on PET film, the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is methyl cyclopentenyl ketone, and inorganic barrier material is ZrO 2, inorganic barrier material diameier 20nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 25%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1.2 μ m, are then cured light intensity 12mW/cm with UV light (λ=365nm) 2, time for exposure 350s;
(6) on the barrier layer of preparing in step (5), adopt method and the material identical with step (5) to repeat to prepare barrier layer 3 times;
(7) covering of PET film: at the PET film edge edge-coating packaging plastic with barrier layer, be cured light intensity 25mW/cm with UV light (λ=365nm) 2, time for exposure 400s; Described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 6.7 × 10 -4, the life-span of organic electroluminescence device is 4,779h(T701000cd/m 2), light transmittance is 73.9%.
Embodiment 6:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of protective layer: adopt mode evaporation ZnS on cathode layer of vacuum evaporation, vacuum degree 1 × 10 -3pa, evaporation rate
Figure BDA00002255189800101
thickness 250nm;
(5) preparation on barrier layer: prepare on PET film, the material on barrier layer is the composite material that organic barrier material and inorganic barrier material form, and organic barrier material is methacrylic resin, and inorganic barrier material is HfO 2, inorganic barrier material diameier 40nm, in mixed membranous layer, the mass fraction that inorganic barrier material accounts for mixed membranous layer is 18%.Adopt the mode of first spin coating post-exposure to prepare, under inert atmosphere, prepare, gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm) 2, time for exposure 300s;
(6) on the barrier layer of preparing in step (5), adopt method and the material identical with step (5) to repeat to prepare barrier layer 3 times;
(7) covering of PET film: at the PET film edge coating packaging plastic with barrier layer, be cured light intensity 15mW/cm with UV light (λ=365nm) 2, time for exposure 300s; Described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device 2day) be 7.5 × 10 -4, the life-span of organic electroluminescence device is 4,609h(T701000cd/m 2), light transmittance is 69.3%.
Effect embodiment
For the beneficial effect of valid certificates organic electroluminescence device of the present invention and preparation method thereof, provide related experiment data as follows.
Table 1. embodiment 1 ~ 6 organic electroluminescence device water oxygen permeability
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
WVTR(g/m 2/day) 3.1×10 -4 4.3×10 -4 5.2×10 -4 6.0×10 -4 6.7×10 -4 7.5×10 -4
Table 2. embodiment 1 ~ 6 organic electro-luminescence device lifetime situation
Figure BDA00002255189800102
Table 3. embodiment 1 ~ 6 organic electroluminescence device light transmittance
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Light transmittance 71.5% 72.3% 73.2% 74.4% 73.9% 69.3%
Table 1 is embodiment 1 ~ 6 organic electroluminescence device water oxygen permeability, and table 2 is embodiment 1 ~ 6 organic electro-luminescence device lifetime situations, and table 3 is embodiment 1 ~ 6 organic electroluminescence device light transmittance situations.
As can be seen from Table 1, the water oxygen permeability of organic electroluminescence device of the present invention (WVTR) reaches 3.1 × 10 -4g/m 2day, as can be seen from Table 2, the life-span of organic electroluminescence device of the present invention reaches 4,600 hours above (T701000cd/m 2), the light transmittance of organic electroluminescence device reaches 69% as can be seen from Table 3.
To sum up; organic electroluminescence device provided by the invention can reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device effectively; thereby device organic functional material and electrode are formed to effective protection; and improve the light transmittance of device; meet the sealing requirements of encapsulation, the life-span that can improve significantly OLED device.

Claims (10)

1. an organic electroluminescence device, comprise the anode conducting substrate stacking gradually, functional layer, luminescent layer, cathode layer and encapsulated layer, anode conducting substrate and encapsulated layer form enclosure space, functional layer, luminescent layer and cathode layer are contained in this enclosure space, it is characterized in that, described encapsulated layer comprises protective layer successively, barrier layer and polyethylene terephthalate film, described barrier layer is multilayer laminated structure, the material on described barrier layer is the composite material that organic barrier material and inorganic barrier material form, wherein, organic barrier material is polytetrafluoroethylene, methacrylic resin or methyl cyclopentenyl ketone, inorganic barrier material is titanium dioxide, zirconium dioxide or hafnium oxide, the mass fraction of described inorganic barrier material in barrier layer is 15~30%.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, described barrier layer is the stepped construction of 4~6 layers.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, described protective layer material is CuPc, N; N'-diphenyl-N; N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, silica, magnesium fluoride or zinc sulphide.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described protective layer is 200nm~300nm.
5. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
(1) on clean conducting glass substrate or conduction organic film substrate, be prepared with the anode pattern of organic electroluminescence devices; Adopt the method for vacuum evaporation on substrate, to prepare successively functional layer, luminescent layer and cathode layer;
(2) adopt the mode of vacuum evaporation on cathode layer, to prepare protective layer;
(3) adopt the mode of first spin coating post-exposure in polyethylene terephthalate film, to prepare barrier layer, the material on described barrier layer is the composite material that organic barrier material and inorganic barrier material form, wherein, organic barrier material is polytetrafluoroethylene, methacrylic resin or methyl cyclopentenyl ketone, inorganic barrier material is titanium dioxide, zirconium dioxide or hafnium oxide, and the mass fraction of described inorganic barrier material in barrier layer is 15~30%;
(4) repeating step (3), obtains having the barrier layer of multilayer laminated structure;
(5) at the PETG film edge coating packaging plastic with barrier layer, be cured with UV light, described organic electroluminescence device is encapsulated in described polyethylene terephthalate film and anode conducting substrate.
6. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described in step (3), the preparation condition on barrier layer is: under inert atmosphere, carry out spin coating and exposure, gluing thickness 1~1.5 μ m, is then cured light intensity 10~15mW/cm with UV light 2, time for exposure 300~400s.
7. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described barrier layer is the stepped construction of 4~6 layers.
8. the preparation method of organic electroluminescence device as claimed in claim 5; it is characterized in that; described in step (2), protective layer material is CuPc, N; N'-diphenyl-N; N'-bis-(1-naphthyl)-1; 1'-biphenyl-4,4'-diamines, oxine aluminium, silica, magnesium fluoride or zinc sulphide.
9. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described in step (2), the condition of protective layer vacuum evaporation is: vacuum degree 1 × 10 -5pa~1 × 10 -3pa, evaporation rate
Figure FDA00002255189700021
10. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described in step (2), the thickness of protective layer is 200nm~300nm.
CN201210388951.1A 2012-10-15 2012-10-15 Organic light-emitting device and preparation method thereof Pending CN103730595A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210388951.1A CN103730595A (en) 2012-10-15 2012-10-15 Organic light-emitting device and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210388951.1A CN103730595A (en) 2012-10-15 2012-10-15 Organic light-emitting device and preparation method thereof

Publications (1)

Publication Number Publication Date
CN103730595A true CN103730595A (en) 2014-04-16

Family

ID=50454593

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210388951.1A Pending CN103730595A (en) 2012-10-15 2012-10-15 Organic light-emitting device and preparation method thereof

Country Status (1)

Country Link
CN (1) CN103730595A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103985821A (en) * 2014-05-30 2014-08-13 云南北方奥雷德光电科技股份有限公司 Film sealing process for top-emission OLED displayer
CN106328810A (en) * 2016-10-17 2017-01-11 武汉华星光电技术有限公司 Flexible OLED substrate structure and the design method thereof
WO2019205329A1 (en) * 2018-04-25 2019-10-31 武汉华星光电半导体显示技术有限公司 Packaging structure and packaging method for oled device
CN111682079A (en) * 2020-06-01 2020-09-18 大连理工大学 Medium/far infrared transparent conductive material system and method for preparing conductive film by using same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103985821A (en) * 2014-05-30 2014-08-13 云南北方奥雷德光电科技股份有限公司 Film sealing process for top-emission OLED displayer
CN106328810A (en) * 2016-10-17 2017-01-11 武汉华星光电技术有限公司 Flexible OLED substrate structure and the design method thereof
CN106328810B (en) * 2016-10-17 2019-03-12 武汉华星光电技术有限公司 Flexible oled substrate structure and design method
WO2019205329A1 (en) * 2018-04-25 2019-10-31 武汉华星光电半导体显示技术有限公司 Packaging structure and packaging method for oled device
CN111682079A (en) * 2020-06-01 2020-09-18 大连理工大学 Medium/far infrared transparent conductive material system and method for preparing conductive film by using same
CN111682079B (en) * 2020-06-01 2021-12-14 大连理工大学 Medium/far infrared transparent conductive material system and method for preparing conductive film by using same

Similar Documents

Publication Publication Date Title
CN103811668A (en) Organic electroluminescent device and method for producing same
CN104638189A (en) Organic light-emitting device and preparation method thereof
CN103730595A (en) Organic light-emitting device and preparation method thereof
CN103730594A (en) Organic light-emitting device and preparation method thereof
CN103855315A (en) Organic light-emitting device and preparation method thereof
CN103730593A (en) Organic light-emitting device and preparation method thereof
CN103855316B (en) A kind of organic electroluminescence device and preparation method thereof
CN103594649A (en) Organic electroluminescent device and preparation method thereof
CN103427035A (en) Organic electroluminescence device and method for manufacturing same
CN103855320B (en) A kind of organic electroluminescence device and preparation method thereof
CN103682119A (en) Organic light-emitting device and preparation method thereof
CN103855321A (en) Organic light-emitting device and preparation method thereof
CN104078595A (en) Organic light-emitting diode and preparation method thereof
CN104078590A (en) Organic light-emitting diode and preparation method thereof
CN103855318B (en) A kind of organic electroluminescence device and preparation method thereof
CN103855308B (en) A kind of organic electroluminescence device and preparation method thereof
CN104103764A (en) Organic light-emitting display and manufacturing method thereof
CN103904239A (en) Organic light-emitting device and preparation method
CN103594647A (en) Organic electroluminescent device and preparation method thereof
CN103594650A (en) Organic electroluminescent device and preparation method thereof
CN103594643A (en) Organic electroluminescent device and preparation method thereof
CN103855317B (en) A kind of organic electroluminescence device and preparation method thereof
CN103855319B (en) A kind of organic electroluminescence device and preparation method thereof
CN103730596A (en) Organic light-emitting device and preparation method thereof
CN104518120A (en) Organic light-emitting device and production method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20140416