CN103730594A - Organic light-emitting device and preparation method thereof - Google Patents
Organic light-emitting device and preparation method thereof Download PDFInfo
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- CN103730594A CN103730594A CN201210388818.6A CN201210388818A CN103730594A CN 103730594 A CN103730594 A CN 103730594A CN 201210388818 A CN201210388818 A CN 201210388818A CN 103730594 A CN103730594 A CN 103730594A
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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
- H10K50/844—Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- 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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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 an organic barrier layer, an inorganic barrier layer and a polyethylene terephthalate film, and the organic barrier layer and the inorganic barrier layer are stacked alternately to form a multilayered structure. 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
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 flexible 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 the anode conducting substrate, functional layer, luminescent layer, cathode layer and the encapsulated layer that stack gradually, anode conducting substrate and encapsulated layer form enclosure space, functional layer, luminescent layer and cathode layer are contained in this enclosure space, described encapsulated layer comprises organic barrier layer, inorganic barrier layer and polyethylene terephthalate (PET) film successively, the alternately laminated formation sandwich construction of described organic barrier layer and inorganic barrier layer;
Described organic barrier layer material is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), CuPc (CuPc), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq
3), 4,4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine (m-MTDATA) or 4,7-diphenyl-1,10-Phen (BCP);
The material of described inorganic barrier layer is by low-index material silica (SiO), magnesium fluoride (MgF
2) and lithium fluoride (LiF) in one and the composite material of a kind of formation in high-index material zinc sulphide (ZnS), zinc selenide (ZnSe) and cadmium sulfide (CdS).
Encapsulated layer comprises organic barrier layer, inorganic barrier layer and PET film successively.
Mode by vacuum evaporation is prepared organic barrier layer on cathode layer, and the existence on organic barrier layer can protect negative electrode to exempt from destruction in subsequent operation process.
Preferably, the thickness on organic barrier layer is 200nm～300nm.
Preferably, in inorganic barrier layer, low-index material SiO, MgF
2or LiF mass fraction is 40～60%.
Preferably, the thickness of inorganic barrier layer is 100nm～200nm.
The material of inorganic barrier layer is the composite material that low-refraction (1.3～1.7) material and high index of refraction (2.1～2.6) material form, and bi-material mixes, and approaches organic barrier layer refractive index, is conducive to improve the light transmittance of organic electroluminescence device.
Preferably, organic barrier layer is identical with the inorganic barrier layer number of plies, is 4～6 layers.
The alternately laminated formation sandwich construction of organic barrier layer and inorganic barrier layer, can reach good packaging effect, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, made up the shortcoming on single inorganic matter barrier layer and single organic substance barrier layer, improve the light transmittance of organic electroluminescence device, extend device lifetime.
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 anode conducting substrate, to prepare successively functional layer, luminescent layer and cathode layer;
(2) adopt the mode of vacuum evaporation on cathode layer, to prepare organic barrier layer, organic barrier layer material is TAPC, CuPc, NPB, Alq
3, m-MTDATA or BCP;
(3) adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the material of inorganic barrier layer is by low-index material SiO, MgF
2with the composite material of a kind of formation in a kind of and high-index material ZnS, ZnSe and CdS in LiF, in inorganic barrier layer, low-index material SiO, MgF
2or LiF mass fraction is 40～60%;
(4) after step (3), adopt method and the material identical with step (2) to prepare organic barrier layer, on described organic barrier layer, adopt again method and the material that step (3) is identical to prepare inorganic barrier layer, by that analogy, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(5) on described inorganic barrier layer surface, cover PET film, then at PET film edge coating packaging plastic, be cured with UV light, described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
Step (2) is prepared organic barrier layer by the mode of vacuum evaporation on cathode layer, and the existence on organic barrier layer can protect negative electrode to exempt from destruction in subsequent operation process.
Preferably, the thickness on organic barrier layer is 200nm～300nm.
Preferably, the vacuum degree 1 × 10 of step (2) vacuum evaporation process
-5pa～1 × 10
-3pa, evaporation rate
Step (3) is prepared inorganic barrier layer by the mode of vacuum evaporation on organic barrier layer,
The material of inorganic barrier layer is mixed and is formed by low-index material and high-index material, and bi-material mixes, and approaches organic barrier layer refractive index, is conducive to improve the light transmittance of organic electroluminescence device.
Low-index material is SiO, MgF
2or LiF.
High-index material is ZnS, ZnSe or CdS.
Preferably, the thickness of inorganic barrier layer is 100nm～200nm.
Preferably, SiO, MgF in inorganic barrier layer
2or the mass fraction of LiF in inorganic barrier layer is 40～60%.
Preferably, the vacuum degree 1 × 10 of step (3) vacuum evaporation process
-5pa～1 × 10
-3pa, evaporation rate
The alternately laminated formation sandwich construction that arranges of organic barrier layer and inorganic barrier layer, can reach good packaging effect.Water, oxygen permeation pathway be can extend on the one hand, outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device effectively reduced; The alternately laminated light transmission efficiency that can improve organic electroluminescence device light that arranges of organic barrier layer and inorganic barrier layer, extends device lifetime on the other hand.
Preferably, described organic barrier layer is identical with the inorganic barrier layer number of plies, is 4～6 layers.
Preferably, anode substrate is conducting glass substrate or conduction organic film substrate.
Adopt the method for vacuum evaporation on anode conducting substrate, to prepare successively 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 for covering PET film on described inorganic barrier layer surface, then at PET film edge coating packaging plastic, is cured with UV light, and described organic electroluminescence device is encapsulated in described PET film and anode conducting substrate.
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 light transmittance, the life-span of improving significantly organic electroluminescence device;
(2) light transmittance of organic electroluminescence device encapsulated layer of the present invention reaches more than 67%, and water resistance (WVTR) reaches 2.3 × 10
-4g/m
2day, the life-span reaches more than 5,700 hours;
(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 mode is simple, and easily large area preparation is suitable for large-scale industrialization and uses.
Accompanying drawing explanation
Fig. 1 is the structural representation of 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 1
3the composite material that doping NPB obtains, MoO
3doping mass fraction be 30%, evaporation all adopts high vacuum coating equipment to carry out, during evaporation, vacuum degree is 1 × 10
-5pa, evaporation rate is
obtain hole injection layer 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, vacuum degree 1 × 10 to adopt 4,4', 4
-5pa, evaporation rate
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, vacuum degree 1 × 10
-5pa, evaporation rate
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, vacuum degree 1 × 10
-5pa, evaporation rate
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%, vacuum degree 1 × 10
-5pa, evaporation rate
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, vacuum degree 1 × 10 successively on electron injecting layer 6
-5pa, evaporation rate
(4) preparation on organic barrier layer 81: adopt the mode of vacuum evaporation to prepare Alq on cathode layer 7
3, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 250nm;
(5) preparation of inorganic barrier layer 82: adopt the mode of vacuum evaporation to prepare inorganic barrier layer 82 on organic barrier layer 81, the composite material that the material of inorganic barrier layer 82 is formed by low-index material and high-index material, low-index material is for being MgF
2, high-index material is ZnSe, MgF
2the mass fraction that accounts for whole rete is 50%, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 150nm;
(6) organic barrier layer 83, 85, 87 and inorganic barrier layer 84, 86, 88 preparation: adopt method and the material identical with step (4) to prepare organic barrier layer 83 at inorganic barrier layer 82 after step (5), on organic barrier layer 83, adopt again method and the material that step (5) is identical to prepare inorganic barrier layer 84, on inorganic barrier layer 84, adopt method and the material identical with step (4) to prepare organic barrier layer 85, on organic barrier layer 85, adopt method and the material that step (5) is identical to prepare inorganic barrier layer 86, on inorganic barrier layer 86, adopt method and the material identical with step (4) to prepare organic barrier layer 87, on organic barrier layer 87, adopt method and the material that step (5) is identical to prepare inorganic barrier layer 88, make inorganic barrier layer and organic barrier layer number of plies respectively reach 4 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film 89: cover PET film 89 on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 89 and anode conducting substrate 1.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 3.7 × 10
-4, the life-span of organic electroluminescence device is 6,005h(T701000cd/m
2), light transmittance is 77%.
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 4 layers of organic barrier layer 81 successively, 83, 85, 87, 4 layers of inorganic barrier layer 82, 84, 86, 88 and PET film 89, ito glass substrate 1 and PET film 89 are sealed and are formed enclosure space by packaging plastic, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6, cathode layer 7, organic barrier layer 81, 83, 85, 87 and inorganic barrier layer 82, 84, 86, 88 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 on organic barrier layer: adopt the mode of vacuum evaporation to prepare CuPc on cathode layer, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 250nm;
(5) preparation of inorganic barrier layer: adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the composite material that the material of inorganic barrier layer is formed by low-index material and high-index material, low-index material is MgF
2, high-index material is ZnSe, MgF
2the mass fraction that accounts for whole rete is 60%, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 100nm;
(6) after step (5), adopt method and the material identical with step (4) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (5) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 5 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film: cover PET film on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 2.9 × 10
-4, the life-span of organic electroluminescence device is 6,111h(T701000cd/m
2), light transmittance is 73%.
Embodiment 3:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation on organic barrier layer: adopt the mode of vacuum evaporation to prepare NPB on cathode layer, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 200nm;
(5) preparation of inorganic barrier layer: adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the composite material that the material of inorganic barrier layer is formed by low-index material and high-index material, low-index material is LiF, high-index material is CdS, the mass fraction that LiF accounts for whole rete is 50%, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 150nm;
(6) after step (5), adopt method and the material identical with step (4) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (5) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 4 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film: cover PET film on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 3.5 × 10
-4, the life-span of organic electroluminescence device is 6,074h(T701000cd/m
2), light transmittance is 74%.
Embodiment 4:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation on organic barrier layer: adopt mode evaporation TAPC on cathode layer of vacuum evaporation, vacuum degree 1 × 10
-5pa, evaporation rate
thickness 300nm;
(5) preparation of inorganic barrier layer: adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the composite material that the material of inorganic barrier layer is formed by low-index material and high-index material, low-index material is SiO, high-index material is ZnS, the mass fraction that SiO accounts for whole rete is 40%, vacuum degree 1 × 10
-5pa, evaporation rate
thickness 200nm;
(6) after step (5), adopt method and the material identical with step (4) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (5) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 6 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film: cover PET film on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 2.3 × 10
-4, the life-span of organic electroluminescence device is 6,213h(T701000cd/m
2), light transmittance is 70%.
Embodiment 5:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation on organic barrier layer: adopt the mode of vacuum evaporation to prepare m-MTDATA on cathode layer, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 270nm;
(5) preparation of inorganic barrier layer: adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the composite material that the material of inorganic barrier layer is formed by low-index material and high-index material, low-index material is SiO, high-index material is CdS, the mass fraction that SiO accounts for whole rete is 50%, vacuum degree 5 × 10
-5pa, evaporation rate
thickness 150nm;
(6) after step (5), adopt method and the material identical with step (4) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (5) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 4 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film: cover PET film on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 4.2 × 10
-4, the life-span of organic electroluminescence device is 5,901h(T701000cd/m
2), light transmittance is 69%.
Embodiment 6:
A preparation method for organic electroluminescence device, comprises the following steps:
(1), (2), (3) are with embodiment 1;
(4) preparation on organic barrier layer: adopt the mode of vacuum evaporation to prepare BCP on cathode layer, vacuum degree 1 × 10
-3pa, evaporation rate
thickness 200nm;
(5) preparation of inorganic barrier layer: adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the composite material that the material of inorganic barrier layer is formed by low-index material and high-index material, low-index material is LiF, high-index material is ZnS, the mass fraction that LiF accounts for whole rete is 45%, vacuum degree 1 × 10
-3pa, evaporation rate
thickness 180nm;
(6) after step (5), adopt method and the material identical with step (4) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (5) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 4 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer.
(7) covering of PET film: cover PET film on the sandwich construction surface of described organic barrier layer and the alternately laminated formation of inorganic barrier layer, then at PET film edge coating packaging plastic, 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 5.1 × 10
-4, the life-span of organic electroluminescence device is 5,782h(T701000cd/m
2), light transmittance is 67%.
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
| |
|
|
|
|
|
|
| WVTR(g/m 2/day) | 3.7×10 -4 | 2.9×10 -4 | 3.5×10 -4 | 2.3×10 -4 | 4.2×10 -4 | 5.1×10 -4 |
Table 2. embodiment 1 ~ 6 organic electro-luminescence device lifetime situation
Table 3. embodiment 1 ~ 6 organic electroluminescence device light transmittance
| |
|
|
|
|
|
|
| Light transmittance | 69% | 74% | 77% | 73% | 67% | 73% |
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 2.3 × 10
-4g/m
2day, as can be seen from Table 2, the life-span of organic electroluminescence device of the present invention reaches 5,700 hours above (T701000cd/m
2), the light transmittance of organic electroluminescence device reaches 67% 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, functional layer, luminescent layer, cathode layer and the encapsulated layer that stack gradually, 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 organic barrier layer, inorganic barrier layer and polyethylene terephthalate film successively, the alternately laminated formation sandwich construction of described organic barrier layer and inorganic barrier layer;
Described organic barrier layer material is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, CuPc, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4; 7-diphenyl-1,10-Phen;
A kind of composite material forming in high-index material zinc sulphide, zinc selenide and cadmium sulfide that a kind of and refractive index in low-index material silica, magnesium fluoride and lithium fluoride that the material of described inorganic barrier layer is 1.3～1.7 by refractive index is 2.1～2.6.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, in described inorganic barrier layer, the mass fraction of low-index material silica, magnesium fluoride or lithium fluoride is 40～60%.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of inorganic barrier layer is 100nm～200nm.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness on organic barrier layer is 200nm～300nm.
5. organic electroluminescence device as claimed in claim 1, is characterized in that, described organic barrier layer is identical with the inorganic barrier layer number of plies, is 4～6 layers.
6. 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 anode conducting substrate, to prepare functional layer, luminescent layer and cathode layer;
(2) adopt the mode of vacuum evaporation on cathode layer, to prepare organic barrier layer, organic barrier layer material is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, CuPc, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4 " tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine or 4,7-diphenyl-1,10-Phen;
(3) adopt the mode of vacuum evaporation to prepare inorganic barrier layer on organic barrier layer, the material of inorganic barrier layer is by a kind of composite material forming in a kind of and high-index material zinc sulphide, zinc selenide and cadmium sulfide in low-index material silica, magnesium fluoride and lithium fluoride, in inorganic barrier layer, low-index material silica, magnesium fluoride or lithium fluoride mass fraction are 40～60%;
(4) after step (3), adopt method and the material identical with step (2) to prepare organic barrier layer, on described organic barrier layer, adopt again method and the material that step (3) is identical to prepare inorganic barrier layer, by that analogy, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer;
(5) on described inorganic barrier layer surface, cover PETG film, then at PETG film edge coating packaging plastic, be cured with UV light, described organic electroluminescence device is encapsulated in described polyethylene terephthalate film and anode conducting substrate.
7. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, in described step (2), the thickness on organic barrier layer is 200nm～300nm, and in described step (3), the thickness of inorganic barrier layer is 100nm～200nm.
8. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, in described step (2), organic barrier layer vacuum evaporation condition is: vacuum degree 1 × 10
-5pa～1 × 10
-3pa, evaporation rate
9. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, in described step (3), inorganic barrier layer vacuum evaporation condition is: vacuum degree 1 × 10
-5pa～1 × 10
-3pa, evaporation rate
10. the preparation method of organic electroluminescence device as claimed in claim 6, is characterized in that, described organic barrier layer is identical with the inorganic barrier layer number of plies, is 4～6 layers.
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| CN108630822A (en) * | 2017-03-24 | 2018-10-09 | 京东方科技集团股份有限公司 | A kind of component and top emission OLED device of top emission OLED device |
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Application publication date: 20140416 |