CN103855315A - Organic light-emitting device and preparation method thereof - Google Patents
Organic light-emitting device and preparation method thereof Download PDFInfo
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- CN103855315A CN103855315A CN201210501265.0A CN201210501265A CN103855315A CN 103855315 A CN103855315 A CN 103855315A CN 201210501265 A CN201210501265 A CN 201210501265A CN 103855315 A CN103855315 A CN 103855315A
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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
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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
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- 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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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract
Provided in the invention is an organic light-emitting device comprising an anode conductive substrate, a functional layer, a light-emitting layer, a cathode layer and a packaging layer. The anode conductive substrate, the functional layer, the light-emitting layer, the cathode layer and the packaging layer are successively laminated; the anode conductive substrate and the packaging layer form an enclosed space; and the functional layer, the light-emitting layer, and the cathode layer are accommodated into the enclosed space. The packaging layer successively includes a protection layer, an inorganic blocking layer, an organic blocking layer, a cooling fin and a metal thin sheet. In addition, the invention also provides a preparation method of the organic light-emitting device. With the method, erosion on the organic light-emitting device by moisture and oxygen can be effectively reduced, so that the device organic functional material and the electrode can be effectively protected and thus the service life of the organic light-emitting device can be obviously prolonged. The method is especially suitable for packaging of a flexible organic light-emitting device.
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.In the time 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, thought to be most likely at by insider 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.Throw light on because the whole world is increasing 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.
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, and organic functional material and the electrode of protection organic electroluminescence device exempt from destruction, and 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, and described encapsulated layer comprises protective layer, inorganic barrier layer, organic barrier layer, fin and sheet metal successively;
The material of described inorganic barrier layer is the sulfide material doped with oxide material, and wherein, described sulfide material comprises tungsten disulfide (WS
2), molybdenum bisuphide (MoS
2), tantalum disulfide (TaS
2), curing niobium (NbS
2), antimonous sulfide (Sb
2s
3) or orpiment (As
2s
3) in one; Described oxide material comprises the one in calcium oxide (CaO), barium monoxide (BaO), strontium oxide strontia (SrO) or magnesium oxide (MgO), and the mass fraction of described oxide material in inorganic barrier layer is 20%～40%;
The material on described organic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin.
Inorganic barrier layer material is the composite material of sulfide and oxide, and compactness is high, and waterproof oxygen ability is strong, reduces the destruction that moisture produces device.
Preferably, the mass fraction of described oxide material in inorganic barrier layer is 30%.
Preferably, the thickness of described inorganic barrier layer is 80～150nm.
The existence on organic barrier layer can stop outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device on the one hand, can increase on the other hand the flexibility of encapsulated layer, prevent that crackle from appearring in encapsulated layer, simultaneously organic barrier layer have quality light, prepare the advantages such as easy; The pliability of encapsulated layer has been strengthened in the preparation that repeats on organic barrier layer.
Preferably, the thickness on described organic barrier layer is 1～1.5 μ m.
Preferably, alternately laminated 4～7 layers of described inorganic barrier layer and organic barrier layer.
The alternately laminated formation sandwich construction of organic barrier layer and inorganic barrier layer, water, oxygen permeation pathway are extended, can reach good packaging effect, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, make up the shortcoming on single inorganic barrier layer and single organic barrier layer, extended device lifetime.
The existence of protective layer can protect negative electrode to exempt from destruction in subsequent operation process.
Preferably; described 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 200～300nm.
Adopt sheet metal as fin, can improve device heat-sinking capability, extend device lifetime.
Preferably, the material of described fin is one or more in metallic aluminium, silver or copper, and thickness is 200～500nm.
Adopt sheet metal as cap, can improve device heat-sinking capability, intercept the corrosion of steam and oxygen, be applicable to flexible organic electroluminescent device, can encapsulation be dropped to minimum on the impact of light efficiency.
Preferably, the material of described sheet metal is the one in silver, aluminium, copper or gold.
At sheet metal edge-coating packaging plastic, be cured with UV light, described organic electroluminescence device is encapsulated in described sheet metal and substrate.
Preferably, described anode conducting substrate is conducting glass substrate or conduction organic film substrate.
More preferably, described anode conducting substrate is tin indium oxide (ITO) conducting glass 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, described cathode layer can be non-transparent metals negative electrode (aluminium, silver, gold etc.) layer or transparent cathode layer (dielectric layer/metal level/dielectric layer etc., as ITO/Ag/ITO, ZnS/Ag/ZnS etc.).
More preferably, described cathode layer is aluminium.
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, cathode layer and protective layer;
(2) adopt the method for magnetron sputtering on protective layer, to prepare inorganic barrier layer, the material of described inorganic barrier layer is the sulfide material doped with oxide material, and wherein, described sulfide material comprises WS
2, MoS
2, TaS
2, NbS
2, Sb
2s
3or As
2s
3in one; Described oxide material comprises the one in CaO, BaO, SrO or MgO, and the mass fraction of described oxide material in inorganic barrier layer is 20%～40%;
(3) adopt the method for first spin coating post-exposure on inorganic barrier layer, to prepare organic barrier layer, the material on described organic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin;
(4) adopt the method for vacuum evaporation to prepare fin on organic barrier layer, then covering metal thin slice on fin, at sheet metal edge-coating packaging plastic, be cured with UV light, described organic electroluminescence device is encapsulated in described sheet metal and substrate.
Step (2) adopts the method for magnetron sputtering on protective layer, to prepare inorganic barrier layer, and inorganic barrier layer material is the composite material that sulfide and oxide form, and compactness is high, and waterproof oxygen ability is strong, reduces the destruction that moisture produces device.
Preferably, sputtering target material when magnetron sputtering is the sulfide material doped with oxide material, and wherein, described sulfide material comprises WS
2, MoS
2, TaS
2, NbS
2, Sb
2s
3or As
2s
3in one; Described oxide material comprises the one in CaO, BaO, SrO or MgO, and the mass fraction of described oxide material in target is 20%～40%; Passing into gas is argon gas (Ar), and gas flow is 10～15sccm, and base vacuum degree is 1 × 10
-5～1 × 10
-3pa.
The existence on organic barrier layer can stop outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device on the one hand, can increase on the other hand the flexibility of encapsulated layer, prevent that crackle from appearring in encapsulated layer, simultaneously organic barrier layer have quality light, prepare the advantages such as easy.The pliability of encapsulated layer has been strengthened in the preparation that repeats on organic barrier layer.
Preferably, while adopting the method for first spin coating post-exposure to prepare organic barrier layer, preparation condition is: under inert atmosphere, behind the organic barrier layer of spin coating, be cured with UV light (λ=365nm), light intensity is 10～15mW/cm
2, the time for exposure is 200～300s.
Preferably, after step (3), adopt method and the material identical with step (2) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (3) is identical to prepare organic barrier layer, by that analogy, finally obtain the sandwich construction of alternately laminated 4～7 layers of formation of organic barrier layer and inorganic barrier layer;
The alternately laminated formation sandwich construction of organic barrier layer and inorganic barrier layer, water, oxygen permeation pathway are extended, can reach good packaging effect, effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, make up the shortcoming on single inorganic barrier layer and single organic barrier layer, extended device lifetime.
Method 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.
Preferably, when the method for employing vacuum evaporation is prepared protective layer, vacuum degree is 3 × 10
-5～8 × 10
-5pa, evaporation rate is
Adopt sheet metal as fin, can improve device heat-sinking capability, extend device lifetime.
Preferably, when the method for employing vacuum evaporation is prepared fin, vacuum degree is 3 × 10
-5～8 × 10
-5pa, evaporation rate
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.
Adopt sheet metal as cap, can improve device heat-sinking capability, intercept the corrosion of steam and oxygen, be applicable to flexible organic electroluminescent device, can encapsulation be dropped to minimum on the impact of light efficiency.
Preferably, on fin, when covering metal thin slice, at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), be then cured with UV light (λ=365nm), light intensity is 10～15mW/cm
2, the time for exposure is 300～400s; Described organic electroluminescence device is encapsulated in described sheet metal and substrate.
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 significantly the life-span of organic electroluminescence device;
(2) organic electroluminescence device water resistance of the present invention (WVTR) reaches 1.3E
-4g/m
2day, the life-span reaches more than 9,400 hours;
(3) the inventive method is applicable to the organic electroluminescence device that encapsulation is prepared take electro-conductive glass as anode substrate, also be 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 conducting glass substrate 1 pre-treatment: ITO conducting glass substrate 1 is put into acetone, ethanol, deionized water, ethanol successively, and ultrasonic cleaning 5 minutes, then dries up with nitrogen respectively, 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 conducting glass substrate 1 thickness is 100nm;
(2) preparation of functional layer and luminescent layer:
Hole injection layer 2: evaporation MoO on ITO conducting 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, when evaporation, vacuum degree is 3 × 10
-5pa, evaporation rate is
obtain hole injection layer 2, thickness is 10nm;
Hole transmission layer 3: adopt 4,4', 4 " tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, evaporation TCTA on hole injection layer 2, vacuum degree is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 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, and vacuum degree is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 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, and vacuum degree is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 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 is 30%, vacuum degree is 3 × 10
-5pa, evaporation rate is
evaporation thickness is 20nm;
(3) preparation of cathode layer 7: evaporation metal negative electrode 7 on electron injecting layer 6, metallic cathode 7 adopts aluminium (Al), and thickness is 100nm, and evaporation vacuum degree is 5 × 10
-5pa, evaporation rate is
(4) preparation of protective layer 801: adopt the method for vacuum evaporation to prepare CuPc on cathode layer 7, vacuum degree is 3 × 10
-5pa, evaporation rate is
thickness is 200nm;
(5) preparation of inorganic barrier layer 802: adopt the method for magnetron sputtering to prepare inorganic barrier layer 802 on protective layer 801, the material of inorganic barrier layer 802 is WS
2with the composite material of CaO, the mass fraction that CaO accounts for inorganic barrier layer 802 is 30%, and sputtering target material is WS
2with the composite material of CaO, the mass fraction that CaO accounts for target is 30%, and passing into gas is Ar, and Ar flow is 15sccm, and base vacuum degree is 1 × 10
-5pa, thickness is 80nm;
(6) preparation on organic barrier layer 803: adopt the method for first spin coating post-exposure to prepare organic barrier layer 803 on inorganic barrier layer 802, the material on organic barrier layer 803 is polytetrafluoroethylene, under inert atmosphere, make, gluing thickness is 1 μ m, then be cured with UV light (λ=365nm), light intensity is 10mW/cm
2, the time for exposure is 300s;
(7) inorganic barrier layer 804, 806, 808 and organic barrier layer 805, 807, 809 preparation: adopt method and the material identical with step (5) to prepare inorganic barrier layer 804 after step (6) on organic barrier layer 803, on inorganic barrier layer 804, adopt again method and the material that step (6) is identical to prepare organic barrier layer 805, on organic barrier layer 805, adopt method and the material identical with step (5) to prepare inorganic barrier layer 806, adopt method and the material that step (6) is identical to prepare organic barrier layer 807 at inorganic barrier layer 806, on organic barrier layer 807, adopt method and the material identical with step (5) to prepare inorganic barrier layer 808, on inorganic barrier layer 808, adopt method and the material that step (6) is identical to prepare organic barrier layer 809, 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.
(8) preparation of fin 810: adopt the method for vacuum evaporation to prepare metallic aluminium on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, vacuum degree is 8 × 10
-5pa, evaporation rate is
thickness is 200nm;
(9) covering of sheet metal 811: covering metal thin slice 811 on fin 810, sheet metal material is silver, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s; Organic electroluminescence device is encapsulated in sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 3.2E
-4, the life-span of organic electroluminescence device is 9515h(T70@1000cd/m
2).
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 conducting 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 801, 4 layers of inorganic barrier layer 802, 804, 806, 808, 4 layers of organic barrier layer 803, 805, 807, 809, fin 810 and sheet metal 811, ITO conducting glass substrate 1 and sheet metal 811 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, protective layer 801, inorganic barrier layer 802, 804, 806, 808, organic barrier layer 803, 805, 807, 809, fin 810 is 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 the method for vacuum evaporation to prepare NPB on cathode layer, vacuum degree is 8 × 10
-5pa, evaporation rate is
thickness is 300nm;
(5) preparation of inorganic barrier layer: adopt the method for magnetron sputtering to prepare inorganic barrier layer on protective layer, the material of inorganic barrier layer is MoS
2with the composite material of BaO, the mass fraction that BaO accounts for inorganic barrier layer is 25%, and sputtering target material is MoS
2with the composite material of BaO, the mass fraction that BaO accounts for target is 25%, and passing into gas is Ar, and Ar flow is 10sccm, and base vacuum degree is 2 × 10
-4pa, thickness is 120nm;
(6) preparation on organic barrier layer: adopt the method for first spin coating post-exposure to prepare organic barrier layer on inorganic barrier layer, the material on organic barrier layer is methacrylic resin, under inert atmosphere, make, gluing thickness is 1.5 μ m, then be cured with UV light (λ=365nm), light intensity is 15mW/cm
2, the time for exposure is 200s;
(7) after step (6), adopt method and the material identical with step (5) to prepare inorganic barrier layer, on inorganic barrier layer, adopt again method and the material that step (6) 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.
(8) preparation of fin: adopt the method for vacuum evaporation to prepare argent on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 500nm;
(9) covering of sheet metal: covering metal thin slice on fin, sheet metal material is aluminium, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured with UV light (λ=365nm), light intensity is 10mW/cm
2, the time for exposure is 400s; Organic electroluminescence device is encapsulated in sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 2.7E
-4, the life-span of organic electroluminescence device is 9,914h(T70@1000cd/m
2).
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: adopt the method for vacuum evaporation to prepare Alq on cathode layer
3, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 250nm;
(5) preparation of inorganic barrier layer: adopt the method for magnetron sputtering to prepare inorganic barrier layer on protective layer, the material of inorganic barrier layer is TaS
2with the composite material of SrO, the mass fraction that SrO accounts for inorganic barrier layer is 40%, and sputtering target material is TaS
2with the composite material of SrO, the mass fraction that SrO accounts for target is 40%, and passing into gas is Ar, and Ar flow is 12sccm, and base vacuum degree is 1 × 10
-3pa, thickness is 150nm;
(6) preparation on organic barrier layer: adopt the method for first spin coating post-exposure to prepare organic barrier layer on inorganic barrier layer, the material on organic barrier layer is cycloaliphatic epoxy resin, under inert atmosphere, make, gluing thickness is 1.2 μ m, then be cured with UV light (λ=365nm), light intensity is 11mW/cm
2, the time for exposure is 230s;
(7) after step (6), adopt method and the material identical with step (5) to prepare inorganic barrier layer, on inorganic barrier layer, adopt again method and the material that step (6) 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.
(8) preparation of fin: adopt the method for vacuum evaporation to prepare argent on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, vacuum degree is 3 × 10
-5pa, evaporation rate is
thickness is 300nm;
(9) covering of sheet metal: covering metal thin slice on fin, sheet metal material is copper, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured with UV light (λ=365nm), light intensity is 15mW/cm
2, the time for exposure is 300s; Organic electroluminescence device is encapsulated in sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 3.4E
-4, the life-span of organic electroluminescence device is 9,406h(T70@1000cd/m
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 the method for vacuum evaporation to prepare SiO on cathode layer, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 200nm;
(5) preparation of inorganic barrier layer: adopt the method for magnetron sputtering to prepare inorganic barrier layer on protective layer, the material of inorganic barrier layer is NbS
2with the composite material of MgO, the mass fraction that MgO accounts for inorganic barrier layer is 40%, and sputtering target material is NbS
2with the composite material of MgO, the mass fraction that MgO accounts for target is 40%, and passing into gas is Ar, and Ar flow is 11sccm, and base vacuum degree is 2 × 10
-4pa, thickness is 100nm;
(6) preparation on organic barrier layer: adopt the method for first spin coating post-exposure to prepare organic barrier layer on inorganic barrier layer, the material on organic barrier layer is polytetrafluoroethylene, under inert atmosphere, make, gluing thickness is 1 μ m, then be cured with UV light (λ=365nm), light intensity is 10mW/cm
2, the time for exposure is 200s;
(7) after step (6), adopt method and the material identical with step (5) to prepare inorganic barrier layer, on inorganic barrier layer, adopt again method and the material that step (6) 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;
(8) preparation of fin: adopt the method for vacuum evaporation to prepare albronze on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, the mass ratio of copper and aluminium is 3:1, and vacuum degree is 5 × 10
-5pa, thickness is 500nm;
(9) covering of sheet metal: covering metal thin slice on fin, sheet metal material is gold, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured with UV light (λ=365nm), light intensity is 11mW/cm
2, the time for exposure is 350s; Organic electroluminescence device is encapsulated in sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 2.5E
-4, the life-span of organic electroluminescence device is 10,117h(T70@1000cd/m
2).
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: adopt the method for vacuum evaporation to prepare MgF on cathode layer
2, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 300nm;
(5) preparation of inorganic barrier layer: adopt the method for magnetron sputtering to prepare inorganic barrier layer on protective layer, the material of inorganic barrier layer is Sb
2s
3with the composite material of MgO, the mass fraction that MgO accounts for inorganic barrier layer is 40%, and sputtering target material is Sb
2s
3with the composite material of MgO, the mass fraction that MgO accounts for target is 40%, and passing into gas is Ar, Ar flow 10sccm, and base vacuum degree is 2 × 10
-4pa, thickness is 150nm;
(6) preparation on organic barrier layer: adopt the method for first spin coating post-exposure to prepare organic barrier layer on inorganic barrier layer, the material on organic barrier layer is methacrylic resin, under inert atmosphere, make, gluing thickness is 1.5 μ m, then be cured with UV light (λ=365nm), light intensity is 15mW/cm
2, the time for exposure is 200s;
(7) after step (6), adopt method and the material identical with step (5) to prepare inorganic barrier layer, on inorganic barrier layer, adopt again method and the material that step (6) 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;
(8) preparation of fin: adopt the method for vacuum evaporation to prepare metallic aluminium on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 300nm;
(9) covering of sheet metal: covering metal thin slice on fin, sheet metal material is aluminium, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured with UV light (λ=365nm), light intensity is 15mW/cm
2, the time for exposure is 400s; Organic electroluminescence device is encapsulated in described sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 1.3E
-4, the life-span of organic electroluminescence device is 11,604h(T70@1000cd/m
2).
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 the method for vacuum evaporation to prepare ZnS on cathode layer, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 250nm;
(5) preparation of inorganic barrier layer: adopt the method for magnetron sputtering to prepare inorganic barrier layer on protective layer, the material of inorganic barrier layer is As
2s
3with the composite material of MgO, the mass fraction that MgO accounts for inorganic barrier layer is 20%, and sputtering target material is As
2s
3with the composite material of MgO, the mass fraction that MgO accounts for target is 20%, and passing into gas is Ar, and Ar flow is 11sccm, and base vacuum degree is 2 × 10
-4pa, thickness is 120nm;
(6) preparation on organic barrier layer: adopt the method for first spin coating post-exposure to prepare organic barrier layer on inorganic barrier layer, the material on organic barrier layer is cycloaliphatic epoxy resin, under inert atmosphere, make, gluing thickness is 1.2 μ m, then be cured with UV light (λ=365nm), light intensity is 11mW/cm
2, the time for exposure is 230s;
(7) after step (6), adopt method and the material identical with step (5) to prepare inorganic barrier layer, on inorganic barrier layer, adopt again method and the material that step (6) is identical to prepare organic barrier layer, by that analogy, make inorganic barrier layer and organic barrier layer number of plies respectively reach 7 layers, finally obtain the sandwich construction of organic barrier layer and the alternately laminated formation of inorganic barrier layer;
(8) preparation of fin: adopt the method for vacuum evaporation to prepare metallic aluminium on the sandwich construction surface of inorganic barrier layer and the alternately laminated formation in organic barrier layer, vacuum degree is 5 × 10
-5pa, evaporation rate is
thickness is 300nm;
(9) covering of sheet metal: covering metal thin slice on fin, sheet metal material is silver, then at sheet metal edge-coating packaging plastic, by the dry sclerosis of the mode packaging plastic of ultraviolet curing (UV-Curing), then be cured with UV light (λ=365nm), light intensity is 11mW/cm
2, the time for exposure is 350s; Organic electroluminescence device is encapsulated in sheet metal and substrate.
Water oxygen permeability (WVTR, the g/m of the present embodiment organic electroluminescence device
2day) be 1.8E
-4, the life-span of organic electroluminescence device is 11,220h(T70@1000cd/m
2).
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 is embodiment 1 ~ 6 organic electroluminescence device water oxygen permeability, and table 2 is embodiment 1 ~ 6 organic electro-luminescence device lifetime situations.
Table 1. embodiment 1 ~ 6 organic electroluminescence device water oxygen permeability
| |
Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| WVTR(g/m 2/day) | 3.2E -4 | 2.7E -4 | 3.4E -4 | 2.5E -4 | 1.3E -4 | 1.8E -4 |
Table 2. embodiment 1 ~ 6 organic electro-luminescence device lifetime situation
As can be seen from Table 1, the water oxygen permeability of organic electroluminescence device of the present invention (WVTR) reaches 1.3E
-4g/m
2day, as can be seen from Table 2, the life-span of organic electroluminescence device of the present invention reaches 9,406 hours above (T70@1000cd/m
2).
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; 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 protective layer, inorganic barrier layer, organic barrier layer, fin and sheet metal successively;
The material of described inorganic barrier layer is the sulfide material doped with oxide material, and wherein, described sulfide material comprises the one in tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; Described oxide material comprises the one in calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and the mass fraction of described oxide material in inorganic barrier layer is 20%～40%;
The material on described organic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, in described inorganic barrier layer, the mass fraction of oxide material in inorganic barrier layer is 30%.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described inorganic barrier layer is 80～150nm, and the thickness on described organic barrier layer is 1～1.5 μ m.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, alternately laminated 4～7 layers of described inorganic barrier layer and organic barrier layer.
5. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described fin is one or more in metallic aluminium, silver and copper, and thickness is 200～500nm.
6. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described sheet metal is the one in silver, aluminium, copper or gold.
7. 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 successively functional layer, luminescent layer, cathode layer and protective layer;
(2) adopt the method for magnetron sputtering on protective layer, to prepare inorganic barrier layer, the material of described inorganic barrier layer is the sulfide material doped with oxide material, wherein, described sulfide material comprises the one in tungsten disulfide, molybdenum bisuphide, tantalum disulfide, curing niobium, antimonous sulfide or orpiment; Described oxide material comprises the one in calcium oxide, barium monoxide, strontium oxide strontia or magnesium oxide, and the mass fraction of described oxide material in inorganic barrier layer is 20%～40%;
(3) adopt the method for first spin coating post-exposure on inorganic barrier layer, to prepare organic barrier layer, the material on described organic barrier layer is polytetrafluoroethylene, methacrylic resin or cycloaliphatic epoxy resin;
(4) adopt the method for vacuum evaporation to prepare fin on organic barrier layer, then covering metal thin slice on fin, at sheet metal edge-coating packaging plastic, be cured with UV light, described organic electroluminescence device is encapsulated in described sheet metal and substrate.
8. the preparation method of organic electroluminescence device as claimed in claim 7, is characterized in that, it is argon gas that described step (2) passes into gas, gas flow 10～15sccm, and base vacuum degree is 1 × 10
-5～1 × 10
-3pa.
9. the preparation method of organic electroluminescence device as claimed in claim 7, is characterized in that, the condition on the organic barrier layer of preparation is in described step (3): under inert atmosphere, behind the organic barrier layer of spin coating, be cured with UV light, light intensity is 10～15mW/cm
2, the time for exposure is 200～300s.
10. the preparation method of organic electroluminescence device as claimed in claim 7, it is characterized in that, after step (3), adopt method and the material identical with step (2) to prepare inorganic barrier layer, on described inorganic barrier layer, adopt again method and the material that step (3) is identical to prepare organic barrier layer, by that analogy, finally obtain the sandwich construction of alternately laminated 4～7 layers of formation of organic barrier layer and inorganic barrier layer.
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| CN110850622A (en) * | 2019-11-21 | 2020-02-28 | 京东方科技集团股份有限公司 | Display panel, preparation method thereof and display device |
| CN110993814A (en) * | 2019-11-15 | 2020-04-10 | 深圳市华星光电半导体显示技术有限公司 | Display device and method for manufacturing the same |
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