CN103066214B - A kind of organic electroluminescence device and preparation method thereof - Google Patents
A kind of organic electroluminescence device and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of organic electroluminescence device and preparation method thereof, wherein organic electroluminescence device includes scattering layer, and the material of described scattering layer comprises following component: the first particle diameter scattering particles: 10-60 weight portion；Second particle diameter scattering particles: 5-30 weight portion；Dispersant: 1-60 weight portion；Photoresist: 0-60 weight portion.The particle diameter ratio of described first particle diameter scattering particles and the second particle diameter scattering particles is 4: 1-800: 1.Adopt the such scheme of the present invention, it is possible to be effectively improved the light output efficiency of organic electroluminescence device, it is also possible to be effectively improved the flatness of scattering film.
Description
Technical field
The present invention relates to organic electroluminescence device technical field, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
OLED (OrganicLight-EmittingDiode) i.e. Organic Light Emitting Diode, it arranges luminescence unit on substrate, and luminescence unit includes two electrodes, is provided with electroluminescent material layer between two electrodes.In the prior art, being typically chosen clear glass as substrate, and the refractive index of glass is generally 1.4-1.5, the refractive index of electroluminescent organic material layer is generally 1.7-1.8.Therefore the light that electroluminescent organic material energising sends, air is entered through glass, due to total reflection principle, have most light and be confined in electroluminescent organic material layer, this causes that the light output efficiency of OLED is substantially reduced, only about 20%, there is the light of 80% to be confined or loss cannot rationally be applied in the inside of the electroluminescent organic material of OLED.Therefore the light output efficiency how improving OLED becomes the research and development focus of technical staff.
About the light output efficiency how improving OLED, existing a lot of documents disclose different technical schemes, as existing patent documentation CN102299266A discloses substrate and the manufacture method of a kind of organic electroluminescence device, it includes transparent substrates, having scattering layer at least side of transparent substrates, scattering layer is by TiO2、SiO2Or the nanoparticle of ZnO is constituted, the inner side of transparent substrates is connected with electrode.The manufacture method of this organic electroluminescence device substrate is, is provided with transparent substrates, forms scattering layer in transparent substrates side by sol-gel or hydro-thermal method, and scattering layer is by TiO2、SiO2Or the nanoparticle of ZnO is constituted, the inner side of transparent substrates is provided with electrode by deposition.In technique scheme, by the OLED substrate that hydro-thermal method or sol-gel process produce, change the direction of propagation of light by arranging scattering layer, increase the probability that light is propagated forward the efficiency improving optical coupling, the TiO on scattering layer2、SiO2Or the nanoparticle of ZnO forms the transparent arrays of flakey, column or tubulose, there is higher refractive index, be more beneficial for changing the round of light, improve the light extraction efficiency of OLED.
Wherein, it is a kind of method from growth from solution crystal that hydro-thermal method prepares crystal, its ultimate principle be by material dissolution in water equal solvent, take adequate measures to cause the supersaturation of solution so that crystal forming core wherein also grows.
And sol-gel process prepares the one that film material belongs in wet chemistry method.It is generally referred to as and metallic compound (including metal alkoxide and metal inorganic salt) and catalyst, chelating agen and water etc. are made colloidal sol, then pass through whirl coating, spraying or impregnating method and be coated on substrate by alkoxide sol masking, hydrolysis and polymerization is there is in alkoxide after absorbing the moisture in air, gradually become gel, eventually pass the process that dry, sintering etc. processes.
Technique scheme is simply write out the broad method preparing scattering layer, and has not provided this process how preparing scattering layer.And the quality of the film forming of scattering layer will directly influence the light extraction efficiency of OLED.And the factor that affects scattering layer quality of forming film is a lot, wherein topmost being how selects the component of each material to carry out the proportioning solution for film forming.
For film forming solution, how to select the content of solute to ensure that the scattering layer prepared can have good flatness and improve light outgoing efficiency, be prior art does not have disclosed in.The too high meeting of solutes content causes that solvent film forming or the scattering film surface for preparing cannot have particulate matter out-of-flatness, there is big granule on scattering film surface, and OLED exists the defect of short circuit, poor stability etc.；And the too low meeting of solutes content causes that solvent institute film forming layer does not possess the effect of scattering；Therefore the content how determining solute is the emphasis that those skilled in the art study.
For this, applicant has submitted patent application " preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency " application number on May 31st, 2012: CN201210175471.7, the preparation method that it is disclosed that a kind of high index of refraction scattering layer, comprise the steps: S1, prepare grinding distribution liquid, described grinding distribution liquid includes: high index of refraction scattering particles, and its mass percent is: 10%-60%；Dispersant, its quality accounts for the 1%-60% of described high index of refraction scattering particles；Anti-settling agent, its mass percent is: 0-5%；Photoresist, its mass percent is: 0-60%；Organic solvent, its mass percent is: 20%-89.9%；S2, employing filtering holes aperture, at the grinding distribution liquid prepared of step S1 described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain film making solution；Described film making solution prepared by S3, described step S2 prepares high index of refraction scattering layer through photoetching spin coating.
Although rationally have selected the mass ratio relation of the mass percent of high index of refraction scattering particles and dispersant and high index of refraction scattering particles so that after prepared by the high index of refraction scattering layer that the program provides, there is good flatness and dispersion effect.But applicant found in the later stage, utilize the scattering layer that said method prepares, in the interface that scattering layer and luminescent layer join, owing to the refractive index ratio of photoresist is relatively low, make light beam from luminescent layer incide scattering layer time, having total reflection in the interface of two-layer handing-over to occur, a part of light can not export, and light output efficiency is high not enough；Additionally, adopt single particle size scattering particles, the flatness of the high index of refraction scattering layer prepared can be influenced by certain impact.Therefore, in such scheme, the space that also can promote in improving light output efficiency and flatness two.
Summary of the invention
The technical problem to be solved is the scattering layer that in prior art, the preparation method of scattering layer obtains, affect light output efficiency owing to the refractive index of photoresist is relatively low and affect the flatness of scattering film owing to there is gap between height refraction scattering particles particle diameter, thus providing a kind of by rationally selecting different-grain diameter scattering particles to be equipped with film making solution with organic electroluminescence device that is that prepare the light extraction efficiency of scattering layer raising OLED and that improve scattering layer flatness and preparation method thereof.
For solving above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of organic electroluminescence device, including substrate and the scattering layer sequentially formed on the substrate, the first electrode, organic function layer and the second electrode, the material of described scattering layer comprises following component:
First particle diameter scattering particles: 10-60 weight portion；
Second particle diameter scattering particles: 5-30 weight portion；
Dispersant: 1-60 weight portion；
Photoresist: 0-60 weight portion；
The particle diameter ratio of described first particle diameter scattering particles and described second particle diameter scattering particles is 4: 1-800: 1.
The particle diameter of described first particle diameter scattering particles is 200nm-800nm；
The particle diameter of described second particle diameter scattering particles is 1nm-50nm.
The particle diameter of described first particle diameter scattering particles is 350nm-450nm；
The particle diameter of described second particle diameter scattering particles is 15nm-35nm.
Wherein said organic function layer may select independent luminescent layer, can also being made up of luminescent layer and functional layer, functional layer therein includes the one or more combination in hole injection layer, electronic barrier layer, hole transmission layer, electron transfer layer, hole blocking layer, electron injecting layer.
Wherein luminescent layer can be HONGGUANG, green glow or blue light.The main body RH of HONGGUANG is Bebq2(double; two (10-hydroxy benzo [h] quinoline) beryllium), dyestuff RD are Ir (piq)2(acac)；The main body GH of green glow is CBP (4,4 '-Bis (9H-carbazol-9-yl) biphenyl), dyestuff GD is Ir (ppy)3；Blue light main body BH is AND (9,10-Di (naphtha-2-yl) anthracene), dyestuff BD is DPAVB (4-(di-p-tolylamino)-4 '-[(di-p-tolylamino) styryl] stilbene)；Electron transfer layer is Bphen.
The material of described first particle diameter scattering particles and described second particle diameter scattering particles can be the same or different, and is respectively selected from TiO2、ZrO2、SiO2, a kind of or wherein several mixture in SiO, TiO.
The thickness of described scattering layer is 0.3 μm-3 μm.
Described dispersant is titanium white dispersant.
The light transmittance of described photoresist is 80%-99%.
A kind of method preparing above-mentioned organic electroluminescence device, comprises the steps:
S1: by base-plate cleaning, drying；
S2: form scattering layer on the substrate；
S3: evaporation forms the first electrode, organic function layer and the second electrode successively on described scattering layer；
S4: be coated with packaging plastic around described organic function layer, cap be fastened on described packaging plastic and be packaged.
The step forming described scattering layer in described step S2 is as follows:
S21, preparing grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S22, employing filter paper aperture, at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain film making solution；
S23, described film making solution are spun on described substrate through photoetching and obtain described scattering layer.
The step forming described scattering layer in described step S2 is as follows:
S2A, preparing grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant and photoresist, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S2B, employing filter paper aperture, at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain film making solution；
S2C, described film making solution are spun on described substrate through photoetching and obtain described scattering layer.
The step forming described scattering layer in described step S2 is as follows:
S2a, preparing grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S2b, employing filter paper aperture, at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain preformed solution；
S2c, in described preformed solution add photoresist mixing after obtain film making solution；
S2d, described film making solution are spun on described substrate through photoetching and obtain described scattering layer.
Described filter paper aperture is 0.8 μm.
Before described step S4, also comprise the steps:
A1: with the described scattering layer of described packaging plastic corresponding region when being etched away encapsulation.
Before described step S4, also comprise the steps:
A2: when being etched away encapsulation with described packaging plastic corresponding region and outside described scattering layer.
The technique scheme of the present invention has the advantage that compared to existing technology
(1) organic electroluminescence device of the present invention, scattering layer therein has the first particle diameter scattering particles and the second particle diameter scattering particles, and the first particle diameter and the second particle diameter are different, the two varies, and the particle diameter ratio of the first particle diameter scattering particles and the second particle diameter scattering particles is 4: 1-800: 1.When so there is space between the first particle diameter scattering particles, it is possible to fill space by the second particle diameter scattering particles, thus can improve the flatness of scattering film.And, doped with after the second scattering particles among photoresist, the refractive index on scattering film surface can be improved, make light from luminescent layer incide scattering layer time, not only by the first particle diameter scattering particles, light can be scattered, can also reducing light by the scattering film surface after improving refractive index and the probability of total reflection occurs, the two combines and light output efficiency can be made to be effectively improved.
(2) organic electroluminescence device of the present invention, select the scattering particles of the first particle diameter scattering particles 200nm-800nm and the scattering particles of the second particle diameter scattering particles 1nm-50nm, second particle diameter is when 1nm-50nm, the refractive index of the scattering film formed after coordinating with photoresist can improve a lot, and the first particle diameter is at least four times of the second particle diameter, the second particle diameter can play the effect better filling space.
(3) in the method preparing organic electroluminescence device of the present invention, when preparing scattering layer, can select to add photoresist makes the scattering layer prepared have better flatness, and in order to prevent from losing most photoresist when filtering, can select first by the first particle diameter scattering particles, second particle diameter scattering particles, dispersant is dissolved in organic solvent to be ground in dispersion liquid the particle diameter granule less than 1 μm and accounts for more than the 80% of integral particle quantitative proportion, after filter paper filtering, add photoresist be mixed to get film making solution, adopt such step can avoid the loss of photoresist.
(4) method preparing organic electroluminescence device provided in the present invention, the scattering layer corresponding owing to being etched away packaging plastic, the OLED after encapsulation can be made to have better seal performance, because the air in the external world and moisture are likely scattered that layer enters causes inside OLED that the luminous organic material water suction in OLED was lost efficacy or oxidized, if therefore scattering layer corresponding for packaging plastic can be etched away during encapsulation, it is possible to effectively prevent the luminous organic material water suction in OLED to lose efficacy or oxidized.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below in conjunction with accompanying drawing, the present invention is further detailed explanation, wherein,
Fig. 1 is the embodiment of the present invention 1 OLED side view containing scattering layer；
Fig. 2 be the embodiment of the present invention 4 etching remove packaging plastic corresponding region and outside OLED side view.
Fig. 3 is the OLED side view that the embodiment of the present invention 5 etching removes encapsulation corresponding region scattering layer；
Wherein accompanying drawing is labeled as: 1-substrate, 2-scattering layer, 3-the first electrode, 4-organic function layer, 5-the second electrode, 6-packaging plastic, 7-cap.
Detailed description of the invention
Embodiment 1
The present embodiment provides a kind of organic electroluminescence device, including substrate 1 and scattering layer the 2, first electrode 3 sequentially formed on described substrate 1, organic function layer 4 and the second electrode 5, described scattering layer 2 is prepared from by following component: the first particle diameter scattering particles: 18 weight portions；Second particle diameter scattering particles: 9 weight portions；Dispersant: 8 weight portions；Photoresist: 60 weight portions；The particle diameter of described first particle diameter scattering particles and the second particle diameter scattering particles is than for 20:1.
The present embodiment provides a kind of method preparing above-mentioned organic electroluminescence device, comprises the steps:
S1: substrate 1 is cleaned, dries；
S2: form scattering layer 2 on described substrate 1；
S3: evaporation forms the first electrode 3, organic function layer 4 and the second electrode 5 successively on described scattering layer 2；
Utilize the first electrode layer that vapour deposition method prepares ITO；Described first electrode layer etches the first electrode 3；ITO target is indium stannum alloy, its component ratio In:Sn=90%:10%.In preparation process, partial pressure of oxygen is 0.4Sccm, and argon partial pressure is 20Sccm；
The process preparing organic function layer 4 on described first electrode 3 is as follows: be deposited with hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer successively on described first electrode 3；Evaporation process middle chamber pressure is lower than 5.0 × 10-3Pa, first evaporation 40nm thickness NPB is as hole transmission layer；Being deposited with ADN and TBPe thick for 30nm as luminescent layer using the method that double source steams altogether, it is 7% that through-rate controls TBPe ratio in ADN；The Alq3 of evaporation 20nm is as electron transfer layer；The LiF of evaporation 0.5nm is as electron injecting layer；Described organic function layer 4 is deposited with the Al of 150nm as the second electrode 5；
S4: be coated with packaging plastic 6 around described organic function layer 4, cap 7 be fastened on described packaging plastic 6 and be packaged.
Wherein, when preparing described scattering layer 2, adopt following steps:
S1, prepare grinding distribution liquid: by the first particle diameter scattering particles TiO2, the second particle diameter scattering particles TiO2, titanium white dispersant, photoresist be dissolved in organic solvent and grind 3 hours so that the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion.
In the present embodiment, described first particle diameter scattering particles and described second particle diameter scattering particles are all chosen as TiO2, described first particle diameter scattering particles 400nm, its weight is chosen as 15g, accounts for 18 weight portions；Described second particle diameter scattering particles 20nm, its weight is chosen as 7.5g, and it accounts for 9 weight portions；Described titanium white dispersant is used for disperseing described first particle diameter scattering particles and described second particle diameter scattering particles, such as can select afcma-4010, disperbyk-110, disperbyk-180, disperbyk-163, dispers655, dispers628 etc. that Byk Chemie GmbH produces, its weight is chosen as 1.2g, and it accounts for 8 weight portions；Described organic solvent selects propylene glycol methyl ether acetate, and its weight is chosen as 60g；
The above-mentioned solution prepared is put in grinding pot, fixes grinding pot and grind post, adding 90ml zirconium pearl (note: the amount of zirconium pearl is depending on the volume of grinding pot), with gauze elimination zirconium pearl after grinding 3 hours, prepare described grinding distribution liquid；
As organic solvent, as long as above-mentioned material can be dissolved and the solvent that do not react with above-mentioned material can properly select use.Therefore except propylene glycol methyl ether acetate, it is also possible to select:
The alcohols such as methanol, ethanol, benzyl alcohol；
(gathering) alkane glycol monoalkyl ethers such as glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol propyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diglycol monotertiary n-butyl ether, triethylene glycol monomethyl ether, 2,2'-ethylenedioxybis(ethanol). list ether, propylene glycol monomethyl ether, dihydroxypropane single-ether, dipropylene glycol monomethyl ether, DPE, dipropylene glycol list positive propyl ether, dipropylene glycol mono-n-butyl ether, Tripropylene glycol monomethyl Ether, tripropylene glycol list ether；
(gathering) alkane glycol monoalkyl acetate esters such as ethylene glycol monomethyl ether acetate, ethylene glycol monoethylether acetate, ethylene glycol propyl ether acetas, ethylene glycol mono-n-butyl ether acetas, diethylene glycol monomethyl ether acetas, diethylene glycol monoethyl ether acetas, diglycol monotertiary positive propyl ether acetas, diglycol monotertiary n-butyl ether acetas, the third diethylene glycol monomethyl ether acetas, propylene glycol monoethyl ether acetate, 3-methoxybutyl acetas；
Other ethers such as diethylene glycol dimethyl ether, diethylene glycol methyl ethyl ether, diethyl carbitol, oxolane；
The ketones such as oneself-2-ketone of methyl ethyl ketone, cyclohexanone, 2-heptanone, 3-heptanone, DAA (4-hydroxy-4-methyl penta-2-ketone), 4-hydroxy-4-methyl；
The oxalic acid esters such as propylene-glycol diacetate, 1,3 butylene glycol diacetate esters, 1,6-HD diacetate esters；
The lactic acid alkyl ester class such as methyl lactate, ethyl lactate；
Ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, formic acid n-pentyl ester, acetic acid isopentyl ester, 3-methoxybutyl acetas, 3-methyl-3-methoxybutyl acetas, n-butyl propionate, 3-methyl-3-methoxybutyl propionic ester, ethyl n-butyrate., propyl butyrate, isopropyl isobutyrate, the positive butyl ester of butanoic acid, hydroxyl ethyl acetate, ethoxy ethyl acetate, 3-methoxy methyl propionate, 3-methoxypropionate, 3-ethoxypropanoate, 3-ethoxyl ethyl propionate, methyl pyruvate, ethyl pyruvate, acetone acid n-propyl, methyl acetoacetate, ethyl acetoacetate, 2-hydroxy-2-methyl ethyl propionate, 2-hydroxy-3-methyl methyl butyrate, 2-supports for other esters such as ethyl n-butyrate .s；
Toluene, dimethylbenzene etc. are aromatic hydrocarbon based；
The amide-types such as N-Methyl pyrrolidone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide；
In these solvents, from dissolubility, pigment-dispersing, coating angularly sets out, preferred benzyl alcohol, ethylene glycol mono-n-butyl ether, propylene glycol monomethyl ether, dihydroxypropane single-ether, ethylene glycol monomethyl ether acetate, ethylene glycol mono-n-butyl ether acetas, diglycol monotertiary n-butyl ether acetas, propylene glycol methyl ether acetate, propylene glycol monoethyl ether acetate, diethylene glycol dimethyl ether, diethylene glycol methyl ethyl ether, Ketohexamethylene, 2-heptanone, 3-heptanone, propylene-glycol diacetate, 1, 3-butanediol diacetate esters, n-butyl acetate, isobutyl acetate, formic acid n-pentyl ester, isoamyl acetate, 3-methoxybutyl acetas, n-buty formate, ethyl n-butyrate., isopropyl isobutyrate, the positive butyl ester of butanoic acid, 3-methoxypropionate, 3-ethoxypropanoate, 3-ethoxyl ethyl propionate, 3-methyl-3-methoxybutyl propionic ester, ethyl pyruvate etc..
Above-mentioned solvent can independent or two or more mixing use.
Furthermore it is also possible to be used in conjunction the high boiling solvents such as benzylisoeugenol, di-n-hexyl ether, acetonyl acetone, isophorone, caproic acid, sad, 1-capryl alcohol, 1 nonyl alcohol, benzyl acetate, ethyl benzoate, ethyl oxalate, ethyl maleate., gamma-butyrolacton, ethylene carbonate, propylene carbonate, ethylene glycol list phenyl ether acetate together with above-mentioned solvent.Above-mentioned high boiling solvent can independent or two or more mixing use.
S2, employing filtering holes aperture, at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm, obtain film making solution；
S3, described film making solution prepare 2 μm of scattering layers through photoetching spin coating.
Adopting the OLED that in the present embodiment prepared by preparation method, its structure is as shown in Figure 1.
Embodiment 2
The present embodiment does following improvement on the basis of embodiment 1, and in the present embodiment, when preparing described scattering layer 2, described first particle diameter scattering particles are chosen as ZrO2, its particle diameter is 800nm, accounts for 10 weight portions；Described second particle diameter scattering particles are chosen as ZrO2, its particle diameter is 50nm, accounts for 30 weight portions；Titanium white dispersant, accounts for 20 weight portions；
Propylene glycol methyl ether acetate is as organic solvent, and weight is chosen as 70g；
The thickness of described scattering layer is 0.3 μm in the present embodiment.
Embodiment 3
The present embodiment does following improvement on the basis of embodiment 1, the method preparing described scattering layer 2 that the present embodiment provides, and comprises the steps:
S2A: selecting described first particle diameter scattering particles is SiO2, its particle diameter is 200nm, accounts for 60 weight portions；Described second particle diameter scattering particles are chosen as SiO2, its particle diameter is 1nm, accounts for 5 weight portions；Described titanium white dispersant is: 60 weight portions；
Selecting photoresist is ZEOCOAT photoresist, and 50 weight portions, the light transmittance of described photoresist is 80%；
Described organic solvent selects propylene glycol methyl ether acetate, and weight is chosen as 50g；
S2B, employing filtering holes aperture, at grinding distribution liquid described in the filter paper filter pressing of 0.9 μm, obtain film making solution；
S2C, described film making solution are spun on described substrate 1 through photoetching and obtain described scattering layer 2.
The thickness of described scattering layer is 3 μm in the present embodiment.
Embodiment 4
The present embodiment does following improvement on the basis of embodiment 1, the preparation method of the described scattering layer 2 that the present embodiment provides, and comprises the steps:
S2A: described first particle diameter scattering particles select SiO, and its particle diameter is 350nm, accounts for 30 weight portions；Described second particle diameter scattering particles select SiO, and its particle diameter is 15nm, accounts for 20 weight portions；
Described titanium white dispersant is: 1 weight portion；
Described photoresist is transparent OC glue, 60 weight portions, and the light transmittance of described photoresist is 99%
Described organic solvent selects 2-hydroxy-3-methyl methyl butyrate, and weight is chosen as 60g；
S2B: adopt filtering holes aperture at grinding distribution liquid described in the filter paper filter pressing of 1.2 μm, obtain film making solution；
S2C: described film making solution is spun on described substrate 1 through photoetching and obtains described scattering layer 2, and the thickness of described scattering layer 2 is 2.5 μm in the present embodiment.
The method preparing organic electroluminescence device in the present embodiment does following improvement on the basis of embodiment 1, when also comprising the steps: to be etched away encapsulation before described step S4 with described packaging plastic 6 corresponding region and outside described scattering layer 2, the region of the described scattering layer 2 being wherein etched away is more than packaging area 2mm, as shown in Figure 2.
The scattering layer corresponding owing to being etched away packaging plastic, the OLED after encapsulation can be made to have better seal performance, because the air in the external world and moisture are likely scattered that layer enters causes inside OLED that the luminous organic material water suction in OLED was lost efficacy or oxidized, if therefore scattering layer corresponding for packaging plastic can be etched away during encapsulation, it is possible to effectively prevent the luminous organic material water suction in OLED to lose efficacy or oxidized.
Embodiment 5
The present embodiment does following improvement on the basis of embodiment 1, the method preparing described scattering layer 2 in the present embodiment, adopts following steps:
S2A: described first particle diameter scattering particles select TiO, and its particle diameter is 600nm, accounts for 45 weight portions；Described second particle diameter scattering particles select TiO, and its particle diameter is 35nm, accounts for 25 weight portions；
Described titanium white dispersant is 35 weight portions；
Described photoresist is auspicious red RZJ304,10 weight portions, and the light transmittance of described photoresist is 85%；
3-methoxypropionate is as organic solvent, and weight is chosen as 80g；
S2B: adopt filtering holes aperture at grinding distribution liquid described in the filter paper filter pressing of 1.2 μm, obtain film making solution；
S2C: described film making solution is spun on described substrate 1 through photoetching and prepares described scattering layer 2.
The method preparing organic electroluminescence device in the present embodiment, different with embodiment 4, it is before described step S4, when being etched away encapsulation with described packaging plastic 6 corresponding region and outside described scattering layer 2, adopt its structure of OLED that in the present embodiment prepared by preparation method as shown in Figure 3.
Embodiment 6
The present embodiment does following improvement on the basis of embodiment 1, the method preparing described scattering layer 2 in the present embodiment, comprises the steps:
S2A: described first particle diameter scattering particles select TiO2, its particle diameter is 450nm, accounts for 20 weight portions；Described second particle diameter scattering particles ZrO2, its particle diameter is 25nm, accounts for 15 weight portions；
Titanium white dispersant, is 5 weight portions；
Photoresist selects ZEOCOAT, and 40 weight portions, the light transmittance of described photoresist is 95%；
Propylene glycol methyl ether acetate is as organic solvent, and weight is chosen as 60g；
S2B: adopt filtering holes aperture at grinding distribution liquid described in the filter paper filter pressing of 1.0 μm, obtain film making solution；
S2C: described film making solution is spun on described substrate 1 through photoetching and prepares described scattering layer 2.
The method preparing organic electroluminescence device in the present embodiment is identical with embodiment 4.
In the above-described embodiments, described first particle diameter scattering particles and described second particle diameter scattering particles are selected from TiO2、ZrO2、SiO2, one in SiO, TiO；And the optional conventional titanium white dispersant of described dispersant, described titanium white dispersant may select all dispersants being applicable to disperse described first particle diameter scattering particles and described second particle diameter scattering particles；Such as: afcma-4010, disperbyk-110, disperbyk-180, disperbyk-163, dispers655, dispers628 etc. that Byk Chemie GmbH produces；And described photoresist primarily as low-refraction host doped in film making solution, in above-described embodiment photoresist EOC130 purchased from Yongguang Chemical Industry Co., Ltd., Taiwan, transparent OC glue purchased from DNP fine chemistry industry, ZEOCOAT purchased from Japanese auspicious father-in-law (Zeon) Electronic Materials Corp, auspicious red RZJ304 purchased from Suzhou Ruihong Electronic Chemical Product Co., Ltd..Photoresist of the present invention can be substituted at other photoresists being commercially available on the market, but the translucent effect that its translucent effect is likely not to have photoresist selected by the present invention is good.
Embodiment 7
In the present embodiment different with above-described embodiment, the preparation method of wherein preparing described scattering layer 2, adopt following steps:
S2a: selecting described first particle diameter scattering particles is TiO2, its particle diameter is 450nm, accounts for 20 weight portions；Selecting described second particle diameter scattering particles is ZrO2, its particle diameter is 5nm, accounts for 15 weight portions；
Titanium white dispersant is 5 weight portions；
Propylene glycol methyl ether acetate is as organic solvent, and weight is chosen as 60g；
S2b: adopt filtering holes aperture at grinding distribution liquid described in the filter paper filter pressing of 1.0 μm, obtain preformed solution；
S2c: obtain film making solution after adding the photoresist mixing of 30 weight portions in described preformed solution；Photoresist directly can be joined in preformed solution stirring by this step and obtain film making solution, it is also possible to photoresist be joined in preformed solution and be placed in ultrasonic environment to be stirred obtaining film making solution；
S2d: described film making solution is spun on described substrate 1 through photoetching and prepares scattering layer.
The method preparing organic electroluminescence device in the present embodiment is identical with embodiment 4.
As optional embodiment, it is also possible on the basis of embodiment 1 to embodiment 6 any embodiment, making following change, in described organic electroluminescence device, other each layers are all constant, and simply described organic function layer 4 can make following change:
Described organic function layer 4 may select independent luminescent layer；
Described organic function layer 4 can also be made up of luminescent layer and functional layer, and functional layer therein includes the one or more combination in hole injection layer, electronic barrier layer, hole transmission layer, electron transfer layer, hole blocking layer, electron injecting layer.
Wherein luminescent layer can be HONGGUANG, green glow or blue light.The main body RH of HONGGUANG is Bebq2(double; two (10-hydroxy benzo [h] quinoline) beryllium), dyestuff RD are Ir (piq)2(acac)；The main body GH of green glow is CBP (4,4 '-Bis (9H-carbazol-9-yl) biphenyl), dyestuff GD is Ir (ppy)3；Blue light main body BH is AND (9,10-Di (naphtha-2-yl) anthracene), dyestuff BD is DPAVB (4-(di-p-tolylamino)-4 '-[(di-p-tolylamino) styryl] stilbene)；Electron transfer layer is Bphen.
Comparative example 1-2:
The scattering particles of scattering layer 2 described in comparative example 1-2 are respectively adopted the first particle diameter scattering particles in embodiment 1 and embodiment 2, and remainder is with embodiment 1 and embodiment 2；
Comparative example 3-4:
The scattering particles of scattering layer 2 described in comparative example 3-4 are respectively adopted the second particle diameter scattering particles in embodiment 1 and embodiment 2, and remainder is with embodiment 1 and embodiment 2.
For the light extraction efficiency of the organic electroluminescence device prepared, above-mentioned comparative example and each embodiment are tested, set its electric current density identical when, be 10mA, compare its luminosity and flatness, comparative result is as follows:
Obviously, when additive method and material are all identical, adopt the scattering layer that the different-grain diameter scattering particles that the embodiment of the present application provides prepare to be applied in OLED, it is possible to be effectively improved the light extraction efficiency of OLED and the flatness of scattering layer.
Obviously, above-described embodiment is only for clearly demonstrating example, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the apparent change thus extended out or variation are still among the protection domain of the invention.
Claims (12)
1. an organic electroluminescence device, including substrate (1) and the scattering layer (2) sequentially formed on described substrate (1), the first electrode (3), organic function layer (4) and the second electrode (5), it is characterised in that: the material of described scattering layer (2) comprises following component:
First particle diameter scattering particles: 10-60 weight portion；
Second particle diameter scattering particles: 5-30 weight portion；
Dispersant: 1-60 weight portion；
Photoresist: 0-60 weight portion, the light transmittance of described photoresist is 80%-99%；
The particle diameter ratio of described first particle diameter scattering particles and described second particle diameter scattering particles is 4: 1-800: 1；
The particle diameter of described first particle diameter scattering particles is 200nm-800nm；
The particle diameter of described second particle diameter scattering particles is 1nm-50nm.
2. organic electroluminescence device according to claim 1, it is characterised in that:
The particle diameter of described first particle diameter scattering particles is 350nm-450nm；
The particle diameter of described second particle diameter scattering particles is 15nm-35nm.
3. organic electroluminescence device according to claim 1 and 2, it is characterised in that:
The material of described first particle diameter scattering particles and described second particle diameter scattering particles can be the same or different, and is respectively selected from TiO2、ZrO2、SiO2, a kind of or wherein several mixture in SiO, TiO.
4. organic electroluminescence device according to claim 1, it is characterised in that:
The thickness of described scattering layer (2) is 0.3 μm-3 μm.
5. organic electroluminescence device according to claim 1, it is characterised in that:
Described dispersant is titanium white dispersant.
6. the method preparing the arbitrary described organic electroluminescence device of claim 1-5, it is characterised in that comprise the steps:
S1: substrate (1) is cleaned, dries；
S2: form scattering layer (2) on described substrate (1)；
S3: evaporation forms the first electrode (3), organic function layer (4) and the second electrode (5) successively on described scattering layer (2)；
S4: be coated with packaging plastic (6) around described organic function layer (4), is fastened on described packaging plastic (6) by cap (7) and is packaged.
7. the method preparing organic electroluminescence device according to claim 6, it is characterised in that the step forming described scattering layer (2) in described step S2 is as follows:
S21: prepare grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S22: adopt filter paper aperture at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain film making solution；
S23: described film making solution is spun on described substrate (1) through photoetching and obtains described scattering layer (2).
8. the method preparing organic electroluminescence device according to claim 6, it is characterised in that the step forming described scattering layer (2) in described step S2 is as follows:
S2A: prepare grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant and photoresist, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S2B: adopt filter paper aperture at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain film making solution；
S2C: described film making solution is spun on described substrate (1) through photoetching and obtains described scattering layer (2).
9. the method preparing organic electroluminescence device according to claim 6, it is characterised in that the step forming described scattering layer (2) in described step S2 is as follows:
S2a: prepare grinding distribution liquid: be dissolved in organic solvent by the first particle diameter scattering particles, the second particle diameter scattering particles, dispersant, being ground in dispersion liquid the particle diameter granule less than 1 μm accounts for more than the 80% of integral particle quantitative proportion；
S2b: adopt filter paper aperture at grinding distribution liquid described in the filter paper filter pressing of 0.8 μm-1.2 μm, obtain preformed solution；
S2c: obtain film making solution after adding photoresist mixing in described preformed solution；
S2d: described film making solution is spun on described substrate (1) through photoetching and obtains described scattering layer (2).
10. according to the arbitrary described method preparing organic electroluminescence device of claim 7-9, it is characterised in that:
Described filter paper aperture is 0.8 μm.
11. the method preparing organic electroluminescence device according to claim 10, it is characterised in that:
Before described step S4, also comprise the steps:
A1: with the described scattering layer (2) of described packaging plastic (6) corresponding region when being etched away encapsulation.
12. the method preparing organic electroluminescence device according to claim 10, it is characterised in that:
Before described step S4, also comprise the steps:
A2: when being etched away encapsulation with described packaging plastic (6) corresponding region and outside described scattering layer (2).
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| CN105789475A (en) * | 2014-12-24 | 2016-07-20 | 固安翌光科技有限公司 | Organic light-emitting device and preparation method thereof |
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| CN101901825A (en) * | 2009-03-05 | 2010-12-01 | 富士胶片株式会社 | Organic electroluminescence device |
| CN102709489A (en) * | 2012-05-31 | 2012-10-03 | 昆山维信诺显示技术有限公司 | Preparation method for high-refractivity scattering layer and preparation method for organic light-emitting diode (OLED) with high luminous efficiency |
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