CN102709489B - The preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency - Google Patents
The preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency, and comprise the steps: S1, prepare grinding distribution liquid, comprising: high index of refraction scattering particles, 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, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8 μm-1.2 μm prepared by step S1, 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.The OLED of the high light-emitting efficiency in the present invention arranges the light extraction efficiency that above-mentioned high index of refraction scattering layer can improve OLED greatly between substrate and electrode.
Description
Technical field
The present invention relates to the preparation method of organic electroluminescence device, be specifically related to a kind of preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency.
Background technology
OLED(Organic Light-Emitting Diode) i.e. Organic Light Emitting Diode, it arranges luminescence unit on substrate, and luminescence unit comprises two electrodes, is provided with electroluminescent material layer between two electrodes.In the prior art, general clear glass of selecting is as substrate, and the refractive index of glass is generally 1.4-1.5, and the refractive index of electroluminescent organic material layer is generally 1.7-1.8.Therefore electroluminescent organic material is energized the light sent, air is entered through glass, due to total reflection principle, having most light is confined in electroluminescent organic material layer, this causes the light output efficiency of OLED to only have greatly reducing, only have an appointment 20%, have the light of 80% to be limited to or loss cannot rationally be applied in the inside of OLED electroluminescent organic material.Therefore the light output efficiency how improving OLED becomes the research and development focus of technical staff.
Existing patent documentation CN102299266A discloses a kind of substrate and manufacture method of organic electroluminescence device, it comprises transparent substrates, have scattering layer at least side of transparent substrates, scattering layer is made up of the nano particle of TiO2, SiO2 or ZnO, the inner side of transparent substrates and Electrode connection.The manufacture method of this organic electroluminescence device substrate is, be provided with transparent substrates, form scattering layer in transparent substrates side by sol-gel or hydro thermal method, scattering layer is made up of the nano particle of TiO2, SiO2 or ZnO, and 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 are produced, the direction of propagation of light is changed by arranging scattering layer, increase the probability of light forward direction and improve the efficiency of optical coupling, the nano particle of TiO2, SiO2 or ZnO on scattering layer forms the transparent arrays of flakey, column or tubulose, there is higher refractive index, be more conducive to the round changing 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, and its general principle is dissolved in water equal solvent by raw material, takes adequate measures to cause the supersaturation of solution, makes crystal forming core growing wherein.
And sol-gel process is prepared film material and is belonged to one in wet chemistry method.Generally refer to and metallic compound (comprising metal alkoxide and metal inorganic salt) and catalyst, chelating agent and water etc. are made colloidal sol, then by whirl coating, spraying or impregnating method, alkoxide sol is coated in masking on substrate, hydrolysis and polymerization is there is in alkoxide after absorbing the moisture in air, become gel gradually, eventually pass the process of the process such as drying, sintering.
In technique scheme, just write out the broad method preparing scattering layer, and do not provide this process how preparing scattering layer.And the quality of the film forming of scattering layer will directly have influence on the light extraction efficiency of OLED.And the factor affecting scattering layer quality of forming film is a lot, wherein topmost is exactly how to select the component of each material to carry out the solution of proportioning for film forming.
For film forming solution, how to select the content of solute to ensure that the scattering layer for preparing can have good evenness and improve light outgoing efficiency, be do not have in prior art disclosed in.The too high meeting of solutes content causes solvent film forming or the scattering film surface for preparing cannot have particle out-of-flatness, and there is large particle on scattering film surface, OLED exists the defect of short circuit, poor stability etc.; And the too low meeting of solutes content causes solvent institute film forming layer not possess the effect of scattering; Therefore how to determine that the content of solute is the emphasis that those skilled in the art study.
In addition, because the scattering particles in film forming solvent are dissolved by the particle of certain particle diameter to be formed in organic solvent, therefore may there is the situation of precipitation in solute, and solute is deposited in the process of spin-coating film and can causes the in uneven thickness of scattering film, make the poor flatness of film surface,, how to solve the scattering film film surface poor flatness problem caused due to solute precipitates be also do not have in prior art disclosed in.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of high index of refraction scattering layer and the OLED preparation method of high light-emitting efficiency.
For solving the problems of the technologies described above, the invention provides a kind of preparation method of high index of refraction scattering layer, comprising the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, 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, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um-1.2um prepared by step S1, 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.
Described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
Described dispersant adopts titanium white dispersant.
Described anti-settling agent adopts titanium white anti-settling agent.
Filter paper aperture described in described step S2 is 0.8um.
The thickness of described scattering layer is 0.3um-3um.
The present invention also provides a kind of high index of refraction scattering layer utilizing the preparation method of above-mentioned high index of refraction scattering layer to prepare.
The present invention also provides a kind of OLED preparation method of high light-emitting efficiency, comprises the steps:
I. on substrate, prepare high index of refraction scattering layer according to the preparation method of above-mentioned preparation high index of refraction scattering layer;
II. on described high index of refraction scattering layer, prepare the first electrode;
III. prepare organic function layer on the first electrode;
IV. on described organic function layer, prepare the second electrode;
V. encapsulation.
Also comprise the steps: after described step I
I. I: when being etched away encapsulation and the high index of refraction scattering layer of packaging plastic corresponding region.
Described step I. in I, all high index of refraction scattering layers when being etched away encapsulation and outside packaging plastic corresponding region.
Technique scheme tool of the present invention has the following advantages:
(1) preparation method of high index of refraction scattering layer provided by the invention, simple to operate, extra equipment is not needed to realize, and the mass percent of high index of refraction scattering particles and the mass ratio relation of dispersant and high index of refraction scattering particles due to choose reasonable, make after prepared by high index of refraction scattering layer provided by the invention, there is good evenness, and there is splendid dispersion effect, adopt the high index of refraction scattering layer provided in the present invention in OLED, the light extraction efficiency of OLED can be made to improve 50%-100%.
(2) preparation method of the high index of refraction scattering layer provided in the present invention, owing to the addition of anti-settling agent, effectively can avoid the precipitation of film making solution, therefore film making solution is even, and the high index of refraction scattering layer obtained after photoetching spin coating has good evenness and uniform dispersion effect.
(3) the OLED preparation method of the high light-emitting efficiency provided in the present invention, owing to adding high index of refraction scattering layer, makes the OLED light extraction efficiency prepared to improve 50%-100%.
(4) the OLED preparation method of the high light-emitting efficiency provided in the present invention, owing to being etched away high index of refraction scattering layer corresponding to packaging plastic, the OLED after encapsulating can be made to have better sealing property, because the air in the external world and moisture likely enter OLED inside through high index of refraction scattering layer cause the water suction of the luminous organic material in OLED inefficacy or oxidized, if high index of refraction scattering layer corresponding for packaging plastic can be etched away when therefore encapsulating, the water suction of the luminous organic material in OLED inefficacy or oxidized effectively can be prevented.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein:
Fig. 1 is the OLED end view that the embodiment of the present invention contains high index of refraction scattering layer;
Fig. 2 is the OLED vertical view that embodiment of the present invention etching removes packaging area high index of refraction scattering layer;
Fig. 3 is the OLED end view that embodiment of the present invention etching removes high index of refraction scattering layer outside packaging plastic.
Wherein Reference numeral is: 1-substrate, 2-high index of refraction scattering layer, 3-ITO first electrode, 4-organic function layer, 5-second electrode, 6-UV packaging plastic, 7-cap.
Embodiment
Provide specific embodiments of the invention below.
embodiment 1
The present embodiment provides a kind of preparation method of high index of refraction scattering layer, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, in the present embodiment, described high index of refraction scattering particles are chosen as TiO
2, its weight is chosen as 15g, and its mass percent is 18.6%;
Dispersant, the byk-163 that described dispersant selects Byk Chemie GmbH to produce is as dispersant, and its weight is chosen as 1.2g, and its quality accounts for 8% of described high index of refraction scattering particles;
Organic solvent, select 1-Methoxy-2-propyl acetate as organic solvent, its weight is chosen as 60g, and its mass percent is 78.74%;
The above-mentioned solution prepared is put into grinding pot, fixes grinding pot and grinding post, add 90ml zirconium pearl (note: the amount of zirconium pearl is depending on the volume of grinding pot), grind use gauze elimination zirconium pearl after 3 hours, obtain grinding distribution liquid;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um prepared by step S1, 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.
The present embodiment also provides a kind of high index of refraction scattering layer utilizing the preparation method of above-mentioned high index of refraction scattering layer to prepare.
The OLED preparation method of what the present embodiment provided prepare high light-emitting efficiency, substrate arranges above-mentioned high index of refraction scattering layer, comprises the steps:
I. prepare high index of refraction scattering layer 2 on substrate 1 according to the preparation method of above-mentioned preparation high index of refraction scattering layer;
II. on described high index of refraction scattering layer 2, prepare the first electrode 3; Direct current magnetron sputtering process is utilized to prepare first electrode layer of ITO; Described first electrode layer etches ITO 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;
III. on described first electrode 3, prepare organic function layer 4; Evaporation hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer successively on described ITO first electrode 3; Evaporate process middle chamber pressure is lower than 5.0 × 10-3Pa, and first the thick NPB of evaporation 40nm is as hole transmission layer; Thick ADN and TBPe of the method evaporation 30nm steamed altogether using double source is as luminescent layer, and the ratio of through-rate control TBPe in ADN is 7%; The Alq3 of evaporation 20nm is as electron transfer layer; The LiF of evaporation 0.5nm is as electron injecting layer;
IV. on described organic function layer 4, prepare the second electrode 5, the Al of evaporation 150nm is as the second electrode 5;
V. encapsulation: after employing UV packaging plastic 6, cap 7 utilize conventional packaged type to encapsulate, make OLED.
Adopt the OLED that in the present embodiment prepared by preparation method, as shown in Figure 1, its light extraction efficiency improves 80% to its structure.
embodiment 2
The present embodiment does following improvement on the basis of embodiment 1, in described grinding distribution liquid, add anti-settling agent, and select the byk-410 that Byk Chemie GmbH produces, its weight is chosen as 0.8g, and its mass percent is 1.03%;
Further, in the present embodiment, also comprise the steps: to add photoresist in the described described film making solution prepared at described step S2 between described step S2 and described step S3; In the present embodiment, select described photoresist to mix with described film making solution, the mass percent of described photoresist is 40%.
The thickness of described scattering layer is 0.6um in the present embodiment.Adopt the OLED that in the present embodiment prepared by preparation method, its light extraction efficiency improves 100%.
embodiment 3
The preparation method of the high index of refraction scattering layer that the present embodiment provides, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 36% of described high index of refraction scattering particles, and namely its mass percent is 3.6%;
Anti-settling agent, its mass percent is: 5%;
Photoresist, its mass percent is: 51.5%;
Organic solvent, its mass percent is: 30%;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.9um prepared by step S1, 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.
In the present embodiment, described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
The method preparing OLED in the present embodiment is consistent with embodiment 1, and adopt the OLED that in the present embodiment prepared by preparation method, its light extraction efficiency improves 50%.
embodiment 4
The preparation method of the high index of refraction scattering layer that the present embodiment provides, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, its mass percent is: 30%;
Dispersant, its quality accounts for 1% of described high index of refraction scattering particles, and namely its mass percent is 0.3%;
Anti-settling agent, its mass percent is: 3%;
Organic solvent, its mass percent is: 66.7%;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um prepared by step S1, 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.
In the present embodiment, described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
The method preparing OLED in the present embodiment does following improvement on the basis of embodiment 1, when also comprising the steps: to be etched away encapsulation after completing steps I and the high index of refraction scattering layer of packaging plastic 6 corresponding region.The both sides, scattering layer region be wherein etched away are greater than packaging area 2mm; As optional execution mode, all high index of refraction scattering layers when also can be etched away encapsulation and outside packaging plastic 6 corresponding region.
Owing to being etched away high index of refraction scattering layer corresponding to packaging plastic, can prevent extraneous air and moisture from likely entering OLED inside through high index of refraction scattering layer and cause the water suction of the luminous organic material in OLED inefficacy or oxidized, if high index of refraction scattering layer corresponding for packaging plastic can be etched away when therefore encapsulating, the water suction of the luminous organic material in OLED inefficacy or oxidized effectively can be prevented.
Adopt the preparation method of the OLED in the present embodiment, its light extraction efficiency improves 63%.
embodiment 5
The preparation method of the high index of refraction scattering layer that the present embodiment provides, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, its mass percent is: 60%;
Dispersant, its quality accounts for 15% of described high index of refraction scattering particles;
Photoresist, its mass percent is: 5%;
Organic solvent, its mass percent is: 20%;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 1.2um prepared by step S1, 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.
Prepare the method for OLED in the present embodiment, different with embodiment 4, it is in described step I. in I, and all high index of refraction scattering layers when being etched away encapsulation and outside packaging plastic 6 corresponding region.As shown in Figure 3, its light extraction efficiency improves 77% to its structure of OLED that in employing the present embodiment prepared by preparation method.
embodiment 6
The preparation method of the high index of refraction scattering layer that the present embodiment provides, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 20% of described high index of refraction scattering particles, and namely its mass percent is 2%;
Anti-settling agent, its mass percent is: 5%;
Photoresist, its mass percent is: 60%;
Organic solvent, its mass percent is: 23%;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um prepared by step S1, 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.
In the present embodiment, described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
The method preparing OLED in the present embodiment is identical with embodiment 4, and adopt the OLED that in the present embodiment prepared by preparation method, its light extraction efficiency improves 66%.
embodiment 7
The preparation method of the high index of refraction scattering layer that the present embodiment provides, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 1% of described high index of refraction scattering particles, and namely its mass percent is 0.1%;
Organic solvent, its mass percent is: 89.9%;
S2, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um prepared by step S1, 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.
In the present embodiment, described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
The method preparing OLED in the present embodiment is identical with embodiment 4, and adopt the OLED that in the present embodiment prepared by preparation method, its light extraction efficiency improves 66%.
In the above-described embodiments, described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO; And described dispersant can select conventional titanium white dispersant, is selected from conventional titanium white class dispersant, described titanium white dispersant is applicable to the dispersant disperseing described high index of refraction scattering particles; Such as: afcma-4010, disperbyk-110, disperbyk-180, disperbyk-163, dispers655, dispers628 etc. that Byk Chemie GmbH produces; And described photoresist mainly as low-refraction host doped in film making solution, if there are other low-refraction matrix also can substitute described photoresist; Described anti-settling agent is chosen as conventional titanium white anti-settling agent, as byk-410, byk-430 etc. that Byk Chemie GmbH produces., described titanium white anti-settling agent is the anti-settling agent for preventing described high index of refraction scattering particles from precipitating.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all execution modes.And thus the apparent change of extending out or variation be still among the protection range of the invention.
Claims (10)
1. a preparation method for high index of refraction scattering layer, is characterized in that, comprises the steps:
S1, prepare grinding distribution liquid, described grinding distribution liquid comprises:
High index of refraction scattering particles, 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, the employing filter bores aperture grinding distribution liquid that described in the filter paper press filtration of 0.8um-1.2um prepared by step S1, 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.
2. the preparation method of high index of refraction scattering layer according to claim 1, is characterized in that:
Described high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, one in SiO, TiO.
3. the preparation method of high index of refraction scattering layer according to claim 1 and 2, is characterized in that:
Described dispersant adopts titanium white dispersant.
4. the preparation method of high index of refraction scattering layer according to claim 1, is characterized in that:
Described anti-settling agent adopts titanium white anti-settling agent.
5. the preparation method of high index of refraction scattering layer according to claim 1, is characterized in that:
Filter paper aperture described in described step S2 is 0.8um.
6. the preparation method of high index of refraction scattering layer according to claim 1, is characterized in that:
The thickness of described scattering layer is 0.3um-3um.
7. the high index of refraction scattering layer utilizing the preparation method of the arbitrary described high index of refraction scattering layer of claim 1-6 to prepare.
8. an OLED preparation method for high light-emitting efficiency, is characterized in that: comprise the steps:
I. above high index of refraction scattering layer (2) is prepared according to the preparation method of the arbitrary described preparation high index of refraction scattering layer of claim 1-6 at substrate (1);
II. at upper preparation first electrode (3) of described high index of refraction scattering layer (2);
III. on described first electrode (3), organic function layer (4) is prepared;
IV. on described organic function layer (4), the second electrode lay (5) is prepared;
V. encapsulate.
9. the OLED preparation method of high light-emitting efficiency according to claim 8, is characterized in that:
Also comprise the steps after described step I
I.I: when being etched away encapsulation and the high index of refraction scattering layer of packaging plastic (6) corresponding region.
10. the OLED preparation method of high light-emitting efficiency according to claim 9, is characterized in that:
In described step I.I, all high index of refraction scattering layers when being etched away encapsulation and outside packaging plastic (6) corresponding region.
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| CN103066214B (en) * | 2012-12-28 | 2016-06-29 | 固安翌光科技有限公司 | A kind of organic electroluminescence device and preparation method thereof |
| CN104124393A (en) * | 2013-04-24 | 2014-10-29 | 海洋王照明科技股份有限公司 | Organic light-emitting device and preparation method thereof |
| CN104124360A (en) * | 2013-04-24 | 2014-10-29 | 海洋王照明科技股份有限公司 | Organic light-emitting device and preparation method thereof |
| CN104124359A (en) * | 2013-04-24 | 2014-10-29 | 海洋王照明科技股份有限公司 | Organic light-emitting device and preparation method thereof |
| CN104124396A (en) * | 2013-04-24 | 2014-10-29 | 海洋王照明科技股份有限公司 | Organic electroluminescent device and preparation method thereof |
| 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 |
| CN105810841B (en) * | 2014-12-29 | 2018-05-01 | 固安翌光科技有限公司 | A kind of organic electroluminescence device |
| CN106206980A (en) * | 2016-07-15 | 2016-12-07 | 深圳市华星光电技术有限公司 | A kind of OLED its preparation method improving light extraction efficiency |
| CN106299151A (en) * | 2016-08-23 | 2017-01-04 | 深圳市华星光电技术有限公司 | OLED display panel and the manufacture method of OLED display panel |
| KR20190130837A (en) * | 2018-05-15 | 2019-11-25 | 코닝 인코포레이티드 | Coating solution for light extraction layer of organic light emitting device and method of fabricating light extraction substrate of organic light emitting device using the same |
| JP7234514B2 (en) * | 2018-06-13 | 2023-03-08 | Ａｇｃ株式会社 | optical laminate |
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Effective date of registration: 20160128 Address after: 065500 Guan County, Hebei Province emerging industry demonstration park Patentee after: GU'AN YEOLIGHT TECHNOLOGY CO., LTD. Address before: 215300 Suzhou Province, Kunshan City, Kunshan hi tech Zone, Feng Feng Road, No. 188, No. Patentee before: Weixinnuo Display Tech Co., Ltd. Patentee before: Weixinnuo Science and Technology Co., Ltd., Beijing |