CN102709489A - Preparation method for high-refractivity scattering layer and preparation method for organic light-emitting diode (OLED) with high luminous efficiency - Google Patents
Preparation method for high-refractivity scattering layer and preparation method for organic light-emitting diode (OLED) with high luminous efficiency Download PDFInfo
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Abstract
The invention discloses a preparation method for a high-refractivity scattering layer and a preparation method for an organic light-emitting diode (OLED) with high luminous efficiency. The preparation method for the high-refractivity scattering layer comprises the following steps of: S1, preparing grinding dispersion, wherein the grinding dispersion comprises 10 to 60 mass percent of high-refractivity scattering particle, a dispersing agent of which the mass is 1 to 60 percent based on the mass of the high-refractivity scattering particles, 0 to 5 mass percent of anti-settling agent, 0 to 60 mass percent of photoresist and 20 to 89.9 mass percent of organic solvent; S2, filter-pressing the grinding dispersion prepared by the step S1 by using filter paper with filtering hole apertures of 0.8 to 1.2 mu m to obtain a film preparation solution; and S3, photoetching and spinning the film preparation solution prepared by the step S2 to obtain the high-refractivity scattering layer. When the high-refractivity scattering layer is arranged between a substrate and an electrode of the OLED with the high luminous efficiency, the luminous efficiency of the OLED can be greatly improved.
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) is an Organic Light Emitting Diode, and it is provided with luminescence unit on substrate, and luminescence unit comprises two electrodes, between two electrodes, is provided with the organic electro luminescent material layer.In the prior art, generally select 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 sends of electroluminescent organic material energising; When getting into air through glass; Because total reflection principle has most light and is confined in the electroluminescent organic material layer, this causes the light output efficiency of OLED to have only reduction greatly; Only have an appointment 20%, have 80% light to be limited to or loss can't rational Application in the inside of OLED electroluminescent organic material.Therefore the light output efficiency that how to improve OLED becomes technical staff's research and development focus.
Existing patent documentation CN102299266A discloses a kind of substrate and manufacturing approach of organic electroluminescence device; It comprises transparent substrates; At least one side in transparent substrates has scattering layer, and scattering layer is made up of the nano particle of TiO2, SiO2 or ZnO, and the inboard of transparent substrates is connected with electrode.The manufacturing approach of this organic electroluminescence device substrate does; Be provided with transparent substrates; Form scattering layer in transparent substrates one side through sol-gel or hydro thermal method, scattering layer is made up of the nano particle of TiO2, SiO2 or ZnO, and the inboard of transparent substrates is provided with electrode through deposition.In the technique scheme; Through the oled substrate of hydro thermal method or sol-gel process production, through the direction of propagation that scattering layer changes light being set, probability that increase light is propagated forward and the efficient that improves optical coupling; The nano particle of TiO2 on the scattering layer, SiO2 or ZnO forms the transparent array of flakey, column or tubulose; Have higher refractive index, more help changing the round of light, improve the light extraction efficiency of OLED device.
Wherein, the Hydrothermal Preparation crystal is a kind of method from the growth from solution crystal, and its basic principle is that raw material is dissolved in the water equal solvent, takes adequate measures to cause the supersaturation of solution, makes crystal forming core and growth therein.
And preparing the film material, sol-gel process belongs to a kind of in the wet chemistry method.Generally refer to metallic compound (comprising metal alkoxide and metal inorganic salt) and catalyst, chelating agent and water etc. are processed colloidal sol; Through whirl coating, spraying or impregnating method alkoxide sol is coated in then and makes film on the substrate; Hydrolysis and polymerization take place after absorbing airborne moisture in alkoxide; Become gel gradually, the process of handling through super-dry, sintering etc. at last.
In technique scheme, just write out the broad method of preparation scattering layer, and do not provided this process that how to prepare scattering layer.And the quality of the film forming of scattering layer will directly have influence on the light extraction efficiency of OLED device.And the factor that influences the scattering layer quality of forming film is a lot, and wherein topmost is exactly how to select the component of each material to come proportioning to be used for the solution of film forming.
For film forming solution, content how to select solute can have preferably evenness and improve light outgoing efficient to guarantee the scattering layer for preparing, be do not have in the prior art disclosed.The too high meeting of solutes content cause solvent can't film forming or the scattering film surface for preparing the particle out-of-flatness is arranged, have big particle on the scattering film surface, there is the defective of short circuit, poor stability etc. in the OLED device; And solutes content is crossed and low can be caused solvent institute film forming layer not possess the effect of scattering; Therefore how to confirm that the content of solute is the emphasis that those skilled in the art study.
In addition; Because the scattering particles in the film forming solvent are the particles by certain grain size to be dissolved in the organic solvent and to form; Therefore the solute situation that may occur precipitating, and solute is deposited in and can causes the in uneven thickness of scattering film in the process of spin-coating film makes the poor flatness of film surface;, how to solve since the scattering film film surface poor flatness problem that solute deposition causes also be do not have in the prior art disclosed.
Summary of the invention
Technical problem to be solved by this invention provides 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 present invention provides a kind of preparation method of high index of refraction scattering layer, comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 10%-60%;
Dispersant, its quality accounts for the 1%-60% of said 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 obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um-1.2um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
Said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
Said dispersant adopts the titanium white dispersant.
Said anti-settling agent adopts the titanium white anti-settling agent.
The said filter paper of said step S2 aperture is 0.8um.
The thickness of said scattering layer is 0.3um-3um.
The high index of refraction scattering layer that the present invention also provides a kind of preparation method who utilizes 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. the preparation method according to above-mentioned preparation high index of refraction scattering layer prepares the high index of refraction scattering layer on substrate;
II. preparation first electrode on said high index of refraction scattering layer;
III. on said first electrode, prepare organic function layer;
IV. preparation second electrode on said organic function layer;
V. encapsulation.
Also comprise the steps: after the said step I
I. I: be etched away when encapsulating and the high index of refraction scattering layer of packaging plastic corresponding region.
Said step I. in the I, be etched away when encapsulating and all high index of refraction scattering layers outside the packaging plastic corresponding region.
Technique scheme of the present invention has following advantage:
(1) preparation method of high index of refraction scattering layer provided by the invention; Simple to operate; Do not need additional apparatus to realize, and since choose reasonable the mass ratio relation of mass percent and dispersant and high index of refraction scattering particles of high index of refraction scattering particles, make after the high index of refraction scattering layer preparation completion provided by the invention; Has good evenness; And have splendid dispersion effect, adopt the high index of refraction scattering layer that provides among the present invention in the OLED device, can make the light extraction efficiency of OLED device improve 50%-100%.
The preparation method of the high index of refraction scattering layer that (2) provides among the present invention; Owing to added anti-settling agent; Can effectively avoid the deposition of film making solution, so film making solution is even, the high index of refraction scattering layer that after the photoetching spin coating, obtains has evenness and uniform dispersion effect preferably.
The OLED preparation method of the high light-emitting efficiency that (3) provides among the present invention owing to added the high index of refraction scattering layer, makes the OLED light extraction efficiency of preparing can improve 50%-100%.
The OLED preparation method of the high light-emitting efficiency that (4) provides among the present invention; Owing to be etched away the corresponding high index of refraction scattering layer of packaging plastic; Can make the OLED after the encapsulation have better sealing property; Because might getting into the OLED device inside through the high index of refraction scattering layer, extraneous air and moisture causes luminous organic material suction inefficacy in the OLED or oxidized; Therefore, can prevent effectively that luminous organic material suction in the OLED device was lost efficacy or oxidized if can be etched away by the high index of refraction scattering layer that packaging plastic is corresponding during encapsulation.
Description of drawings
For content of the present invention is more clearly understood, below according to a particular embodiment of the invention and combine accompanying drawing, the present invention is done further detailed explanation, wherein:
Fig. 1 contains the OLED device-side view of high index of refraction scattering layer for the embodiment of the invention;
Fig. 2 removes the OLED device vertical view of packaging area high index of refraction scattering layer for embodiment of the invention etching;
Fig. 3 removes the OLED device-side view of high index of refraction scattering layer outside the packaging plastic for embodiment of the invention etching.
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 embodiment of the present invention below.
Embodiment 1
Present embodiment provides a kind of preparation method of high index of refraction scattering layer, comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, in the present embodiment, said 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, said dispersant select the byk-163 of Bi Ke chemistry Co., Ltd production as dispersant, and its weight is chosen as 1.2g, and its quality accounts for 8% of said high index of refraction scattering particles;
Organic solvent selects 1-Methoxy-2-propyl acetate as organic solvent, and its weight is chosen as 60g, and its mass percent is 78.74%;
The above-mentioned solution for preparing is put into grinding pot, fix grinding pot and grind post, add 90ml zirconium pearl (annotate: the amount of zirconium pearl is looked the volume of grinding pot and decided), grind after 3 hours, make the grinding dispersion liquid with gauze elimination zirconium pearl;
S2, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
The high index of refraction scattering layer that present embodiment also provides a kind of preparation method who utilizes above-mentioned high index of refraction scattering layer to prepare.
The OLED preparation method of the preparation high light-emitting efficiency that present embodiment provides is provided with above-mentioned high index of refraction scattering layer on substrate, comprise the steps:
I. the preparation method according to above-mentioned preparation high index of refraction scattering layer prepares high index of refraction scattering layer 2 on substrate 1;
II. preparation first electrode 3 on said high index of refraction scattering layer 2; Utilize direct current magnetron sputtering process to prepare first electrode layer of ITO; On said first electrode layer, etch ITO first electrode 3; The ITO target is an indium stannum alloy, its composition ratio In:Sn=90%:10%.Partial pressure of oxygen is 0.4Sccm in the preparation process, and argon partial pressure is 20Sccm;
III. preparation organic function layer 4 on said first electrode 3; Vapor deposition hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer successively on said ITO first electrode 3; Evaporate process middle chamber pressure is lower than 5.0 * 10-3Pa, and at first the thick NPB of vapor deposition 40nm is as hole transmission layer; ADN that the method vapor deposition 30nm that steams altogether with double source is thick and TBPe are as luminescent layer, and the ratio of through-rate control TBPe in ADN is 7%; The Alq3 of vapor deposition 20nm is as electron transfer layer; The LiF of vapor deposition 0.5nm is as electron injecting layer;
IV. preparation second electrode 5 on said organic function layer 4, the Al of vapor deposition 150nm is as second electrode 5;
V. encapsulation: after adopting UV packaging plastic 6, cap 7 to utilize conventional packaged type encapsulation, process the OLED device.
Adopt the OLED device of preparation method's preparation in the present embodiment, its structure is as shown in Figure 1, and its light extraction efficiency has improved 80%.
Present embodiment is done following improvement on the basis of embodiment 1, in said grinding dispersion liquid, add anti-settling agent, the byk-410 that selects Bi Ke chemistry Co., Ltd to produce, and its weight is chosen as 0.8g, and its mass percent is 1.03%;
And, in the present embodiment, also comprise the steps: between said step S2 and the said step S3 to add photoresist to said in the said film making solution of said step S2 preparation; In the present embodiment, select said photoresist to mix with said film making solution, the mass percent of said photoresist is 40%.
The thickness of said scattering layer is 0.6um in the present embodiment.Adopt the OLED device of preparation method's preparation in the present embodiment, its light extraction efficiency has improved 100%.
The preparation method of the high index of refraction scattering layer that present embodiment provides comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 36% of said high index of refraction scattering particles, and promptly 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, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.9um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
In the present embodiment, said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
Consistent among the method for preparing the OLED device in the present embodiment and the embodiment 1, adopt the OLED device of preparation method's preparation in the present embodiment, its light extraction efficiency has improved 50%.
Embodiment 4
The preparation method of the high index of refraction scattering layer that present embodiment provides comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 30%;
Dispersant, its quality accounts for 1% of said high index of refraction scattering particles, and promptly its mass percent is 0.3%;
Anti-settling agent, its mass percent is: 3%;
Organic solvent, its mass percent is: 66.7%;
S2, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
In the present embodiment, said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
The method for preparing the OLED device in the present embodiment is done following improvement on the basis of embodiment 1, after the completing steps I, also comprise the steps: to be etched away when encapsulating and the high index of refraction scattering layer of packaging plastic 6 corresponding regions.The both sides, scattering layer zone that wherein are etched away are greater than packaging area 2mm; As optional execution mode, also can be etched away when encapsulating and all high index of refraction scattering layers outside packaging plastic 6 corresponding regions.
Owing to be etched away the corresponding high index of refraction scattering layer of packaging plastic; Can prevent that extraneous air and moisture from might get into the OLED device inside through the high index of refraction scattering layer and cause luminous organic material suction inefficacy in the OLED or oxidized; Therefore, can prevent effectively that luminous organic material suction in the OLED device was lost efficacy or oxidized if can be etched away by the high index of refraction scattering layer that packaging plastic is corresponding during encapsulation.
Adopt the OLED preparation of devices method in the present embodiment, its light extraction efficiency has improved 63%.
The preparation method of the high index of refraction scattering layer that present embodiment provides comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 60%;
Dispersant, its quality accounts for 15% of said high index of refraction scattering particles;
Photoresist, its mass percent is: 5%;
Organic solvent, its mass percent is: 20%;
S2, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 1.2um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
The method for preparing the OLED device in the present embodiment, different with embodiment 4, it is in said step I. in the I, is etched away when encapsulating and all high index of refraction scattering layers outside packaging plastic 6 corresponding regions.Adopt its structure of OLED device of preparation method's preparation in the present embodiment as shown in Figure 3, its light extraction efficiency has improved 77%.
The preparation method of the high index of refraction scattering layer that present embodiment provides comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 20% of said high index of refraction scattering particles, and promptly 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, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
In the present embodiment, said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
The method for preparing the OLED device in the present embodiment is identical with embodiment 4, adopts the OLED device of preparation method's preparation in the present embodiment, and its light extraction efficiency has improved 66%.
Embodiment 7
The preparation method of the high index of refraction scattering layer that present embodiment provides comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 10%;
Dispersant, its quality accounts for 1% of said high index of refraction scattering particles, and promptly its mass percent is 0.1%;
Organic solvent, its mass percent is: 89.9%;
S2, employing filtering holes aperture obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
In the present embodiment, said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
The method for preparing the OLED device in the present embodiment is identical with embodiment 4, adopts the OLED device of preparation method's preparation in the present embodiment, and its light extraction efficiency has improved 66%.
In the above-described embodiments, said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO; And said dispersant can be selected conventional titanium white dispersant, is selected from conventional titanium white class dispersant,, said titanium white dispersant is applicable to the dispersant that disperses said high index of refraction scattering particles; Such as: the afcma-4010 that Bi Ke chemistry Co., Ltd produces, disperbyk-110, disperbyk-180, disperbyk-163, dispers655, dispers628 etc.; And said photoresist mainly is to be entrained in the film making solution as low-refraction matrix, if there are other low-refraction matrix also can substitute said photoresist; Said anti-settling agent is chosen as conventional titanium white anti-settling agent, the byk-410 that produces like Bi Ke chemistry Co., Ltd, byk-430 etc., said titanium white anti-settling agent is the anti-settling agent that is used to prevent said high index of refraction scattering particles deposition.
Obviously, the foregoing description only be for explanation clearly done for example, and be not qualification to execution mode.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here need not also can't give exhaustive to all execution modes.And conspicuous variation of being extended out thus or change still are among the protection range of the invention.
Claims (10)
1. the preparation method of a high index of refraction scattering layer is characterized in that, comprises the steps:
Dispersion liquid is ground in S1, preparation, and said grinding dispersion liquid comprises:
The high index of refraction scattering particles, its mass percent is: 10%-60%;
Dispersant, its quality accounts for the 1%-60% of said 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 obtain film making solution at the grinding dispersion liquid that the said step S1 of the filter paper press filtration of 0.8um-1.2um prepares;
The said film making solution of S3, said step S2 preparation prepares the high index of refraction scattering layer through the photoetching spin coating.
2. the preparation method of high index of refraction scattering layer according to claim 1 is characterized in that:
Said high index of refraction scattering particles are selected from TiO
2, ZrO
2, SiO
2, a kind of among the SiO, TiO.
3. the preparation method of high index of refraction scattering layer according to claim 1 and 2 is characterized in that:
Said dispersant adopts the titanium white dispersant.
4. according to the preparation method of the arbitrary described high index of refraction scattering layer of claim 1-3, it is characterized in that:
Said anti-settling agent adopts the titanium white anti-settling agent.
5. according to the preparation method of the arbitrary described high index of refraction scattering layer of claim 1-4, it is characterized in that:
The said filter paper of said step S2 aperture is 0.8um.
6. according to the preparation method of the arbitrary described high index of refraction scattering layer of claim 1-5, it is characterized in that:
The thickness of said scattering layer is 0.3um-3um.
7. high index of refraction scattering layer that the preparation method who utilizes the arbitrary described high index of refraction scattering layer of claim 1-6 prepares.
8. the OLED preparation method of a high light-emitting efficiency is characterized in that: comprise the steps:
I. the preparation method according to the arbitrary described preparation high index of refraction scattering layer of claim 1-6 goes up preparation high index of refraction scattering layer (2) at substrate (1);
II. go up preparation first electrode (3) at said high index of refraction scattering layer (2);
III. go up preparation organic function layer (4) at said first electrode (3);
IV. go up preparation second electrode (5) at said organic function layer (4);
V. encapsulation.
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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 |
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 |
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 |
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 |
CN105810841A (en) * | 2014-12-29 | 2016-07-27 | 固安翌光科技有限公司 | Organic electroluminescent device |
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 |
CN112219290A (en) * | 2018-05-15 | 2021-01-12 | 康宁公司 | Coating solution for light extraction layer of organic light emitting device and method of manufacturing light extraction substrate of organic light emitting device by using the same |
JP2019215458A (en) * | 2018-06-13 | 2019-12-19 | Agc株式会社 | Optical laminate |
JP7234514B2 (en) | 2018-06-13 | 2023-03-08 | Agc株式会社 | optical laminate |
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