CN114316680B - UV curing composition and application thereof in preparation of OLED light extraction component - Google Patents
UV curing composition and application thereof in preparation of OLED light extraction component Download PDFInfo
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Abstract
The invention relates to a UV curing composition and application thereof in preparing an OLED light extraction component, and belongs to the technical field of UV curing compositions. In order to solve the problems that an OLED light extraction component printing material can only be cured in a nitrogen environment, the production efficiency is low, and the energy consumption is high, the invention provides a UV curing composition, which comprises metal oxide nanoparticles, an epoxy resin active diluent, a photoinitiator and a leveling agent, wherein the viscosity of the UV curing composition is less than 50cp at room temperature, the ink-jet printing requirement is met, the problem of oxygen inhibition does not exist, the rapid curing can be realized in an air environment, the production energy consumption is reduced, and the production efficiency is obviously improved. The OLED light extraction component prepared by taking the UV curing composition as a raw material has high refraction, high transmission and high flatness, the refractive index can reach 1.615-1.802, the transmission rate can reach more than 95%, and the light extraction efficiency can be obviously improved.
Description
Technical Field
The invention belongs to the technical field of UV curing compositions, and particularly relates to a UV curing composition and application thereof in preparation of OLED light extraction components.
Background
An Organic light-Emitting Diode (OLED), also called an Organic electroluminescent Display (OELD), is thinner and lighter than an LCD, and has the characteristics of high brightness, low power consumption, fast response, high definition, good flexibility, and high light-Emitting efficiency.
The OLED device comprises a substrate, a cathode, an anode, a Hole Injection Layer (HIL), an Electron Injection Layer (EIL), a Hole Transport Layer (HTL), an electron transport layer (RTL), an Electron Blocking Layer (EBL), a Hole Blocking Layer (HBL), an emitting layer (EML) and the like. The OLED belongs to a current-type organic light emitting device, and under the action of an electric field, holes generated by an anode and electrons generated by a cathode move, are respectively injected into a hole transport layer and an electron transport layer, and migrate to a light emitting layer. When the two meet at the light-emitting layer, energy excitons are generated to excite the light-emitting molecules to finally generate visible light.
Due to reflection caused by refractive index matching of materials of each layer in the OLED device, most of light emitted by the light emitting layer forms total reflection at a plurality of interfaces, so that the light is trapped in the display device, and the light emitting efficiency of the light emitting device is reduced. The high refraction light extraction layer can change the traveling route of light rays and reduce the light rays confined in the OLED device.
The invention patent application publication No. CN113316609A, "solventless formulation and nanocomposite material", provides a high refractive index acrylic formulation embedded with metal oxide nanocrystals having an average particle size of less than 30nm, which uses acrylic monomers containing unsaturated double bonds or resin-dispersed metal oxide nanocrystals to prepare UV curable light extractable printing materials. Because the printing requires a material with a low viscosity, only mono-or trifunctional acrylic monomers can be selected for dilution, which results in a narrow range of initiators for UV-curable materials, resulting in an oxygen inhibition effect causing a slower cure. In order to prevent the oxygen inhibition effect, the curing can be only carried out in a nitrogen environment, the requirement on equipment is high, the production efficiency is reduced, and the energy consumption is greatly increased.
Disclosure of Invention
In order to solve the problems that the printing material of the existing light extraction component can only be cured in a nitrogen environment, the production efficiency is low, and the energy consumption is high, the invention provides a UV curing composition and application thereof in preparing an OLED light extraction component.
The technical scheme of the invention is as follows:
the UV curing composition comprises the following components in parts by mass: 10 to 70 portions of metal oxide nano particles, 10 to 80 portions of epoxy resin reactive diluent, 0.5 to 5 portions of photoinitiator and 0.01 to 1 portion of flatting agent.
Further, the metal oxide nanoparticles comprise one or a combination of several of aluminum oxide nanoparticles, zinc oxide nanoparticles, hafnium oxide nanoparticles, zirconium oxide nanoparticles or titanium oxide nanoparticles, and the particle size of the metal oxide nanoparticles is not more than 10nm.
The metal oxide nanoparticles used in the present invention are obtained from SZR-MIBK SERIES, sakai chemical industry Co., ltd, and MHI FUNCTIONAL SERIES, japan imperial pigment Co., ltd, and the surface of the metal oxide nanoparticles used in the present invention is grafted with an organic group, and can be dispersed in an epoxy system more preferably.
Further, the epoxy resin reactive diluent comprises a mono-functional, di-functional or tri-functional epoxy compound containing an epoxy group, wherein the epoxy group is a propylene oxide structure or an oxetane structure.
Furthermore, the epoxy resin reactive diluent also contains unsaturated double bonds.
Further, the epoxy resin reactive diluent comprises one or a combination of several of the following compounds:
further, the photoinitiator includes a cationic initiator of a sulfonium salt or an iodonium salt.
Further, the photoinitiator specifically comprises BASF250 or BASF290.
Further, the leveling agent comprises BYK361N, BYK3500, BYK3510, BYK3550, BYK361N, BYK378 or BYK333. Leveling agents conventionally used in the art may be compounded with the UV curable composition of the present invention to further improve the flatness of the light extraction features.
Use of a UV curable composition as described in the present invention for the preparation of an OLED light extraction feature.
Furthermore, the OLED light extraction component is obtained by taking any one of the UV curing compositions as a raw material and carrying out UV curing after ink-jet printing, spin coating, spray coating, blade coating, slit coating, screen printing or embossing printing.
The invention has the beneficial effects that:
the UV curing composition provided by the invention has the viscosity of less than 50cp at room temperature, and can meet the requirements of ink-jet printing. According to the invention, epoxy resin cation curing is adopted, so that the problem of oxygen inhibition does not exist in the UV curing process, and the rapid curing can be realized in the air environment; compared with the existing acrylate curing system, the method has the advantages that the requirement on supporting equipment is reduced, the production energy consumption is reduced, and meanwhile, the production efficiency is obviously improved.
The OLED light extraction component prepared by taking the UV curing composition as a raw material has high refraction, high transmission and high flatness, the refractive index can reach 1.615-1.802, the transmission rate can reach more than 95%, and the light extraction efficiency can be obviously improved. Because the UV curing printing material does not have the problem of oxygen inhibition, the thickness of the high-refraction light extraction layer film prepared by the UV curing printing material is thinner than that of the existing film, and can reach 5-30 mu m, and the performance of an OLED display device can be further improved.
Based on the UV curing composition provided by the invention, conventional functional auxiliaries in the field such as a surfactant, a wetting agent, an antioxidant, a dispersing agent, a plasticizer, a toughening agent, a thickening agent, a dispersing agent, a softening agent and the like can be compounded according to conventional addition amounts, so that the performances of the UV curing composition and a light extraction component prepared from the UV curing composition are further improved.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, all technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
The metal oxide nanoparticles used in the following examples were obtained from SZR-MIBK SERIES, made by Sakai chemical industry Co., ltd, and MHI FUNCTIONAL SERIES, made by Yukai pigment Co., ltd, and the metal oxide nanoparticles used were surface-grafted with an organic group and were more preferably dispersed in an epoxy system; the particle size of the metal oxide nanoparticles is not more than 10nm, more preferably not more than 5nm, so as to avoid high optical haze caused by excessive particle size.
Example 1
This example provides a UV curable composition comprising the components in parts by mass as shown in table 1.
TABLE 1
Preparation method of UV-curable composition: the components shown in Table 1 were weighed precisely in parts by mass, mixed for 1 to 2 hours by mechanical stirring or magnetic stirring, and filtered with a 1 μm filter membrane after uniform mixing to obtain a UV curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 30cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 2
This example provides a UV curable composition comprising the components in parts by mass as shown in table 2.
TABLE 2
Preparation method of UV-curable composition: the components shown in Table 2 were weighed precisely in parts by mass, mixed for 1 to 2 hours by mechanical stirring or magnetic stirring, and filtered with a 1 μm filter membrane after uniform mixing to obtain a UV curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 40cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 3
The present embodiment provides a UV curable printing material including the components in parts by mass as shown in table 3.
TABLE 3
Preparation method of UV curable composition: the components shown in Table 3 were weighed precisely in parts by mass, mixed for 1 to 2 hours by mechanical stirring or magnetic stirring, and filtered with a 1 μm filter membrane after uniform mixing to obtain a UV curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV curing composition prepared by the embodiment is detected to be 40cp by a BROOKFILED viscometer at 25 ℃, and the requirement of ink-jet printing is met.
Example 4
The present embodiment provides a UV curable printing material including the components in parts by mass as shown in table 4.
TABLE 4
Preparation method of UV-curable composition: the components shown in Table 4 were weighed precisely in parts by mass, mixed for 1 to 2 hours by mechanical stirring or magnetic stirring, and filtered with a 1 μm filter membrane after uniform mixing to obtain a UV-curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 40cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 5
The present embodiment provides a UV curable printing material including the components in parts by mass as shown in table 5.
TABLE 5
Preparation method of UV curable composition: the components shown in Table 5 were weighed precisely in parts by mass, mixed for 1 to 2 hours by mechanical stirring or magnetic stirring, and filtered with a 1 μm filter membrane after uniform mixing to obtain a UV-curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 40cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 6
The present embodiment provides a UV curable printing material including the components in parts by mass as shown in table 6.
TABLE 6
Preparation method of UV curable composition: the components shown in table 6 were weighed precisely in parts by mass, mixed for 1 to 2 hours with mechanical stirring or magnetic stirring, and filtered with a 1 μm filtration membrane after being mixed uniformly to obtain a UV curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 40cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 7
The present embodiment provides a UV curable printing material including the components in parts by mass as shown in table 7.
TABLE 7
Preparation method of UV-curable composition: the components shown in table 7 were weighed precisely in parts by mass, mixed for 1 to 2 hours with mechanical stirring or magnetic stirring, and filtered with a 1 μm filtration membrane after being mixed uniformly to obtain a UV curable composition.
Viscosity test method of UV curable composition: the viscosity of the UV-curable composition prepared in this example was measured to be 40cp at 25 ℃ using a BROOKFILED viscometer, which meets the requirements of ink-jet printing.
Example 8
This example prepares a light extraction member for application to an OLED by inkjet printing using the UV curable composition prepared in example 1 to example 7 as a raw material, and examines the refractive index and transmittance of the prepared light extraction member.
The printing and curing method adopted by the embodiment comprises the following steps: the spray head is selected from KM1024i (30 pl), and is cured by 395nm LED UV light source with the light illumination of 1000mw/s/cm 2 *2s, and the curing time is 1-10 s.
In this example, the light extraction members prepared by printing and curing were each a light extraction layer having a thickness of 20 μm, and the refractive index of each light extraction layer was measured by an ellipsometer (wuhan Yilight), and the transmittance of each light extraction layer was measured by an ULtra SCAN VIS. The results are shown in Table 8.
TABLE 8
| Light extraction member | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 |
| Refractive index | 1.698 | 1.703 | 1.653 | 1.720 | 1.736 | 1.653 | 1.743 |
| Transmittance (%) | 96.8 | 96.3 | 97.0 | 96.2 | 96.8 | 97.2 | 95.9 |
As can be seen from the data in Table 8, the UV curable composition provided by the invention is used for preparing OLED light extraction components, and higher refractive index and transmittance are obtained. According to the OLED device design structure, the light extraction component with high refractive index can well reduce the total reflection of an OLED light emitting layer, improve the light emitting efficiency of the OLED and has good transmittance. Compared with an OLED device without the light extraction layer, the light extraction efficiency of the OLED device can be improved by 20%.
Claims (3)
1. The UV curing composition is characterized by comprising the following components in parts by mass:
50 parts of zirconia nano particles,
A cationic initiator IRGACURE 250 parts and a flatting agent BYK361N 0.1 part; or comprises the following components in parts by mass:
50 parts of zinc oxide nano particles,
250 parts of cationic initiator IRGACURE and 3500.05 parts of flatting agent BYK; or comprises the following components in parts by mass:
50 parts of titanium oxide nano particles,
0.5 part of cationic initiator IRGACURE 290 and 0.05 part of flatting agent BYK 3510; or comprises the following components in parts by mass:
50 parts of alumina nano particles,
0.5 part of cationic initiator IRGACURE 290 and 0.03 part of flatting agent BYK 3550; or comprises the following components in parts by mass:
40 parts of titanium oxide nano particles,
0.5 part of cationic initiator IRGACURE 290 and 0.02 part of leveling agent BYK 361N; or comprises the following components in parts by mass:
50 parts of hafnium oxide nano particles,
0.5 part of cationic initiator IRGACURE 290 and 0.01 part of flatting agent BYK 378; or comprises the following components in parts by mass:
50 parts of zirconia nano particles,
0.5 part of cationic initiator IRGACURE 290 and 1 part of leveling agent BYK333.
2. Use of the UV curable composition of claim 1 for the preparation of an OLED light extraction feature.
3. The use of the UV-curable composition according to claim 2 for the preparation of an OLED light extraction member, wherein the OLED light extraction member is obtained by UV-curing after inkjet printing, spin coating, spray coating, blade coating, slot coating, screen printing or flexo printing, using the UV-curable composition according to claim 1 as a raw material.
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| CN102208566A (en) * | 2011-04-18 | 2011-10-05 | 电子科技大学 | Substrate used in luminescent device and preparation method thereof |
| CN102208555B (en) * | 2011-04-18 | 2013-07-31 | 电子科技大学 | Substrate used in luminescent device and preparation method thereof |
| CN102208563B (en) * | 2011-04-18 | 2013-01-30 | 电子科技大学 | Substrate for flexible luminescent device and preparation method thereof |
| CN107987216B (en) * | 2017-11-12 | 2020-07-28 | 江门职业技术学院 | Photosensitive three-dimensional printing structural color material and preparation method thereof |
| CN108130029A (en) * | 2017-12-22 | 2018-06-08 | 烟台德邦科技有限公司 | A kind of conductive silver glue of UV retardation of curing and preparation method thereof |
| CN111607289B (en) * | 2020-06-15 | 2021-07-06 | 中国科学技术大学 | Ultraviolet curing ink-jet printing ink with double curing mechanisms and preparation method thereof |
| CN113717350B (en) * | 2021-08-19 | 2024-02-23 | 浙江福斯特新材料研究院有限公司 | Photocurable composition, package structure, and semiconductor device |
| CN114031893A (en) * | 2021-10-29 | 2022-02-11 | 武汉尚赛光电科技有限公司 | High-refractive-index photocuring composition and preparation method and application thereof |
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