CN110819165A - Printable OLED electronic ink and preparation method thereof - Google Patents
Printable OLED electronic ink and preparation method thereof Download PDFInfo
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Abstract
The invention provides printable OLED electronic ink and a preparation method thereof, wherein the electronic ink is prepared by taking silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator, an OLED organic luminescent material and water as raw materials to prepare the OLED organic luminescent material loaded on aerogel, then taking nano alloy particles, P-type nano metal oxide particles and an alcohol solvent as raw materials to prepare dispersion liquid, and then mixing and stirring the dispersion liquid with an alkali metal complex doping material, a surface tension regulator, a viscosity regulator, a polar mixed solvent and an auxiliary solvent. The OLED material in the OLED electronic ink provided by the invention has good dispersibility, and the physical properties of the composite ink, such as viscosity, surface tension, boiling point and the like, can meet the requirements of the existing ink-jet printing equipment, and has good printing smoothness and wide application prospect.
Description
Technical Field
The invention relates to the technical field of OLED manufacturing, in particular to printable OLED electronic ink and a preparation method thereof.
Background
In the era of rapid display technology change, the Organic Light Emitting Diode (OLED) display technology, which is a next generation display technology, has a series of outstanding advantages of self-luminescence, high contrast, wide color gamut, large viewing angle, fast response speed, flexible display and the like, and is considered as a next generation novel flat panel display technology with the most potential, and is once becoming a hot topic of the industry. At present, since the cost of OLED is too high and mass production is difficult, OLED cannot meet the market demand, and the fabrication process is difficult to escape from the responsibility.
At present, there are two distinct manufacturing processes in the OLED display technology, one is FMM evaporation process, and the other is inkjet printing process, which are very different from manufacturing equipment and manufacturing materials. The evaporation process is that in vacuum, evaporated material is evaporated into atoms or molecules by means of current heating, electron beam bombardment heating, laser heating and the like, and the atoms or molecules move linearly with great freedom and collide with the surface of the substrate to be condensed to form a film. And the main material of the ink-jet printing OLED panel is OLED organic material, and then the material fused by the solvent is directly jet-printed on the substrate through a high-precision nozzle, so that the RGB organic light-emitting layer is formed.
In summary, the evaporation process has the disadvantages of complex equipment and process, high energy consumption, large material waste, high cost, and the like, and the inkjet printing is gradually becoming the mainstream manufacturing process of the OLED panel by virtue of its unique technical characteristics and manufacturing advantages, and will change the mode of the whole display industry. In the current common structure of the OLED device for ink-jet printing, the hole injection layer, the hole transport layer and the light-emitting layer are printed, but the electron transport layer and the cathode are still in the evaporation process. Most OLED organic materials are materials dissolved by organic solvents, and are difficult to disperse after being prepared into ink, and mutual solubility phenomenon is easy to exist between the OLED organic materials and a light-emitting layer, so that the device preparation in the full-solution process is difficult. In order to realize the all-solution process, the development of the OLED material electronic ink without damaging the light emitting layer is required.
Chinese patent application No. 201810153650.8 discloses an ink composition for inkjet printing comprising polythiophene, and provides an ink composition comprising polythiophene and polymethylsiloxane, which is formulated for inkjet printing a Hole Injection Layer (HIL) of an Organic Light Emitting Diode (OLED). The Chinese patent application No. 201310089765.2 discloses a transparent carbon nanotube polymer composite conductive ink and a preparation method thereof, wherein the conductive ink is composed of modified carbon nanotubes, conductive polymers, a water-soluble polymer cosolvent, a polymer modification auxiliary agent, a surfactant and deionized water, and is prepared by a solution blending process technology.
In order to maintain the advantages of OLED inkjet printing and avoid the problems that ink configured by an OLED light-emitting material is difficult to disperse, mutual solubility between light-emitting layers is easy to occur, the light-emitting layers are damaged, and the like, it is necessary to provide a novel printable OLED electronic ink, thereby promoting the development and application of an inkjet printing OLED device.
Disclosure of Invention
Aiming at the problems that the OLED luminescent material is prepared into ink at present, the dispersion is difficult, the luminescent layer is damaged, and the like, the invention provides the printable OLED electronic ink and the preparation method thereof, so that the problem of material agglomeration in the OLED electronic ink is effectively avoided, the dispersibility of the ink is improved, the luminescent layer is not damaged, and the requirements of the existing OLED ink-jet printing can be effectively met.
In order to solve the problems, the invention adopts the following technical scheme:
the printable OLED electronic ink is prepared by taking silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator, an OLED organic light-emitting material and water as raw materials to prepare the OLED organic light-emitting material loaded on aerogel, then taking nano alloy particles, P-type nano metal oxide particles and an alcohol solvent as raw materials to prepare dispersion liquid, and then mixing and stirring the dispersion liquid with an alkali metal complex doping material, a surface tension regulator, a viscosity regulator, a polar mixed solvent and an auxiliary solvent.
Preferably, the silicate is one of ethyl orthosilicate, methyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
Preferably, the organic solvent is one of ethanol, methanol, propanol, butanol and acetone.
Preferably, the silane coupling agent is one or the combination of more than two of gamma-aminopropyl triethoxysilane, gamma-chloropropyl triethoxysilane, vinyl trichlorosilane, vinyl triethoxysilane, gamma-aminopropyl trimethoxysilane and gamma-chloropropyl trimethoxysilane.
Preferably, the polymer monomer is a monomer for preparing a transparent flexible polymer, and the transparent flexible polymer is one of polymethyl methacrylate, polystyrene, polyurethane and silane modified polyether.
Preferably, the initiator is one of benzoyl peroxide and azobisisobutyronitrile.
Preferably, the OLED organic light-emitting material is one or a combination of more than two of a phosphorescent material, a delayed fluorescence material and a rare earth complex material.
Preferably, the nano alloy particles are spherical alloy particles of two or more elements of gold, silver, aluminum, copper, iron, nickel and platinum, and the diameter of the nano alloy spherical particles is 2-100 nm.
Preferably, the P-type nano metal oxide particles are one or a combination of more than two of nano nickel oxide particles, nano molybdenum oxide particles and nano tungsten oxide particles.
Preferably, the alcohol solvent is one of methanol, ethanol, n-propanol, isopropanol, n-butanol, 2-butanol, tert-butanol, and 2-methyl-1-propanol.
Preferably, the alkali metal complex doping material is 8-hydroxyquinolinolato lithium.
Preferably, the polar mixed solvent is a polyol compound.
Preferably, the surface tension regulator is one or a combination of more than two of a cosolvent, a surfactant and a small molecular compound for regulating the surface tension, and the small molecular compound for regulating the surface tension is one or a combination of more than two of imidazole and derivatives thereof, phenol and hydroquinone.
Preferably, the viscosity regulator comprises one or more of alcohol, ether, ester, phenol and amine compounds.
Preferably, the auxiliary solvent is one of alcohols, ketones, ethers, esters and amides.
The invention also provides a preparation method of the printable OLED electronic ink, which comprises the following specific steps:
(1) uniformly mixing silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator and water to prepare a mixed solution, adding an OLED organic light-emitting material, and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at a preset temperature for a preset time to form wet gel, and then converting the wet gel into aerogel by using a supercritical drying method to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding the nano alloy particles and the P type nano metal oxide particles into an alcohol solvent, and uniformly dispersing to obtain a dispersion liquid of the nano alloy particles and the P type nano metal oxide particles;
(4) and dissolving the OLED organic luminescent material and the alkali metal complex doping material loaded on the aerogel into the polar mixed solvent, uniformly mixing, adding the surface tension regulator, the viscosity regulator, the dispersion liquid and the auxiliary solvent, and uniformly stirring at a certain temperature to obtain the printable OLED electronic ink.
Preferably, in the mixed solution in the step (1), the molar ratio of the silicate ester, the organic solvent, the silane coupling agent, the polymer monomer, the initiator and the water is 1:0.1-0.3: 0.02-0.08: 0.3-0.7: 0.15-0.4: 1-3.
Preferably, in the mixed system in the step (1), the mass ratio of the mixed solution to the OLED organic light-emitting material is 100: 10-20.
Preferably, the preset temperature in the step (2) is 60-70 ℃, and the preset time is 24-28 h.
Preferably, the supercritical drying in the step (2) adopts supercritical carbon dioxide drying, the temperature is 30-35 ℃, and the pressure is 8-15 MPa.
Preferably, in the dispersion liquid in the step (3), the mass ratio of the alcohol solvent, the nano alloy particles and the P-type nano metal oxide particles is 100:5-15: 8-18.
Preferably, the stirring temperature in step (4) is 0 to 80 ℃.
Preferably, in the electronic ink in the step (4), the mass ratio of the polar mixed solvent, the OLED organic light-emitting material loaded on the aerogel, the alkali metal complex doping material, the surface tension regulator, the viscosity regulator, the dispersion liquid and the auxiliary solvent is 100:10-15:8-12: 0.5-3: 0.5-3: 10-20: 15-25.
As is known, the method for manufacturing an OLED screen by inkjet printing mainly includes dissolving OLED organic materials with a solvent, and then directly inkjet printing the materials on the surface of a substrate to form R (red), G (green), and B (blue) organic light emitting layers. Compared with the evaporation technology, the inkjet printing OLED technology has obvious advantages in the aspects of manufacturing process, yield, cost and the like, but the inkjet printing technology is limited in development due to a series of difficulties existing in the process. Most OLED organic materials are materials dissolved by organic solvents, and are difficult to disperse after being prepared into electronic ink, and mutual solubility phenomenon is easy to exist between the OLED organic materials and a light-emitting layer, so that the device preparation in the full-solution process is difficult.
The invention prepares the silicon dioxide/organic polymer hybrid aerogel by a supercritical drying method. The silicon dioxide aerogel is a porous, light and amorphous nano solid material with a continuous three-dimensional network structure and formed by the existence of interconnected nano particles, has the characteristics of high specific surface area, low density, high porosity and the like, introduces an organic group which does not undergo hydrolysis on silicon atoms, can effectively improve the mechanical property of the aerogel, and simultaneously utilizes a supercritical drying method to obtain the hybrid aerogel with the characteristics of elasticity, light weight, excellent mechanical property and the like.
Furthermore, the silicon dioxide/organic polymer hybrid aerogel is used as a matrix to load the OLED organic light-emitting material, so that the OLED material is orderly and controllably dispersed in the three-dimensional network framework structure of the aerogel, the agglomeration of the OLED material can be effectively avoided, the dispersibility is improved, the mutual solubility with the light-emitting layer is avoided, and the problem that the light-emitting layer is damaged is prevented.
Furthermore, spherical nano alloy particles, P-type nano metal oxide particles, a surface tension regulator, a viscosity regulator and the like are added in the electronic ink configuration, so that the viscosity and the surface tension of the ink can be effectively reduced, a printer nozzle cannot be blocked in ink-jet printing, and the printing fluency can be effectively improved.
The existing ink prepared by the OLED luminescent material has the problems of difficult dispersion, damage to a luminescent layer and the like, and the application of the existing ink is limited. In view of the above, the invention provides a printable OLED electronic ink and a preparation method thereof, silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator and water are uniformly mixed, and then an OLED organic light-emitting material is added and uniformly mixed; reacting the obtained system at a preset temperature for a preset time to form wet gel; and converting the obtained wet gel into aerogel by using a supercritical drying method to obtain the OLED organic light-emitting material loaded on the aerogel. Dispersing the nano alloy particles and the P-type nano metal oxide particles in an alcohol solvent to obtain a nano alloy particle and P-type nano metal oxide particle dispersion liquid; and dissolving the OLED organic luminescent material loaded on the aerogel and the alkali metal complex doping material in a polar mixed solvent, uniformly mixing, adding a surface tension regulator, a viscosity regulator, a dispersion liquid and an auxiliary solvent, and uniformly stirring to obtain the printable OLED electronic ink. The OLED material in the OLED electronic ink provided by the invention has good dispersibility, and the physical properties such as the agglomerated viscosity, surface tension, boiling point and the like of the composite ink can meet the requirements of the existing ink-jet printing equipment, and the OLED electronic ink has good printing smoothness and wide application prospect.
Compared with the prior art, the invention provides the printable OLED electronic ink and the preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. the composite ink provided by the invention has physical properties such as viscosity, surface tension, boiling point and the like which can meet the requirements of the existing ink-jet printing equipment, and has good printing fluency.
2. According to the invention, the silicon dioxide/organic polymer hybrid aerogel is used as a matrix to load the OLED organic light-emitting material, so that the OLED material is orderly and controllably dispersed in the three-dimensional network skeleton structure of the aerogel, the agglomeration of the OLED material can be effectively avoided, the overlapping rate of the OLED material is reduced, the prepared ink has good dispersibility, and the existing ink-jet printing equipment can be met.
Drawings
FIG. 1 is a print flow diagram of example 1;
figure 2 is a flow chart of the print of comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Uniformly mixing 1mol of ethyl orthosilicate, 0.15mol of ethanol, 0.04 mol of gamma-aminopropyltriethoxysilane, 0.4mol of polymethyl methacrylate, 0.2mol of benzoyl peroxide and 2.5mol of water to prepare a mixed solution, and then adding 13 parts by weight of phosphorescent material into 100 parts by weight of the mixed solution and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at 62 ℃ for 27h to form wet gel, drying by using supercritical carbon dioxide, and drying at 31 ℃ and 10MPa to convert the wet gel into aerogel so as to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding 8 parts by weight of spherical gold and silver alloy particles with the average diameter of 30nm and 12 parts by weight of nano nickel oxide particles into 100 parts by weight of methanol, and uniformly dispersing to obtain a dispersion liquid of nano alloy particles and P-type nano metal oxide particles;
(4) and (2) dissolving 12 parts by weight of the OLED organic luminescent material loaded on the aerogel and 9 parts by weight of 8-hydroxyquinoline lithium in 100 parts by weight of the polyol compound, uniformly mixing, then adding 1 part by weight of imidazole, 1 part by weight of the alcohol compound, 12 parts by weight of the dispersion liquid and 17 parts by weight of the alcohol compound, and uniformly stirring at 10 ℃ to obtain the printable OLED electronic ink.
Example 2
(1) Uniformly mixing 1mol of methyl orthosilicate, 0.25mol of methanol, 0.07 mol of gamma-chloropropyltriethoxysilane, 06 mol of polystyrene, 0.3mol of azobisisobutyronitrile and 2.5mol of water to prepare a mixed solution, and then adding 18 parts by weight of delayed fluorescent material into 100 parts by weight of the mixed solution and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at 68 ℃ for 25h to form wet gel, drying by using supercritical carbon dioxide, and drying at the temperature of 34 ℃ and the pressure of 12MPa to convert the wet gel into aerogel so as to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding 12 parts by weight of spherical aluminum and copper alloy particles with the average diameter of 80nm and 15 parts by weight of nano molybdenum oxide particles into 100 parts by weight of n-propanol, and uniformly dispersing to obtain a dispersion liquid of the nano alloy particles and the P-type nano metal oxide particles;
(4) and (2) dissolving 14 parts by weight of the OLED organic luminescent material loaded on the aerogel and 11 parts by weight of 8-hydroxyquinoline lithium in 100 parts by weight of the polyol compound, uniformly mixing, adding 2 parts by weight of phenol, 2 parts by weight of the ether compound, 18 parts by weight of the dispersion liquid and 22 parts by weight of the ketone compound, and uniformly stirring at 70 ℃ to obtain the printable OLED electronic ink.
Example 3
(1) Uniformly mixing 1mol of propyl orthosilicate, 0.1mol of propanol, 0.02 mol of vinyl trichlorosilane, 0.3mol of polyurethane, 0.15mol of benzoyl peroxide and 1mol of water to prepare a mixed solution, and then adding 10 parts by weight of rare earth complex material into 100 parts by weight of the mixed solution and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at 60 ℃ for 28h to form wet gel, drying by using supercritical carbon dioxide, and drying at the temperature of 30 ℃ and the pressure of 8MPa to convert the wet gel into aerogel so as to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding 5 parts by weight of spherical iron and nickel alloy particles with the average diameter of 10nm and 8 parts by weight of nano tungsten oxide particles into 100 parts by weight of isopropanol, and uniformly dispersing to obtain a dispersion liquid of the nano alloy particles and the P-type nano metal oxide particles;
(4) dissolving 10 parts by weight of OLED organic luminescent material loaded on aerogel and 8 parts by weight of 8-hydroxyquinoline lithium in 100 parts by weight of polyol compound, uniformly mixing, then adding 0.5 part by weight of hydroquinone, 0.5 part by weight of ester compound, 10 parts by weight of dispersion liquid and 15 parts by weight of ether compound, and uniformly stirring at 0 ℃ to obtain the printable OLED electronic ink.
Example 4
(1) Uniformly mixing 1mol of n-butyl orthosilicate, 0.3mol of butanol, 0.08 mol of vinyl triethoxysilane, 0.7 mol of silane modified polyether, 0.4mol of azobisisobutyronitrile and 3mol of water to prepare a mixed solution, adding 20 parts by weight of phosphorescent material into 100 parts by weight of the mixed solution, and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at 70 ℃ for 24h to form wet gel, drying by using supercritical carbon dioxide, and drying at 35 ℃ and 15MPa to convert the wet gel into aerogel so as to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding 15 parts by weight of spherical nickel with the average diameter of 100nm, platinum alloy particles and 18 parts by weight of nano nickel oxide particles into 100 parts by weight of n-butyl alcohol, and uniformly dispersing to obtain a dispersion liquid of nano alloy particles and P-type nano metal oxide particles;
(4) and (2) dissolving 15 parts by weight of the OLED organic luminescent material loaded on the aerogel and 12 parts by weight of 8-hydroxyquinoline lithium in 100 parts by weight of the polyol compound, uniformly mixing, adding 3 parts by weight of imidazole, 3 parts by weight of the phenol compound, 20 parts by weight of the dispersion liquid and 25 parts by weight of the ester compound, and uniformly stirring at 80 ℃ to obtain the printable OLED electronic ink.
Example 5
(1) Uniformly mixing 1mol of ethyl orthosilicate, 0.2mol of acetone, 0.05 mol of gamma-chloropropyltrimethoxysilane, 5mol of polymethyl methacrylate, 0.25mol of benzoyl peroxide and 2mol of water to prepare a mixed solution, adding 15 parts by weight of phosphorescent material into 100 parts by weight of the mixed solution, and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at 65 ℃ for 26h to form wet gel, drying by using supercritical carbon dioxide, and drying at 32 ℃ and under the pressure of 12MPa to convert the wet gel into aerogel so as to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding 10 parts by weight of spherical gold with the average diameter of 50nm, platinum alloy particles and 13 parts by weight of nano nickel oxide particles into 100 parts by weight of 2-butanol, and uniformly dispersing to obtain a dispersion liquid of the nano alloy particles and the P-type nano metal oxide particles;
(4) and (2) dissolving 12 parts by weight of the OLED organic luminescent material loaded on the aerogel and 10 parts by weight of 8-hydroxyquinoline lithium in 100 parts by weight of the polyol compound, uniformly mixing, adding 2 parts by weight of hydroquinone, 2 parts by weight of the amine compound, 15 parts by weight of the dispersion liquid and 20 parts by weight of the amide compound, and uniformly stirring at 40 ℃ to obtain the printable OLED electronic ink.
Comparative example 1
Comparative example 1 no silica/organic polymer hybrid aerogel was used as a matrix to support the OLED organic light emitting material, and the rest of the preparation process was referred to example 1.
The test method comprises the following steps:
and (3) viscosity testing: the viscosities of the inks of examples 1 to 5 and comparative example 1 were measured using a rotary viscometer;
surface tension test: pouring the inks in the examples 1-5 and the comparative example 1 into a beaker, carrying out constant-temperature water bath to 40 ℃, and detecting by adopting a dynamic surface tension meter;
printing fluency test: the inks of example 1 and comparative example 1, which were stable in standing, were passed through a 2 μm filter head, placed in a liquid reservoir of an ink jet printer, subjected to ink jet printing, and observed for smoothness and clogging of the head. FIG. 1 is a printing flow diagram of example 1, and the printing flow of the ink obtained in example 1 is uniform and has no floating, as shown in FIG. 1; FIG. 2 is a flow chart of printing of comparative example 1, and the ink of comparative example 1 prints with uneven flow and ink break, as shown in FIG. 2.
The test results are shown in table 1;
table 1:
therefore, the ink disclosed by the invention is low in viscosity and surface tension, is not easy to agglomerate to cause blockage of a printer nozzle, and has a wide application prospect.
Claims (10)
1. The printable OLED electronic ink is characterized in that silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator, an OLED organic light-emitting material and water are used as raw materials to prepare the OLED organic light-emitting material loaded on aerogel, then nano alloy particles, P-type nano metal oxide particles and an alcohol solvent are used as raw materials to prepare dispersion liquid, and then the dispersion liquid is mixed and stirred with an alkali metal complex doping material, a surface tension regulator, a viscosity regulator, a polar mixed solvent and an auxiliary solvent to prepare the printable OLED electronic ink.
2. The printable OLED electronic ink, according to claim 1,
the silicate is one of ethyl orthosilicate, methyl orthosilicate, propyl orthosilicate and butyl orthosilicate;
the organic solvent is one of ethanol, methanol, propanol, butanol and acetone;
the silane coupling agent is one or the combination of more than two of gamma-aminopropyl triethoxysilane, gamma-chloropropyl triethoxysilane, vinyl trichlorosilane, vinyl triethoxysilane, gamma-aminopropyl trimethoxysilane and gamma-chloropropyl trimethoxysilane;
the polymer monomer is used for preparing a transparent flexible polymer, and the transparent flexible polymer is one of polymethyl methacrylate, polystyrene, polyurethane and silane modified polyether;
the initiator is one of benzoyl peroxide and azobisisobutyronitrile;
the OLED organic light-emitting material is one or a combination of more than two of a phosphorescent material, a delayed fluorescence material and a rare earth complex material;
the nano alloy particles are two or more of spherical gold, silver, aluminum, copper, iron, nickel and platinum alloy particles, and the diameter of the nano alloy spherical particles is 2-100 nm;
the P-type nano metal oxide particles are one or the combination of more than two of nano nickel oxide particles, nano molybdenum oxide particles and nano tungsten oxide particles;
the alcohol solvent is one of methanol, ethanol, n-propanol, isopropanol, n-butanol, 2-butanol, tert-butanol and 2-methyl-1-propanol;
the alkali metal complex doping material is 8-hydroxyquinoline lithium;
the polar mixed solvent is a polyol compound;
the surface tension regulator is one or the combination of more than two of a cosolvent, a surfactant and a small molecular compound for regulating the surface tension, and the small molecular compound for regulating the surface tension is one or the combination of more than two of imidazole and derivatives thereof, phenol and hydroquinone;
the viscosity regulator comprises one or the combination of more than two of alcohol, ether, ester, phenol and amine compounds;
the auxiliary solvent is one of alcohols, ketones, ethers, esters and amides.
3. The method for preparing the printable OLED electronic ink as claimed in any one of claims 1-2, wherein the specific preparation method is as follows:
(1) uniformly mixing silicate ester, an organic solvent, a silane coupling agent, a polymer monomer, an initiator and water to prepare a mixed solution, adding an OLED organic light-emitting material, and uniformly mixing to obtain a mixed system;
(2) reacting the obtained mixed system at a preset temperature for a preset time to form wet gel, and then converting the wet gel into aerogel by using a supercritical drying method to obtain the OLED organic light-emitting material loaded on the aerogel;
(3) adding the nano alloy particles and the P type nano metal oxide particles into an alcohol solvent, and uniformly dispersing to obtain a dispersion liquid of the nano alloy particles and the P type nano metal oxide particles;
(4) and dissolving the OLED organic luminescent material and the alkali metal complex doping material loaded on the aerogel into the polar mixed solvent, uniformly mixing, adding the surface tension regulator, the viscosity regulator, the dispersion liquid and the auxiliary solvent, and uniformly stirring at a certain temperature to obtain the printable OLED electronic ink.
4. The method of claim 3, wherein the mixed solution of silicate ester, organic solvent, silane coupling agent, polymer monomer, initiator and water in the step (1) has a molar ratio of 1:0.1-0.3: 0.02-0.08: 0.3-0.7: 0.15-0.4: 1-3.
5. The method of claim 3, wherein in the step (1), the mass ratio of the mixed solution to the OLED organic light-emitting material is 100: 10-20.
6. The method for preparing printable OLED electronic ink according to claim 3, wherein the preset temperature in step (2) is 60-70 ℃ and the preset time is 24-28 h.
7. The method of claim 3, wherein the supercritical drying in step (2) is performed with supercritical carbon dioxide at 30-35 ℃ and under a pressure of 8-15 MPa.
8. The method of claim 3, wherein in the dispersion of step (3), the mass ratio of the alcohol solvent to the nano-alloy particles to the P-type nano-metal oxide particles is 100:5-15: 8-18.
9. The method of claim 3, wherein the stirring temperature in step (4) is 0-80 ℃.
10. The method for preparing printable OLED electronic ink according to claim 3, wherein in the electronic ink in step (4), the mass ratio of the polar mixed solvent, the OLED organic light emitting material supported on the aerogel, the alkali metal complex doping material, the surface tension regulator, the viscosity regulator, the dispersion liquid, and the auxiliary solvent is 100:10-15:8-12: 0.5-3: 0.5-3: 10-20: 15-25.
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| WO2023070618A1 (en) * | 2021-10-30 | 2023-05-04 | 华为技术有限公司 | Light-emitting element ink and application of polymer in same, and display apparatus and manufacturing method therefor |
-
2019
- 2019-11-18 CN CN201911127526.5A patent/CN110819165A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023070618A1 (en) * | 2021-10-30 | 2023-05-04 | 华为技术有限公司 | Light-emitting element ink and application of polymer in same, and display apparatus and manufacturing method therefor |
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