CN114058298B - Functional glue and preparation method thereof, quantum dot functional glue solution and preparation method thereof - Google Patents

Functional glue and preparation method thereof, quantum dot functional glue solution and preparation method thereof Download PDF

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CN114058298B
CN114058298B CN202111457733.4A CN202111457733A CN114058298B CN 114058298 B CN114058298 B CN 114058298B CN 202111457733 A CN202111457733 A CN 202111457733A CN 114058298 B CN114058298 B CN 114058298B
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quantum dot
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parts
functional glue
glue
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CN114058298A (en
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张超
庄永漳
仉旭
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Laiyu Optoelectronic Technology Suzhou Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/10—Homopolymers or copolymers of methacrylic acid esters
    • C09J133/12—Homopolymers or copolymers of methyl methacrylate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
    • C09J167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0806—Silver
    • C—CHEMISTRY; METALLURGY
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0812—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
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    • C08K2003/0881—Titanium
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention provides functional glue and a preparation method thereof, quantum dot functional glue solution and a preparation method thereof, wherein the functional glue comprises 0.1-30 parts by weight of functional material, 25-49 parts by weight of polymer resin, 30-70 parts by weight of organic solvent and 1-5 parts by weight of photosensitive material, wherein the functional material is a material with oxidation performance. The invention can solve the problems that in the prior art, due to the existence of oxygen, the quantum dot is easily oxidized by taking the defect as the center, the surface defect is increased, the non-radiative recombination is increased, the structure of the quantum dot is collapsed, and the light conversion capability is reduced or even completely lost.

Description

Functional glue and preparation method thereof, quantum dot functional glue solution and preparation method thereof
Technical Field
The invention relates to the technical field of quantum dots, in particular to functional glue and a preparation method thereof, quantum dot functional glue solution and a preparation method thereof, and a display device for realizing light color conversion by using the quantum dot functional glue solution.
Background
The quantum dot display device has the advantages of high spectral purity, wide color gamut, high brightness and the like, and is considered to be an important development direction in the future of the display industry. The development of the quantum dot high-precision photoetching patterning technology has important significance for realizing the application of the quantum dot high-precision photoetching patterning technology in the display field. In the existing majority of quantum dot display products, the quantum dots mainly convert the blue backlight source of the liquid crystal display into red light and green light, and play a role in improving the color gamut and brightness of the display. In order to further use quantum dots as color conversion materials for Micro light-emitting diodes (Micro-LEDs) or directly use the electroluminescent properties of quantum dots to construct more advantageous active quantum dot electro-luminescent diodes (QLEDs) display devices, it is necessary to perform pixelation processing on the quantum dots. Therefore, the development of a patterning method of a quantum dot film has important significance for realizing the application of the quantum dot film in the fields of display and other photoelectric devices. While the use of photolithographic processes for the construction of quantum dot patterns has considerable advantages and development potential.
However, the quantum dots are easily damaged by external environments such as oxygen, water vapor and the like, and the luminous efficiency is greatly affected, so that one of the related technologies of the quantum dots is how to increase the stability of the quantum dots and keep the excellent luminous property of the quantum dots. In the existing formation process of quantum dot photoresist, quantum dots are generally dispersed in a polymer resin main body material to form quantum dot colloid, and then the quantum dot colloid is packaged into a film and the like to exist as a light conversion device. However, no matter how the packaging technology is mature, the capability of the polymer as one of the packaging materials to isolate external water vapor and oxygen is certain, and part of water vapor and oxygen can remain in the quantum dot colloid, which can cause great damage to the quantum dot and affect the service life and luminous performance of the quantum dot.
Disclosure of Invention
Aiming at the technical problems, the invention provides functional glue and a preparation method thereof, quantum dot functional glue solution and a preparation method thereof, and a display device for realizing light color conversion by using the quantum dot functional glue solution, so as to solve the problems that in the prior art, the quantum dot glue is easy to oxidize by taking defects as the center and increasing surface defects to cause non-radiative recombination increase, thereby causing collapse of a quantum dot structure, and the light conversion capability is reduced or even completely lost due to the existence of oxygen.
In order to achieve the above purpose, the invention provides functional glue, which comprises 0.1-30 parts by weight of functional material, 25-49 parts by weight of polymer resin, 30-70 parts by weight of organic solvent and 1-5 parts by weight of photosensitive material, wherein the functional material is a material with oxidation performance.
Preferably, the functional glue comprises, by weight, 5-25 parts of functional materials, 30-45 parts of polymer resins, 45-70 parts of organic solvents and 1-5 parts of photosensitive materials.
Preferably, the functional material comprises one or a mixture of several of nano aluminum, nano silver, nano zirconium, nano titanium, nano silicon, nano calcium and nano barium.
Preferably, the particle size of the functional material is 3nm to 500nm.
Preferably, the polymer resin comprises one or more of polymethyl methacrylate, polyethyl methacrylate, polyester acrylate, epoxy acrylate, polyurethane acrylate, acrylic resin and methyl methacrylate.
Preferably, the organic solvent comprises one or a mixture of a plurality of monofunctional reactive diluents, difunctional reactive diluents, polyfunctional reactive diluents, vinyl ether reactive diluents and methacrylate reactive diluents.
Preferably, the monofunctional reactive diluents comprise one or a mixture of more of propyl methacrylate, isobornyl acrylate and octadecyl acrylate; the difunctional reactive diluent comprises one or more of dipropylene glycol diacrylate, propoxylated glycerol triacrylate, tripropylene glycol diacrylate, ethylene glycol diacrylate and propylene glycol diacrylate; the multifunctional reactive diluent comprises one or more of trimethylolpropane triacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate and propylene glycol methyl ether acetate.
Preferably, the photosensitive material comprises one or a mixture of a plurality of cleavage type free radical photoinitiators, hydrogen abstraction type free radical photoinitiators, cationic photoinitiators, macromolecular photoinitiators, polymerizable photoinitiators, UV-LED photoinitiators and visible light initiators.
Preferably, the polymerizable photoinitiator comprises di-t-butyl peroxide; the cationic photoinitiator comprises one or two of an arylferrocenium salt and an aryldiazonium salt; the macromolecular photoinitiator comprises macromolecular benzophenone; the cracking type free radical photoinitiator comprises azodiisobutyronitrile, diphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide and one or a mixture of more of trimethylbenzoyl-diphenyl phosphine oxides.
The invention also provides a preparation method of the functional glue, which comprises the following steps: and stirring the mixture of the polymer resin, the photosensitive material, the organic solvent and the functional material for 1-20 hours to obtain the functional glue, wherein the stirring temperature is 25-50 ℃.
The invention also provides a quantum dot functional glue solution, which comprises the quantum dots and the functional glue solution, wherein the quantum dots are more than 0 part and less than or equal to 20 parts in parts by weight.
Preferably, the quantum dots comprise CdSe, cdS, cdZnSe, cdZnS, cdZnSeS, znSeS, znSe, cuInS, cuInSe, inP, inZnP and a mixture of one or more of perovskite quantum dots.
Preferably, the quantum dots are of the homogeneous hybrid type, gradient hybrid type or core-shell type.
Preferably, the quantum dot contains a ligand, wherein the ligand comprises one or a mixture of a C6-C18 saturated amine, an unsaturated amine, a saturated acid and an unsaturated acid.
Preferably, the ligand contained in the quantum dot is one or a mixture of more than one of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, octadecenoic acid, hexadecanoic acid, heptadecanoic acid, octadecenoic acid, tributylamine, tri-n-octylamine and oleylamine.
The invention also provides a preparation method of the quantum dot functional glue solution, which comprises the following steps: and mixing and stirring the quantum dots and the functional glue for 1-20 hours to obtain the quantum dot functional glue solution, wherein the stirring temperature is 25-50 ℃.
The invention also provides a display device, which comprises a display substrate and a quantum dot functional adhesive layer arranged on the display substrate, wherein the quantum dot functional adhesive layer is formed by spin coating the quantum dot functional adhesive layer.
Compared with the prior art, the invention introduces functional materials such as nano aluminum, nano zirconium, nano silver, nano titanium, nano silicon, nano calcium, nano barium and other nano materials to combine with polymer resin, photosensitive materials and organic solvents to form functional glue, and then combines the functional glue with quantum dots to form quantum dot functional glue solution. Then when the obtained quantum dot functional glue solution is spin-coated, because the quantum dot functional glue solution (photoresist) contains polymer resin and photosensitive material, the introduced functional material can be preferentially combined with free oxygen in the glue solution to form corresponding nano oxide or corresponding nano salt (such as BaSO 4 ，CaCO 3 Etc.) that in turn can serve as examples of light diffusion to enhance light scattering and transmission. In addition, the nano particles with the particle size of 3-500 nm are selected, and the nano particles with smaller particle size have higher surface energy and are easier to combine and react with oxygen and water vapor, so that oxygen and water vapor in the quantum dot functional glue solution are consumed, and the damage to the quantum dots is avoided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic state diagram of a quantum dot functional glue solution prepared in embodiment 1 of the present invention;
FIG. 2 is a schematic diagram of the quantum dot functional glue solution prepared in example 1 after spin coating into an optical film;
fig. 3A and 3B are schematic diagrams after spin-coating an optical film using the quantum dot dope prepared in comparative examples 1 and 2, respectively.
Detailed Description
For a further understanding of the objects, construction, features, and functions of the invention, reference should be made to the following detailed description of the preferred embodiments.
The invention provides functional glue which comprises, by weight, 0.1-30 parts of a functional material, 25-49 parts of a polymer resin, 30-70 parts of an organic solvent and 1-5 parts of a photosensitive material, wherein the functional material is a material with oxidation performance. Wherein, preferably, the components of the functional glue are respectively 5 to 25 parts of functional materials, 30 to 45 parts of polymer resin, 45 to 70 parts of organic solvents and 1 to 5 parts of photosensitive materials according to parts by weight.
In addition, preferably, the functional material is selected from one or a mixture of several of nano aluminum, nano silver, nano zirconium, nano titanium, nano silicon, nano calcium and nano barium. In the functional glue, the functional material contains polymer resin and photosensitive material, and the introduced functional material can be combined with free oxygen in the glue solution to form corresponding nano oxide or corresponding nano salt (such as BaSO 4 ，CaCO 3 Etc.) that in turn can serve as examples of light diffusion to enhance light scattering and transmission. Specific reaction formulae are, for example, as follows: al (Al) 3+ +O -2 →Al 2 O 3 ，Zr 2+ +O -2 →ZrO，Ag 2+ +O -2 →AgO，Ti 2+ +O -2 →TiO，Si 2+ +O -2 →SiO，Ca 2+ +CO 3 -2 →CaCO 3 ，Ba 2+ +SO 4 -2 →BaSO 3 . Preferably, the functional material is a small-particle-size material, and the particle size of the functional material is 3 nm-500 nm; more preferably, the particle size of the functional material is 3 nm-200 nm, because the nano particles with smaller particle size have higher surface energy and are easier to combine and react with oxygen and water vapor, so that oxygen and water vapor in the quantum dot functional glue solution are consumed, and damage to the quantum dots is avoided.
Further, the polymer resin comprises one or more of polymethyl methacrylate, polyethyl methacrylate, polyester acrylate, epoxy acrylate, polyurethane acrylate, acrylic resin and methyl methacrylate.
Preferably, the organic solvent comprises one or a mixture of a plurality of monofunctional reactive diluents, difunctional reactive diluents, polyfunctional reactive diluents, vinyl ether reactive diluents and methacrylate reactive diluents. Specifically, for example, the monofunctional reactive diluents include one or a mixture of several of propyl methacrylate, isobornyl acrylate and octadecyl acrylate; the difunctional reactive diluent comprises one or more of dipropylene glycol diacrylate, propoxylated glycerol triacrylate, tripropylene glycol diacrylate, ethylene glycol diacrylate and propylene glycol diacrylate; the multifunctional reactive diluent comprises one or more of trimethylolpropane triacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate and propylene glycol methyl ether acetate.
In addition, the photosensitive material comprises one or more of a cracking type free radical photoinitiator, a hydrogen abstraction type free radical photoinitiator, a cationic photoinitiator, a macromolecular photoinitiator, a polymerizable photoinitiator, a UV-LED photoinitiator and a visible light initiator. Specifically, for example, the polymerizable photoinitiator includes di-t-butyl peroxide; the cationic photoinitiator comprises one or two of an arylferrocenium salt and an aryldiazonium salt; the macromolecular photoinitiator comprises macromolecular benzophenone; the cracking type free radical photoinitiator comprises azodiisobutyronitrile, diphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide and one or a mixture of more of trimethylbenzoyl-diphenyl phosphine oxides.
In addition, the invention also provides a preparation method of the functional glue, which comprises the following steps: and stirring the mixture of the polymer resin, the photosensitive material, the organic solvent and the functional material for 1-20 hours to obtain the functional glue, wherein the stirring temperature is 25-50 ℃.
The invention also provides a quantum dot functional glue solution, which comprises the quantum dots and the functional glue solution, wherein the quantum dots are more than 0 part and less than or equal to 20 parts in parts by weight.
Preferably, the quantum dots include CdSe (cadmium selenide), cdS (cadmium sulfide), cdZnSe, cdZnS, cdZnSeS, znSeS, znSe (zinc selenide), cuInS, cuInSe, inP (indium phosphide), inZnP, and perovskite (e.g., PVK, csPbBr) x ) One or a mixture of several quantum dots. The quantum dots can be of a uniform mixed type, a gradient mixed type or a core-shell type, namely the quantum dots can be uniformly mixed quantum dots, can be mixed quantum dots with gradient concentration, and can also be quantum dots with a core-shell structure. For example, the quantum dots are red CdSe/ZnS type quantum dots or green CdSe/ZnS type quantum dots. The red quantum dots can emit red light under the excitation of blue light, and the green quantum dots can emit green light under the excitation of blue light. The quantum dot photo-curing glue can be composed of quantum dots which emit different colors, each quantum dot selects corresponding quantum dots according to the different colors which can be emitted, for example, when red light is required to be emitted, red CdSe/ZnS quantum dots can be selected; when green light is required to be emitted, green CdSe/ZnS quantum dots can be selected. The type of quantum dot selected in this embodiment is not limited as long as it can emit light of different colors as needed.
In addition, the quantum dot contains a ligand, and the ligand comprises one or a mixture of more of saturated amine, unsaturated amine, saturated acid and unsaturated acid of C6-C18. And preferably, the ligand contained in the quantum dot is, for example, one or a mixture of several of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, octadecenoic acid, hexadecanoic acid, heptadecanoic acid, octadecenoic acid, tributylamine, tri-n-octylamine and oleylamine. One of the effects of ligands on the surface of the quantum dot is to increase the hydrophobicity of the surface of the quantum dot and to reduce the mutual aggregation of the quantum dots in a solvent.
In addition, the invention also provides a preparation method of the quantum dot functional glue solution, which comprises the following steps: and mixing and stirring the quantum dots and the functional glue for 1-20 hours to obtain the quantum dot functional glue solution, wherein the stirring temperature is 25-50 ℃.
In addition, the invention also provides a display device, which comprises a display substrate and a quantum dot functional adhesive layer arranged on the display substrate, wherein the quantum dot functional adhesive layer is formed by spin coating the quantum dot functional adhesive layer. The light color conversion is realized by arranging the quantum dot functional adhesive layer on the display substrate. The display device can be applied to any products or components with display functions, such as a display, a notebook computer, a tablet computer, electronic paper, a mobile phone, a television, a VR display, a digital photo frame, a navigator, an AR display, a vehicle-mounted display, and the like.
The invention is further illustrated below in connection with specific examples.
Example 1
1g of green Cd quantum dot is dissolved in 5ml of PGMEA solvent, then mixed with 0.1 part of nano aluminum, 10 parts of polyester acrylate, 15 parts of acrylic resin, 70 parts of PGMEA and 5 parts of azodiisobutyronitrile by mechanical stirring at 25 ℃ to obtain quantum dot functional glue solution, spin-coated to form a film, ultraviolet (UV) cured for 5 minutes and thermally cured at 110 ℃ for 5 minutes.
Example 2
1g of red Cd quantum dot is dissolved in 5ml of PGMEA solvent, and then mixed with 10 parts of nano zirconium, 22 parts of polyester acrylic ester, 16 parts of acrylic resin, 50 parts of PGMEA, 10 parts of isobornyl acrylate (IBOA) and 1.9 parts of azodiisobutyronitrile by mechanical stirring at 25 ℃ to obtain quantum dot functional glue solution, spin-coating the obtained quantum dot functional glue solution into a film, carrying out UV curing for 5 minutes and carrying out heat curing at 110 ℃ for 5 minutes.
Example 3
1.5g of green In quantum dot is dissolved In 5ml of PGMEA solvent, and then mixed with 30 parts of nano titanium, 20 parts of polyurethane acrylic ester, 9 parts of acrylic resin, 30 parts of PGMEA, 10 parts of IBOA and 1 part of azodiisobutyronitrile by mechanical stirring at 25 ℃ to obtain quantum dot functional glue solution, spin-coating the obtained quantum dot functional glue solution into a film, carrying out UV curing for 5 minutes and carrying out heat curing at 110 ℃ for 5 minutes.
Example 4
3g of red In quantum dot is dissolved In 8ml of PGMEA solvent, and then mixed with 20 parts of nano silver, 40 parts of polyester acrylic ester, 9 parts of acrylic resin, 20 parts of PGMEA, 10 parts of IBOA and 1 part of azodiisobutyronitrile by mechanical stirring at 25 ℃ to obtain quantum dot functional glue solution, spin-coating the obtained quantum dot functional glue solution into a film, carrying out UV curing for 5 minutes and carrying out heat curing at 110 ℃ for 5 minutes.
Comparative example 1
Preparation using non-functional material glue
1g of green Cd-based quantum dot is dissolved in 5ml of PGMEA solvent, and then mixed with 20 parts of polyester acrylate, 15 parts of acrylic resin, 40 parts of PGMEA, 20 parts of glycol diacrylate and 5 parts of di-tert-butyl peroxide by mechanical stirring at 25 ℃ to obtain quantum dot glue solution, and the obtained quantum dot glue solution is subjected to spin coating to form a film, UV curing for 5 minutes and heat curing at 110 ℃ for 5 minutes.
Comparative example 2
1g of red Cd quantum dot is dissolved in 5ml of PGMEA solvent, and then mixed with 22 parts of polyurethane acrylate, 16 parts of polyester acrylate, 50 parts of PGMEA, 6 parts of tripropylene glycol diacrylate and 6 parts of azodiisobutyronitrile by mechanical stirring at 25 ℃ to obtain quantum dot glue solution, the obtained quantum dot glue solution is spin-coated into a film, and is subjected to UV curing for 5 minutes and heat curing at 110 ℃ for 5 minutes.
The quantum dot functional glue solution of the present invention obtained in examples 1-4 and the quantum dot glue solution obtained in comparative examples 1-2 were spin-coated into optical films, respectively, and tested, and the test results are shown in the following table 1 and fig. 1-3B, and fig. 1 is a schematic state diagram of the quantum dot functional glue solution prepared in example 1 of the present invention; FIG. 2 is a schematic diagram of the quantum dot functional glue solution prepared in example 1 after spin coating into an optical film; fig. 3A and 3B are schematic diagrams after spin-coating an optical film using the quantum dot dope prepared in comparative examples 1 and 2, respectively.
Table 1 test results of spin-coating of quantum dot functional glue solutions obtained in examples and comparative examples into optical films
Figure BDA0003388388720000101
As can be seen from table 1, the effective conversion efficiency of photoluminescence quantum yield (PLQY) of the quantum dot functional glue in this example is significantly improved compared to that of the luminescent quantum yield (PLQY) in comparative examples 1-2, and the retention rate of quantum dot PLQY is very high. In addition, the optical film formed by spin coating the quantum dot functional glue solution in the embodiment of the invention has good film surface uniformity, no bubbles or granular feel (as shown in figure 2), and very high blue light absorptivity. In contrast, the optical film prepared by the conventional method has a non-uniform film surface and bubbles (as shown in fig. 3A and 3B).
In summary, the functional material such as nano aluminum, nano zirconium, nano silver, nano titanium, nano silicon, nano calcium, nano barium and the like is introduced to be combined with the polymer resin, the photosensitive material and the organic solvent to form the functional glue, and then the functional glue is combined with the quantum dots to form the quantum dot functional glue solution. Then when the obtained quantum dot functional glue solution is spin-coated, because the quantum dot functional glue solution (photoresist) contains polymer resin and photosensitive material, the introduced functional material can be preferentially combined with free oxygen in the glue solution to form corresponding nano oxide or corresponding nano salt (such as BaSO 4 ，CaCO 3 Etc.) that in turn can serve as examples of light diffusion to enhance light scattering and transmission. In addition, the nano particles with the particle size of 3-500 nm are selected, and the nano particles with smaller particle size have higher surface energy and are easier to combine and react with oxygen and water vapor, so that oxygen and water vapor in the quantum dot functional glue solution are consumed, and the damage to the quantum dots is avoided.
The invention has been described with respect to the above-described embodiments, however, the above-described embodiments are merely examples of practicing the invention. In addition, the technical features described above in the different embodiments of the present invention may be combined with each other as long as they do not collide with each other. It should be noted that the disclosed embodiments do not limit the scope of the invention. On the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (16)

1. The functional glue is characterized by comprising 0.1-30 parts of functional materials, 25-49 parts of polymer resins, 30-70 parts of organic solvents and 1-5 parts of photosensitive materials in parts by weight, wherein the functional materials comprise one or more of nano aluminum, nano silver, nano zirconium, nano titanium, nano silicon, nano calcium and nano barium.
2. The functional glue as claimed in claim 1, wherein the components of the functional glue are respectively 5-25 parts by weight of functional material, 30-45 parts by weight of polymer resin, 45-70 parts by weight of organic solvent and 1-5 parts by weight of photosensitive material.
3. The functional glue according to claim 1, wherein the particle size of the functional material is 3nm to 500nm.
4. The functional glue of claim 1, wherein the polymer resin comprises one or a mixture of polymethyl methacrylate, polyethyl methacrylate, polyester acrylate, epoxy acrylate and polyurethane acrylate.
5. The functional glue of claim 1, wherein the organic solvent comprises one or a mixture of more of a monofunctional reactive diluent, a difunctional reactive diluent, and a multifunctional reactive diluent.
6. The functional glue of claim 5, wherein the monofunctional reactive diluent comprises one or more of propyl methacrylate, isobornyl acrylate, and octadecyl acrylate; the difunctional reactive diluent comprises one or a mixture of more of ethylene glycol diacrylate and propylene glycol diacrylate; the multifunctional reactive diluent comprises one or a mixture of a plurality of trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol pentaacrylate.
7. The functional glue of claim 1, wherein the photosensitive material comprises one or more of a split-type radical photoinitiator, a hydrogen abstraction type radical photoinitiator, a cationic photoinitiator, a macromolecular photoinitiator, a polymerizable photoinitiator, a UV-LED photoinitiator, and a visible light initiator.
8. The functional glue of claim 7, wherein the cationic photoinitiator comprises one or both of an arylferrocenium salt and an aryldiazonium salt; the macromolecular photoinitiator comprises macromolecular benzophenone; the cracking type free radical photoinitiator comprises azodiisobutyronitrile, diphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide and one or a mixture of more of trimethylbenzoyl-diphenyl phosphine oxides.
9. A method of preparing a functional glue according to any one of claims 1 to 8, comprising: and stirring the mixture of the polymer resin, the photosensitive material, the organic solvent and the functional material for 1-20 hours to obtain the functional glue, wherein the stirring temperature is 25-50 ℃.
10. A quantum dot functional glue solution, which is characterized by comprising quantum dots and the functional glue solution according to any one of claims 1-8, wherein the quantum dots are more than 0 parts and less than or equal to 20 parts by weight.
11. The quantum dot functional glue of claim 10, wherein the quantum dot comprises one or a mixture of a plurality of CdSe, cdS, cdZnSe, cdZnS, cdZnSeS, znSeS, znSe, cuInS, cuInSe, inP, inZnP and perovskite quantum dots.
12. The quantum dot functional glue of claim 11, wherein the quantum dot is of a homogeneous blend type, a gradient blend type, or a core-shell type.
13. The quantum dot functional glue of claim 10, wherein the quantum dot comprises a ligand comprising one or a mixture of C6-C18 saturated amines, unsaturated amines, saturated acids, and unsaturated acids.
14. The quantum dot functional glue solution of claim 13, wherein the ligand contained in the quantum dot is one or a mixture of several of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecenoic acid, tributylamine, tri-n-octylamine and oleylamine.
15. A method for preparing the quantum dot functional glue solution according to claim 10, wherein the preparation method comprises the following steps: and mixing and stirring the quantum dots and the functional glue for 1-20 hours to obtain the quantum dot functional glue solution, wherein the stirring temperature is 25-50 ℃.
16. A display device, characterized in that the display device comprises a display substrate and a quantum dot functional glue layer arranged on the display substrate, wherein the quantum dot functional glue layer is formed by spin coating the quantum dot functional glue solution according to claim 10.
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