CN111038034A - Edge-closed quantum dot reinforced membrane and preparation method thereof - Google Patents
Edge-closed quantum dot reinforced membrane and preparation method thereof Download PDFInfo
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- CN111038034A CN111038034A CN201811193137.8A CN201811193137A CN111038034A CN 111038034 A CN111038034 A CN 111038034A CN 201811193137 A CN201811193137 A CN 201811193137A CN 111038034 A CN111038034 A CN 111038034A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
Abstract
The invention discloses an edge-closed quantum dot reinforced film which has a multilayer structure and comprises two outer base films, two inner barrier layers and a middle quantum dot layer, wherein the two inner barrier layers are positioned on the outer sides of the middle quantum dot layer, the two outer base films are positioned on the outer sides of the two inner barrier layers, the thickness of the outer base film is 50-125 mu m, the thickness of the inner barrier layer is 0.001-0.5 mu m, and the thickness of the middle quantum dot layer is 50-150 mu m; the quantum dot layer is composed of matrix resin, quantum dots, a quantum dot stabilizer, scattering particles, an initiator and a diluent. The invention also discloses a preparation method of the edge-closed quantum dot reinforced film. The method is simple to operate, time-consuming and labor-consuming coating of a specific area is not needed, and only the whole quantum dot film is immersed. In addition, the method can coat multiple layers of ultrathin films with the minimum of only 20nm, and has little influence on the optical performance of products.
Description
Technical Field
The invention relates to an edge-closed quantum dot reinforced film.
The invention also relates to a preparation method of the edge-closed quantum dot reinforced film.
The invention also relates to a preparation method of the quantum dot film slurry, in particular to a preparation method of the quantum dot film slurry suitable for being prepared by a slit coating method. .
Background
Quantum Dots (QDs) are semiconductor nanoparticles with a size of 1-10nm, and can confine conductive particles, holes, and excitons in three directions due to their small physical structure, thereby having a Quantum effect. The quantum dots can be applied to various fields such as luminescent devices, solar cells, biological fluorescent labels and the like due to the structure of the quantum dots, and have wide application prospects.
At present, the most extensive and profound application field of quantum dots is in the optical field. The quantum dot film prepared by mixing and curing the quantum dot and the thermosetting or photo-curing glue to form a film is applied to a Liquid crystal display (Liquid crystal display), the NTSC color gamut can be improved to about 110 percent, the NTSC color gamut of the current Liquid crystal display can only be about 72 percent, and the NTSC color gamut is only 90 percent even if the Liquid crystal display is an organic light-emitting diode OLED. Therefore, the quantum dot television has better color expression and fidelity.
According to the current quantum dot film production mode, quantum dots and thermosetting or photocuring glue are mixed and then combined with two base films with barrier layers through slit coating, so that the quantum dot film coil with a 5-layer structure is formed. Further, it is desirable to cut different sized films from a large roll and then apply them to a liquid crystal display. In the process of coil forming and cutting, the marginal part is exposed in air and steam, and after long-time exposure, air and moisture can permeate quantum dot membrane inlayer, and take place the chemical reaction with the quantum dot for quantum dot fluorescence yield reduces, causes the quantum dot to lose original color, causes the quantum dot membrane edge to whiten, loses its orange yellow color originally.
Some patents have started to reduce the edge effect of the quantum dot film by closing the edge (chinese patent CN 104501043 a, chinese patent CN 106189826 a), but the above-mentioned edge-closed quantum dot film has some disadvantages: (1) the production efficiency can be greatly reduced by coating the adhesive layer on the edge of the quantum dot film; (2) areas such as membrane positioning holes where the adhesive layer is difficult to coat cannot be improved; (3) the adoption of the mode of curing the liquid microcapsules at the edge means that the liquid microcapsules are arranged in the whole quantum dot film, and the curing and forming mode is difficult to ensure that the liquid microcapsules are not cured when the glue is cured; (4) the liquid microcapsule will affect the optical performance and mechanical property of the quantum dot film, and it is difficult to ensure that the quantum dot film does not deform under the action of external force.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an edge-closed quantum dot reinforced film.
The invention also aims to solve the technical problem of providing a preparation method of the edge-closed quantum dot reinforced film.
The technical scheme adopted by the invention is as follows:
an edge-closed quantum dot reinforced film has a multilayer structure and comprises two outer base films, two inner barrier layers and a middle quantum dot layer, wherein the two inner barrier layers are positioned on the outer sides of the middle quantum dot layer, the two outer base films are positioned on the outer sides of the two inner barrier layers, the thickness of the outer base film is 50-125 mu m, the thickness of the inner barrier layer is 0.001-0.5 mu m, and the thickness of the middle quantum dot layer is 50-150 mu m; the quantum dot layer is composed of matrix resin, quantum dots, a quantum dot stabilizer, scattering particles, an initiator and a diluent.
Furthermore, the base film is made of one or more of Polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), Polycarbonate (PC), polyethylene glycol Phthalate (PET) and polymethyl methacrylate (PMMA).
Further, the matrix resin is one or more of silicone resin, epoxy resin, polyacrylamide, polyurethane, isocyanate, light-cured resin and heat-cured resin.
Further, the quantum dots are one or more of MgS, CdTe, CdSe, CdS, CdZnS, ZnSe, ZnTe, ZnS, ZnO, GaAs, GaN, GaP, InP, InAs, InN, InSb, AlP and AlSb.
Furthermore, the structure of the quantum dot is a core-shell structure, the core-shell structure is a quantum dot central core structure and an outer shell structure, and the materials used by the core-shell structure are semiconductors.
Further, the quantum dot stabilizer is one or more of toluene, n-hexane, chloroform and isobornyl acrylate.
Further, the scattering particles are at least one of inorganic particles and organic particles.
Further, the inorganic particles are one or more of nano silicon dioxide, nano titanium dioxide, nano calcium dioxide and nano zirconium dioxide; the organic particles are one or more of organic silicon nanoparticles and acrylic acid nanoparticles.
Further, the initiator is one or more of a photoinitiator and a thermal initiator.
Further, the diluent is one or more of toluene, acetone, butanone, acetonitrile, ethanol, acetic acid, ethyl acetate, butyl acetate and n-butyl ether.
A preparation method of an edge-closed quantum dot reinforced film comprises the following steps: the quantum dots are dissolved in the quantum dot stabilizer to obtain a quantum dot solution, the quantum dot solution is mixed with matrix resin, scattering particles, an initiator and a diluent, and then is attached to the upper and lower base films with the barrier layers through slit coating, and under the action of illumination and heat, the middle quantum dot layer is cured, so that a multilayer structure is formed and is wound into the quantum dot film coiled material.
Further, after cutting and punching the positioning holes, the quantum dot film coiled material is subjected to wet coating treatment, namely, the quantum dot film subjected to cutting and punching treatment is soaked in the coating liquid, and then the soaked quantum dot film is taken out of the coating liquid at a certain speed; after the quantum dot film taken out from the coating liquid is kept stand for a certain time, the solvent in the coating liquid attached to the surface layer of the quantum dot film is volatilized, a layer of transparent film is left on the surface layer, and the layer of transparent film can completely cover the whole quantum dot film which is cut; the thickness of the transparent film can be adjusted by controlling the speed of taking out the quantum dot film from the coating liquid, and the thickness range is 20nm-50 μm.
Further, the quantum dot film may be subjected to a single or multiple wet coating processes, thereby forming a multi-layered transparent thin film.
Further, the main component of the coating liquid used in the wet coating process is one or more of SiOx, SiOxNy, Si, azotriazolone, AlOx, silane, silicon nitride, silicon oxynitride, polyvinylidene chloride, ethylene, vinyl alcohol copolymer, polyamide, polyester, and polyimide.
Furthermore, the quantum dot film can be coated with the inorganic thin film layer and the organic thin film layer discontinuously, so that a structure that the organic thin film layer and the inorganic thin film layer are distributed discontinuously is formed.
The invention achieves the following beneficial effects: the method is simple to operate, time-consuming and labor-consuming coating of a specific area is not needed, and only the whole quantum dot film is immersed. In addition, the method can coat multiple layers of ultrathin films with the minimum of only 20nm, and has little influence on the optical performance of products.
Drawings
Fig. 1 is a view showing the structure of the quantum dot of the present invention.
Fig. 2 is a schematic cross-sectional view of a quantum dot film of the present invention.
FIG. 3 is a schematic view of a wet coating process of the present invention.
Fig. 4 is a schematic cross-sectional view of a closed quantum dot film after wet coating according to the present invention.
Fig. 5 is a schematic cross-sectional view of a multilayer closed quantum dot film of the present invention.
Detailed Description
For the purpose of enhancing an understanding of the present invention, the following detailed description of the present invention is provided in conjunction with the accompanying drawings, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
Referring to fig. 1, the structure of the quantum dot of the present invention includes a quantum dot central core structure 101 and an outer shell structure 102, both the quantum dot central core structure 101 and the outer shell structure 102 are made of semiconductor materials, and the components of the quantum dot central core structure 101 and the outer shell structure 102 are one or more of MgS, CdTe, CdSe, CdS, CdZnS, ZnSe, ZnTe, ZnS, ZnO, GaAs, GaN, GaP, InP, InAs, InN, InSb, AlP, and AlSb;
as shown in fig. 2, an edge-sealed quantum dot reinforced film of the present invention has a multilayer structure, and includes two outer base films 201, two inner barrier layers 202, and a middle quantum dot layer 203, wherein the two inner barrier layers 202 are located outside the middle quantum dot layer 203, and the two outer base films 201 are located outside the two inner barrier layers 202. The arrangement of the structure can protect the intermediate quantum dot layer 203 from contacting with water vapor and air in the air to the maximum extent. Wherein, the thickness of the outer base film 201 is 50-125 μm, the thickness of the barrier layer 202 is 0.001-0.5 μm, and the thickness of the intermediate quantum dot layer 203 is 50-150 μm. The quantum dot layer 203 is composed of green quantum dots 204, red quantum dots 205, scattering particles 206, and a matrix resin 207.
The base film 201 is made of one or more of Polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), Polycarbonate (PC), polyethylene glycol Phthalate (PET) and polymethyl methacrylate (PMMA).
The matrix resin 207 is one or more of silicone resin, epoxy resin, polyacrylamide, polyurethane, isocyanate, light-curable resin, and heat-curable resin.
The quantum dot stabilizer is one or more of toluene, n-hexane, chloroform and isobornyl acrylate.
The scattering particles 206 are at least one of inorganic particles and organic particles; the inorganic particles are one or more of nano silicon dioxide, nano titanium dioxide, nano calcium dioxide, nano zirconium dioxide and organic particles; the organic particles are one or more of organic silicon nanoparticles and acrylic nanoparticles.
The initiator is one or more of a photoinitiator and a thermal initiator.
The diluent is one or more of toluene, acetone, butanone, acetonitrile, ethanol, acetic acid, ethyl acetate, butyl acetate and n-butyl ether.
The quantum dots are dissolved in the quantum dot stabilizer to obtain a quantum dot solution, the quantum dot solution is mixed with matrix resin, scattering particles, an initiator and a diluent, and then is attached to the upper and lower base films with the barrier layers through slit coating, and under the action of illumination and heat, the middle quantum dot layer 203 is cured, so that a multilayer structure is formed and is wound into the quantum dot film coiled material.
After cutting and punching the positioning holes on the quantum dot film coil, performing wet coating, wherein the wet coating is a technology for uniformly coating or infiltrating resin dissolved in an organic solvent or liquid on a base film, namely infiltrating the quantum dot film 301 subjected to cutting and punching into a coating liquid 302, and then taking the infiltrated quantum dot film 301 out of the coating liquid 302 at a certain speed; standing the taken quantum dot film for a certain time, volatilizing the solvent in the coating liquid attached to the surface layer of the quantum dot film, and leaving a layer of transparent film 303 on the surface layer, wherein the layer of transparent film can completely cover the whole cut quantum dot film; the thickness of the transparent thin film 303 can be adjusted by controlling the speed of taking out the quantum dot film 301 from the coating liquid 302, and the thickness range is 20nm to 50 μm.
The quantum dot film can be subjected to a single or multiple wet coating processes, the quantum dot film is repeatedly soaked in the coating liquid 302, the solvent is volatilized after the quantum dot film is taken out to form a layer of transparent film, and the process is repeated for multiple times, so that a multilayer transparent film is formed, and the oxygen-blocking and water-blocking performances of the quantum dot film can be further improved.
The coating liquid 302 used in the wet coating process is mainly composed of one or more of SiOx, SiOxNy, Si, azotriazolone, AlOx, silane, silicon nitride, silicon oxynitride, polyvinylidene chloride, ethylene, vinyl alcohol copolymer, polyamide, polyester, and polyimide.
Example 1
(1) Preparation of Quantum dot films
Dissolving green CdSe quantum dots with average particle diameter of 3nm and red CdSe quantum dots with average particle diameter of 7nm in toluene at 1 wt%, polyacrylic resin as matrix resin, and SiO as scattering particles2The photoinitiator 1173 and the diluent acetic acid were mixed and attached to the PET base film 201 with the barrier layer 202 by slit coating, followed by UV irradiation at 390 nm. At this time, the intermediate glue layer is cured into the quantum dot layer 203 under the irradiation of UV light, and a multilayer structure having a total thickness of 350 μm is formed, and the quantum dot layer thickness is 100 μm.
(2) Cutting of quantum dot films
And cutting the quantum dot film into required patterns according to required sizes and punching the sheet according to the requirement.
(3) Wet coating encapsulation of quantum dot film
After the quantum dot film coil is cut and punched to form the positioning holes, wet coating is performed, that is, the cut and punched quantum dot film 301 is soaked in the coating liquid 302, and then the soaked quantum dot film 301 is taken out from the coating liquid 302 at a certain speed. Standing the taken quantum dot film for a certain time, volatilizing the solvent in the coating liquid attached to the surface layer of the quantum dot film, and leaving a layer of transparent film 303 on the surface layer, wherein the layer of transparent film can completely cover the whole cut quantum dot film; the thickness of the transparent thin film 303 can be adjusted by controlling the speed of taking out the quantum dot film 301 from the coating liquid 302, and the thickness range is 20nm to 50 μm.
Example 2
Preparing a quantum dot film: dissolving green CdSe quantum dots with average particle diameter of 3nm and red CdSe quantum dots with average particle diameter of 7nm in n-hexane at 1 wt%, polyacrylic resin as matrix resin, and CaO as scattering particle2The thermal initiator and the diluent toluene were mixed and attached to the PET base film 201 with the barrier layer 202 by slit coating, followed by UV irradiation at 390 nm. At this time, the intermediate glue layer is cured into the quantum dot layer 203 under the irradiation of UV light, and a multilayer structure having a total thickness of 350 μm is formed, and the quantum dot layer thickness is 100 μm.
Example 3
Preparing a quantum dot film: dissolving green CdSe quantum dots with average particle diameter of 3nm and 7nm in isobornyl acrylate at 1 wt%, polyacrylic resin, mercapto resin, and TiO as matrix resin2The mixture of the photoinitiator 1173 and the ethyl acetate diluent is adhered to the PET base film 201 with the barrier layer 202 through slit coating, the total thickness of the barrier layer 202 and the PET base film 201 is 50 μm, and then the PET base film is irradiated by UV light with 390nm and is dried in an oven at a high temperature of 80 ℃. At this time, the intermediate glue layer is cured into a quantum dot layer 203 with a thickness of 100 μm under UV light and high temperature, forming a multi-layered structure with a total thickness of 200 μm.
Example 4
Preparing a quantum dot film: dissolving green CdSe quantum dots with average particle diameter of 3nm and red CdSe quantum dots with average particle diameter of 7nm in isobornyl acrylate at 1 wt%, polyacrylic resin, mercapto resin, and scattering particles ZrO2The mixture of the photoinitiator 1173 and the diluent acetic acid is adhered to the PET base film 201 with the barrier layer 202 through slit coating, the total thickness of the barrier layer 202 and the PET base film 201 is 50 μm, and then the PET base film is irradiated by UV light with 390nm and is dried in an oven at a high temperature of 80 ℃. At this time, the intermediate glue layer is cured into the quantum dot layer 203 with a thickness of 50 μm under UV light and high temperature to form a multi-layered structure with a total thickness of 150 μm.
Example 5
Dissolving green CdSe quantum dots with average particle diameter of 3nm and red CdSe quantum dots with average particle diameter of 7nm in chloroform at 1 wt%, polyacrylic resin as matrix resin, and SiO as scattering particles2The photoinitiator 1173 and the diluent acetonitrile are mixed and then attached to the PET base film 201 with the barrier layer 202 by slit coating, followed by UV irradiation at 390 nm. At this time, the intermediate glue layer is cured into the quantum dot layer 203 under the irradiation of UV light, and a multilayer structure having a total thickness of 350 μm is formed, and the quantum dot layer thickness is 100 μm.
The quantum dot film coated in the embodiments 2 to 5 can be cut into various sizes such as 55 inches, 60 inches, 65 inches, 75 inches and the like according to different requirements after being cut as described in the embodiment 1. And slowly immersing the quantum dot film with the size into an ethyl acetate solution in which epoxy resin is dissolved, slowly taking out the quantum dot film, forming a layer of epoxy resin organic film on the surface after the solvent is completely volatilized, then entering the ethyl acetate solution in which SiOx and SiNx are dissolved, and slowly taking out the quantum dot film, and forming a layer of SiOx and SiOxNx inorganic film on the surface of the diaphragm after the solvent is completely volatilized. The process is repeated, so that a plurality of layers of organic and inorganic films can be generated outside the quantum dot film, and the organic and inorganic films can further improve the water and oxygen resisting capacity of the quantum dot.
Claims (15)
1. An edge-sealed quantum dot enhancement film, characterized in that: the quantum dot reinforced film has a multilayer structure and comprises two outer base films, two inner barrier layers and a middle quantum dot layer, wherein the two inner barrier layers are positioned on the outer sides of the middle quantum dot layer, the two outer base films are positioned on the outer sides of the two inner barrier layers, the thickness of the outer base film is 50-125 mu m, the thickness of the inner barrier layer is 0.001-0.5 mu m, and the thickness of the middle quantum dot layer is 50-150 mu m; the quantum dot layer is composed of matrix resin, quantum dots, a quantum dot stabilizer, scattering particles, an initiator and a diluent.
2. The edge-capped quantum dot enhancement film of claim 1, wherein: the base film is made of one or more of Polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), Polycarbonate (PC), polyethylene glycol Phthalate (PET) and polymethyl methacrylate (PMMA).
3. The edge-capped quantum dot enhancement film of claim 1, wherein: the matrix resin is one or more of organic silicon resin, epoxy resin, polyacrylamide, polyurethane, isocyanate, light-cured resin and heat-cured resin.
4. The edge-capped quantum dot enhancement film of claim 1, wherein: the quantum dots are one or more of MgS, CdTe, CdSe, CdS, CdZnS, ZnSe, ZnTe, ZnS, ZnO, GaAs, GaN, GaP, InP, InAs, InN, InSb, AlP and AlSb.
5. The edge-capped quantum dot enhancement film of claim 1, wherein: the structure of the quantum dot is a core-shell structure, the core-shell structure is a quantum dot central core structure and an outer shell structure, and materials used by the core-shell structure are semiconductors.
6. The edge-capped quantum dot enhancement film of claim 1, wherein: the quantum dot stabilizer is one or more of toluene, n-hexane, chloroform and isobornyl acrylate.
7. The edge-capped quantum dot enhancement film of claim 1, wherein: the scattering particles are at least one of inorganic particles and organic particles.
8. The edge-capped quantum dot enhancement film of claim 7, wherein: the inorganic particles are one or more of nano silicon dioxide, nano titanium dioxide, nano calcium dioxide and nano zirconium dioxide; the organic particles are one or more of organic silicon nanoparticles and acrylic acid nanoparticles.
9. The edge-capped quantum dot enhancement film of claim 1, wherein: the initiator is one or more of a photoinitiator and a thermal initiator.
10. The edge-capped quantum dot enhancement film of claim 1, wherein: the diluent is one or more of toluene, acetone, butanone, acetonitrile, ethanol, acetic acid, ethyl acetate, butyl acetate and n-butyl ether.
11. The preparation method of the edge-closed quantum dot reinforced film is characterized by comprising the following steps of: the quantum dots are dissolved in the quantum dot stabilizer to obtain a quantum dot solution, the quantum dot solution is mixed with matrix resin, scattering particles, an initiator and a diluent, and then is attached to the upper and lower base films with the barrier layers through slit coating, and under the action of illumination and heat, the middle quantum dot layer is cured, so that a multilayer structure is formed and is wound into the quantum dot film coiled material.
12. The method for preparing an edge-sealed quantum dot reinforced film according to claim 11, wherein: after cutting and punching the positioning holes on the quantum dot film coiled material, carrying out wet coating treatment, namely soaking the cut and punched quantum dot film in a coating liquid, and then taking out the soaked quantum dot film from the coating liquid at a certain speed; after the quantum dot film taken out from the coating liquid is kept stand for a certain time, the solvent in the coating liquid attached to the surface layer of the quantum dot film is volatilized, a layer of transparent film is left on the surface layer, and the layer of transparent film can completely cover the whole quantum dot film which is cut; the thickness of the transparent film can be adjusted by controlling the speed of taking out the quantum dot film from the coating liquid, and the thickness range is 20nm-50 μm.
13. The method for preparing an edge-sealed quantum dot reinforced film according to claim 12, wherein: the quantum dot film may be subjected to a single or multiple wet coating processes to form a multilayer transparent thin film.
14. The method for preparing an edge-sealed quantum dot reinforced film according to claim 12, wherein: the main component of the coating liquid used in the wet coating process is one or more of SiOx, SiOxNy, Si, azotriazolone, AlOx, silane, silicon nitride, silicon oxynitride, polyvinylidene chloride, ethylene, vinyl alcohol copolymer, polyamide, polyester and polyimide.
15. The method for preparing an edge-sealed quantum dot reinforced film according to claim 12, wherein: the quantum dot film can be coated with the inorganic thin film layer and the organic thin film layer discontinuously, so that a structure that the organic thin film layer and the inorganic thin film layer are distributed discontinuously is formed.
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