CN117143420A - Quantum dot foaming diffusion plate and preparation method thereof - Google Patents
Quantum dot foaming diffusion plate and preparation method thereof Download PDFInfo
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- CN117143420A CN117143420A CN202311431328.4A CN202311431328A CN117143420A CN 117143420 A CN117143420 A CN 117143420A CN 202311431328 A CN202311431328 A CN 202311431328A CN 117143420 A CN117143420 A CN 117143420A
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- quantum dot
- foaming
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- plate body
- diffusion plate
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 45
- 238000005187 foaming Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229920001709 polysilazane Polymers 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
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- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
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- 238000000034 method Methods 0.000 claims abstract description 9
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- 239000000463 material Substances 0.000 claims description 21
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- 239000002270 dispersing agent Substances 0.000 claims description 16
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- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
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- 229910052623 talc Inorganic materials 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
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- 238000003756 stirring Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 6
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- 210000004027 cell Anatomy 0.000 description 16
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- FXRLMCRCYDHQFW-UHFFFAOYSA-N 2,3,3,3-tetrafluoropropene Chemical compound FC(=C)C(F)(F)F FXRLMCRCYDHQFW-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- CDOOAUSHHFGWSA-UPHRSURJSA-N (z)-1,3,3,3-tetrafluoroprop-1-ene Chemical compound F\C=C/C(F)(F)F CDOOAUSHHFGWSA-UPHRSURJSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
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- 150000004706 metal oxides Chemical class 0.000 description 2
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
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- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- OGFYGJDCQZJOFN-UHFFFAOYSA-N [O].[Si].[Si] Chemical group [O].[Si].[Si] OGFYGJDCQZJOFN-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001348 alkyl chlorides Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- COOGPNLGKIHLSK-UHFFFAOYSA-N aluminium sulfide Chemical compound [Al+3].[Al+3].[S-2].[S-2].[S-2] COOGPNLGKIHLSK-UHFFFAOYSA-N 0.000 description 1
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- ORECYURYFJYPKY-UHFFFAOYSA-N n,n'-bis(2,2,6,6-tetramethylpiperidin-4-yl)hexane-1,6-diamine;2,4,6-trichloro-1,3,5-triazine;2,4,4-trimethylpentan-2-amine Chemical compound CC(C)(C)CC(C)(C)N.ClC1=NC(Cl)=NC(Cl)=N1.C1C(C)(C)NC(C)(C)CC1NCCCCCCNC1CC(C)(C)NC(C)(C)C1 ORECYURYFJYPKY-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- NIEHEMAZEULEKB-UHFFFAOYSA-N ortho-ethylanisole Natural products CCC1=CC=CC=C1OC NIEHEMAZEULEKB-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
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- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of 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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
Abstract
The invention relates to the technical field of display screens, in particular to a foaming diffusion plate applied to quantum dots and a preparation method thereof. According to the invention, by combining the foaming technology with the quantum dot diffusion plate technology, in the process of forming and stabilizing the cells, the waste heat of the plate body and the humidity atmosphere of the plate body enable the perhydro polysilazane in the plate body to react with water quickly to form a protective layer made of silicon dioxide, on one hand, the hard silicon dioxide formed by hydrolyzing the silazane prevents the cells from being combined and enlarged, and the maintained microporous structure has a good light homogenizing effect; on the other hand, a silicon dioxide structure with a water-oxygen blocking effect is formed on the surface and in the plate body, and meanwhile, the plate body has the property of resisting warp deformation.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to a quantum dot foaming diffusion plate and a preparation method thereof.
Background
Quantum dot display technology is becoming accepted by more and more brand vendors and consumers as the most cost effective wide color gamut display scheme. With the big explosion of Mini-LED technology, brand manufacturers such as samsung, TCL, chuangwei and Hai have successively introduced the Mini-LED products carrying the quantum dot technology. The quantum dot scheme is far ahead of other emerging technologies in the market share of TV products, and along with the acceleration of technical innovation and industrialization, the cost is continuously reduced, and the quantum dot scheme is expected to become display standard. However, the quantum dots are greatly affected by water, high temperature and humidity due to the vulnerability of the quantum dots, and the quantum dots need to be protected. Water-oxygen barrier films are currently used as barrier layers to prevent the quantum dots from decomposing due to moisture.
To reduce production costs, industry strives to disperse quantum dots in diffusion plates. However, the quantum dots are very easily oxidized, which limits the production and application of quantum dot diffusion plates. The prior art discloses a quantum dot optical function board, which is prepared by using a raw material containing a chemical foaming agent to prepare resin-based granules containing holes, loading quantum dots in the holes, mixing other components such as a high-temperature foaming agent, and extruding and molding. For example, chinese patent application CN202010812282.0, entitled "light diffusion plate and method for manufacturing the same", discloses a foam quantum dot diffusion plate, where the diameter of the cells is 60-400 μm, and it is obvious that the number of times of reflection and refraction of light passing through the cells is less due to larger pore diameter and lower distribution uniformity of the chemical foaming agent, so that the light homogenizing effect is poor, and the strength of the quantum dot optical functional plate is reduced due to larger pore diameter, especially, the problem of deformation and warpage easily occurs in a high-temperature and high-humidity environment, so that the problem of larger brightness attenuation is caused.
The patent publication No. CN216870976U, the patent name is a kind of optical function board and device Chinese patent application publication discloses a foaming quantum dot diffusion plate, wherein the diameter of the foam cells is 0.5-500 μm, the patent application claims to control the diameter of the foam cells according to the density of the light beads of the LED chip, and the high density requires the diameter of the foam cells to be small so as to ensure the diffusion effect. However, it does not disclose a method of controlling the cell diameter.
Disclosure of Invention
In order to solve the defects existing in the existing quantum dot diffusion plate production technology, the invention provides a quantum dot foaming diffusion plate and a preparation method thereof, and the preparation method is realized by the following technical scheme:
the quantum dot foam diffusion plate comprises a plurality of quantum dots and foam cells formed by foaming and used for light homogenizing, wherein the surface of the plate is provided with a hard protection layer formed by hydrolysis of perhydro polysilazane, the inside of the plate is provided with a hard aggregate formed by hydrolysis of perhydro polysilazane, and the diameter of the foam cells is only 5-50 mu m under the limit of the hard aggregate.
The preparation method of the quantum dot foaming diffusion plate is characterized by comprising the following steps of:
step 1, adding quantum dots, a light dispersing agent, a foaming agent, perhydro polysilazane and other auxiliary agents into a resin base material, and stirring to form a uniform mixed material;
step 2, heating the mixed material in an extruder to a preset temperature and extruding the mixed material into a plate body; the water vapor and oxygen in the air permeate into the plate body, and the waste heat of the plate body is combined, the perhydro polysilazane is hydrolyzed, a hard protection layer is formed on the surface of the plate body, and hard aggregate is formed inside the plate body; the hard aggregate partially wraps or completely wraps the core or the shell of the quantum dot, so that the water-oxygen barrier effect of the quantum dot is enhanced; and the hard aggregate prevents unordered expansion of the cells, improves the uniformity of the cells, and ensures that the diameter of the cells is 5-50 mu m.
The preparation method of the quantum dot foaming diffusion plate is further designed in that the components of the mixed material in the step 1 are as follows: 100 parts of resin base material, 0.1-0.5 part of quantum dot, 0.5-10 parts of light dispersing agent, 0.5-5 parts of foaming agent, 1-5 parts of perhydro polysilazane and 0.2-3 parts of other auxiliary agents.
The preparation method of the quantum dot foaming diffusion plate is further designed in that the resin base material is one or more of polystyrene, polymethyl methacrylate, styrene-polymethyl methacrylate copolymer or polycarbonate.
The preparation method of the quantum dot foaming diffusion plate is further designed in that the light diffusing agent is inorganic light diffusing particles or organic light diffusing particles.
The preparation method of the quantum dot foaming diffusion plate is further designed in that the foaming agent is any one inorganic powder of talcum, kaolin, mica, silicon dioxide, calcium carbonate, barium sulfate, titanium oxide, aluminum oxide, clay, bentonite and diatomite.
The preparation method of the quantum dot foaming diffusion plate is further designed in that the relative humidity of the environment is not less than 50%.
The invention has the beneficial effects that:
the high-quality quantum dot foaming diffusion plate is realized through the quantum dot foaming diffusion plate and the preparation method thereof, the linear expansion coefficient of the quantum dot diffusion plate is obviously reduced, the deformation resistance is better, the large-size quantum dot diffusion plate has excellent dimensional stability, the high-performance and low-cost light-emitting diode (LED) quantum dot optical function plate which is required by the market and is convenient to assemble is provided, and the mass production cost of Mini LED display equipment is greatly reduced; meanwhile, the silazane can effectively promote foaming of the foaming particles, well stabilize the cells while generating the cells, effectively prevent the physical foaming agent remained in the cells after extrusion foaming from being dissipated into the atmosphere, and generate better uniformity of the cells. During the reaction, silazane was consumed and the shape was maintained. The invention realizes the excellent water-oxygen barrier property and the excellent high temperature resistance of the quantum dot optical plate,
drawings
Fig. 1 is a schematic diagram of a quantum dot foaming diffusion plate structure.
FIG. 2 is a molecular structure diagram of perhydro polysilazane (PHPS).
FIG. 3 is a schematic illustration of the reaction process of perhydro polysilazane in an air, moisture atmosphere.
FIG. 4 is an electron microscope image of a slice of example 1 of the present invention.
FIG. 5 is an electron microscope image of a slice of example 2 of the present invention.
FIG. 6 is an electron micrograph of a comparative example 1 slice of the present invention.
FIG. 7 is an electron micrograph of a comparative example 2 slice of the present invention.
FIG. 8 is a table of performance data for an embodiment of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples in conjunction with the description:
the quantum dot foaming diffusion plate comprises a plurality of quantum dots 1 and foam holes 2 for light homogenizing, wherein the surface of the plate is provided with a hard protection layer 3 made of silicon dioxide generated by hydrolysis of silazane, the inside of the plate is provided with a hard aggregate 4 made of silicon dioxide generated by hydrolysis of silazane, and the diameter of the foam holes is 5-50 mu m.
The preparation method of the quantum dot foaming diffusion plate is characterized by comprising the following steps of:
and step 1, adding quantum dots, a light dispersing agent, a foaming agent, perhydro polysilazane and other auxiliary agents into a resin substrate, and stirring to form a uniform mixed material.
Step 2, heating the mixed material in an extruder to a preset temperature and extruding the mixed material into a plate body; under the preset humidity environment, water and oxygen permeate into the plate body, and the waste heat of the plate body is combined, the perhydro polysilazane is hydrolyzed, a hard protection layer is formed on the surface of the plate body, and hard aggregate is formed inside the plate body; the hard aggregate partially wraps or completely wraps the core or the shell of the quantum dot, so that the water-oxygen barrier effect of the quantum dot is enhanced; and the hard aggregate prevents unordered expansion of the cells, improves the uniformity of the cells, and ensures that the diameter of the cells is 5-50 mu m.
The components of the mixture in the step 1 are as follows: 100 parts of resin base material, 0.1-0.5 part of quantum dot, 0.5-10 parts of light dispersing agent, 0.5-5 parts of foaming agent, 1-5 parts of perhydro polysilazane, 0.2-3 parts of other auxiliary agents (0.01-0.8 part of light stabilizer, 0.2-1 part of antioxidant and 0.1-5 parts of toughening agent).
The resin base material is one or more of polystyrene, polymethyl methacrylate, styrene-polymethyl methacrylate copolymer or polycarbonate.
The light diffusing agent is inorganic light diffusing particles or organic light diffusing particles. The inorganic light diffusion particles are one or more of silicon dioxide, calcium carbonate, nano barium sulfate, cadmium selenide, indium phosphide, perovskite, titanium dioxide, barium sulfate, magnesium sulfate, aluminum oxide, aluminum sulfide, aluminum hydroxide, zirconium oxide, zinc oxide, calcium carbonate and magnesium silicate. The organic light diffusion particles can be one or more of polymethyl methacrylate, polybutyl methacrylate, polyurethane, polystyrene, polyethylene, polyamide, polyethylene terephthalate, polyacrylic acid, polyacrylonitrile, polyurethane, polyvinyl chloride and organic silicon resin. The foaming agent is any one inorganic powder of talcum, kaolin, mica, silicon dioxide, calcium carbonate, barium sulfate, titanium oxide, aluminum oxide, clay, bentonite and diatomite.
And the quantum dot adopts a binary or multi-element semiconductor compound of the core or the shell of the IV group, the II-VI group, the II-V group, the III-VI group, the I-III-VI group, the II-IV-VI group and the II-IV-V group, or perovskite nano particles, metal nano particles or metal oxide nano particles or a mixture of the perovskite nano particles, the metal nano particles and the metal oxide nano particles, wherein the perovskite nano particles are of the chemical formula of APbX3 (in the APbX3, A=Cs or MA, X=Cl, br or I). The quantum dot takes one or more of organic solvents such as styrene, toluene, cyclohexane, n-hexane, ethanol, methanol, isopropanol, acetone, ethyl acetate, anisole or tetrahydrofuran as a solvent to form a quantum dot solution, wherein the concentration of the quantum dot in the quantum dot solution is 10-30 wt.%. The quantum dot solution is added to ensure that the mass part of the quantum dot is 0.1 to 0.5 part.
Known chemical foaming agents such as talc, kaolin, mica, silica, calcium carbonate, barium sulfate, titanium oxide, alumina, clay, bentonite, diatomaceous earth and other inorganic powder, azodicarbonamide may be used, and organic physical foaming agents and/or inorganic physical foaming agents may be used. Examples of the organic physical blowing agent include saturated hydrocarbons having 3 to 5 carbon atoms, aliphatic alcohols having 1 to 5 carbon atoms, hydrofluoroolefins (HFOs), ethers, and alkyl chlorides. Inorganic physical blowing agents such as water, carbon dioxide, nitrogen, and the like. These foaming agents may be used alone or in combination of 2 or more. Examples of the Hydrofluoroolefins (HFOs) include fluorounsaturated hydrocarbons such as trans-1, 3,3, 3-tetrafluoropropene (transHFO-1234 ze), cis-1, 3,3, 3-tetrafluoropropene (cis HFO-1234 ze), 1, 1, 1, 2-tetrafluoropropene (HFO-1234 yf), 2,3,3, 3-tetrafluoropropene, and chlorofluorounsaturated hydrocarbons such as 1-chloro-3, 3, 3-trifluoropropene. In the method of the present invention, the extruded foam sheet contains at least 1 selected from 1, 3,3, 3-tetrafluoropropene, 2,3,3, 3-tetrafluoropropene, 1-chloro-3, 3, 3-trifluoropropene, and long-term heat insulation is preferably achieved.
The relative humidity of the environment is not less than 50%. On one hand, certain water in the environment is ensured to enter the plate body, and on the other hand, the infiltration amount is adapted to the addition amount of the perhydro polysilazane, so that the water entering the plate body is gradually consumed through hydrolysis reaction after being fast and slow along with the temperature change.
After the reaction is completed, the average diameter of the cells of the micro-point foaming diffusion plate is 5-50 mu m. The thickness of the whole plate body can be controlled to be 0.2-3mm according to the requirement.
At the moment of extruding the plate body, the foaming agent foams, and meanwhile, the waste heat of the plate body and the humidity atmosphere of the plate body enable the perhydro polysilazane in the plate body to react with water quickly to form a protective layer of a silicon-oxygen-silicon structure, so that the protection of quantum dots is realized, the water-oxygen barrier property and the high-temperature resistance are excellent, the Mini-LED quantum dot optical function plate with high performance, low cost and convenient assembly required by the market is provided, and the mass production cost of Mini-LED display equipment is greatly reduced.
The raw materials in examples and comparative examples are all commercially available; unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
The raw materials and sources used in examples 1 to 9 are specifically as follows:
resin: GPPS, supplied by the company Jiangsu seeglong, or PMMA, supplied by the company Mitsubishi, japan;
the quantum dot adopts self-made CdZnSeS or CsPbBr3; the foaming agent adopts EM304 of water accumulation company or commercially available azodicarbonamide; the silazane is organic silazane with the model of IOTA OPSZ 9150K or inorganic silazane with the model of IOTA-PHPS; the dispersing agent adopts organosilicon light dispersing agent KMP-590 provided by the Xinyue company; the antioxidant adopts Irganox antioxidant 1010 hindered phenol antioxidant provided by Pasteur, and the light stabilizer adopts Chimassorb 944 provided by Pasteur; the toughening agent adopts MBS B-522 toughening agent of Japanese brillouin.
Example 1:
100 parts by mass of a GPPS resin; 2 parts by mass of an EM304 foaming agent; 2 parts by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Example 2:
100 parts by mass of a GPPS resin; 2 parts by mass of an EM304 foaming agent; 1 part by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Example 3:
100 parts by mass of a GPPS resin; 2 parts by mass of an EM304 foaming agent; 3 parts by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Example 4:
100 parts by mass of a GPPS resin; 2 parts by mass of an EM304 foaming agent; 5 parts by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Example 5:
100 parts by mass of a GPPS resin; 2 parts by mass of an azodicarbonamide foaming agent; 1 part by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Example 6:
100 parts by mass of PMMA resin; 2 parts by mass of an EM304 foaming agent; 2 parts by mass of perhydro polysilazane; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
After the ingredients in the embodiment are mixed, the mixture is subjected to melt mixing and extrusion molding, and the plate body is subjected to decomposition of perhydro polysilazane to form a protective layer of silicon dioxide in a preset humidity environment, so that the quantum dot diffusion plate with the thickness of 1.5 mm is obtained.
Correspondingly, the material ratios of the comparative examples are as follows:
comparative example 1:
100 parts by mass of a GPPS resin; 2 parts by mass of an EM304 foaming agent; 0.2 parts by mass of CsPbBr3 quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
Comparative example 2:
100 parts by mass of PMMA resin; 2 parts by mass of an EM304 foaming agent; 0.2 parts by mass of CdZnSeS quantum dots; 8 parts by mass of a dispersing agent; 0.4 parts by mass of an antioxidant; 0.2 parts by mass of a light stabilizer; 2.5 parts by mass of a toughening agent.
The performance test is carried out on the quantum dot diffusion plates prepared in the embodiment and the comparative example, and the specific method is as follows:
(1) Foaming diameter:
cutting the quantum dot diffusion plate along the vertical direction of extrusion to obtain a quantum dot diffusion plate section, and measuring the average diameter of cells in the section by using a scanning electron microscope;
(2) Stability:
placing the quantum dot diffusion plate at 60deg.C under 90% RH humidity for 1000 hr, detecting brightness values before and after placement,
calculating to obtain a brightness attenuation rate, wherein the brightness attenuation= (brightness value before aging-brightness value after aging)/brightness value before aging is 100%;
the brightness detection method comprises the following steps: and (3) placing the quantum dot diffusion plate under a blue light backlight module, and testing the brightness of the central point by using a color analyzer, fixing the current by 400A and fixing the voltage by 42V. The detection is shown in FIG. 8.
As can be seen from examples 1 to 6, by adding perhydro polysilazane into the quantum dot foaming plate, a stable protective layer is formed on the surface of the quantum dot by using the silazane, so that the quantum dot has excellent water-oxygen barrier property and excellent high temperature resistance, the linear expansion coefficient of the quantum dot diffusion plate is remarkably reduced, the deformation resistance is better, and the large-size quantum dot diffusion plate has excellent dimensional stability; the influence of light, temperature, humidity, oxygen and the like on the quantum dots is effectively reduced, the stability of the quantum dot foaming plate is enhanced, the brightness attenuation rate is less than 10%, and the requirement of the display backlight module is met. Whereas the perovskite quantum dot obtained in comparative example 1 failed directly; comparative examples 1 and 2 caused attenuation of more than 50% due to no protection of silica.
In the extruded foam sheet obtained by the present invention, the escape of a physical foaming agent, particularly foaming gas, is effectively prevented, and the inflow of air from the atmosphere into cells is prevented, thereby forming a foam sheet having a long-term heat insulation property superior to that of conventional extruded foam sheets.
Claims (7)
1. The quantum dot foam diffusion plate is characterized in that the surface of the plate body is provided with a hard protective layer made of silicon dioxide material generated by hydrolysis of perhydro polysilazane, the inside of the plate body is provided with a hard aggregate made of silicon dioxide material generated by hydrolysis of perhydro polysilazane, and the diameter of the foam hole is only 5-50 mu m under the limit of the hard aggregate.
2. The preparation method of the quantum dot foaming diffusion plate is characterized by comprising the following steps of:
step 1, adding quantum dots, a light dispersing agent, a foaming agent, perhydro polysilazane and other auxiliary agents into a resin base material, and stirring to form a uniform mixed material; wherein the mass ratio of each component is as follows: 100 parts of resin base material, 0.1-0.5 part of quantum dot, 0.5-10 parts of light dispersing agent, 0.5-5 parts of foaming agent, 1-5 parts of perhydro polysilazane and 0-3 parts of other auxiliary agents;
step 2, heating the mixed material in an extruder to a preset temperature and extruding the mixed material into a plate body; under a preset humidity environment, water and oxygen permeate into the plate body, and the waste heat of the plate body is combined, the perhydro polysilazane is hydrolyzed, a hard protective layer made of silicon dioxide is formed on the surface of the plate body, and a hard aggregate of silicon dioxide is formed inside the plate body; the hard aggregate partially wraps or completely wraps the core or the shell of the quantum dot, so that the water-oxygen barrier effect of the quantum dot is enhanced; and the rigid aggregate prevents unordered expansion of foam cells formed by foaming, improves the uniformity of the foam cells, and ensures that the diameter of the foam cells is 5-50 mu m.
3. The method for preparing a quantum dot foaming diffusion plate according to claim 2, wherein the resin base material is one or more of polystyrene, polymethyl methacrylate, styrene-polymethyl methacrylate copolymer or polycarbonate.
4. The method of manufacturing a quantum dot foaming diffusion plate according to claim 2, wherein the light diffusing agent is inorganic light diffusing particles or organic light diffusing particles.
5. The method for preparing a quantum dot foaming diffusion plate according to claim 2, wherein the foaming agent is any one of inorganic powder of talcum, kaolin, mica, silicon dioxide, calcium carbonate, barium sulfate, titanium oxide, aluminum oxide, clay, bentonite and diatomite.
6. The method of manufacturing a quantum dot foaming diffusion plate according to claim 2, wherein the plate body is placed in an environment with a relative humidity of not less than 50% after extrusion.
7. The method for preparing a quantum dot foaming diffusion plate according to claim 2, wherein the other auxiliary agents comprise 0.01-0.8 part of light stabilizer, 0.2-1 part of antioxidant and 0.1-1 part of toughening agent.
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CN109880156A (en) * | 2019-02-24 | 2019-06-14 | 成都市水泷头化工科技有限公司 | A kind of polystyrene foam sheet and preparation method for interior/exterior decoration |
CN114355491A (en) * | 2021-12-03 | 2022-04-15 | 金发科技股份有限公司 | High-stability micro-foaming quantum dot diffusion plate and preparation method and application thereof |
CN114488615A (en) * | 2022-02-11 | 2022-05-13 | 深圳市华星光电半导体显示技术有限公司 | Display panel, manufacturing method thereof and quantum dot film |
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CN109880156A (en) * | 2019-02-24 | 2019-06-14 | 成都市水泷头化工科技有限公司 | A kind of polystyrene foam sheet and preparation method for interior/exterior decoration |
CN114355491A (en) * | 2021-12-03 | 2022-04-15 | 金发科技股份有限公司 | High-stability micro-foaming quantum dot diffusion plate and preparation method and application thereof |
CN114488615A (en) * | 2022-02-11 | 2022-05-13 | 深圳市华星光电半导体显示技术有限公司 | Display panel, manufacturing method thereof and quantum dot film |
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