CN112175604A - Composite powder with multilayer coating structure, preparation method and application - Google Patents
Composite powder with multilayer coating structure, preparation method and application Download PDFInfo
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- CN112175604A CN112175604A CN201910597799.XA CN201910597799A CN112175604A CN 112175604 A CN112175604 A CN 112175604A CN 201910597799 A CN201910597799 A CN 201910597799A CN 112175604 A CN112175604 A CN 112175604A
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- 239000000843 powder Substances 0.000 title claims abstract description 91
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 239000011248 coating agent Substances 0.000 title claims abstract description 60
- 238000000576 coating method Methods 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 239000002096 quantum dot Substances 0.000 claims abstract description 119
- 239000004005 microsphere Substances 0.000 claims abstract description 96
- 229920000620 organic polymer Polymers 0.000 claims abstract description 79
- 239000010410 layer Substances 0.000 claims abstract description 74
- 239000011159 matrix material Substances 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000011247 coating layer Substances 0.000 claims abstract description 29
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 59
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- 239000005033 polyvinylidene chloride Substances 0.000 claims description 44
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims description 41
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- 239000003292 glue Substances 0.000 claims description 33
- 239000000178 monomer Substances 0.000 claims description 33
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- 238000000034 method Methods 0.000 claims description 18
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- 239000000126 substance Substances 0.000 claims description 13
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- 229910052725 zinc Inorganic materials 0.000 claims description 4
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- 238000005253 cladding Methods 0.000 claims description 3
- COBLIZNSZVKDMR-UHFFFAOYSA-N furan-2,5-dione;octadec-1-ene Chemical compound O=C1OC(=O)C=C1.CCCCCCCCCCCCCCCCC=C COBLIZNSZVKDMR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
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- 239000002243 precursor Substances 0.000 claims description 3
- MJQWABQELVFQJL-UHFFFAOYSA-N 3-Mercapto-2-butanol Chemical compound CC(O)C(C)S MJQWABQELVFQJL-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
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- 239000007788 liquid Substances 0.000 description 15
- 238000000926 separation method Methods 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
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- 229910052906 cristobalite Inorganic materials 0.000 description 7
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- 238000001035 drying Methods 0.000 description 7
- 238000002189 fluorescence spectrum Methods 0.000 description 7
- 239000003999 initiator Substances 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
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- 229910052905 tridymite Inorganic materials 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000006862 quantum yield reaction Methods 0.000 description 4
- 238000009777 vacuum freeze-drying Methods 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
Images
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
-
- 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
- H01L33/502—Wavelength conversion materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Abstract
The application discloses a composite powder with a multilayer coating structure, and a preparation method and application thereof. The composite powder comprises a microsphere matrix, a quantum dot material and a coating layer; the quantum dot material is embedded and attached on the microsphere matrix to form a quantum dot/microsphere matrix; the coating layer is coated on the quantum dot/microsphere matrix; wherein the clad layer comprises at least one organic polymer layer. The material maintains high quantum dot light efficiency, has the advantage of good weather resistance, and is an excellent fluorescence conversion material particularly under the environment of high temperature and high humidity.
Description
Technical Field
The application relates to a composite powder with a multilayer coating structure, a preparation method and application thereof, belonging to the technical field of lighting materials.
Background
The quantum dots have optical properties of continuously adjustable luminescence peak positions (from ultraviolet to infrared), narrow half-peak widths (<4eV) and the like, so that the display color gamut of the quantum dots can be effectively improved, the development of the quantum dots in the display field is stimulated by the advantage, at the moment, the biggest problem of hindering the application of the quantum dots is the stability problem of the quantum dots, the contact of the quantum dots with oxygen and moisture is reduced as far as possible, and the initial optical properties of the quantum dots are kept as far as possible.
In the prior art, a microscopic coating strategy of coating the quantum dots by using inorganic oxides as units and a macroscopic coating strategy of embedding the quantum dots into a matrix block are used. The macro coating strategy has the problems of self absorption, spectrum redshift and reduction of luminous efficiency caused by quantum dot agglomeration, limited application field of quantum dot blocks and the like, and the problems of quantum dot stability reduction caused by block cracks and the like. Compared with the prior art, the microcosmic coating strategy takes each quantum dot as a unit, avoids the quantum dot agglomeration, is easy to prepare powder with high luminous efficiency, and has wider application field and higher stability retention degree.
However, the fluorescent quantum dots of the powder coated with the quantum dots in a microscopic manner have low yield and low fluorescence intensity in a high-temperature and high-humidity environment, and a better microscopic packaging structure is still required to improve the chemical stability of the quantum dots.
Disclosure of Invention
According to an aspect of the present application, there is provided a composite powder of a multilayer coating structure, which maintains high efficiency of quantum dot light emission and has an advantage of good stability under high temperature, high humidity conditions, and is an excellent fluorescence conversion type material.
The composite powder body with a multilayer coating structure comprises a microsphere substrate, a quantum dot material and a coating layer;
the quantum dot material is adsorbed in the microsphere matrix to form a quantum dot/microsphere matrix;
the coating layer is coated on the surface of the microsphere matrix;
wherein the clad layer comprises at least one organic polymer layer.
Optionally, the cladding layer is an organic polymer layer.
Optionally, the cladding layer is two organic polymer layers.
Specifically, in the present application, it is preferable that the two organic polymer layers are different organic polymers.
Optionally, the coating layer is an organic polymer layer and an inorganic oxide layer;
wherein, the surface of the substrate of the extending microsphere extends outwards and is sequentially provided with an organic polymer layer and an inorganic oxide layer;
the inorganic oxide layer is selected from any one of silicon dioxide, aluminum oxide and titanium oxide.
Specifically, the organic polymer layer is an inner layer and directly coats the quantum dot/microsphere matrix, and the inorganic oxide layer is an outer layer and coats the organic polymer layer.
The inorganic oxide layer is selected from the group consisting of oxides: silicon dioxide (SiO)2) Aluminum oxide (Al)2O3) Titanium oxide (TiO)2) At least one of (1).
Optionally, the microsphere matrix is selected from at least one of an organic silicon microsphere, a silicon dioxide microsphere, a polymethyl methacrylate microsphere, a polystyrene microsphere and an iron oxide microsphere.
Specifically, the microsphere matrix is 0.5-10 microns in size.
Optionally, the organic polymer layer is selected from at least one of polyvinyl chloride, polymethyl methacrylate, polyvinyl acetate, cellulose acetate, polyamide, polyimide, polycarbonate, polystyrene, polyvinylidene chloride, polyvinylidene fluoride, polyvinyl alcohol, transparent ABS plastic, polyacrylonitrile, polyolefin elastomer, thermoplastic polyurethane, polyvinyl carbazole.
In particular, the organic polymer layer is selected from polymers: at least one of polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), polyvinyl acetate (PVAc), Cellulose Acetate (CA), Polyamide (PA), Polyimide (PI), Polycarbonate (PC), Polystyrene (PS), polyvinylidene chloride (PVDC), polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVA), transparent ABS plastic (ABS), Polyacrylonitrile (PAN), polyolefin elastomer (POE), Thermoplastic Polyurethane (TPU), polyvinyl carbazole (PVK).
Optionally, the quantum dot material is a quantum dot or a quantum dot modified by an organic substance;
the organic matter is at least one selected from 6-mercapto-1-hexanol, 2-mercapto-3-butanol, 3-mercapto-1-propanol, 2, 3-dimercaptopropanol and poly-octadecene-maleic anhydride.
Wherein the molecular weight of poly-octadecene-maleic anhydride is xx-xx.
Optionally, the quantum dots are selected from at least one of a substance I with a chemical formula shown in a formula I, a substance II with a chemical formula shown in a formula II and a substance III with a chemical formula shown in a formula III;
AM formula I
EFQ2Formula II
GHX3Formula III
Wherein A is selected from at least one of Cd, Zn, Pb and In;
m and Q are independently selected from at least one of S, Se, Te and P;
e is selected from at least one of Cu, Ag and Zn;
f is selected from at least one of Al, Ga and In;
g is selected from CH3NH3、CH(NH)NH3At least one of Cs;
h is selected from at least one of Ag, Sb, Bi, Pb, In and Al;
x is selected from at least one of halogen;
the size of the quantum dots is 2-39 nm.
Optionally, the particle size of the composite powder with the multilayer coating structure is 1-20 microns.
Optionally, the solid content of the quantum dot material in the composite powder is 2 wt% to 50 wt%.
According to another aspect of the present application, there is provided a method for preparing the composite powder with a multilayer coating structure, comprising at least the following steps:
a) heating a material containing a quantum dot material and a microsphere matrix to obtain the quantum dot/microsphere matrix;
b) and coating the coating layer on the surface of the microsphere matrix to obtain the composite powder.
Specifically, in the present application, the quantum dot material includes any one of quantum dots, organic-modified quantum dots.
In the present application, the method for preparing the quantum dot is a method commonly used in the art, and the present application is not limited to this.
The preparation method of the quantum dot modified by the organic matter is not strictly limited in the application. A better preparation method is described below, quantum dots and organic matters are dispersed in an organic solvent, heated for 1h at 120 ℃, and washed and dried after solid-liquid separation, so that the quantum dots modified by the organic matters can be obtained.
Optionally, in step a), the mass ratio of the quantum dot material to the microsphere matrix is 1% to 10%.
Optionally, in the step a), heating to 50-70 ℃; until the solvent in the material is completely evaporated.
Optionally, the step b) comprises:
b-1) carrying out solid-liquid separation on a mixture a containing the quantum dot/microsphere matrix and the first coating layer source to obtain a quantum dot/microsphere matrix/coating layer I;
b-2) carrying out solid-liquid separation on a mixture b containing the quantum dot/microsphere matrix/coating layer I and a second coating layer source to obtain a quantum dot/microsphere matrix/coating layer I/coating layer II;
wherein, the first coating layer source is selected from any one of organic polymer glue solution and organic polymer monomer;
the second coating layer source is selected from any one of organic polymer glue solution, organic polymer monomer and inorganic oxide precursor.
Optionally, the organic polymer glue solution is at least one selected from a polyvinyl chloride glue solution, a polymethyl methacrylate glue solution, a polyvinyl acetate glue solution, a cellulose acetate glue solution, a polyamide glue solution, a polyimide glue solution, a polycarbonate glue solution, a polystyrene glue solution, a polyvinylidene chloride glue solution, a polyvinylidene fluoride glue solution, a polyvinyl alcohol glue solution, a transparent ABS plastic glue solution, a polyacrylonitrile glue solution, a polyolefin elastomer glue solution, a thermoplastic polyurethane glue solution and a polyvinyl carbazole glue solution.
Specifically, the solute in the polyvinyl chloride glue solution is polyvinyl chloride, and the solvent is any one of N, N-dimethylformamide, acetone, tetrahydrofuran and ethyl acetate.
Similarly, the solvent in the organic polymer dope may be selected from any one of N, N-dimethylformamide, acetone, tetrahydrofuran and ethyl acetate.
Optionally, the organic polymer monomer is selected from at least one of a polyvinyl chloride monomer, a polymethyl methacrylate monomer, a polyvinyl acetate monomer, a cellulose acetate monomer, a polyamide monomer, a polyimide monomer, a polycarbonate monomer, a polystyrene monomer, a polyvinylidene chloride monomer, a polyvinylidene fluoride monomer, a polyvinyl alcohol monomer, a transparent ABS plastic monomer, a polyacrylonitrile monomer, a polyolefin elastomer monomer, a thermoplastic polyurethane monomer, and a polyvinyl carbazole monomer.
Optionally, the inorganic oxide precursor is selected from any one of ethyl orthosilicate, aluminum isopropoxide, and tetrabutyl titanate.
Optionally, the step b) comprises:
b-1) carrying out solid-liquid separation on a mixture a containing the quantum dot/microsphere matrix and the organic polymer glue solution to obtain a quantum dot/microsphere matrix/organic polymer layer I;
b-2) carrying out solid-liquid separation on a mixture b containing the quantum dot/microsphere matrix/organic polymer layer I and an organic polymer monomer to obtain a quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II;
wherein the organic polymer layer I and the organic polymer layer II are different organic polymers.
Optionally, the mixture b further comprises an initiator and a dispersant.
Specifically, in the step b-2), the quantum dot/microsphere matrix/organic polymer layer I, the organic polymer monomer, the initiator and the dispersant are mixed at the temperature of 55-70 ℃, and after centrifugal solid-liquid separation, the quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II is obtained.
Further, mixing was performed in an inert atmosphere. For example, mixing in a nitrogen atmosphere.
Optionally, the step b) comprises:
b-1) carrying out solid-liquid separation on a mixture a containing the quantum dot/microsphere matrix and the organic polymer monomer to obtain a quantum dot/microsphere matrix/organic polymer layer I;
b-2) carrying out solid-liquid separation on a mixture b containing the quantum dot/microsphere matrix/organic polymer layer I and an organic polymer glue solution to obtain a quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II;
wherein the organic polymer layer I and the organic polymer layer II are different organic polymers.
Optionally, in the mixture a, an initiator and a dispersant are also included.
Specifically, in the step b-1), the quantum dot/microsphere matrix, the organic polymer monomer, the initiator and the dispersing agent are mixed at the temperature of 55-70 ℃, and after centrifugal solid-liquid separation, the quantum dot/microsphere matrix/organic polymer layer I is obtained.
Further, mixing was performed in an inert atmosphere. For example, mixing in a nitrogen atmosphere.
Optionally, the initiator is selected from any one of azoisobutyronitrile, benzoyl peroxide and potassium persulfate.
The dispersant is selected from any one of water, ethanol and methanol.
A preferred method for preparing the composite powder is as follows:
the method comprises the following steps:
dispersing the microsphere matrix and the quantum dot material in an organic solvent to obtain quantum dot @ microsphere composite powder; mixing with polymer glue solution to obtain quantum dot @ microsphere/polymer powder; polymerizing the monomers to obtain the composite powder with the multilayer coating structure.
Specifically speaking:
1. dispersing the quantum dot material and the microsphere matrix in an organic solvent, and heating to 50-70 ℃; keeping the temperature for 22-26 h, enabling the quantum dot material to enter the microsphere matrix, and cleaning and drying the quantum dot material after solid-liquid separation to obtain quantum dot/microsphere matrix powder;
2. adding the quantum dot/microsphere matrix powder obtained in the step 1 into a polymer coating material glue solution, uniformly mixing, carrying out solid-liquid separation, cleaning with a poor solvent, and carrying out vacuum freeze drying to obtain quantum dot/microsphere matrix/organic polymer layer I powder;
3. and (3) mixing the powder of the quantum dot/microsphere matrix/organic polymer layer I obtained in the step (2) with a polymer coating material monomer, an initiator and a dispersing agent, heating and stirring (50-60 ℃, 4-6 hours), carrying out solid-liquid separation, cleaning and drying to obtain the quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II, namely the composite powder with a multilayer coating structure.
Method two
Dispersing the microsphere matrix and the quantum dot material in an organic solvent to obtain quantum dot @ microsphere composite powder; polymerizing the monomers to obtain quantum dot @ microsphere/polymer powder; and mixing with polymer glue solution to obtain the composite powder with the multilayer coating structure.
Specifically speaking:
1. dispersing the quantum dot material and the microsphere matrix in an organic solvent, and heating to 50-70 ℃; keeping the temperature for 22-26 h, enabling the quantum dot material to enter the microsphere matrix, and cleaning and drying the quantum dot material after solid-liquid separation to obtain quantum dot/microsphere matrix powder;
2. mixing the quantum dot/microsphere matrix powder obtained in the step 1 with a polymer coating material monomer, an initiator and a dispersing agent, heating and stirring (50-60 ℃, 4-6 h), carrying out solid-liquid separation, and then cleaning and drying to obtain quantum dot/microsphere matrix/organic polymer layer I powder;
3. and (3) adding the quantum dot/microsphere matrix/organic polymer layer I powder obtained in the step (2) into a polymer coating material glue solution, uniformly mixing, carrying out solid-liquid separation, cleaning by using a poor solvent, and carrying out vacuum freeze drying to obtain quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II powder, namely the composite powder with a multilayer coating structure.
The composite powder body with the multilayer coating structure comprises a microsphere substrate and two transparent polymer coating materials, the specific existence forms of the microsphere substrate and the two transparent polymer coating materials are shown in figure 1, quantum dots are embedded in the microspheres, and the quantum dots @ microspheres are wrapped by at least two transparent polymers, so that the effects of water resistance and oxygen resistance are well achieved. Wherein the solid content of the quantum dots is 2 wt% -50 wt%.
The yield of the fluorescence quantum of the composite powder with the multilayer coating structure is about 70%, and the fluorescence integral area is still kept above 80% after the composite powder is aged for 600 hours under the conditions of high temperature of 60 ℃ and high humidity of 90%.
According to another aspect of the present application, the composite powder of a multilayer coating structure described in any one of the above and the composite powder of a multilayer coating structure prepared by the method described in any one of the above are applied in the fields of illumination and display.
In particular, the composite powder based on the multilayer coating structure is used for illumination and display.
According to another aspect of the present application, there is provided a display device including a light guide plate, a chip, and a composite powder of a multilayer clad structure;
the chip is positioned on the side of the light guide plate;
the composite powder with the multilayer coating structure comprises any one of the composite powder with the multilayer coating structure and the composite powder with the multilayer coating structure prepared by the method.
Optionally, the composite powder of the multilayer coating structure is attached to a surface of the chip facing the light guide plate.
Specifically, the composite powder is attached to the surface of the chip facing the light guide plate to form a surface mount type packaging backlight structure.
Optionally, the composite powder of the multilayer coating structure is attached to a side surface of the light guide plate facing the chip.
Specifically, the composite powder is attached to the side surface of the light guide plate facing the chip to form a side tube type packaging backlight structure.
The beneficial effects that this application can produce include:
1) the composite powder with the multilayer coating structure keeps high quantum dot luminous efficiency, has the advantage of good weather resistance, and is an excellent fluorescence conversion material particularly in a high-temperature and high-humidity environment.
2) The composite powder with the multilayer coating structure overcomes the defects of single coating material and poor stability of a quantum dot composite material in the prior art, and overcomes the defect that a quantum dot block is difficult to integrate.
3) The application provides a leaded light material of powder class, and this composite powder can directly adhere in the side of display device's chip or light guide plate, and the quantum dot's in the composite powder that has significantly reduced quantity has greatly practiced thrift the cost.
4) According to the preparation method of the composite powder, the stability of the quantum dots under the conditions of high temperature and high humidity is improved while the light efficiency of the quantum dots is maintained; the powder is directly applied to surface mount type packaging, and later processing is facilitated.
Drawings
Fig. 1 is a schematic structural diagram of a specific existence form of a substance in a composite powder with a multilayer coating structure according to an embodiment of the present disclosure.
Fig. 2 is a schematic flow chart of a process for preparing a composite powder with a multilayer coating structure according to an embodiment of the present disclosure.
FIG. 3 is a scanning electron microscope image of QDs/PMMA and QDs/PMMA/PVDC samples in example 1 of the present application.
FIG. 4 is a TEM image of the samples QDs/PMMA, QDs/PMMA/PVDC and QDs @ PMMA/PVDC/PS of example 1 of the present application.
FIG. 5 is a fluorescence spectrum of a sample of QDs/PMMA/PVDC/PS prepared in example 1.
FIG. 6 is a fluorescence spectrum of a sample of QDs/PS/PVDC/PMMA prepared in example 2.
FIG. 7 is a graph showing the change of fluorescence intensity of the product of example 1 during aging at 60 ℃ and 90% humidity in each coating stage.
Fig. 8 is a schematic diagram of a chip package backlight structure.
FIG. 9 is a schematic view of a side-tube package backlight structure.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The microsphere matrix was obtained from Plaskolite West, and the polymer was obtained from Bayer, Germany and Sigma.
The particle size of the microsphere matrix is 0.5-10 microns.
The quantum dots adopt reference documents: prepared by the method in Wan Ki Bae, et al chem. Mater.2008,20, 531-539.
The analysis method in the examples of the present application is as follows:
and performing morphology characterization on the composite powder with the multilayer coating structure by using a Hitachi S-4800 scanning electron microscope and a Japanese electron JEM-2100F type transmission electron microscope.
And performing fluorescence spectrum characterization on the composite powder with the multilayer coating structure by using a Shanghai shared optical PG2000-Pro back-illuminated spectrometer and a Hamamatsu optical C9920 absolute quantum yield measuring instrument.
The fluorescence quantum yield test was carried out using a C9920-02 absolute quantum efficiency instrument manufactured by Hamamastu.
Example 1
Preparation of sample QDs/PMMA/PVDC/PS
0.5g micron-sized polymethyl methacrylate (PMMA) microspheres are put into normal hexane, heated in a water bath kettle at the temperature of 60 ℃ for 24 hours until the solvent is completely evaporated, and 10ml of gradient alloy quantum dot Cd is addedxZn1-xSeyS1-y(QDs) solution 5mg/mL, 10h incubation. And (3) slowly evaporating the solvent, washing the quantum dots on the surface of the microsphere after the solution is evaporated to dryness, and drying to obtain the QDs/PMMA microsphere.
Adding the QDs/PMMA microspheres into N, N-Dimethylformamide (DMF) solution of polyvinylidene chloride (PVDC) (with the polymerization degree of 2000), stirring, centrifuging at a high speed, adding N-hexane, stirring at a high speed, and carrying out vacuum freeze drying to obtain loose QDs/PMMA/PVDC powder.
Finally, Polystyrene (PS) is coated outside the QDs/PMMA/PVDC by a suspension polymerization method. Taking 30mg of QDs/PMMA/PVDC powder, 5mL of methanol, 180mg of styrene monomer, 66mg of polyvinylpyrrolidone and 5.4mg of azoisobutyronitrile, heating and stirring at 55 ℃ in a nitrogen atmosphere for 5 hours, and centrifuging to obtain QDs/PMMA/PVDC/PS powder, wherein the QDs/PMMA/PVDC/PS powder is marked as sample No. 1.
Example 2
Preparation of sample QDs/PS/PVDC/PMMA
The preparation process of the sample QDs/PS/PVDC/PMMA is similar to that of the sample QDs/PMMA/PVDC/PS in the embodiment 1, except that PMMA microspheres are changed into PS microspheres, a PS coating layer is changed into radical polymerization reaction to form a PMMA layer, and the rest is the same as that of the embodiment 1. The polymerization method of the PMMA layer is as follows: 2nmol of QDs/PS/PVDC, 1g of Methyl Methacrylate (MMA), 0.01g of azoisobutyronitrile, 5mL of methanol, stirring at 70 ℃ for 12h, washing with ethanol three times, and centrifugal drying to obtain QDs/PS/PVDC/PMMA powder, which is designated as sample # 2.
Example 3
Sample QDs/SiO2Preparation of/PVDC/PS
Sample QDs/SiO2The preparation process of/PVDC/PS is similar to that of the sample QDs/PMMA/PVDC/PS in example 1, except that PMMA microspheres are changed to SiO2Microspheres otherwise identical to example 1 gave QDs/SiO2PVDC/PS powder, noted sample # 3.
Example 4
Sample QDs/PMMA/PVDC/SiO2Preparation of
Sample QDs/PMMA/PVDC/SiO2The preparation process of (1) is similar to that of the sample QDs/PMMA/PVDC/PS in example 1, except that the process of forming PS coating layer by free radical is changed to SiO by reverse microemulsion method2The layers were otherwise the same as in example 1. SiO 22The specific method of the layer is as follows: dispersing 2nmol QDs/PMMA/PVDC powder in a mild solution of 100 μ L chloroform and 1mL cyclohexane, adding 80 μ L Tetraethoxysilane (TEOS), 150 μ L ammonia water, stirring at 800r/min for 15min, standing at room temperature in the dark for 5d, washing with 3mL ethanol, and centrifugally drying to obtain QDs/PMMA/PVDC/SiO2Powder, taken as sample # 4.
Example 5
Preparation of sample QDs/PS/PVDC/PMMA
The preparation of the sample QDs/PS/PVDC/PMMA differs from example 1 in that: in this embodiment, a polymer is first polymerized and coated on the surface of the quantum dot by a monomer, and then the polymer is coated on the surface of the quantum dot by a second layer of glue solution.
Preparation of sample QDs/PMMA/PS/PVDC
The preparation of the sample QDs/PMMA/PS/PVDC differs from example 1 in that: in this embodiment, a polymer is first polymerized and coated on the surface of the quantum dot by a monomer, and then the polymer is coated on the surface of the quantum dot by a second layer of glue solution.
The preparation method of the QDs/PMMA microspheres is the same as that of the embodiment 1, and the description is omitted;
PS is coated outside the QDs/PMMA microspheres. And heating and stirring 20mg of QDs/PMMA powder, 5mL of methanol, 180mg of styrene monomer, 66mg of polyvinylpyrrolidone and 5.4mg of azoisobutyronitrile at 55 ℃ in a nitrogen atmosphere for 5 hours, and centrifuging to obtain QDs/PMMA/PS powder.
Adding 100mg of QDs/PMMA/PS powder into 300mg/mL of PVDC-DMF glue solution, stirring, centrifuging at a high speed, adding n-hexane, stirring at a high speed, and carrying out vacuum freeze drying to obtain loose QDs/PMMA/PS/PVDC powder which is marked as sample No. 5.
Example 6 Performance testing
Respectively carrying out appearance characterization on the samples 1# to 5#
The characterization result shows that the particle size of the composite powder with the multilayer coating structure is several to more than ten microns.
Taking sample 1# as a typical representative, fig. 3 is a scanning electron microscope image of QDs/PMMA and QDs/PMMA/PVDC samples, and fig. 4 is a transmission electron microscope image of QDs/PMMA, QDs/PMMA/PVDC and QDs/PMMA/PVDC/PS samples, and as can be seen from fig. 3 and fig. 4, the particle size of the QDs/PMMA/PVDC/PS samples is tens of microns to tens of microns.
And after the quantum dot microspheres are subjected to multilayer coating, the size is increased by several microns.
And respectively carrying out fluorescence spectrum tests on samples 1# to 5 #. Typically, as shown in FIGS. 5 and 6, FIG. 5 is a fluorescence spectrum of the QDs/PMMA/PVDC/PS sample prepared in example 1, FIG. 6 is a fluorescence spectrum of the QDs/PS/PVDC/PMMA sample prepared in example 2, and it can be seen from FIGS. 5 and 6 that the fluorescence spectrum position is red-shifted by 3-4 nm.
The fluorescence quantum yield tests of samples 1# to 5# are respectively carried out, and the test result is represented by sample 1# and shows that the fluorescence quantum yield is reduced from 85% to 70%.
The weather resistance test is performed on the product of each coating stage in sample 1# respectively, and the test result is shown in fig. 7, as can be seen from fig. 7, the stability of the multilayer structure composite powder is greatly improved under the conditions of high temperature (60 ℃) and high humidity (90%), the fluorescence intensity of the pure quantum dot sample is reduced to 75% after aging for 630h, the fluorescence intensity of the QDs/PMMA/PVDC and QDs/PMMA/PVDC/PS samples is still maintained above 80%, and the fluorescence intensity is maintained at 93% and 86%, respectively.
Example 7
The quantum dot multilayer composite powder with high temperature and high humidity stability is suitable for being applied to backlight display, and as shown in fig. 8, the composite powder with a multilayer coating structure is adhered to a chip by being mixed with silica gel.
In the embodiment, the composite powder is only adhered to the chip, so that the using amount of the composite powder is reduced, and the practical cost is greatly reduced. The method is favorable for realizing the surface mount type integration of the light emitting diode with good stability.
Example 8
The quantum dot multilayer composite powder with high temperature and high humidity stability is suitable for being applied to backlight display, and as shown in fig. 9, the composite powder with a multilayer coating structure is adhered to the side surface of the light guide plate by being mixed with silica gel.
In the embodiment, the composite powder is only adhered to the side face of the light guide plate, so that the using amount of the composite powder is reduced, and the practical cost is greatly reduced. The side tube type integration of the light emitting diode with good stability is facilitated.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The composite powder with a multilayer coating structure is characterized by comprising a microsphere matrix, a quantum dot material and a coating layer;
the quantum dot material is adsorbed in the microsphere matrix to form a quantum dot/microsphere matrix;
the coating layer is coated on the surface of the microsphere matrix;
wherein the clad layer comprises at least one organic polymer layer.
2. The composite powder of claim 1, wherein the coating layer is an organic polymer layer;
preferably, the cladding layer is two organic polymer layers;
preferably, the coating layer is an organic polymer layer and an inorganic oxide layer;
wherein, the organic polymer layer and the inorganic oxide layer extend outwards along the surface of the microsphere substrate;
the inorganic oxide layer is selected from any one of silicon dioxide, aluminum oxide and titanium oxide.
3. The composite powder according to claim 1, wherein the microsphere matrix is at least one selected from the group consisting of an organosilicon microsphere, a silica microsphere, a polymethyl methacrylate microsphere, a polystyrene microsphere, and an iron oxide microsphere;
preferably, the organic polymer is selected from at least one of polyvinyl chloride, polymethyl methacrylate, polyvinyl acetate, cellulose acetate, polyamide, polyimide, polycarbonate, polystyrene, polyvinylidene chloride, polyvinylidene fluoride, polyvinyl alcohol, transparent ABS plastic, polyacrylonitrile, polyolefin elastomer, thermoplastic polyurethane, polyvinyl carbazole;
preferably, the quantum dot material is quantum dot or quantum dot modified by organic matter;
wherein the organic matter is at least one selected from 6-mercapto-1-hexanol, 2-mercapto-3-butanol, 3-mercapto-1-propanol, 2, 3-dimercaptopropanol, and poly-octadecene-maleic anhydride;
preferably, the quantum dots are selected from at least one of a substance I with a chemical formula shown in a formula I, a substance II with a chemical formula shown in a formula II and a substance III with a chemical formula shown in a formula III;
AM formula I
EFQ2Formula II
GHX3Formula III
Wherein A is selected from at least one of Cd, Zn, Pb and In;
m and Q are independently selected from at least one of S, Se, Te and P;
e is selected from at least one of Cu, Ag and Zn;
f is selected from at least one of Al, Ga and In;
g is selected from CH3NH3、CH(NH)NH3At least one of Cs;
h is selected from at least one of Ag, Sb, Bi, Pb, In and Al;
x is selected from at least one of halogen;
the size of the quantum dots is 2-39 nm.
4. A method for preparing the composite powder with a multilayer coating structure according to claim 1, which comprises at least the following steps:
a) heating a material containing a quantum dot material and a microsphere matrix to obtain the quantum dot/microsphere matrix;
b) and coating the coating layer on the surface of the microsphere matrix to obtain the composite powder.
5. The method according to claim 4, wherein in step a), the mass ratio of the quantum dot material to the microsphere matrix is 1% to 10%;
preferably, in the step a), the temperature is heated to 50-70 ℃ until the solvent in the material is completely evaporated.
6. The method of claim 4, wherein step b) comprises:
b-1) coating a mixture a containing the quantum dot/microsphere matrix and the first coating layer source to obtain a quantum dot/microsphere matrix/coating layer I;
b-2) coating a mixture b containing the quantum dot/microsphere matrix/coating layer I and a second coating layer source to obtain a quantum dot/microsphere matrix/coating layer I/coating layer II;
wherein, the first coating layer source is selected from any one of organic polymer glue solution and organic polymer monomer;
the second coating layer source is selected from any one of organic polymer glue solution, organic polymer monomer and inorganic oxide precursor;
preferably, the step b) includes:
b-1) uniformly mixing a mixture a containing the quantum dot/microsphere matrix and the organic polymer glue solution to obtain a quantum dot/microsphere matrix/organic polymer layer I;
b-2) carrying out polymerization reaction on a mixture b containing the quantum dot/microsphere matrix/organic polymer layer I and an organic polymer monomer to obtain a quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II;
wherein the organic polymer layer I and the organic polymer layer II are different organic polymers;
preferably, the step b) includes:
b-1) carrying out polymerization reaction on a mixture a containing the quantum dot/microsphere matrix and the organic polymer monomer to obtain a quantum dot/microsphere matrix/organic polymer layer I;
b-2) uniformly mixing a mixture b containing the quantum dot/microsphere matrix/organic polymer layer I and an organic polymer glue solution to obtain a quantum dot/microsphere matrix/organic polymer layer I/organic polymer layer II;
wherein the organic polymer layer I and the organic polymer layer II are different organic polymers.
7. The multilayer coating structure composite powder according to any one of claims 1 to 3 and the multilayer coating structure composite powder prepared by the method according to any one of claims 4 to 6 are applied to the fields of illumination and display.
8. A display device is characterized by comprising a light guide plate, a chip and composite powder with a multilayer coating structure;
the chip is positioned on the side of the light guide plate;
the composite powder with a multilayer coating structure comprises any one of the composite powder with a multilayer coating structure as defined in any one of claims 1 to 3 and the composite powder with a multilayer coating structure prepared by the method as defined in any one of claims 4 to 6.
9. The display device according to claim 8, wherein the composite powder of the multilayer coating structure is attached to a surface of the chip facing the light guide plate.
10. The display device according to claim 8, wherein the composite powder of the multilayer coating structure is attached to a side of the light guide plate facing the chip.
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