CN117567905A - Quantum dot composition, preparation method of compound and color conversion panel containing quantum dot composition - Google Patents
Quantum dot composition, preparation method of compound and color conversion panel containing quantum dot composition Download PDFInfo
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- CN117567905A CN117567905A CN202311492310.5A CN202311492310A CN117567905A CN 117567905 A CN117567905 A CN 117567905A CN 202311492310 A CN202311492310 A CN 202311492310A CN 117567905 A CN117567905 A CN 117567905A
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- quantum dot
- organic compound
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- 238000002360 preparation method Methods 0.000 title description 5
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- 239000000370 acceptor Substances 0.000 claims abstract description 4
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- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- VEBCLRKUSAGCDF-UHFFFAOYSA-N ac1mi23b Chemical compound C1C2C3C(COC(=O)C=C)CCC3C1C(COC(=O)C=C)C2 VEBCLRKUSAGCDF-UHFFFAOYSA-N 0.000 description 1
- IPTNXMGXEGQYSY-UHFFFAOYSA-N acetic acid;1-methoxybutan-1-ol Chemical compound CC(O)=O.CCCC(O)OC IPTNXMGXEGQYSY-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- OCWYEMOEOGEQAN-UHFFFAOYSA-N bumetrizole Chemical compound CC(C)(C)C1=CC(C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O OCWYEMOEOGEQAN-UHFFFAOYSA-N 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000005520 diaryliodonium group Chemical group 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- 150000001989 diazonium salts Chemical class 0.000 description 1
- 229940019778 diethylene glycol diethyl ether Drugs 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- BHXIWUJLHYHGSJ-UHFFFAOYSA-N ethyl 3-ethoxypropanoate Chemical compound CCOCCC(=O)OCC BHXIWUJLHYHGSJ-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012949 free radical photoinitiator Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- BDJSOPWXYLFTNW-UHFFFAOYSA-N methyl 3-methoxypropanoate Chemical compound COCCC(=O)OC BDJSOPWXYLFTNW-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FEUIEHHLVZUGPB-UHFFFAOYSA-N oxolan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC1CCCO1 FEUIEHHLVZUGPB-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229950000688 phenothiazine Drugs 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 229940116351 sebacate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005409 triarylsulfonium group Chemical group 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The present disclosure provides a quantum dot composition, a method of preparing a quantum dot composite, and a color conversion panel; the quantum dot composition includes quantum dots, an organic compound, a polymer precursor, and a photoinitiator, wherein the quantum dots and the organic compound can be uniformly dispersed in the polymer precursor; the molecular weight of the organic compound is less than or equal to 1000, the organic compound is solid at normal temperature, and the molecular polarization rate is 10-4010 ‑24 cm 3 The fusion heat is 50-350kJ/kg, and the number of hydrogen bond acceptors is more than or equal to 1. The organic compound with the characteristics can be uniformly dispersed in an ink system, agglomeration and sedimentation can not occur, and the storage and use stability of the quantum dot composition are improved. In the subsequent application, the crystallization particles can be prevented from being formed after sedimentation and solidification in the printing spray head, and the effect of conventional scattering particles is provided.
Description
Technical Field
The disclosure relates to the technical field of quantum dot photoluminescence, in particular to a quantum dot composition, a compound preparation method and a color conversion panel containing the quantum dot composition.
Background
In photoluminescent inkjet ink systems, the addition of inorganic scattering particles can improve the light efficiency but its tendency to settle has a negative impact on the printing performance. In order to delay the sedimentation of inorganic scattering particles, the main means at present is the surface modification of the inorganic scattering particles so as to improve the dispersibility of the inorganic scattering particles. However, since the particle size of the inorganic scattering particles in the ink jet ink is 100 to 300nm, sedimentation thereof is unavoidable after a long-term storage.
Disclosure of Invention
It is an object of the present disclosure to provide a quantum dot composition having improved storage and use stability, and a composite preparation method and color conversion panel.
In a first aspect of the present application, there is provided a quantum dot composition comprising quantum dots, an organic compound, a polymer precursor, and a photoinitiator, the quantum dots and the organic compound being uniformly dispersible in the polymer precursor; the molecular weight of the organic compound is less than or equal to 1000, the organic compound is solid at normal temperature, and the molecular polarization rate is 10-4010 -24 cm 3 The fusion heat is 50-350kJ/kg, and the number of hydrogen bond acceptors is more than or equal to 1.
Alternatively, the surface tension of the organic compound is 20.0 to 45.0mN/m.
Alternatively, the melting temperature of the organic compound is 80-200 ℃.
Optionally, the organic compound is selected from one or more of the group consisting of lactide, acrylonitrile resin, diethyl terephthalate, methyl styrene, dimethoxy styrene, polyvinylpyrrolidone, 2-hydroxy-4-oxatricyclo [4,2,1,0,37] -5-nonanone, 2-acrylamido-2-methylpropanesulfonic acid.
Alternatively, the polymer precursors include monomers and oligomers containing unsaturated bonds.
Alternatively, the unsaturated bond-containing monomer includes monofunctional and polyfunctional acrylic monomers.
Optionally, the quantum dot composition further comprises a solvent.
Alternatively, the quantum dot composition does not include scattering particles of an inorganic compound.
Optionally, the quantum dot composition further comprises an auxiliary agent, preferably selected from one or more of a dispersant, an antioxidant and a light stabilizer.
Optionally, the quantum dot composition comprises 10-60wt% of quantum dots and 3-15wt% of organic compounds.
In a second aspect of the present application, there is provided a method for preparing a quantum dot composite, comprising preparing any one of the above quantum dot compositions, and photo-curing, wherein the organic compound does not chemically react during the curing process, and the organic compound aggregates to form crystalline particles.
Alternatively, the crystalline particles are platelet-shaped and have a lateral dimension of 20-400nm.
In a third aspect of the present application, there is provided a color conversion panel comprising a substrate, a pixel defining layer, and a black matrix disposed therebetween; the quantum dot composite prepared by any preparation method is positioned in each opening area of the pixel defining layer.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate and explain the exemplary embodiments of the disclosure and together with the description serve to explain the disclosure, and do not constitute an undue limitation on the disclosure. In the drawings:
fig. 1 shows a schematic structural diagram of a quantum dot composite of the present disclosure.
Fig. 2 is a photograph of ink droplets of a quantum dot composition after being ejected by a printing device in accordance with some embodiments of the present disclosure.
Fig. 3 is an optical micrograph of a quantum dot composition printed to a pixel substrate according to some embodiments of the present disclosure.
Fig. 4 is an optical micrograph of a quantum dot composite of some embodiments of the present disclosure.
Fig. 5 is an optical micrograph of a quantum dot composite of a comparative example of the present disclosure.
Fig. 6 shows quantum dot composite melting curves of examples and comparative examples of the present disclosure.
Fig. 7 shows fluorescence emission spectra of quantum dot composites of examples and comparative examples of the present disclosure.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
According to a first aspect of the present invention, there is provided a quantum dot composition comprising quantum dots, an organic compound, a polymer precursor and a photoinitiator, said quantum dots and said organic compound being uniformly dispersible in said polymer precursor; the organic compound has a molecular weight of 1000 or less, is solid at normal temperature, and has a molecular polarizability of 10-4010 - 24 cm 3 The fusion heat is 50-350kJ/kg, and the number of hydrogen bond acceptors is more than or equal to 1. The organic compound with the characteristics can be uniformly dispersed in an ink system, agglomeration and sedimentation can not occur, and the storage and use stability of the quantum dot composition are improved. And in the subsequent application, the formation of crystalline particles after sedimentation and solidification in a printing nozzle can be avoided, and the effect of conventional scattering particles (such as titanium oxide) is provided.
The normal temperature state is 25℃and the normal atmospheric pressure.
In some embodiments, the surface tension of the above-described organic compounds is 20.0-45.0mN/m, thereby making the quantum dot composition more suitable for inkjet printing.
In some embodiments, the melting temperature of the organic compound is 80-200 ℃, thereby making the presence of crystalline particles more stable after solidification of the quantum dot composition. And is suitable for the working temperature of the color conversion panel.
In some embodiments, the organic compound is selected from one or more of the group consisting of lactide (containing L-configuration or D-configuration or LD-configuration), acrylonitrile resin, diethyl terephthalate, methyl styrene, dimethoxy styrene, polyvinylpyrrolidone (preferably having a number average molecular weight of 100 or more), 2-hydroxy-4-oxatricyclo [4,2,1,0,37] -5-nonone, 2-acrylamido-2-methylpropanesulfonic acid.
In some embodiments, the polymer precursors described above include monomers and oligomers containing unsaturated bonds.
In some embodiments, the unsaturated bond-containing monomers described above include mono-and multi-functional acrylic monomers.
The acrylic monomer with a single functional group is selected from one or more of methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, n-propyl acrylate, n-propyl methacrylate, isopropyl acrylate, isopropyl methacrylate, n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate, isobutyl methacrylate, tert-butyl acrylate, tert-butyl methacrylate, isooctyl acrylate, isooctyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate, hydroxybutyl methacrylate, isobornyl acrylate, isobornyl methacrylate, isodecyl acrylate, lauryl methacrylate, 2-phenoxyethyl acrylate, 2-phenoxyethyl methacrylate, 3, 5-trimethylcyclohexane acrylate, tetrahydrofuranyl acrylate and acryloylmorpholine.
The multifunctional acrylic monomer may be a difunctional or trifunctional acrylic monomer. The acrylic monomer with double or three functionalities is selected from one or more of 1, 6-hexanediol diacrylate, triethylene glycol dimethacrylate, tricyclodecane dimethanol diacrylate, tri (2-hydroxyethyl) isocyanic acid triacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate, 3-ethoxy-trimethylolpropane triacrylate, 9-ethoxy-trimethylolpropane triacrylate, propoxy-trimethylolpropane triacrylate and trimethylolpropane trimethacrylate.
In some embodiments, the quantum dot compositions described above do not include a solvent. In some embodiments, the quantum dot compositions described above further comprise a solvent. Specific examples of the solvent include alkylene glycol alkyl ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, and propylene glycol methylethyl ether; diethylene glycol dialkyl ethers such as diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol dipropyl ether, diethylene glycol dibutyl ether, and the like; alkylene glycol alkyl ether acetates such as methyl cellosolve acetate, ethyl cellosolve acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, and propylene glycol monopropyl ether acetate; alkoxyalkyl acetates such as methoxybutyl acetate and methoxypentyl acetate; aromatic hydrocarbons such as benzene, toluene, xylene, and mesitylene; ketones such as methyl ethyl ketone, acetone, methyl amyl ketone, methyl isobutyl ketone, and cyclohexanone; alcohols such as ethanol, propanol, butanol, hexanol, cyclohexanol, ethylene glycol, and glycerin; esters such as ethyl 3-ethoxypropionate and methyl 3-methoxypropionate; cyclic esters such as gamma-butyrolactone, etc.
In some embodiments, the quantum dot compositions described above do not include scattering particles of inorganic compounds. Examples of inorganic compound scattering include, but are not limited to, tiO 2 、ZrO 2 、Al 2 O 3 、SiO 2 、In 2 O 3 ZnO and SnO 2 。
The quantum dots may include at least one of red quantum dots, green quantum dots, and blue quantum dots.
The photoinitiator may include: at least one of benzoin and derivatives, benzil, alkyl benzene ketone, acyl phosphorus oxide, thioxanthone and cationic photoinitiator. The free radical photoinitiator comprises benzoin and derivatives, wherein the benzoin and derivatives can comprise at least one of benzoin, benzoin dimethyl ether, benzoin diethyl ether, benzoin isopropyl ether and benzoin butyl ether; the benzil may include at least one of diphenylethanone, α -dimethoxy- α -phenylacetophenone; the alkylbenzene ketone may include at least one of alpha, alpha-diethoxyacetophenone, alpha-hydroxyalkyl benzophenone, alpha-aminoalkyl benzophenone; the acyl phosphorus oxide may include at least one of aroylphosphine oxide, bisbenzoylphenylphosphine oxide; the thioxanthone may include at least one of a thiopropyloxythioxanthone, an isopropylthioxanthone; the cationic photoinitiator may include at least one of diazonium salts, diaryliodonium salts, triarylsulfonium salts, alkyl sulfonium salts, iron arene salts, sulfonyloxy ketones, and triarylsiloxane ethers. The photoinitiator may be selected from one or more, and the specific type and amount may be selected according to the practice.
In some embodiments, the quantum dot composition further comprises an auxiliary agent, preferably selected from one or more of a dispersant, an antioxidant, and a light stabilizer.
As the resin-type dispersant, a phosphate-type dispersant, a urethane-type dispersant, an acrylic-type dispersant, or the like can be used. Specifically, as a commercial product of the above-mentioned dispersant, a trade name of the Pick company can be used: DISPER BYK-103, DISPER BYK-110, DISPER BYK-111, DISPER BYK-2000, DISPER BYK-2001, DISPER BYK-2070, DISPER BYK-2150, DISPER BYK-160, DISPER BYK-161, DISPER BYK-162, DIPER BYK-163, DIPER BYK-164, DIPER BYK-166, and the like.
The antioxidant may be at least one of 1, 4-hydroquinone, methylhydroquinone, 4-methoxyphenol, p-ethoxyphenol, t-butylcatechol, p-phenol monobutyl ether, p-hydroxyanisole, 2-t-butylhydroquinone, 2, 5-di-t-butylhydroquinone, phenothiazine, phenoxazine, 2, 6-tetramethylpiperidine-1-oxyl, tetramethylpiperidine nitroxide phosphate triester, 2, 6-di-t-butyl-p-methylphenol, 4' -di-warp biphenyl, and bisphenol A.
The light stabilizer can be selected from bis-2, 6-tetramethyl piperidinol sebacate, polymer of succinic acid and 4-hydroxy-2, 6-tetramethyl-1-piperidinol 2- (2H-benzotriazol-2-yl) -4- (1, 3-tetramethylbutyl) phenol, 2- (2-hydroxy-5-methyl-phenyl) -2H-benzotriazol 2-hydroxy-4-n-octoxybenzophenone, 2- (2H-benzotriazol-2-yl) -4, 6-bis (1-methyl-1-phenethyl) -phenol, and 2- (5-chloro-2H-benzotriazol-2-yl) -6- (1, 1-dimethylethyl) -4-methylphenol.
In some embodiments, the quantum dot composition comprises 10-60wt% of the quantum dot and 3-15wt% of the organic compound.
In some embodiments, the quantum dot composition comprises 30-60wt% of the quantum dot and 3-8wt% of the organic compound.
In some embodiments, the quantum dot compositions described above are suitable for use in inkjet printing processes.
According to a second aspect of the present invention, there is provided a method of preparing a quantum dot composite, comprising preparing any one of the above quantum dot compositions, light curing, wherein the organic compound does not undergo chemical reaction during the curing process, and the organic compound aggregates to form crystalline particles.
In the curing process, the polymer precursor gradually polymerizes to form a polymer, the molecular weight is increased, the solubility of the organic compound originally dissolved in the composition in the polymer is reduced, the phase separation phenomenon occurs between the organic compound and the polymer and between the organic compound and the polymer precursor, an organic compound enrichment region and a polymer and polymer precursor enrichment region are formed, and the molecules of the organic compound enrichment region are closely packed to form a crystallization region (or called crystallization), so that the polymer precursor completely reacts to form the polymer. In the finally formed quantum dot composite, the crystalline particles are distributed in the polymer, and the schematic structure of the quantum dot composite is shown in fig. 1. The regular arrangement of the molecular level of the organic compound can not only serve as a scattering component, but also serve as an auxiliary agent for blocking water and oxygen.
In some embodiments, any of the quantum dot compositions described above are prepared, and inkjet printed onto a substrate for photo-curing. The quantum dot composition has good ink jet printing effect, does not block a spray head, and has uniform film layer after being solidified into a compound.
In some embodiments, the crystalline particles are platelet-shaped and have a lateral dimension of 20-400nm. In some embodiments, the lateral dimension of the crystalline particles is 100-400nm.
According to a third aspect of the present invention, there is provided a color conversion panel comprising a substrate including a substrate, a pixel defining layer, and a black matrix disposed therebetween; the quantum dot composite is positioned in each opening area of the pixel defining layer. The color conversion panel is a panel for a display device. The color conversion panel with the quantum dot compound has better light-emitting efficiency. The structure of the above-described substrate may be referred to the prior art.
Hereinafter, the embodiments are described in more detail with reference to specific examples. However, they are illustrative examples of the present disclosure, and the present disclosure is not limited thereto.
Example 1
Preparing a quantum dot composition, taking red quantum dots as an example
The first step: firstly, mixing a Quantum Dot (QD) concentrated solution (solvent toluene) into an acrylic acid monomer, swirling for 30 minutes on a vortex instrument, standing for 30 minutes, and repeating the process until the QD is completely dissolved; and introducing nitrogen for 15min to remove the solvent and oxygen, thus obtaining the QD-propionate monomer mixed solution a.
And a second step of: mixing a crystalline compound (lactide-L/D) into an acrylate monomer, and performing ultrasonic treatment for 30min to obtain a crystalline compound-acrylate monomer mixed solution b.
And thirdly, mixing the two mixed solutions of the a and the b in proportion, adding a photoinitiator and other auxiliary agents, swirling for 30min, and filtering by using a 0.45 mu m filter to obtain the QD printing ink of which the filtrate contains 30-60wt% of QD and 1-8wt% of crystalline compound.
The viscosity of the resulting QD ink was 5 to 25cP (35 ℃ C.) and the surface tension was 25 to 40mN/m.
The quantum dot ink was printed by an inkjet printing apparatus (FUJIFILM Dimatix DMP, 2800) at a printing temperature of 35 ℃ to obtain fig. 2. From the photograph, it can be seen that the ink drops at the outlet of the printing nozzle are round, and have no tailing phenomenon, which indicates good printing performance.
The printing effect of the quantum dot ink on the pixel substrate is shown in fig. 3. The ink can well fill into the pixel pits of the substrate, the position is accurate, the surface is smooth, no overflow exists, and the printing effect is good.
Comparative example 1
The difference from the quantum dot composition of example 1 is that no organic compound for forming crystals is contained. The viscosity of the resulting QD ink was 5 to 25cP (35 ℃ C.) and the surface tension was 25 to 35mN/m.
Characterization test of quantum dot complexes:
the quantum dot inks of example 1 and comparative example 1 were uv cured and observed with an optical microscope (a gyroscope), and the obtained photographs are shown in fig. 4 and 5, respectively. As can be seen from a comparison of the two figures, the quantum dot composite obtained in example 1 has a crystalline region of 20-400nm, which is more uniformly distributed inside the sample. After curing the QD ink of example 1, these organic compounds aggregate and undergo precipitation crystallization, and the crystal particle size approaches the usual scattering particle size.
The melting curves of the cured quantum dot composite sample and the cured quantum dot composite sample are further detected by a Differential Scanning Calorimeter (DSC) and are shown in fig. 6, and it can be seen by comparing the melting curves of the cured quantum dot composite sample and the cured quantum dot composite sample, wherein the melting peak exists in the curve corresponding to the composite prepared by the ink of the embodiment 1, namely crystallization exists, and the melting temperature is 126 ℃.
The quantum dot inks of example 1 and comparative example 1 were uv cured on a transparent glass substrate to give a composite having a thickness of 10 μm and a Quantum Dot (QD) content of 30wt%, wherein the mass fraction of the organic compound forming the crystalline use in the quantum dot ink of example 1 was 4%. And placing the quantum dot compound on a 450nm blue LED backlight source, respectively testing a blue backlight spectrum and a spectrum penetrating through the quantum dot compound material by using an integrating sphere, and calculating the luminous efficiency by using the integral area of the spectrogram. Fig. 7 shows fluorescence emission spectra of the quantum dot composites of the examples and the comparative examples, with blue absorption increased from 90% to 98% and luminous efficiency increased from 65% to 70%. This demonstrates that the addition of the organic compound acts as a scattering particle, not only increasing the blue light absorption of the quantum dot composite, but also increasing the light efficiency.
The foregoing description of the preferred embodiments of the present disclosure is provided only and not intended to limit the disclosure so that various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (13)
1. A quantum dot composition comprising quantum dots, an organic compound, a polymer precursor, and a photoinitiator, wherein the quantum dots and the organic compound are uniformly dispersed in the polymer precursor; the molecular weight of the organic compound is less than or equal to 1000, the organic compound is solid at normal temperature, and the molecular polarization rate is 10-4010 -24 cm 3 The fusion heat is 50-350kJ/kg, and the number of hydrogen bond acceptors is more than or equal to 1.
2. The quantum dot composition of claim 1, wherein the surface tension of the organic compound is 20.0-45.0mN/m.
3. The quantum dot composition of claim 1, wherein the melting temperature of the organic compound is 80-200 ℃.
4. A quantum dot composition according to claim 2 or 3, wherein the organic compound is selected from one or more of the group consisting of lactide, acrylonitrile resin, diethyl terephthalate, methyl styrene, dimethoxystyrene, polyvinylpyrrolidone, 2-hydroxy-4-oxatricyclo [4,2,1,0,37] -5-nonanone, 2-acrylamido-2-methylpropanesulfonic acid.
5. The quantum dot composition of claim 1, wherein the polymer precursor comprises monomers and oligomers containing unsaturation.
6. The quantum dot composition of claim 5, wherein the unsaturated bond-containing monomer comprises mono-and multi-functional acrylic monomers.
7. The quantum dot composition of claim 1, wherein the quantum dot composition further comprises a solvent.
8. The quantum dot composition of claim 1, wherein the quantum dot composition does not include scattering particles of an inorganic compound.
9. The quantum dot composition according to claim 1, characterized in that the quantum dot composition further comprises an auxiliary agent, preferably selected from one or more of dispersants, antioxidants and light stabilizers.
10. The quantum dot composition according to claim 1, wherein the mass fraction of the quantum dots in the quantum dot composition is 10-60wt% and the mass fraction of the organic compound is 3-15wt%.
11. A method of preparing a quantum dot composite comprising preparing a quantum dot composition according to any one of claims 1 to 10, light curing, wherein the organic compound does not chemically react during the curing, and wherein the organic compound aggregates to form crystalline particles.
12. The method of preparing a quantum dot composite according to claim 11, wherein the crystalline particles are in the form of flakes and the lateral dimension of the crystalline particles is 20-400nm.
13. A color conversion panel comprising a substrate, a pixel defining layer, and a black matrix disposed therebetween; further comprising the quantum dot composite prepared by the method of claim 11 or 12, the quantum dot composite being located within each open area of the pixel defining layer.
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