CN111363385A - Preparation method of organic modified barium titanate nanoparticles and preparation method of quantum dot optical film - Google Patents
Preparation method of organic modified barium titanate nanoparticles and preparation method of quantum dot optical film Download PDFInfo
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- barium titanate
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 106
- 239000002096 quantum dot Substances 0.000 title claims abstract description 82
- 239000012788 optical film Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 47
- 239000011259 mixed solution Substances 0.000 claims abstract description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 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 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005416 organic matter Substances 0.000 claims abstract description 13
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- ZUDYPQRUOYEARG-UHFFFAOYSA-L barium(2+);dihydroxide;octahydrate Chemical compound O.O.O.O.O.O.O.O.[OH-].[OH-].[Ba+2] ZUDYPQRUOYEARG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 239000003292 glue Substances 0.000 claims description 11
- -1 titanium ions Chemical class 0.000 claims description 9
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 8
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- VYMPLPIFKRHAAC-UHFFFAOYSA-N 1,2-ethanedithiol Chemical compound SCCS VYMPLPIFKRHAAC-UHFFFAOYSA-N 0.000 claims description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- 229910001422 barium ion Inorganic materials 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 6
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229920000193 polymethacrylate Polymers 0.000 claims description 5
- GJRCLMJHPWCJEI-UHFFFAOYSA-N 1,9-Nonanedithiol Chemical compound SCCCCCCCCCS GJRCLMJHPWCJEI-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- AGBQKNBQESQNJD-UHFFFAOYSA-M lipoate Chemical compound [O-]C(=O)CCCCC1CCSS1 AGBQKNBQESQNJD-UHFFFAOYSA-M 0.000 claims description 3
- 235000019136 lipoic acid Nutrition 0.000 claims description 3
- ZJLMKPKYJBQJNH-UHFFFAOYSA-N propane-1,3-dithiol Chemical compound SCCCS ZJLMKPKYJBQJNH-UHFFFAOYSA-N 0.000 claims description 3
- 229960002663 thioctic acid Drugs 0.000 claims description 3
- PGTWZHXOSWQKCY-UHFFFAOYSA-N 1,8-Octanedithiol Chemical compound SCCCCCCCCS PGTWZHXOSWQKCY-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- KMTUBAIXCBHPIZ-UHFFFAOYSA-N pentane-1,5-dithiol Chemical compound SCCCCCS KMTUBAIXCBHPIZ-UHFFFAOYSA-N 0.000 claims 1
- 229910002113 barium titanate Inorganic materials 0.000 description 20
- 239000002245 particle Substances 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 11
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000000103 photoluminescence spectrum Methods 0.000 description 3
- ZRKMQKLGEQPLNS-UHFFFAOYSA-N 1-Pentanethiol Chemical compound CCCCCS ZRKMQKLGEQPLNS-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- SONHXMAHPHADTF-UHFFFAOYSA-M sodium;2-methylprop-2-enoate Chemical compound [Na+].CC(=C)C([O-])=O SONHXMAHPHADTF-UHFFFAOYSA-M 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical class C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical class [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- WNKMTAQXMLAYHX-UHFFFAOYSA-N barium(2+);dioxido(oxo)titanium Polymers [Ba+2].[O-][Ti]([O-])=O WNKMTAQXMLAYHX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical class [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002290 germanium Chemical class 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical class [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical class [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- GTLQJUQHDTWYJC-UHFFFAOYSA-N zinc;selenium(2-) Chemical class [Zn+2].[Se-2] GTLQJUQHDTWYJC-UHFFFAOYSA-N 0.000 description 1
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- 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
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Abstract
The invention provides a preparation method of organic modified barium titanate nano-particles and a preparation method of a quantum dot optical film, wherein the preparation method of the organic modified barium titanate nano-particles comprises the following steps: adding barium hydroxide octahydrate into deionized water, and uniformly stirring to obtain a barium hydroxide solution; adding tetrabutyl titanate into an ethanol solvent, and uniformly stirring to obtain a tetrabutyl titanate solution; adding the barium hydroxide solution into the tetrabutyl titanate solution to obtain a first mixed solution; adding a sodium hydroxide solution and an organic matter into the first mixed solution to obtain a second mixed solution, wherein the organic matter contains carbon-hydrogen bonds and carbon-oxygen bonds; sealing the second mixed solution in a high-pressure reaction kettle; and carrying out high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution to obtain the organic modified barium titanate nanoparticles.
Description
Technical Field
The application relates to the technical field of semiconductor display, in particular to a preparation method of organic modified barium titanate nano particles and a preparation method of a quantum dot optical film.
Background
Quantum dots are a novel semiconductor material with excellent light-emitting characteristics, mainly composed of elements of II-VI groups, III-V groups, IV groups and the like, and the size of the quantum dots is close to or smaller than the exciton Bohr radius. The wavelength of emitted light in a visible light waveband is adjustable, the half-peak width is narrow, the luminous efficiency is high, and the LED-based light source has strong application potential in the application fields of white LEDs, QLEDs, photoelectric detectors and the like. The quantum dots are applied to the display field, and because the synthesis cost is high and the price is high, in order to reduce the dosage of the quantum dots, scattering particles can be doped to increase the brightness of the quantum dots, and meanwhile, the heavy metal content in unit mass can be reduced, thereby being beneficial to protecting the environment and meeting the standard of commercial application.
The quantum dot scattering film becomes an important functional material in the fields of illumination, optical display, light design and the like, can solve the problem of asymmetric visual angle, can achieve the aim of unifying high efficiency and visual uniformity of an illumination and display system, and provides guarantee for illumination and display equipment with high efficiency, low loss, high uniformity and perfect vision.
The quantum dots can be used as fluorescent conversion materials in the field of LED luminescence for backlight display of mobile phones and televisions, wherein a white light quantum dot film needs to mix red and green quantum dots together, then emits light through excitation of blue light of a chip, and is compounded with emergent light of the chip to obtain white light. The application of the quantum dots in the display field can provide an optical film with wide color gamut, high color rendering index, high brightness and high color purity, and can replace fluorescent powder backlight with low luminous efficiency and low color rendering purity to lead the next generation of display.
However, the barium titanate nanoparticles synthesized by the traditional method are not subjected to organic modification and are easily precipitated in an organic solvent, so that the barium titanate nanoparticles are easily aggregated in acrylic glue, and the uniformity of luminescence of the quantum dot optical film is affected.
Disclosure of Invention
The invention aims to provide a preparation method of organic modified barium titanate nano-particles and a preparation method of a quantum dot optical film, wherein the barium titanate nano-particles synthesized by the traditional method are not subjected to organic modification and are easy to precipitate in an organic solvent, so that the barium titanate nano-particles are easy to aggregate in acrylic glue and influence the light-emitting uniformity of the quantum dot optical film.
In order to achieve the above object, the present invention provides a method for preparing organically modified barium titanate nanoparticles, comprising the steps of: adding barium hydroxide octahydrate into deionized water, and uniformly stirring to obtain a barium hydroxide solution; adding tetrabutyl titanate into an ethanol solvent, and uniformly stirring to obtain a tetrabutyl titanate solution; adding the barium hydroxide solution into the tetrabutyl titanate solution to obtain a first mixed solution; adding a sodium hydroxide solution and an organic matter into the first mixed solution to obtain a second mixed solution, wherein the organic matter contains carbon-hydrogen bonds and carbon-oxygen bonds; sealing the second mixed solution in a high-pressure reaction kettle; and carrying out high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution to obtain the organic modified barium titanate nanoparticles.
Further onThe organic matter is acrylic acid series, COOH- (CH)2) n-COOH series, HS- (CH)2) n-SH series, HS- (CH)2) n-COOH, wherein n is 1. ltoreq.n < 20.
Further, the acrylic acid series includes any one of methacrylic acid and sodium polymethacrylate.
Further, the COOH- (CH)2) The n-COOH series includes any one of malonic acid, succinic acid, glutaric acid, azelaic acid, pimelic acid.
Further, the HS- (CH)2) The n-SH series includes any one of 1, 2-ethanedithiol, 1, 3-propanedithiol, 1, 5-pentanethiol, and 1, 9-nonanedithiol.
Further, the HS- (CH)2) The n-COOH series includes any one of mercaptopropionic acid and lipoic acid.
Further, in the first mixed solution, the molar ratio of titanium ions to barium ions is 1: 1.
Further, in the step of performing high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution, the high-pressure reaction kettle is placed in an oven, the second mixed solution is subjected to high-temperature treatment for 10-30 hours at the temperature of 150-.
In order to achieve the above object, the present invention further provides a method for preparing a quantum dot optical film, comprising the steps of:
providing organically modified barium titanate nanoparticles as described hereinbefore; preparing a blend, wherein the blend comprises the following components in percentage by mass: 2-10 wt% of the organic modified barium titanate nano particles, 0.9-1.5 wt% of the quantum dots and the balance of glue; and coating the mixture on a substrate, and curing to form the quantum dot optical film.
Further, in the step of preparing the blend, the organically modified barium titanate nanoparticles, the quantum dots and the glue are mixed and stirred to obtain the blend; and in the step of coating the mixture on a substrate, curing the mixture by adopting an ultraviolet irradiation mode or a heating mode.
The invention has the technical effects that an organic matter is added in the process of preparing the organic modified barium titanate nano particles, so that the organic modified barium titanate nano particles are controllable in appearance and adjustable in particle size, the crystal structure of the organic modified barium titanate nano particles is a perovskite structure, and the organic modified barium titanate nano particles have high refractive index, namely good scattering capability. The organic modified barium titanate nano-particles are used as scattering particles and applied to the quantum dot optical film, and can play a role in enhancing the brightness of the film, namely after the quantum dots are doped with the scattering particles, the using amount of the quantum dots can be reduced, the utilization rate of blue light can be improved, and the absorption of the blue light is increased. The quantum dots contain heavy metal elements which are harmful to the environment and human bodies, so that the production cost can be saved by reducing the dosage of the quantum dots, and meanwhile, the displayed dosage is also reduced.
Drawings
The technical solution and other advantages of the present application will become apparent from the detailed description of the embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a flowchart of a method for preparing organically modified barium titanate nanoparticles according to an embodiment of the present disclosure.
Fig. 2 is a flowchart of a method for manufacturing a quantum dot optical film according to an embodiment of the present disclosure.
Fig. 3 is a TEM (transmission electron microscope) image of the organically modified barium titanate nanoparticles of the present application.
Fig. 4 is a FT-IR spectrum of barium titanate nanoparticles before modification.
Fig. 5 is a FT-IR spectrum of sodium methacrylate modified barium titanate nanoparticles.
FIG. 6 is a FT-IR spectrum of sodium polymethacrylate modified barium titanate nanoparticles.
Fig. 7 is a FT-IR spectrum of glutaric acid modified barium titanate nanoparticles.
Fig. 8 is a PL spectrum of a quantum dot optical film without and with organically modified barium titanate nanoparticles added.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The following disclosure provides many different embodiments or examples for implementing different features of the application. In order to simplify the disclosure of the present application, specific example components and arrangements are described below. Of course, they are merely examples and are not intended to limit the present application. Moreover, the present application may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, examples of various specific processes and materials are provided herein, but one of ordinary skill in the art may recognize applications of other processes and/or use of other materials.
As shown in fig. 1, the present application provides a method for preparing organically modified barium titanate nanoparticles, including the following steps S1) -S6).
S1) adding barium hydroxide octahydrate into deionized water, and uniformly stirring to obtain a barium hydroxide solution.
S2) adding tetrabutyl titanate into an ethanol solvent, and uniformly stirring to obtain a tetrabutyl titanate solution.
S3) adding the barium hydroxide solution into the tetrabutyl titanate solution to obtain a first mixed solution, wherein the molar ratio of titanium ions to barium ions is 1: 1.
S4) adding a sodium hydroxide solution and an organic matter into the first mixed solution to obtain a second mixed solution, wherein the organic matter contains carbon-hydrogen bonds and carbon-oxygen bonds. In this embodiment, the carbon-oxygen bond of the organic substance may be carbon-oxygenThe single bond may be a carbon-oxygen double bond. The organic matter is acrylic acid series, COOH- (CH)2) n-COOH series, HS- (CH)2) n-SH series, HS- (CH)2) n-COOH, wherein n is 1. ltoreq.n < 20.
S5) sealing the second mixed solution in a high-pressure reaction kettle.
S6) carrying out high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution to obtain the organic modified barium titanate nano-particles.
As shown in fig. 2, the present application also provides a method for manufacturing a quantum dot optical film, including the following steps S101) to S103).
S101) providing the organically modified barium titanate nanoparticles prepared by the preparation method of the organically modified barium titanate nanoparticles.
S102) preparing a blend, wherein the blend comprises the following components in percentage by mass: 2-10 wt% of the organic modified barium titanate nano-particles, 0.9-1.5 wt% of the quantum dots and the balance of glue.
S103) coating the mixture on a substrate, and curing to form the quantum dot optical film.
The application provides an organic modified barium titanate nano-particle, mainly be at the in-process of preparing organic modified barium titanate nano-particle, add the organic matter, can make organic modified barium titanate nano-particle's appearance controllable, the particle diameter is adjustable, and its crystal structure is perovskite type structure, and it possesses the high refractive index simultaneously, possesses good scattering ability promptly. Therefore, in the process of preparing the quantum dot optical film, after the organic modified barium titanate nano-particles and the quantum dots are doped, the dosage of the quantum dots can be reduced, the utilization rate of blue light can be improved, and the absorption of the blue light is increased. The quantum dots contain heavy metal elements which are harmful to the environment and human bodies, so that the production cost can be saved by reducing the dosage of the quantum dots, and meanwhile, the displayed dosage is also reduced.
The following organic substances are acrylic acid series, COOH- (CH)2) n-COOH series, HS- (CH)2) n-SH series, HS- (CH)2) The n-COOH series is illustrated.
Example 1
This example provides a method for preparing organically modified barium titanate nanoparticles, including the following steps S11) -S18). The organic material is an acrylic acid series, the acrylic acid series includes any one of methacrylic acid and sodium polymethacrylate, and the present embodiment will be described in detail by taking methacrylic acid as an example.
S11) adding 200.0mg of barium hydroxide octahydrate into 15mL of deionized water, and uniformly stirring to obtain a barium hydroxide solution. Specifically, the barium hydroxide octahydrate is added into ionized water at the temperature of 50-100 ℃, and the mixture is uniformly stirred to obtain a barium hydroxide solution.
S12) adding 215.8mg of tetrabutyl titanate into 15mL of an ethanol solvent, and stirring uniformly to obtain a tetrabutyl titanate solution. In this example, the ethanol solvent was added to prevent the tetrabutyl titanate from being directly hydrolyzed in the air, and the operation was performed in a glove box under an inert gas atmosphere.
S13) adding the barium hydroxide solution into the tetrabutyl titanate solution to obtain a first mixed solution. Wherein the first mixed solution is a barium titanate solution. In the barium titanate solution, the molar ratio of titanium ions to barium ions is 1:1, so that the titanium ions in the tetrabutyl titanate solution and the barium ions in the barium hydroxide solution can be sufficiently reacted, and free titanium ions or barium ions are prevented from remaining in the first mixed solution.
S14) adding 1mol/L sodium hydroxide solution and 100mg methacrylic acid into the first mixed solution to obtain a second mixed solution, wherein the methacrylic acid contains carbon-hydrogen bonds and carbon-oxygen bonds. In this embodiment, the sodium hydroxide solution is added to adjust the PH of the first mixed solution to 9 to 14, where the sodium hydroxide solution is an alkaline solution, and in this embodiment, other alkaline solutions may also be used instead of the sodium hydroxide solution, such as ammonia water. In this embodiment, the sodium methacrylate is added to modify the first mixed solution to serve as an organic group of the barium titanate solution, thereby preventing the barium titanate solution from precipitating in the organic solvent and improving the dispersibility of the barium titanate solution in the organic solvent.
S15) sealing the second mixed solution in a high-pressure reaction kettle.
S16) carrying out high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution to obtain the organic modified barium titanate nano-particles. Specifically, the high-pressure reaction kettle is placed in an oven, the second mixed solution is subjected to high-temperature treatment for 10-30 hours at the temperature of 150-300 ℃, and after cooling to room temperature, centrifugal separation and purification treatment are carried out to obtain powdery organic modified barium titanate nanoparticles. And washing the organic modified barium titanate nanoparticles after cooling by adopting an ethanol solution to obtain purified organic modified barium titanate nanoparticles.
The embodiment provides a preparation method of an organic modified barium titanate nanoparticle, which is characterized in that organic methacrylic acid is adopted to modify the barium titanate nanoparticle to obtain the organic modified barium titanate nanoparticle, the preparation method of the organic modified barium titanate nanoparticle is simple, the morphology is controllable, the particle size is adjustable, the crystal structure of the organic modified barium titanate nanoparticle is a perovskite structure, and meanwhile, the organic modified barium titanate nanoparticle has a high refractive index which is greater than 2.4, namely, the organic modified barium titanate nanoparticle has good scattering ability. However, the barium titanate nanoparticles synthesized by the traditional method are not subjected to organic modification and are easy to precipitate in an organic solvent. Therefore, the organic group is modified on the surface of the barium titanate nano-particle by the organic modified barium titanate nano-particle prepared by the method, the dispersibility of the barium titanate nano-particle in an organic solvent is improved, and the film forming effect of the barium titanate nano-particle in glue is improved. In addition, organic matters are added into the barium titanate solution to modify the barium titanate, so that secondary experiments are avoided, and the production cost is saved.
The present embodiment also provides a method for producing a quantum dot optical film including the following steps S111) to S113).
S111) providing the organically modified barium titanate nanoparticles.
S112) preparing a blend, wherein the blend comprises the following components in percentage by mass: 2-10 wt% of the organic modified barium titanate nano-particles, 0.9-1.5 wt% of the quantum dots and the balance of glue. Specifically, the organic modified barium titanate nanoparticles, the quantum dots and the glue are mixed and stirred to obtain the blend. The organic modified barium titanate nano-particles are added, so that the dosage of the quantum dots can be reduced, and the compatibility of the quantum dots and glue is effectively improved.
S113) coating the mixture on a substrate, and curing to form the quantum dot optical film. Specifically, the blend is cured by ultraviolet irradiation or heating. In this embodiment, the quantum dots include silicon quantum dots, germanium quantum dots, cadmium sulfide quantum dots, cadmium selenide quantum dots, cadmium telluride quantum dots, zinc selenide quantum dots, lead sulfide quantum dots, lead selenide quantum dots, indium phosphide quantum dots, indium arsenide quantum dots, and CsPbBr3、CsPbI3Or CsPbCl3Or a mixture of at least two thereof. The thickness of the quantum dot optical film is 50-200 μm, preferably 120 μm, and when the quantum dot optical film is applied to a display panel, the display quality of the display panel can be effectively improved, and the display panel is light and thin.
The embodiment provides a method for preparing a quantum dot optical film, wherein organic modified barium titanate nanoparticles are used as scattering particles, and the organic modified barium titanate nanoparticles can enhance the brightness of the optical film, that is, after the quantum dots are doped with the organic modified barium titanate nanoparticles, the dosage of the quantum dots can be reduced, the utilization rate of blue light can be improved, and the absorption of the blue light is increased. However, the quantum dots contain heavy metal elements and are harmful to the environment and human bodies, so that the quantum dots can be used in the film in a reduced amount while the brightness of the quantum dot optical film is increased, and the production cost can be saved. In addition, the embodiment provides a preparation method of the quantum dot optical film, which is simple in synthesis method and suitable for industrial mass production.
Example 2
This example provides a method for preparing organically modified barium titanate nanoparticles and a method for preparing a quantum dot optical film, including most of the technical solutions of example 1, except that the organic substance is acrylic acid series and is replaced with COOH- (CH) —2) n-COOH series, said COOH- (CH)2) Any one of n-COOH series malonic acid, succinic acid, glutaric acid, azelaic acid and pimelic acid, and this embodiment will be described in detail with glutaric acid as an example.
Specifically, in the second mixed solution preparation step of the preparation method of the organically modified barium titanate nanoparticles, 1mol/L sodium hydroxide solution and 100mg glutaric acid are added to the first mixed solution to obtain a second mixed solution. Wherein the glutaric acid contains carbon-hydrogen bonds and carbon-oxygen bonds.
Example 3
This example provides a method for preparing organically modified barium titanate nanoparticles and a method for preparing a quantum dot optical film, including most of the technical solutions of example 1, except that the organic substance is an acrylic acid series and is replaced with HS- (CH)2) n-SH series, said HS- (CH)2) The n-SH series includes any one of 1, 2-ethanedithiol, 1, 3-propanedithiol, 1, 5-pentanethiol, and 1, 9-nonanedithiol, and this example will be described in detail with 1, 2-ethanedithiol as an example.
Specifically, in the second mixed solution preparation step of the preparation method of the organically modified barium titanate nanoparticles, 1mol/L sodium hydroxide solution and 1.0mL of 1, 2-ethanedithiol are added to the first mixed solution to obtain a second mixed solution. Wherein the 1, 2-ethanedithiol contains a carbon-hydrogen bond and a carbon-oxygen bond.
Example 4
This example provides a method for preparing organically modified barium titanate nanoparticles and a method for preparing a quantum dot optical film, including most of the technical solutions of example 1, except that the organic substance is an acrylic acid series and is replaced with HS- (CH)2) n-COOH series, said HS- (CH)2) The n-COOH series includes any one of mercaptopropionic acid and lipoic acid, and this example will be described in detail with mercaptopropionic acid as an example.
Specifically, in the second mixed solution preparation step of the preparation method of the organically modified barium titanate nanoparticles, 1mol/L sodium hydroxide solution and 1.0mL mercaptopropionic acid are added to the first mixed solution to obtain a second mixed solution. Wherein, the mercaptopropionic acid contains carbon-hydrogen bonds and carbon-oxygen bonds.
In summary, the present application provides a method for preparing organically modified barium titanate nanoparticles and a method for preparing a quantum dot optical film.
As shown in fig. 3, fig. 3 is a transmission electron microscope image of organically modified barium titanate nanoparticles, and the average particle size of the nanoparticles is about 78-85nm, preferably 81nm and 82nm, which is beneficial to enhancing scattering of blue light and improving utilization rate of blue light.
As shown in FIG. 4, FIG. 4 is a Fourier infrared (FT-IR) spectrum of barium titanate nanoparticles before modification at 2800 and 3000cm-1The characteristic absorption peak of the organic C-H bond is very weak, which indicates that the surface organic content of the nano-particles is low, 1453cm-1 is the characteristic absorption peak of Ba-Ti, and 614cm-1 is the characteristic absorption peak of Ti-O bond.
As shown in FIG. 5, FIG. 5 is a FT-IR spectrum of sodium methacrylate-modified barium titanate nanoparticles (2924 cm)-1Is a characteristic absorption peak of the C-H bond of sodium methacrylate. Compared with the barium titanate nanoparticles before modification, the nanoparticles are at 1078cm-1The characteristic peak of C-O bond appears at the position, so that the shape of the organic modified barium titanate nano particle can be controlled, the particle size can be adjusted, the crystal structure is a perovskite structure, and the organic modified barium titanate nano particle has high refractive index, namely good scattering capability.
As shown in FIG. 6, FIG. 6 is a FT-IR spectrum of sodium polymethacrylate-modified barium titanate nanoparticles (2893 cm)-1And 2972cm-1Is a characteristic absorption peak of a C-H bond, 1752cm-1Is a characteristic peak of C ═ O bond, 1089cm-1The characteristic peak of the C-O bond appears at the position, is derived from sodium polymethacrylate, can control the appearance and adjust the particle size of the organic modified barium titanate nano-particles, has a perovskite structure as a crystal structure, and has high refractive index, namely good scattering ability.
As shown in FIG. 7, FIG. 7 is an FT-IR spectrum of glutaric acid-modified barium titanate nanoparticles at 1752cm-1Is a characteristic peak of C ═ O bond, 1056cm-1The characteristic peak of C-O bond appears at the position, is derived from glutaric acid, and can ensure that the organically modified barium titanate is nanoThe shape of the particles is controllable, the particle size is adjustable, the crystal structure of the particles is a perovskite structure, and meanwhile, the particles have high refractive index, namely, good scattering capability.
Therefore, the application provides a preparation method of organic modified barium titanate nanoparticles and a preparation method of a quantum dot optical film, the organic modified barium titanate nanoparticles are used as scattering particles and applied to the quantum dot optical film, the barium titanate nanoparticles can play a role in enhancing the brightness of the film, namely after the quantum dots are doped with the scattering particles, the using amount of the quantum dots can be reduced, the utilization rate of blue light can be improved, the absorption of the quantum dots to the blue light is increased, more quantum dots are excited by the blue light, and the brightness and the fluorescence emission intensity of the optical film are increased. The quantum dots contain heavy metal elements which are harmful to the environment and human bodies, so that the production cost can be saved by reducing the dosage of the quantum dots, and meanwhile, the displayed dosage is also reduced.
As shown in table (1), table 1 is a comparison table of the conventional quantum dot optical film and the quantum dot optical film of the present application.
Watch (1)
As can be seen from Table (1), the luminance of the conventional quantum dot optical film was 1221cd/m2About, the quantum dot optical film of this application increases along with organic modified barium titanate nano-particle's quantity, the luminance of quantum dot optical film increases, and its dispersion effect is also preferred, and does not have obvious aggregation phenomenon. In the application, the mass percentage of the organically modified barium titanate nanoparticles is preferably 5 wt%, 5.5 wt%, 6.2 wt%, 6.8 wt% and 7.1 wt%, so that the subsequently formed quantum dot optical film has a good dispersion effect, and meanwhile, the waste of the nanoparticles is not caused, and the cost is saved.
As shown in fig. 8, fig. 8 is a PL (photoluminescence) spectrum of the quantum dot optical film without and with the organic modified barium titanate nanoparticles added. Wherein, the dotted line represents the PL spectrum of the quantum dot optical film without the added organic modified barium titanate nanoparticles, and the solid line represents the PL spectrum of the quantum dot optical film with the added organic modified barium titanate nanoparticles. As can be seen from the figure, the quantum dot optical film without the organic modified barium titanate nanoparticles has poor absorption capability on blue light (450nm), however, the quantum dot optical film with the organic modified barium titanate nanoparticles increases the absorption capability on blue light, and benefits from scattering particles with high refractive index to scatter blue light, so that the utilization rate of blue light is increased, more quantum dots are excited by blue light, and therefore, the intensity of a green light emission peak (530nm) is increased very obviously.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above detailed description is made on the preparation method of the organic modified barium titanate nanoparticle and the preparation method of the quantum dot optical film provided in the embodiments of the present application, and specific examples are applied herein to explain the principle and the implementation manner of the present application, and the description of the above embodiments is only used to help understanding the technical scheme and the core idea of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A preparation method of organic modified barium titanate nanoparticles is characterized by comprising the following steps:
adding barium hydroxide octahydrate into deionized water, and uniformly stirring to obtain a barium hydroxide solution;
adding tetrabutyl titanate into an ethanol solvent, and uniformly stirring to obtain a tetrabutyl titanate solution;
adding the barium hydroxide solution into the tetrabutyl titanate solution to obtain a first mixed solution;
adding a sodium hydroxide solution and an organic matter into the first mixed solution to obtain a second mixed solution, wherein the organic matter contains carbon-hydrogen bonds and carbon-oxygen bonds;
sealing the second mixed solution in a high-pressure reaction kettle; and
and carrying out high-temperature high-pressure reaction and centrifugal separation and purification treatment on the second mixed solution to obtain the organic modified barium titanate nano-particles.
2. The method for producing organically modified barium titanate nanoparticles according to claim 1,
the organic matter is acrylic acid series, COOH- (CH)2) n-COOH series, HS- (CH)2) n-SH series, HS- (CH)2) n-COOH, wherein n is 1. ltoreq.n < 20.
3. The method for producing organically modified barium titanate nanoparticles according to claim 2,
the acrylic acid series includes any one of methacrylic acid and sodium polymethacrylate.
4. The method for producing organically modified barium titanate nanoparticles according to claim 2,
the COOH- (CH)2) The n-COOH series includes any one of malonic acid, succinic acid, glutaric acid, azelaic acid, pimelic acid.
5. The method for producing organically modified barium titanate nanoparticles according to claim 2,
the HS- (CH)2) The n-SH series includes any one of 1, 2-ethanedithiol, 1, 3-propanedithiol, 1, 5-pentanedithiol, 1, 8-octanedithiol, and 1, 9-nonanedithiol.
6. The method for producing organically modified barium titanate nanoparticles according to claim 2,
the HS- (CH)2) The n-COOH series includes any one of mercaptopropionic acid and lipoic acid.
7. The method for producing organically modified barium titanate nanoparticles according to claim 1,
in the first mixed solution, the molar ratio of titanium ions to barium ions is 1: 1.
8. The method for producing organically modified barium titanate nanoparticles according to claim 1,
in the step of carrying out high-temperature high-pressure reaction and centrifugal separation purification treatment on the second mixed solution,
and (3) placing the high-pressure reaction kettle in an oven, carrying out high-temperature treatment on the second mixed solution for 10-30 hours at the temperature of 150-300 ℃, cooling to room temperature, and carrying out centrifugal separation and purification treatment to obtain powdery organic modified barium titanate nanoparticles.
9. A preparation method of a quantum dot optical film is characterized by comprising the following steps:
providing organically modified barium titanate nanoparticles prepared according to the method for preparing organically modified barium titanate nanoparticles of claim 1;
preparing a blend, wherein the blend comprises the following components in percentage by mass:
2-10 wt% of the organic modified barium titanate nano particles, 0.9-1.5 wt% of the quantum dots and glue; and
and coating the mixture on a substrate, and curing to form the quantum dot optical film.
10. The method of manufacturing a quantum dot optical film according to claim 9,
in the step of preparing the blend, mixing and stirring the organic modified barium titanate nanoparticles, the quantum dots and the glue to obtain the blend;
and in the step of coating the mixture on a substrate, curing the mixture by adopting an ultraviolet irradiation mode or a heating mode.
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