CN115418105A - Quantum dot-MOF composite color filter membrane and preparation method thereof - Google Patents

Quantum dot-MOF composite color filter membrane and preparation method thereof Download PDF

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CN115418105A
CN115418105A CN202211054757.XA CN202211054757A CN115418105A CN 115418105 A CN115418105 A CN 115418105A CN 202211054757 A CN202211054757 A CN 202211054757A CN 115418105 A CN115418105 A CN 115418105A
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mof
quantum dot
color filter
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王亮
黄宝健
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Jiangyin Jinshujian New Material Technology Co ltd
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
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    • 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
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    • C08J2387/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds

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Abstract

The invention discloses a preparation method of a quantum dot-MOF composite color filter membrane, which comprises the following steps: synthesizing quantum dots; modifying the surface of the quantum dot; synthesizing nano MOF; compounding the modified quantum dots and the MOF to form a solution containing the quantum dot-MOF composite material; adding a solution comprising a quantum dot-MOF composite material on a substrate; carrying out photo/thermal curing on the solution containing the quantum dot-MOF composite material on the substrate to form a prefabricated film; and carrying out light/heat treatment on the prefabricated film to form a color filter film. The invention realizes the effective transfer of excitation energy from MOF to quantum dots, and obviously improves the fluorescence efficiency of the quantum dots; the holes of the MOF material increase the steric hindrance between the quantum dots, thereby avoiding the possibility of quantum dot agglomeration and ion exchange and improving the stability of the quantum dots; the quantum dot-MOF color filter membrane provided by the invention has higher color purity and high blue light absorption coefficient, improves the color gamut of a liquid crystal display device and improves the light utilization rate of exciting light.

Description

Quantum dot-MOF composite color filter membrane and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a quantum dot-MOF composite color filter membrane and a preparation method thereof.
Background
In a Liquid Crystal Display (LCD), a Color Filter (CF) is an indispensable important part of a Display module for realizing Color rendering. Conventional color filters use pigmented photoresists to obtain the desired color by absorbing light at other wavelengths. However, the color filter film has low light utilization rate and low color purity (half-peak width > 50 nm), and cannot realize wide color gamut display.
Quantum Dots (QDs) as a novel semiconductor nanomaterial have the advantages of adjustable emission spectrum, narrow half-peak width, high fluorescence efficiency and the like, so that the Quantum Dots are widely applied to the field of liquid crystal display to effectively improve the color saturation and color gamut of a display, and are luminescent materials with great prospects in the future display market. However, quantum dots in the market are mainly in the form of optical films or diffusion plates in liquid crystal displays, and are not applied to color filter films on the upper layers of the liquid crystal displays. One of the main reasons is that the existing quantum dots have low light/heat stability and cannot meet the process requirements of the color filter film; secondly, the quantum dots with high fluorescence efficiency are usually dissolved in a non-polar solvent, and serious aggregation and light efficiency loss can occur when the quantum dots are directly added into a color filter film. Therefore, an effective quantum dot color filter film is urgently needed to solve the above technical problems, so as to realize the rapid development of the quantum dot color filter film in the liquid crystal display.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a quantum dot-MOF composite color filter membrane and a preparation method thereof. The prepared quantum dot-MOF composite color filter film has narrow half-peak width, high fluorescence yield and good stability, and is beneficial to realizing the mass production of the liquid crystal display panel of the quantum dot color filter.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the quantum dot-MOF composite color filter membrane comprises the following steps: s1, synthesizing quantum dots; s2, carrying out surface modification on the quantum dots by using a surface modifier; s3, synthesizing nano MOF; s4, compounding the modified quantum dots and the MOF to form a solution containing the quantum dot-MOF composite material, and S5, adding the solution containing the quantum dot-MOF composite material on the substrate; s6, carrying out photo/thermal curing on the solution containing the quantum dot-MOF composite material on the substrate to form a prefabricated film; and S7, carrying out light/heat treatment on the prefabricated film to form a color filter film.
Preferably, the quantum dots include, but are not limited to, cdSe, cdZnSe, cdSe/ZnS, cdZnSe/ZnS, cdSe/ZnSe, cdZnSe/ZnSe, cdSe/ZnSe/ZnS, cdZnSe/ZnSe/ZnS, inP/ZnSe/ZnS, csPbBr 3 、CsPbCl 3 、CsPbI 3 、CsPb(Cl/Br) 3 、CsPb(Br/I) 3 Any one or more of;
the surface modifier comprises any one or more of oleylamine, oleic acid, C6-C20 alkyl thiol, triphenylphosphine oxide, trioctylphosphine oxide, mercapto polyethylene glycol fatty acid ester, mercapto polypropylene glycol fatty acid ester, mercapto polyglycerol fatty acid ester and mercapto-sorbitan fatty acid ester;
the nano MOF comprises any one or more of, but is not limited to, uiO-67, uiO-66, MOF-5, MOF-1 and MOF-74.
Preferably, the modified quantum dots are compounded with MOF by adding an initiator.
Preferably, the initiator includes, but is not limited to, any one or more of 2-hydroxy-2-methyl-1-phenyl acetone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester, 2-dimethylamino-2-benzyl 1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, methyl benzoylformate, 2,4-dihydroxybenzophenone, and diphenyl- (2,4,6-trimethylbenzoyl) oxyphosphorus.
Preferably, in the above technical solution, a solvent is added to the solution containing the quantum dot-MOF composite material, and the solvent includes, but is not limited to, dodecyl methacrylate, 2-methyl-2-adamantyl methacrylate, isobornyl methacrylate, tripropylene glycol diacrylate
The quantum dot-MOF composite color filter membrane is prepared by the preparation method.
The invention has the beneficial effects that:
1. according to the invention, the quantum dots are embedded into the holes of the MOF material, so that the effective transfer of excitation energy from the MOF to the quantum dots is realized, and the fluorescence efficiency of the quantum dots is obviously improved;
the holes of the MOF material increase the steric hindrance between the quantum dots, avoid the possibility of quantum dot agglomeration and ion exchange, and improve the stability (thermal stability, irradiation stability, humidity stability and the like) of the quantum dots;
3. the quantum dot-MOF color filter membrane provided by the invention has higher color purity and high blue light absorption coefficient, improves the color gamut of a liquid crystal display device and improves the light utilization rate of exciting light.
Drawings
FIG. 1 is a fluorescence emission spectrum of a quantum dot-MOF material prepared in example 1;
fig. 2 is a fluorescence emission spectrum of the color filter in comparative example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Preparation of cadmium selenide quantum dot-MOF nano composite material
1) Preparing cadmium selenide quantum dots:
adding 0.5mmoL of cadmium oxide, 2mL of oleic acid, 15mL of 1-octadecene and 1mmoL of zinc acetate into a three-neck flask, vacuumizing for 2 hours at 120 ℃ to remove water and oxygen, then heating to 290 ℃, quickly injecting 0.8mmoL of TOP-Se, keeping for 5, 30 and 60 minutes, cooling to room temperature, purifying products by using n-hexane and acetone, dissolving the precipitate into the n-hexane, and finishing the reaction to form red, green and blue cadmium selenide quantum dot hexane solutions;
2) Modification of quantum dots:
cadmium selenide quantum dots (1 mL) were exchanged with pyridine by reprecipitating and dispersing in pyridine (1 mL) with acetone and heating in a glass tube at 80 ℃ for 24 hours to complete the ligand exchange with pyridine. After the suspension became clear, the solution was cooled to room temperature, excess hexane was added to precipitate the quantum dots and redispersed in 1mL pyridine to a concentration of 100mg/mL as a quantum dot stock solution for subsequent experiments;
3) Synthesis of MOF-3:
0.16mmol of zinc acetate was dissolved in DMF (2 mL) and added rapidly to a solution of 2-aminoterephthalic acid (0.059 mmol) in DMF (3 mL) and the mixture was stirred at room temperature for 30 min. Centrifuging to collect the product, washing with DMF/ethanol for 3 times, and drying under reduced pressure to obtain MOF-3 white powder;
4) Preparation of quantum dot-MOF composite material:
powdered nanoscale MOF-3 was dispersed in DMF (5 mL) using sonication. Pyridine-capped cadmium selenide quantum dots (0.1 mL) were then rapidly injected into the above solvent with stirring. And stirring the suspension at room temperature for 5 minutes again, obtaining the quantum dot-MOF-3 by centrifugal separation, then adding dodecyl triethoxysilane, a BYK-361N flatting agent and a BYK-1790 defoaming agent, and completely dissolving to obtain the quantum dot-MOF composite material solution.
Example 2
1) Preparing the indium phosphide quantum dots:
adding 5mL of indium tetradecanoate and 10mL of 1-octadecene into a three-neck flask, vacuumizing at 120 ℃ for 2 hours to remove water and oxygen, then cooling to room temperature, adding 0.1mmol of tris (trimethylsilyl) phosphine, heating to 290 ℃ and keeping for 1, 15 and 40 minutes, then cooling to room temperature, purifying a product by using n-hexane and acetone, dissolving a precipitate in the n-hexane, and finishing the reaction to form red, green and blue indium phosphide quantum dot hexane solutions;
2) Modification of quantum dots:
indium phosphide quantum dots (1 mL) were heated in a glass tube at 80 ℃ for 24 hours by reprecipitating and dispersing in pyridine (1 mL) with acetone to complete the exchange of the ligand with pyridine. After the suspension became clear, the solution was cooled to room temperature, excess hexane was added to precipitate the quantum dots and redispersed in 1mL pyridine to a concentration of 100mg/mL as a quantum dot stock solution for subsequent experiments;
3) The preparation of the MOF and quantum dot-MOF composite material is the same as the 3) 4) step of the example 1.
Example 3
Preparation of perovskite quantum dot-MOF nano composite material
1) Preparing perovskite quantum dots:
0.75mmol formamidine acetate, 0.2mmol lead acetate trihydrate, 2mL oleic acid, 0.6mmol oleylamine halide (blue-oleylamine chloride, green-oleylamine bromide, red-oleylamine iodide), and 8mL n-octane were mixed in a 50mL beaker. And then placing the beaker and the mixed solution under a high-energy ultrasonic column, carrying out reaction in an atmospheric environment, and detecting the reaction temperature of the solution in real time by using a temperature detector carried by the instrument. The obtained product is centrifugally purified twice by ethyl acetate to remove unreacted precursors and impurities. The resulting precipitate was finally dispersed in n-hexane solvent.
2) Modification of perovskite quantum dots:
perovskite quantum dots (1 mL) were prepared by reprecipitating and dispersing in pyridine (1 mL) with ethyl acetate and heating in a glass tube at 50 ℃ for 48 hours to complete the ligand exchange with pyridine. After the suspension became clear, the solution was cooled to room temperature, excess ethyl acetate was added to precipitate the quantum dots and redispersed in 1mL pyridine to a concentration of 100mg/mL as a quantum dot stock solution for subsequent experiments;
3) The preparation of the MOF and quantum dot-MOF composite material is the same as the 3) 4) step of the example 1.
Comparative example 1
Just like the first two steps of the step of the embodiment 2, the preparation of the indium phosphide quantum dots is carried out, and the quantum dots are directly added into the color filter coating.
Preparing a quantum dot color light filtering film:
1) The glass substrate is provided with a plurality of pixel isolation structures, and the obtained quantum dot composite material solution is printed on the glass substrate in an ink-jet mode;
2) Ultraviolet light with 365nm wavelength is adopted at 2000mJ/cm 2 UV curing at an intensity of (1) for 10 minutes to form a prefabricated film;
3) And (3) heating the prefabricated film for 40 minutes at the heating temperature of 80 ℃, and drying to obtain the quantum dot light filter film.
The color filters obtained in examples 1 to 3 and comparative example 1 were subjected to performance testing, and the test data are shown in the following table:
quantum yield Quantum yield after 100 hours at 95 DEG C 95% humidity, quantum yield after 100 hours
Example 1 92％ 90％ 92％
Example 2 85％ 80％ 82％
Example 3 97％ 85％ 87％
Comparative example 1 86％ 44％ 51％
The fluorescence emission spectrum of the quantum dot-MOF material prepared in example 1 is shown in fig. 1. It can be seen that the quantum dots still have high fluorescence properties after being compounded with MOFs. The fluorescence emission spectrum of the color filter in comparative example 1 is shown in fig. 2. The comparison can show that the quantum dot film has poor stability and serious fluorescence intensity attenuation without the existence of MOF.
Having described preferred embodiments of the present invention in detail, it is to be understood that modifications and variations may be resorted to without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. The preparation method of the quantum dot-MOF composite color filter membrane is characterized by comprising the following steps of: s1, synthesizing quantum dots; s2, carrying out surface modification on the quantum dots by using a surface modifier; s3, synthesizing nano MOF; s4, compounding the modified quantum dots and the MOF to form a solution containing the quantum dot-MOF composite material, and S5, adding the solution containing the quantum dot-MOF composite material on the substrate; s6, carrying out photo/thermal curing on the solution containing the quantum dot-MOF composite material on the substrate to form a prefabricated film; and S7, carrying out light/heat treatment on the prefabricated film to form a color filter film.
2. The method for preparing the quantum dot-MOF composite color filter film according to claim 1, the quantum dots include, but are not limited to, cdSe, cdZnSe, cdSe/ZnS, cdZnSe/ZnS, cdSe/ZnSe, cdZnSe/ZnSe, cdSe/ZnSe/ZnS, cdZnSe/ZnSe/ZnS, inP/ZnSe/ZnS, csPbBr 3 、CsPbCl 3 、CsPbI 3 、CsPb(Cl/Br) 3 、CsPb(Br/I) 3 Any one or more of;
the surface modifier comprises any one or more of oleylamine, oleic acid, C6-C20 alkyl thiol, triphenylphosphine oxide, trioctylphosphine oxide, mercapto polyethylene glycol fatty acid ester, mercapto polypropylene glycol fatty acid ester, mercapto polyglycerol fatty acid ester and mercapto-sorbitan fatty acid ester;
the nano MOF comprises any one or more of, but is not limited to, uiO-67, uiO-66, MOF-5, MOF-1 and MOF-74.
3. The method for preparing the quantum dot-MOF composite color filter membrane as claimed in claim 2, wherein an initiator is added into the modified quantum dots, and then the modified quantum dots are compounded with MOF.
4. The method for preparing a quantum dot-MOF composite color filter according to claim 3, wherein the initiator comprises any one or more of but not limited to 2-hydroxy-2-methyl-1-phenyl acetone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone, 2,4,6-trimethylbenzoylphenyl phosphonic acid ethyl ester, 2-dimethylamino-2-benzyl 1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, methyl benzoylformate, 2,4-dihydroxybenzophenone, diphenyl- (2,4,6-trimethylbenzoyl) oxyphosphor.
5. The method for preparing a quantum dot-MOF composite color filter film according to claim 4, wherein a solvent is added to the solution containing the quantum dot-MOF composite material, and the solvent includes but is not limited to dodecyl methacrylate, 2-methyl-2-adamantyl methacrylate, isobornyl methacrylate, tripropylene glycol diacrylate.
6. A quantum dot-MOF composite color filter film, characterized by being prepared by the preparation method in claim 4 or 5.
CN202211054757.XA 2022-08-31 2022-08-31 Quantum dot-MOF composite color filter membrane and preparation method thereof Pending CN115418105A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108774511A (en) * 2018-05-31 2018-11-09 兰州大学 The preparation of full-inorganic perovskite quantum dot/mesoporous MOF-5 composite luminescent materials and application in the led
CN111607234A (en) * 2020-06-15 2020-09-01 Tcl华星光电技术有限公司 Quantum dot composition and preparation method thereof, quantum dot patterning method and patterned quantum dot solid film
CN112143287A (en) * 2020-09-22 2020-12-29 苏州星烁纳米科技有限公司 Quantum dot ink, color filter film, display device and preparation method of color filter film
WO2021258690A1 (en) * 2020-06-24 2021-12-30 Tcl科技集团股份有限公司 Quantum dot material and preparation method, and quantum dot light-emitting diode and preparation method
CN114316970A (en) * 2021-12-30 2022-04-12 宁波东旭成新材料科技有限公司 Preparation method of quantum dot film
CN114958154A (en) * 2022-04-28 2022-08-30 阳明量子科技(深圳)有限公司 Preparation method of green-light perovskite quantum dot optical film

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108774511A (en) * 2018-05-31 2018-11-09 兰州大学 The preparation of full-inorganic perovskite quantum dot/mesoporous MOF-5 composite luminescent materials and application in the led
CN111607234A (en) * 2020-06-15 2020-09-01 Tcl华星光电技术有限公司 Quantum dot composition and preparation method thereof, quantum dot patterning method and patterned quantum dot solid film
WO2021258690A1 (en) * 2020-06-24 2021-12-30 Tcl科技集团股份有限公司 Quantum dot material and preparation method, and quantum dot light-emitting diode and preparation method
CN112143287A (en) * 2020-09-22 2020-12-29 苏州星烁纳米科技有限公司 Quantum dot ink, color filter film, display device and preparation method of color filter film
CN114316970A (en) * 2021-12-30 2022-04-12 宁波东旭成新材料科技有限公司 Preparation method of quantum dot film
CN114958154A (en) * 2022-04-28 2022-08-30 阳明量子科技(深圳)有限公司 Preparation method of green-light perovskite quantum dot optical film

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Application publication date: 20221202