CN107382744B - Perovskite quantum dot film, preparation method thereof, backlight module and display device - Google Patents
Perovskite quantum dot film, preparation method thereof, backlight module and display device Download PDFInfo
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- CN107382744B CN107382744B CN201710537400.XA CN201710537400A CN107382744B CN 107382744 B CN107382744 B CN 107382744B CN 201710537400 A CN201710537400 A CN 201710537400A CN 107382744 B CN107382744 B CN 107382744B
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- 238000006243 chemical reaction Methods 0.000 claims description 7
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C211/00—Compounds containing amino groups bound to a carbon skeleton
- C07C211/01—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms
- C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C211/03—Monoamines
- C07C211/04—Mono-, di- or tri-methylamine
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/1336—Illuminating devices
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/1336—Illuminating devices
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Abstract
The invention discloses a perovskite quantum dot film, a preparation method thereof and a backlight module, and belongs to the field of liquid crystal display backlight modules. The quantum dot film includes: perovskite quantum dots and polyamidoamine dendrimer; the perovskite quantum dots are dispersed in gaps formed by side groups of the polyamidoamine dendrimer. The preparation method comprises the following steps: adding perovskite quantum dot perovskite quantum dots into a polyamidoamine dendrimer solution to obtain a mixed solution, coating the mixed solution on a substrate, and curing to obtain a cured film, thereby obtaining the perovskite quantum dot film. The backlight module includes: perovskite quantum dot membrane, structural component and backlight and reflector plate. According to the invention, the perovskite quantum dots are dispersed by using the side group structure of the polyamidoamine dendrimer, and the side group of the polyamidoamine dendrimer plays a role in separating and fixing the perovskite quantum dots, so that the agglomeration or overlapping among the perovskite quantum dots is reduced.
Description
Technical Field
The invention relates to the field of liquid crystal display backlight modules, in particular to a perovskite quantum dot film and a preparation method thereof, a backlight module and a display device.
Background
The backlight module of the liquid crystal display is characterized in that a light source with sufficient brightness and uniform distribution is supplied, so that the backlight module can normally display images, luminescent materials (such as fluorescent powder) can be added into the backlight module to be used as a component in the backlight module, when the perovskite quantum dot film is irradiated by monochromatic light of the light source such as a light emitting diode in the backlight module, different fluorescent powder can emit light with different colors due to photoluminescence, the light with different colors can form white light after being mixed, and a color image obtained after the filtering treatment of a color filter has good color development, so that the color gamut expression of the liquid crystal display can be improved, and the color is more vivid. As a novel luminescent material, the perovskite quantum dot film has photoluminescence performance and feasibility of being applied to a backlight module.
The perovskite quantum dot is a quasi-zero-dimensional perovskite nano material, can be understood as perovskite with three dimensions below 100 nanometers, and the perovskite is a molecular general formula ABX3In which A is usually an organic cation (e.g. CH) in the organic-inorganic perovskite3NH3 +) B is typically a divalent metal cation (e.g., Pb)2+) X is typically a halide anion (e.g., Cl)-). At present, the perovskite quantum dot film is prepared as follows to prepare CH3NH3PbBr3For quantum dots as an example, first, a predetermined molar ratio of methyl ammonium bromide CH is used as a raw material3NH3Br, lead bromide PbBr2Dissolving a surface modifier (e.g., octylamine) in Dimethylformamide (DMF) to form a precursor solution, dropping a predetermined amount of the precursor solution into toluene and stirring, spin-coating the resulting solution on a substrate, and drying to obtain CH3NH3PbBr3The quantum dot film can be prepared into perovskite quantum dot films emitting different colors after photoluminescence by changing raw materials and the same preparation method.
In the process of implementing the invention, the inventor finds that the prior art has at least the following problems:
in the above method of forming the quantum dots into a solution first and then coating and drying, when the content of the quantum dots is high, the quantum dots are easily agglomerated in the solution, causing the quantum dots to exist in an agglomerated state in the quantum dot film after forming into the quantum dot film, thereby blocking absorption of excitation light among the quantum dots, and finally resulting in low fluorescence quantum efficiency.
Disclosure of Invention
In order to solve the above problems in the prior art, embodiments of the present invention provide a perovskite quantum dot film, a preparation method and an application thereof. The technical scheme is as follows:
in a first aspect, the present invention provides a perovskite quantum dot film, the quantum dot film comprising: perovskite quantum dots and polyamidoamine dendrimer;
the perovskite quantum dots are dispersed in gaps formed by the side groups of the polyamidoamine dendrimer.
Preferably, the polyamidoamine dendrimer is obtained by reacting a diamine monomer and an unsaturated ester.
Preferably, the pendant groups of the polyamidoamine dendrimer form a gap of width of 2-8 nm.
Preferably, the perovskite quantum dots comprise at least one of green perovskite quantum dots, red perovskite quantum dots and blue perovskite quantum dots, and the green perovskite quantum dots, the red perovskite quantum dots and the blue perovskite quantum dots are respectively CH3NH3PbBr3、CH3NH3PbBr1.5I1.5And CH3NH3PbBrCl2。
In a second aspect, the present invention provides a method for preparing a perovskite quantum dot film, the method comprising:
and 2, coating the mixed solution on a polyethylene terephthalate substrate for curing to obtain a cured film, and taking down the cured film from the polyethylene terephthalate substrate to obtain the perovskite quantum dot film.
Preferably, the polyamidoamine dendrimer solution in the step 1 is prepared by the following method:
adding unsaturated ester monomer into diamine monomer for addition reaction;
adding diamine monomers into the product of the addition reaction for substitution reaction to obtain a 1-generation polyamidoamine dendrimer;
repeatedly adding the unsaturated ester monomer and the diamine monomer into the 1-generation polyamidoamine dendrimer for N-1 times to obtain the N-generation polyamidoamine dendrimer, wherein N is an integer greater than or equal to 2;
adding monoamine to terminate the reaction, and obtaining the polyamidoamine dendrimer of which the width of the gap formed by the side group is in a preset range.
Specifically, the diamine monomer comprises: one of octadecyl diamine, ethylene diamine, butanediamine, p-phenylenediamine and naphthalene diamine, and the unsaturated ester monomer comprises 3-butyl phenylacrylate.
Preferably, said N is 6.
Preferably, the green perovskite quantum dot, the red perovskite quantum dot and the blue perovskite quantum dot are respectively prepared by the following methods:
mixing and dissolving organic amine salt and lead bromide in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the green-light perovskite quantum dot;
mixing and dissolving organic amine salt, lead bromide and lead iodide in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the red-light perovskite quantum dots;
and mixing and dissolving organic amine salt, lead bromide and lead chloride in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the blue-light perovskite quantum dot.
Preferably, the organic ammonium salt is methyl ammonium bromide.
Preferably, the methyl amine bromide is mixed with the lead bromide in a molar ratio of 3:1-2, the methyl amine bromide is mixed with the lead bromide and the lead iodide in a molar ratio of (2-3):1:1, and the methyl amine bromide is mixed with the lead bromide and the lead chloride in a molar ratio of (3-4):2: 1.
Preferably, the organic solvent is a dimethylformamide solution.
Preferably, the dimethyl phthalein amine solution accounts for 80% by volume.
Preferably, the surface modifying agents are oleylamine and octylamine.
Preferably, the toluene is added, specifically, under the condition of 70 ℃ water bath, the toluene is added until the system is irradiated by ultraviolet light and the exciting light is a constant value.
In a third aspect, the present invention provides a backlight module, which includes the above perovskite quantum dot film, a structural component, a backlight and a reflector plate.
In a fourth aspect, the present invention provides a display device, which includes the backlight module provided in the third aspect.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
according to the perovskite quantum dot film provided by the embodiment of the invention, perovskite quantum dots are dispersed by utilizing a side group structure of the polyamidoamine dendrimer, the side group of the polyamidoamine dendrimer plays a role in separating and fixing the perovskite quantum dots, and the perovskite quantum dots are regularly dispersed in gaps formed by the side group of the polyamidoamine dendrimer, so that the uniformity and consistency of the perovskite quantum dot distribution are improved, and the phenomenon of agglomeration or overlapping easily occurring among the perovskite quantum dots is avoided.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a backlight module with a perovskite quantum dot film added according to embodiment 2 of the present invention;
FIG. 2 is a photoluminescence spectrum provided in characterization example 3 of the present invention.
Wherein the drawings are described as follows: 1. a structural component; 2. a perovskite quantum dot film; 3. a backlight and a reflector plate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
In a first aspect, embodiments of the present invention provide a perovskite quantum dot film, the quantum dot film comprising: perovskite quantum dots and polyamidoamine dendrimer;
the perovskite quantum dots are dispersed in gaps formed by the side groups of the polyamidoamine dendrimer.
According to the perovskite quantum dot film provided by the embodiment of the invention, perovskite quantum dots are dispersed by utilizing a side group structure of the polyamidoamine dendrimer, the side group of the polyamidoamine dendrimer plays a role in separating and fixing the perovskite quantum dots, and the perovskite quantum dots are regularly dispersed in gaps formed by the side group of the polyamidoamine dendrimer, so that the uniformity and consistency of the distribution of the perovskite quantum dots are improved, the phenomenon of agglomeration or overlapping which is easy to occur among the perovskite quantum dots is avoided, meanwhile, the mutual influence of light absorption of the perovskite quantum dots with different colors can be reduced, and the fluorescence quantum efficiency of the perovskite quantum dot film is improved.
The quantum dots emit light at a full angle of 360 ° upon light excitation, and the wavelength of light absorbed by the quantum dots is shorter than that of light emitted by the quantum dots, so that the quantum dots of one color may absorb light emitted by the quantum dots of another color, which may cause loss of light inside the perovskite quantum dot film material, resulting in low fluorescence quantum efficiency. The embodiment of the invention improves the uniformity and consistency of the distribution of the perovskite quantum dots, and when the perovskite quantum dots with different colors exist in the perovskite quantum dot film provided by the embodiment of the invention, the mutual influence of the absorbed lights of the quantum dots with different colors can be reduced, and the fluorescence quantum efficiency of the perovskite quantum dot film is improved. In addition, the perovskite quantum dot film provided by the embodiment of the invention wraps perovskite quantum dots which have large specific surface areas and are easy to oxidize by using polyamidoamine dendrimer, so that the perovskite quantum dots are prevented from being oxidized.
Further, the polyamidoamine dendrimer is obtained by reacting diamine monomers and unsaturated esters. The polyamidoamine dendrimer is characterized in that a diamine monomer is used as an initiation core to perform addition reaction with unsaturated ester to form a short-chain side group, an ester group functional group on the short-chain side group is used as a basis to perform chain growth reaction with the diamine monomer to grow the short-chain side group, and the polyamidoamine dendrimer can be obtained after multiple reactions. The diamine monomer comprises one of octadecyl diamine, ethylenediamine, butanediamine, p-phenylenediamine and naphthalene diamine, and the unsaturated ester monomer comprises 3-butyl phenylacrylate.
The width of the gap formed by the side group of the polyamidoamine dendrimer is 2-8nm, and is preferably 4.4 nm. The uniformity and consistency of the perovskite quantum dot distribution are ensured through the limitation of the gap width.
The perovskite quantum dot comprises CH3NH3PbBr3Quantum dot, CH3NH3PbBr1.5I1.5Quantum dots and CH3NH3PbBrCl2At least one of quantum dots. The general molecular formula of the perovskite quantum dot is ABX3Wherein A in the organic-inorganic perovskite is usually an organic cation (e.g. CH)3NH3 +) B is typically a divalent metal cation (e.g., Pb)2+) X is typically a halide anion (e.g., Cl)-). Different perovskite quantum dot films emit light with different colors due to photoluminescence after being irradiated by a light-emitting diode, and the principle is that the forbidden bandwidth of the organic-inorganic perovskite quantum dot can be controlled by controlling the proportion of halogen atoms X, so that the light-emitting wavelength of the organic-inorganic perovskite quantum dot is regulated and controlled. With CH3NH3PbBr3Quantum dot based, Cl-The increase of the components enables the forbidden bandwidth of the organic-inorganic perovskite quantum dot to be increased and the luminescent peak position to be blue-shifted; i is-The increase of the components can reduce the forbidden bandwidth of the organic-inorganic perovskite quantum dots and red shift the luminescence peak position. Perovskite quantum dot CH described above3NH3PbBr3、CH3NH3PbBr1.5I1.5And CH3NH3PbBrCl2Under the excitation of ultraviolet light, green light, red light and blue light are respectively emitted.
In a second aspect, an embodiment of the present invention provides a method for preparing a perovskite quantum dot film, where the method includes:
and 2, coating the mixed solution on a polyethylene terephthalate substrate for curing to obtain a cured film, and taking down the cured film from the polyethylene terephthalate substrate to obtain the perovskite quantum dot film.
According to the preparation method, the perovskite quantum dots are added into the polyamidoamine dendrimer solution, the perovskite quantum dots are regularly dispersed in gaps formed by the side groups of the polyamidoamine dendrimer, the uniformity and consistency of the perovskite quantum dots are high, and the phenomenon that the perovskite quantum dots are easy to agglomerate or overlap is avoided.
Specifically, when preparing a monochromatic perovskite quantum dot film, green light or red light or blue light perovskite quantum dots are added into a solution of polyamidoamine dendrimer, so that the perovskite quantum dots are regularly dispersed in gaps formed by side groups of the polyamidoamine dendrimer.
When preparing a green light and red light bicolor perovskite quantum dot film, respectively adding green light perovskite quantum dots and red light perovskite quantum dots into 2 parts of polyamidoamine dendrimer solution to obtain a mixed solution, and then mixing the 2 parts of solution to obtain a mixed solution; and then send out the light of different colours through photoluminescence, the light of different colours forms white light after mixing, can be applied to backlight unit with the bicolor perovskite quantum dot membrane that obtains.
When preparing green light, red light and blue light bicolor perovskite quantum dot films, respectively adding green light perovskite quantum dots, red light perovskite quantum dots and blue light perovskite quantum dots into 3 parts of polyamidoamine dendrimer solution to obtain mixed solution, and then mixing the 3 parts of solution to obtain mixed solution; and then send out the light of different colours through photoluminescence, the light of different colours forms white light after mixing, can be applied to backlight unit with the bicolor perovskite quantum dot membrane that obtains.
In the above-described preparation method, the polyamidoamine dendrimer solution in the step 1 is prepared by the following method:
adding unsaturated ester monomer into diamine monomer for addition reaction;
adding diamine monomers into the product of the addition reaction for substitution reaction to obtain a 1-generation polyamidoamine dendrimer;
repeatedly adding the unsaturated ester monomer and the diamine monomer into the 1-generation polyamidoamine dendrimer for N-1 times to obtain the N-generation polyamidoamine dendrimer, wherein N is an integer greater than or equal to 2;
adding excessive monoamine to terminate the reaction, and obtaining the polyamidoamine dendrimer of which the width of the gap formed by the side group is in a preset range. The monoamine may be a long-chain alkylamine, and for example, the monoamine may be a monoamine having an even number of carbon atoms in hexa-to octadecylamine.
Specifically, before adding an unsaturated ester monomer into a diamine monomer for addition reaction, heating the diamine monomer at 70-80 ℃, wherein the diamine monomer comprises: one of octadecyl diamine, ethylene diamine, butanediamine, p-phenylenediamine and naphthalene diamine, and the unsaturated ester monomer comprises 3-butyl phenyl acrylate and methyl acrylate. Through Michelal addition reaction of unsaturated ester monomers and diamine monomers, the diamine monomers are preferably long-chain diamine monomers, such as octa-to-octadecyl diamine, can be used as a warp-wise template chain of a polyamide-amine dendrimer, and a side group is formed on the basis of the template chain, so that the uniformity and consistency of the distribution of perovskite quantum dots can be improved. Adding excessive diamine monomer into the product of the addition reaction to carry out substitution reaction to obtain alcohol and 1-generation polyamidoamine dendrimer, and then repeatedly adding unsaturated ester monomer N-1 times to carry out addition reaction and repeatedly adding diamine monomer N-1 times to carry out substitution reaction, wherein the unsaturated ester monomer is preferably unsaturated ester containing benzene ring or naphthalene ring, such as naphthalene diamine, p-phenylenediamine and the like, and can be used as a latitudinal template chain of the polyamidoamine dendrimer to keep the structural rigidity and macroscopic compactness of the polyamidoamine dendrimer. Preferably, N is 6, to obtain a 6-generation polyamidoamine dendrimer.
In addition, a small amount of unsaturated polyester may be added during the addition reaction of the unsaturated ester monomer to the diamine monomer to prevent the formation of impurities due to the amidation reaction. Wherein, the unsaturated polyester can be obtained by condensation of dibasic acid and dihydric alcohol, and the dibasic acid can be phthalic acid and adipic acid. The diacid, when used, may be in the form of an anhydride, such as phthalic anhydride, adipic anhydride. The dihydric alcohol can be propylene glycol or diethylene glycol.
In the preparation method, the green perovskite quantum dot, the red perovskite quantum dot and the blue perovskite quantum dot are respectively prepared by the following methods:
mixing and dissolving organic amine salt and lead bromide in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the green-light perovskite quantum dot;
mixing and dissolving organic amine salt, lead bromide and lead iodide in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the red-light perovskite quantum dots;
and mixing and dissolving organic amine salt, lead bromide and lead chloride in an organic solvent, adding the dissolved solution into a polyamidoamine dendrimer solution, adding a surface modifier, and adding toluene to obtain the blue-light perovskite quantum dot.
Specifically, the organic ammonium salt is methyl ammonium bromide. The methyl amine bromide and the lead bromide are mixed according to a molar ratio of 3:1-2, the methyl amine bromide, the lead bromide and the lead iodide are mixed according to a molar ratio of (2-3):1:1, and the methyl amine bromide, the lead bromide and the lead chloride are mixed according to a molar ratio of (3-4):2: 1. The organic solvent is a dimethylformamide solution. The dimethyl phthalide amine solution accounts for 80% of the volume fraction. The surface modifier is oleylamine and octylamine, and the molar ratio of the oleylamine to the octylamine is 1 (1-4). And adding toluene, namely adding toluene under the condition of 70 ℃ water bath until the system is irradiated by ultraviolet light to ensure that the exciting light is a constant value.
In the step 2, the mixed solution is coated on a polyethylene terephthalate substrate to be cured to obtain a cured film, and specifically, the mixed solution is evaporated to dryness to obtain the cured film under the conditions that the temperature is 70 ℃ and the negative pressure is 0.08 Mpa.
According to the preparation method, perovskite quantum dots are formed in situ in the polyamidoamine dendrimer solution with constant gap width formed by the side groups, and the perovskite quantum dots with fixed and uniform particle size can be obtained, namely the perovskite quantum dots are uniformly distributed in the gaps formed by the side groups of the polyamidoamine dendrimer.
In a third aspect, the embodiment of the present invention provides a backlight module, referring to fig. 1, which includes a perovskite quantum dot film 2, a structural component 1, and a backlight and reflector sheet 3.
Covering barrier layers on two sides of the perovskite quantum dot film, wherein the barrier layers are aluminum oxide layers or silicon oxide layers, and then adding the perovskite quantum dot film covered with the barrier layers into the backlight module.
The perovskite quantum dot film is high in color purity and strong in stability, and due to the fact that the phenomenon that agglomeration or overlapping easily occurs among perovskite quantum dots is avoided, the perovskite quantum dots with different colors can be prevented from absorbing mutual influence among light, loss of light in the material is reduced, and fluorescence quantum efficiency of the perovskite quantum dot film is high. The backlight module is suitable for being applied to the backlight module.
In a fourth aspect, an embodiment of the present invention provides a display device, including the backlight module provided in the third aspect.
The technical scheme of the invention is illustrated by specific preparation examples, application examples and characterization examples as follows:
in the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer. The raw materials are conventional products which can be obtained commercially by manufacturers and specifications.
Preparation of example 1
The embodiment provides a perovskite quantum dot film comprising three colors of red, green and blue, and the perovskite quantum dot film is prepared by the following method:
preparation of polyamidoamine dendrimers
Heating 0.1mol of octadecyldiamine to 73 ℃, then adding 0.095mol of 3-butyl phenylacrylate, and adding a small amount of poly (propylene glycol adipate);
adding 0.22mol of naphthalene diamine to obtain a 1-generation polyamidoamine dendrimer;
adding 0.1mol of 3-phenyl butyl acrylate into the 1 generation polyamidoamine dendrimer;
then 0.1mol of naphthalene diamine is added to obtain 2-generation polyamidoamine dendrimer;
repeatedly adding 0.1mol of 3-butyl phenylacrylate and 0.1mol of naphthalene diamine into the 2 generation polyamidoamine dendrimer for 4 times to obtain 6 generation polyamidoamine dendrimer;
finally, 0.05mol of octadecylamine is added to stop the reaction, and the concentration of 5X 10 is obtained-4The polyamide amine dendrimer is prepared from an ethanol solution of polyamide amine dendrimer in mol/L, and the width of a gap formed by the side group of the polyamide amine dendrimer is 4.4 nm.
Preparation of perovskite quantum dot film
a) Mixing methyl amine bromide and lead bromide in a molar ratio of 3:2, dissolving the mixture in a dimethylformamide solution, wherein the volume fraction of the dimethylformamide solution is 80%, adding the solution into the obtained polyamidoamine dendrimer solution, adding oleylamine and octylamine, wherein the total adding amount of the oleylamine and the octylamine is 0.02mol, the molar ratio of the oleylamine to the octylamine is 1:4, adding toluene under the condition of 70 ℃ water bath until the system color is green, and stopping adding the toluene when ultraviolet light irradiates an exciting light to be a constant value to obtain the polyamidoamine dendrimer solutionCH with the mass fraction of 0.85% in the solution3NH3PbBr3Quantum dots; the reason that the toluene is stopped being added when the exciting light is irradiated by the ultraviolet light to be a constant value is that a plurality of light-emitting peak values may appear when the exciting light is irradiated by the ultraviolet light in the initial stage of toluene dropping, the peak values are unified to be a constant peak value along with the reaction, and at the moment, the quantum dots are good in uniformity and the light-emitting peak values are stable;
b) mixing methyl amine bromide, lead bromide and lead iodide in a molar ratio of 2:1:1, adding toluene in a water bath at 70 ℃ in the same process until the system color is red, and stopping adding the toluene when ultraviolet light irradiates exciting light to be a constant value to obtain CH with the mass fraction of 0.45% formed in the polyamidoamine dendrimer solution3NH3PbBr1.5I1.5Quantum dots;
c) mixing methyl amine bromide, lead bromide and lead chloride in a molar ratio of 3:2:1, adding toluene in a water bath at 70 ℃ in the same process until the system color is blue, and stopping adding the toluene when ultraviolet light irradiates exciting light with a constant value to obtain the 1% CH by mass in the polyamidoamine dendrimer solution3NH3PbBrCl2Quantum dots;
d) forming the CH in the polyamidoamine dendrimer solution3NH3PbBr3Quantum dot, CH3NH3PbBr1.5I1.5Quantum dots and CH3NH3PbBrCl2The quantum dots are mixed in equal amount to obtain a mixed solution of the perovskite quantum dots and the polyamide amine;
e) and coating the mixed solution on a polyethylene glycol terephthalate substrate, evaporating the mixed solution to dryness under the conditions that the temperature is 70 ℃ and the negative pressure is 0.08Mpa to obtain a cured film, and taking down the cured film from the polyethylene glycol terephthalate substrate to obtain the perovskite quantum dot film.
Similarly, the preparation processes of the single-color perovskite quantum dot film and the double-color perovskite quantum dot film are similar to those described above, and those skilled in the art can obtain different types of quantum dot films by referring to the preparation principle and method described above, and no further description is given here. The following preparation examples 2-4 are examples of preparing three single-color perovskite quantum dot films.
Preparation of example 2
A monochromatic quantum dot film, i.e., CH, was prepared in the same manner as in example 1, except that the above-described steps b), c) and d) were not included3NH3PbBr3Quantum dot films, i.e., green quantum dot films.
Preparation of example 3
A monochromatic quantum dot film, i.e., CH, was prepared in the same manner as in example 1, except that the above-described steps a), c) and d) were not included3NH3PbBr1.5I1.5Quantum dot films, i.e., red quantum dot films.
Preparation of example 4
A monochromatic quantum dot film, i.e., CH, was prepared in the same manner as in example 1, except that the above-described steps a), b) and d) were not included3NH3PbBrCl2Quantum dot films, i.e., blue quantum dot films.
Application examples 5 to 8
In this example, the perovskite quantum dot film 2 prepared in the preparation examples 1 to 4 was assembled with the structural member 1, the backlight and the reflector 3, respectively, to be applied to a backlight module of a liquid crystal display device. The structure of the backlight module added with the perovskite quantum dot film is shown in the attached figure 1.
Characterization example 9
This example will prepare three quantum dot films, i.e., CH, obtained by examples 2-43NH3PbBr3Quantum dot film, CH3NH3PbBr1.5I1.5Quantum dot film, CH3NH3PbBrCl2The quantum dot films are respectively excited by ultraviolet light to obtain photoluminescence spectrograms in the attached figure 2. And measuring the fluorescence quantum efficiency of the three quantum dot films respectively by adopting 365nm light as exciting light and adopting a fluorescence spectrometer (HORIBA) with the model of FluoroMax-4 to test the absorption of the fluorescence quantum dots in an integrating sphere (high beam) with the model of EVERFINE-0.5mSpectrum and excitation light spectrum, and obtaining fluorescence quantum efficiency by the following formula: fluorescence quantum efficiency (η) is the number of photons emitted/absorbed.
CH can be seen from FIG. 23NH3PbBr3The quantum dot film has a peak between 500-600nm, which shows that the film can emit green light under the excitation of ultraviolet light, and the fluorescence quantum efficiency of the green light is measured to be 40.6%. CH (CH)3NH3PbBr1.5I1.5The quantum dot film has a peak between 600-700nm, which shows that the film can emit red light under the excitation of ultraviolet light, and the fluorescence quantum efficiency of the red light is measured to be 65.8%. CH (CH)3NH3PbBrCl2The quantum dot film has a peak between 400 and 500nm, which shows that the quantum dot film can emit blue light under the excitation of ultraviolet light, and the fluorescence quantum efficiency of the blue light is measured to be 10.1%. From the above, it can be seen that the fluorescence quantum efficiency of the quantum dot film for various colors is high under the excitation of ultraviolet light.
Preparation of comparative example 1
(1) Mixing 0.5mol of methyl amine bromide and lead bromide with the molar ratio of 3:2, dissolving the mixture in 2.5L of dimethylformamide, adding oleylamine and octylamine to form a precursor solution, wherein the total amount of the oleylamine and the octylamine is 0.06mol, the molar ratio of the oleylamine to the octylamine is 1:4,
then, 0.5mol of the above precursor solution was dropped into 2.5L of toluene and stirred to obtain CH3NH3PbBr3The quantum dot concentration is 0.05mol/L solution,
the obtained solution is spin-coated on a polyethylene terephthalate substrate, and CH can be obtained after drying3NH3PbBr3A quantum dot film.
(2) Mixing 0.4mol of methyl amine bromide, lead bromide and lead iodide in a molar ratio of 2:1:1, dissolving the mixture in 2.5L of dimethylformamide, and adding oleylamine and octylamine to form a precursor solution, wherein the total amount of oleylamine and octylamine added is 0.04mol, and the molar ratio of oleylamine to octylamine is 1:3
Then, 0.4mol of the precursor solution was dropped into 2.5L of toluene and stirred to obtain CH3NH3PbBr1.5I1.5Solution with quantum dot concentration of 0.04mol/L，
The obtained solution is spin-coated on a polyethylene terephthalate substrate, and CH can be obtained after drying3NH3PbBr1.5I1.5A quantum dot film.
(3) Mixing 0.6mol of methyl amine bromide, lead bromide and lead chloride in a molar ratio of 3:2:1, dissolving the mixture in 2.5L of dimethylformamide, adding oleylamine and octylamine to form a precursor solution, wherein the total amount of oleylamine and octylamine added is 0.05mol, and the molar ratio of oleylamine to octylamine is 1:4,
then, 0.6mol of the above precursor solution was dropped into 2.5L of toluene and stirred to obtain CH3NH3PbBrCl2The quantum dot concentration is 0.06mol/L solution,
the obtained solution is spin-coated on a polyethylene terephthalate substrate, and CH can be obtained after drying3NH3PbBrCl2A quantum dot film.
Respectively obtaining CH by the preparation process3NH3PbBr3Quantum dot film, CH3NH3PbBr1.5I1.5Quantum dot film and CH3NH3PbBrCl2A quantum dot film.
Comparative application example 2
In this embodiment, the perovskite quantum dot film 2 prepared by the preparation comparative example 1 is respectively assembled with the structural component 1, the backlight and the reflector plate 3 to be applied to the backlight module of the liquid crystal display device. Wherein, the perovskite quantum dot film 2 is CH3NH3PbBr3Quantum dot film, CH3NH3PbBr1.5I1.5Quantum dot film and CH3NH3PbBrCl2The quantum dot film 3 is formed as an integral structure of the perovskite quantum dot film 2 shown in fig. 1 after the quantum dot films are bonded together.
Characterization comparative example 3
This example will be obtained by preparing CH as obtained in comparative example 13NH3PbBr3Quantum dot film, CH3NH3PbBr1.5I1.5Quantum dot film and CH3NH3PbBrCl2QuantumThe dot films were measured for fluorescence quantum efficiency, respectively, in the same manner as in characterization example 9.
CH3NH3PbBr3The fluorescence quantum efficiency of the quantum dot film is 30%, CH3NH3PbBr1.5I1.5The fluorescence quantum efficiency of the quantum dot film is 50%, CH3NH3PbBrCl2The fluorescence quantum efficiency of the quantum dot film was 8%.
In conclusion, comparing the results of characterizing example 9 and characterizing comparative example 3, it can be seen that CH was obtained by the inventive preparation example 23NH3PbBr3The fluorescence quantum efficiency of the quantum dot film is higher than that of CH in the comparative example3NH3PbBr3The fluorescence quantum efficiency of the quantum dot film,
preparation of CH obtained in example 3 by the invention3NH3PbBr1.5I1.5The fluorescence quantum efficiency of the quantum dot film is higher than that of CH in the comparative example3NH3PbBr1.5I1.5The fluorescence quantum efficiency of the quantum dot film,
preparation of CH from example 4 by the invention3NH3PbBrCl2The fluorescence quantum efficiency of the quantum dot film is higher than that of CH in the comparative example3NH3PbBrCl2Fluorescence quantum efficiency of the quantum dot film.
All the above optional technical solutions may be combined arbitrarily to form the optional embodiments of the present disclosure, and are not described herein again.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A perovskite quantum dot film, wherein the quantum dot film comprises: perovskite quantum dots and polyamidoamine dendrimer;
the perovskite quantum dots are dispersed in gaps formed by the side groups of the polyamidoamine dendrimer;
the width of a gap formed by the side group of the polyamidoamine dendrimer is 2-8 nm;
the polyamidoamine dendrimer is a 6-generation polyamidoamine dendrimer;
the polyamidoamine dendrimer is obtained by reacting diamine monomers and unsaturated esters;
the perovskite quantum dots are selected from at least one of green perovskite quantum dots, red perovskite quantum dots and blue perovskite quantum dots;
the general molecular formula of the perovskite quantum dot is ABX3Wherein A is an organic cation which is CH3NH3 +B is a divalent metal cation, X is a halide anion;
the green perovskite quantum dots, the red perovskite quantum dots and the blue perovskite quantum dots are respectively CH3NH3PbBr3、CH3NH3PbBr1.5I1.5And CH3NH3PbBrCl2；
The diamine monomer is selected from: one of octadecyl diamine, ethylene diamine, butanediamine, p-phenylenediamine and naphthalene diamine, and the unsaturated ester monomer is 3-butyl phenyl acrylate.
2. A method of making the perovskite quantum dot film of claim 1, comprising:
step 1, adding perovskite quantum dots into a solution of polyamidoamine dendrimer to obtain a mixed solution, wherein the polyamidoamine dendrimer has a gap capable of accommodating the perovskite quantum dots;
and 2, coating the mixed solution on a polyethylene terephthalate substrate for curing to obtain a cured film, and taking down the cured film from the polyethylene terephthalate substrate to obtain the perovskite quantum dot film.
3. The method of claim 2, wherein the polyamidoamine dendrimer solution of step 1 is prepared by:
adding unsaturated ester monomer into diamine monomer for addition reaction;
adding diamine monomers into the product of the addition reaction for substitution reaction to obtain a 1-generation polyamidoamine dendrimer;
repeatedly adding the unsaturated ester monomer and the diamine monomer into the 1-generation polyamidoamine dendrimer for N-1 times to obtain the N-generation polyamidoamine dendrimer, wherein N is an integer greater than or equal to 2;
adding monoamine to terminate the reaction, and obtaining the polyamidoamine dendrimer of which the width of the gap formed by the side group is in a preset range.
4. The method according to claim 3, characterized in that said diamine-based monomers are selected from: one of octadecyl diamine, ethylene diamine, butanediamine, p-phenylenediamine and naphthalene diamine, and the unsaturated ester monomer is 3-butyl phenyl acrylate.
5. The method of claim 3, wherein N is 6.
6. A backlight module, characterized in that the backlight module comprises the perovskite quantum dot film of claim 1.
7. A display device, comprising the backlight module of claim 6.
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| CN106170877A (en) * | 2014-02-26 | 2016-11-30 | 联邦科学和工业研究组织 | The method forming the photosensitive layer of perovskite light-sensitive unit |
| CN104861958A (en) * | 2015-05-14 | 2015-08-26 | 北京理工大学 | Perovskite/polymer composite luminescent material and preparation method thereof |
| CN105957970A (en) * | 2016-05-30 | 2016-09-21 | 哈尔滨工业大学 | Preparation method of large-size mono-crystal perovskite film |
| CN106653875A (en) * | 2017-02-20 | 2017-05-10 | 江苏欧耐尔新型材料股份有限公司 | Nano light absorption composite material and preparation method thereof, and coated film preparation method |
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