CN111410748A - Perovskite quantum dot composition and preparation method thereof, perovskite quantum dot film and preparation method thereof - Google Patents
Perovskite quantum dot composition and preparation method thereof, perovskite quantum dot film and preparation method thereof Download PDFInfo
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Abstract
The application provides a manufacturing method of a perovskite quantum dot composition, which comprises the following steps: providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol; mixing the first glue solution and the second glue solution; adding perovskite quantum dots; and performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer. Therefore, the stable perovskite quantum dot composition can be prepared, and the red shift of the emission wavelength is realized.
Description
Technical Field
The application belongs to the field of quantum dots, and particularly relates to a perovskite quantum dot composition and a perovskite quantum dot film.
Background
Perovskite quantum dots refer to compounds having a perovskite crystal structure. The perovskite crystal structure is meant to correspond to CaTiO3Three-dimensional of the crystal structure of(3D) A crystal structure. Quantum dots are nanoparticles that are all less than 100 nanometers in three-dimensional size.
The chemical formula of the perovskite quantum dot is generally expressed as [ A ]][B][X]3. Wherein in the formula, a is at least one monovalent organic cation, at least one monovalent inorganic cation, or any combination thereof, B is at least one divalent inorganic cation, and X is at least one monovalent anion. Wherein, X is a halogen element such as-Cl, -Br, -I.
When A is Cs and B is Pb, X is-Cl, and the perovskite quantum dot CsPbCl3The light emission range of (a) is generally in the blue wavelength range; when A is Cs and B is Pb, X is-Br, perovskite quantum dot CsPbBr3The light emission range of (a) is generally in the green wavelength range; when A is Cs and B is Pb, X is-I, perovskite quantum dot CsPbBr3Generally in the red wavelength range.
However, in the actual preparation process, especially the wavelength of PbCsBr3 can only reach 518nm, so that it is difficult to prepare green perovskite quantum dots with large wavelength, such as green light with the wavelength of 520-530 nm.
At present, in order to realize the green perovskite quantum dot with large wavelength, iodine elements are doped in the PbCsBr3 quantum dot, so that the PbCsBr3 quantum dot is subjected to light red shift, and the green perovskite quantum dot with large wavelength is realized. However, the doped PbCsBr3 quantum dots are unstable, so that the service life of the perovskite quantum dot film manufactured in the later period is greatly reduced.
Therefore, a method for preparing a stable green-light PbCsBr3 quantum dot composition with a large wavelength is urgently needed.
Disclosure of Invention
Aiming at the technical problems, the application provides a manufacturing method of a perovskite quantum dot composition, which can be used for preparing a stable green light PbCsBr3 quantum dot composition, and the emission wavelength is within the range of 520-540 nm.
According to an aspect of the present application, there is provided a method of preparing a perovskite quantum dot composition, comprising:
providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol;
mixing the first glue solution and the second glue solution;
adding perovskite quantum dots;
and performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
Preferably, the mass ratio of the first glue solution to the second glue solution is 1: 100-1: 1.
preferably, the perovskite quantum dots comprise CsPbCl3、CsPbBr3Or CsPbI3At least one of (1).
Preferably, the isocyanate includes at least one of monoisocyanate, diisocyanate, and polyisocyanate.
Preferably, the diisocyanate includes at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate.
Preferably, the polyether polyol comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000 and PPG-2000; and/or the polyester polyol comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol.
In another aspect of the present application, there is provided a perovskite quantum dot composition which is a perovskite quantum dot-polyurethane coordination polymer comprising a perovskite quantum dot and a polyurethane coordinated to the perovskite quantum dot.
In another aspect of the present application, there is provided a method for preparing a perovskite quantum dot film, including:
providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol;
mixing the first glue solution and the second glue solution;
adding perovskite quantum dots;
and performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
And curing the coordination polymer to form a film, thereby forming the perovskite quantum dot film.
In another aspect of the present application, a perovskite quantum dot film is provided, which is obtained by the above preparation method.
Preferably, the perovskite quantum dot film contains CsPbBr3The light emitted by the perovskite quantum dot film is green light with the wavelength of 520-540 nm;
the perovskite quantum dot film contains CsPbCl3The light emitting wavelength of the perovskite quantum dot film is 460-480 nm; or
The perovskite quantum dot film contains CsPbI3And the light emitted by the perovskite quantum dot film is red light with the wavelength of 660-760 nm.
Has the advantages that:
according to the preparation method, the perovskite quantum dots are directly added during the preparation of polyurethane, in the addition polymerization reaction of a first glue solution containing isocyanate and a second glue solution containing polyether polyol and/or polyester polyol, the perovskite quantum dots are coordinated with urethane bonds (-NHCOO-) and fixed in the polyurethane, and along with the polymerization reaction of the first glue solution and the second glue solution, the perovskite quantum dots are also aggregated therewith, so that the composition is finally prepared: the perovskite quantum dot-polyurethane coordination polymer can emit green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm.
Different from the prior art in which perovskite quantum dots are directly added into polyurethane, the perovskite quantum dots are added in the preparation process of the polyurethane, and the perovskite quantum dots and the coordination complexing in the preparation process of the polyurethane are ingeniously utilized, so that the luminescent red shift of the perovskite quantum dot composition is realized.
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FIG. 1 is a flow chart of a method of preparing a perovskite quantum dot composition according to an embodiment of the present application;
FIG. 2 is a flow chart of a method of making a perovskite quantum dot film according to an embodiment of the present disclosure;
FIG. 3 is a luminescence test plot of a perovskite quantum dot film according to an embodiment of the present application;
FIG. 4 is a luminescence test plot of a perovskite quantum dot film according to another embodiment of the present application;
FIG. 5 is a luminescence test plot of a perovskite quantum dot film according to another embodiment of the present application;
fig. 6 is a luminescence test chart of a perovskite quantum dot film according to another embodiment of the present application.
Detailed Description
The technical solutions in the examples of the present application will be described in detail below with reference to the embodiments of the present application. It should be noted that the described embodiments are only some embodiments of the present application, and not all embodiments.
As used herein, a statement such as "at least one (one)" modifies an entire list of elements as it precedes or succeeds the list of elements without modifying individual elements of the list. Unless otherwise defined, all terms (including technical and scientific terms) in the specification may be defined as commonly understood by one of ordinary skill in the art. Terms defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure, and may not be interpreted in an idealized or overly formal sense unless expressly so defined. Furthermore, unless expressly stated to the contrary, the terms "comprises" and "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, elements, components, and/or groups thereof. Thus, the above wording will be understood to mean that the stated elements are included, but not to exclude any other elements.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The term "or" means "and/or". The expression "at least one of" when preceding or following a list of elements modifies the entire list of elements without modifying individual elements of the list.
It will be understood that, although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms are only used to distinguish one element, component, region, layer or section from another element, component, region, layer or section. Thus, a first element, component, region, layer or section discussed below could be termed a second element, component, region, layer or section without departing from the teachings of the present embodiments.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
As used herein, "about" or "approximately" includes the stated value and is meant to be within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art in view of the measurement in question and the error associated with measurement of the particular quantity (i.e., limitations of the measurement system). For example, "about" may mean a deviation from the stated value within one or more standard deviation ranges, or within ± 10%, 5%.
As used herein, the term "dispersion" refers to a dispersion in which the dispersed phase is a solid and the continuous phase comprises a liquid. For example, the term "dispersion" may refer to a colloidal dispersion in which the dispersed phase has a size of about 1nm to about 1 micrometer (μm).
As used herein, "combination" includes all types of combinations, including blends, alloys, solutions, and the like.
The source of the quantum dots is not particularly limited. The quantum dots can be prepared by any known method or are commercially available.
The quantum dots can have a size (e.g., particle diameter, or in the case of non-spherical particles, diameter calculated from the two-dimensional area of an electron microscope image of the particle) of about 1nm to about 100 nm. In some embodiments, the quantum dots can have a particle size of from about 1nm to about 50nm, such as from 2nm (or from 3nm) to 35 nm. In some embodiments, the quantum dots have a diameter of greater than or equal to about 1nm, greater than or equal to about 2nm, greater than or equal to about 3nm, greater than or equal to about 4nm, or greater than or equal to about 5 nm. In some embodiments, the quantum dots have a diameter of less than or equal to about 50nm, less than or equal to about 45nm, less than or equal to about 40nm, less than or equal to about 35nm, less than or equal to about 30nm, less than or equal to about 25nm, less than or equal to about 20nm, less than or equal to about 19nm, less than or equal to about 18nm, less than or equal to about 17nm, less than or equal to about 16nm, or less than or equal to about 15 nm.
The quantum dots may have a Full Width Half Maximum (FWHM) of less than or equal to about 45nm, such as less than or equal to about 40nm, or less than or equal to about 30 nm. While not wanting to be bound by theory, it is understood that within such a range, a device including the quantum dots may have enhanced color purity or improved color reproducibility.
Perovskite quantum dots refer to compounds having a perovskite crystal structure. The perovskite crystal structure is meant to correspond to CaTiO3The chemical formula of the perovskite quantum dot is generally represented by [ A ]][B][X]3. Wherein in the formula, a is at least one monovalent organic cation, at least one monovalent inorganic cation, or any combination thereof, B is at least one divalent inorganic cation, and X is at least one monovalent anion. Wherein, X is a halogen element such as-Cl, -Br, -I. When A is Cs and B is Pb, X is-Br, perovskite quantum dot CsPbBr3Generally in the green wavelength range.
However, in the actual preparation process, especially the wavelength of PbCsBr3 can only reach 518nm, so that it is difficult to prepare green perovskite quantum dots with large wavelength, such as green light with the wavelength of 520-540 nm.
The method and the device can enable the PbCsBr3 quantum dots to emit red shift under the condition of not doping iodine elements, and can prepare green perovskite quantum dots with emission wavelengths of 520-540 nm.
The inventor finds that, when the polyurethane is prepared, the perovskite quantum dots are directly added, in the addition polymerization reaction of a first glue solution containing isocyanate and a second glue solution containing polyether polyol and/or polyester polyol, the perovskite quantum dots are coordinated with urethane bonds (-NHCOO-) and are fixed in the polyurethane, and the perovskite quantum dots are also aggregated along with the polymerization reaction of the first glue solution and the second glue solution, so that the composition is finally prepared: the perovskite quantum dot-polyurethane coordination polymer can emit green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm.
Similarly, the perovskite quantum dot film contains CsPbCl3The red shift can also be realized by the quantum dots, and the light-emitting wavelength of the perovskite quantum dot film is 460-480 nm; or the perovskite quantum dot film contains CsPbI3The quantum dot can also realize red shift, and the light emitting wavelength of the perovskite quantum dot film is 660-760 nm. This document is not repeated here.
Different from the technical scheme of directly adding the perovskite quantum dots into the polyurethane, the perovskite quantum dots are added in the preparation process of the polyurethane, and the perovskite quantum dots and the coordination complexing in the preparation process of the polyurethane are ingeniously utilized, so that the luminescent red shift of the perovskite quantum dot composition is realized.
Fig. 1 is a flow chart of a method for preparing a perovskite quantum dot composition according to an embodiment of the present disclosure. A method of preparing a perovskite quantum dot composition, comprising:
step S101, providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol.
The first glue solution contains isocyanate, and the second glue solution contains at least one of polyether polyol and polyester polyol. The parts of the first glue solution and the parts of the second glue solution are configured according to a certain proportion, for example, the mass ratio of the first glue solution to the second glue solution is 1: 100-1: 1. that is, when the polyurethane is synthesized, the amount of the isocyanate, the amount of the polyether polyol and the amount of the polyester polyol are combined in a certain ratio, and the ratio of the first glue solution to the second glue solution is controlled to control the amount of the reaction product. For example, the mass ratio of isocyanate to polyester polyol is 1:1 or 1:10 or 1:20 or 1:30 or 1:40 or 1:50 or 1:60 or 1:70 or 1:80 or 1:90 or 1: 100.
Specifically, the isocyanate contained in the first glue solution may include at least one of monoisocyanate, diisocyanate, and polyisocyanate. For example, the diisocyanate includes at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate. The polyether polyol contained in the second glue solution comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000 and PPG-2000; the polyester polyol contained in the second glue solution comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol. The second glue solution can comprise both polyether polyol and polyester polyol, and also can only contain polyether polyol or only contain polyester polyol. The present application is not limited thereto.
Step S102, mixing the first glue solution and the second glue solution;
and mixing the first glue solution and the second glue solution which are prepared in the step S101.
Step S103, adding perovskite quantum dots;
in some exemplary embodiments of the present application, the perovskite quantum dots may be surrounded by, for example, at least one ligand. The ligands may increase the stability of the perovskite quantum dots and protect the perovskite quantum dots from deleterious external conditions (e.g., high temperature, high strength, external gases and/or moisture).
In the step S102, perovskite quantum dots are added to the mixture of the first glue solution and the second glue solution, and in the present application, the perovskite quantum dots are PbCsBr3 quantum dots. Before adding the perovskite quantum dots, the perovskite quantum dots can be added after the first glue solution and the second glue solution react for a period of time, for example, 1 minute to 30 minutes, to form a part of liquid polyurethane glue solution. The perovskite quantum dots are generally dissolved in a toluene solvent, and when the perovskite quantum dots are added, the toluene solvent of the perovskite quantum dots is directly added into a mixed solution of the first glue and the second glue. The solvent for the perovskite quantum dots is not limited to toluene, but may be a chloroform solvent, a heptane solvent, or the like, and the present application is not limited thereto.
And step S104, performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
After the perovskite quantum dots are added in step S103, the mixed solution of the first glue solution and the second glue solution is kept stable for a certain time, for example, 1 hour to 12 hours, until a clear mixed solution is formed. At this time, urethane bonds (-NHCOO-) in the polyurethane provide lone pair electrons, and coordinate with the empty orbitals of the metal ions in the perovskite quantum dots to form a coordination compound. And forming a perovskite quantum dot-polyurethane coordination polymer along with the addition polymerization reaction of the first glue solution and the second glue solution, wherein the perovskite quantum dots are aggregated along with the polymerization of polyurethane, so that the luminescence red shift of the reaction product perovskite quantum dot composition is realized.
Through coordination of the perovskite quantum dots and the urethane bonds (-NHCOO-) and fixation of the perovskite quantum dots in polyurethane, the perovskite quantum dot-polyurethane coordination polymer can emit green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm. Compared with the method for preparing the green light quantum dots with large wavelength by doping iodine elements in PbCsBr3, the preparation method of the application does not cause adverse effect on the stability of the perovskite quantum dots, and improves the stability of the perovskite quantum dots by inversely complexing the perovskite quantum dots with polyurethane.
In another embodiment of the present application, a perovskite quantum dot composition is provided, the perovskite quantum dot composition being a perovskite quantum dot-polyurethane coordination polymer, the coordination polymer comprising a perovskite quantum dot and a polyurethane coordinated to the perovskite quantum dot. The perovskite quantum dot is a PbCsBr3 quantum dot, and the light emitting range of the perovskite quantum dot composition is 520-540 nm. Further, the perovskite quantum dot composition is prepared by the following method:
firstly, providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol. The first glue solution contains isocyanate, and the second glue solution contains at least one of polyether polyol and polyester polyol. The parts of the first glue solution and the parts of the second glue solution are configured according to a certain proportion, for example, the mass ratio of the first glue solution to the second glue solution is 1:100 to 1. That is, when the polyurethane is synthesized, the amount of the isocyanate, the amount of the polyether polyol and the amount of the polyester polyol are combined in a certain ratio, and the ratio of the first glue solution to the second glue solution is controlled to control the amount of the reaction product. For example, the mass of isocyanate to polyester polyol is 1:1 or 1:10 or 1:20 or 1:30 or 1:40 or 1:50 or 1:60 or 1:70 or 1:80 or 1:90 or 1: 100.
Specifically, the isocyanate contained in the first glue solution may include at least one of monoisocyanate, diisocyanate, and polyisocyanate. For example, the diisocyanate includes at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate. The polyether polyol contained in the second glue solution comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000 and PPG-2000; the polyester polyol contained in the second glue solution comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol. The second glue solution can comprise both polyether polyol and polyester polyol, and also can only contain polyether polyol or only contain polyester polyol. The present application is not limited thereto.
Secondly, mixing the first glue solution and the second glue solution, and then adding perovskite quantum dots;
and adding perovskite quantum dots into the mixture of the first glue solution and the second glue solution, wherein the perovskite quantum dots are PbCsBr3 quantum dots. Before adding the perovskite quantum dots, the perovskite quantum dots can be added after the first glue solution and the second glue solution react for a period of time, for example, 1 minute to 30 minutes, to form a part of liquid polyurethane glue solution. The perovskite quantum dots are generally dissolved in a toluene solvent, and when the perovskite quantum dots are added, the toluene solvent of the perovskite quantum dots is directly added into a mixed solution of the first glue and the second glue. The solvent for the perovskite quantum dots is not limited to toluene, but may be a chloroform solvent, a heptane solvent, or the like, and the present application is not limited thereto.
And finally, performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer. After the perovskite quantum dots are added, the mixed solution of the first glue solution and the second glue solution is kept stable for a certain time, for example, 1 hour to 12 hours, until a clear mixed solution is formed. At this time, urethane bonds (-NHCOO-) in the polyurethane provide lone pair electrons, and coordinate with the empty orbitals of the metal ions in the perovskite quantum dots to form a coordination compound. And forming a perovskite quantum dot-polyurethane coordination polymer along with the addition polymerization reaction of the first glue solution and the second glue solution, wherein the perovskite quantum dots are aggregated along with the polymerization of polyurethane, so that the luminescence red shift of the reaction product perovskite quantum dot composition is realized. Finally, the perovskite quantum dot composition emits green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm. And the stability of the perovskite quantum dots is improved through the coordination and complexation of the perovskite quantum dots and the polyurethane.
Fig. 2 is a flowchart of a method for producing a perovskite quantum dot film according to an embodiment of the present invention. The preparation method of the perovskite quantum dot film comprises the following steps:
step S201, providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol.
The first glue solution contains isocyanate, and the second glue solution contains at least one of polyether polyol and polyester polyol. The parts of the first glue solution and the parts of the second glue solution are configured according to a certain proportion, for example, the mass ratio of the first glue solution to the second glue solution is 1: 100-1: 1. that is, when the polyurethane is synthesized, the amount of the isocyanate, the amount of the polyether polyol and the amount of the polyester polyol are combined in a certain ratio, and the ratio of the first glue solution to the second glue solution is controlled to control the amount of the reaction product. For example, the mass ratio of isocyanate to polyester polyol is 1:1 or 1:10 or 1:20 or 1:30 or 1:40 or 1:50 or 1:60 or 1:70 or 1:80 or 1:90 or 1: 100.
Specifically, the isocyanate contained in the first glue solution may include at least one of monoisocyanate, diisocyanate, and polyisocyanate. For example, the diisocyanate includes at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate. The polyether polyol contained in the second glue solution comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000 and PPG-2000; the polyester polyol contained in the second glue solution comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol. The second glue solution can comprise both polyether polyol and polyester polyol, and also can only contain polyether polyol or only contain polyester polyol. The present application is not limited thereto.
Step S202, mixing the first glue solution and the second glue solution;
and mixing the first glue solution and the second glue solution which are prepared in the step S201.
Step S203, adding perovskite quantum dots;
in step S202, perovskite quantum dots are added to the mixture of the first glue solution and the second glue solution, and in this application, the perovskite quantum dots are PbCsBr3 quantum dots. Before adding the perovskite quantum dots, the perovskite quantum dots can be added after the first glue solution and the second glue solution react for a period of time, for example, 1 minute to 30 minutes, to form a part of liquid polyurethane glue solution. The perovskite quantum dots are generally dissolved in a toluene solvent, and when the perovskite quantum dots are added, the toluene solvent of the perovskite quantum dots is directly added into a mixed solution of the first glue and the second glue. The solvent for the perovskite quantum dots is not limited to toluene, but may be a chloroform solvent, a heptane solvent, or the like, and the present application is not limited thereto.
And step S204, performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
After the perovskite quantum dots are added in step S203, the mixed solution of the first glue solution and the second glue solution is kept stable for a certain time, for example, 1 hour to 12 hours, until a clear mixed solution is formed. At this time, urethane bonds (-NHCOO-) in the polyurethane provide lone pair electrons, and coordinate with the empty orbitals of the metal ions in the perovskite quantum dots to form a coordination compound. And forming a perovskite quantum dot-polyurethane coordination polymer along with the addition polymerization reaction of the first glue solution and the second glue solution, wherein the perovskite quantum dots are aggregated along with the polymerization of polyurethane, so that the luminescence red shift of the reaction product perovskite quantum dot composition is realized.
Through coordination of the perovskite quantum dots and the urethane bonds (-NHCOO-) and fixation of the perovskite quantum dots in polyurethane, the perovskite quantum dot-polyurethane coordination polymer can emit green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm. Compared with the method for preparing the green light quantum dots with large wavelength by doping iodine elements in PbCsBr3, the preparation method of the application does not cause adverse effect on the stability of the perovskite quantum dots, and improves the stability of the perovskite quantum dots by inversely complexing the perovskite quantum dots with polyurethane.
And S205, solidifying the coordination polymer to form a film, and forming the perovskite quantum dot film.
The perovskite quantum dot-polyurethane coordination polymer prepared by the above steps is coated on the substrate, for example, in one embodiment of the present application, the perovskite quantum dot-polyurethane coordination polymer is coated on the barrier film, and the coating thickness may be 10 μm to 500 μm. The present application is not limited thereto.
And after coating, forming a wet film, drying the wet film, evaporating the redundant toluene solvent, and finally curing to obtain the perovskite quantum dot film.
Further, in a specific embodiment of the present application, after the perovskite quantum dot film is formed, a barrier film is formed on the quantum dot film, so as to form a good water and oxygen barrier protection for the perovskite quantum dot film.
Further, in an embodiment of the present application, after the perovskite quantum dot film is formed, the quantum dot film may be subjected to a thermal curing process, for example, aging at 40 ℃ for 2 to 3 days; aging at 60 deg.C for 36 hr; aging was carried out at 80 ℃ for 12 hours.
In another embodiment of the present application, there is provided a perovskite quantum dot film, the quantum dot film containing CsPbBr3 quantum dots, the perovskite quantum dot film being prepared by coating a perovskite quantum dot-polyurethane coordination polymer. The light emitting range of the perovskite quantum dot film is 520-540 nm. Specifically, the perovskite quantum dot film is prepared by the following method:
firstly, providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol.
The first glue solution contains isocyanate, and the second glue solution contains at least one of polyether polyol and polyester polyol. The parts of the first glue solution and the parts of the second glue solution are configured according to a certain proportion, for example, the mass ratio of the first glue solution to the second glue solution is 1: 100-1: 1. that is, when the polyurethane is synthesized, the amount of the isocyanate, the amount of the polyether polyol and the amount of the polyester polyol are combined in a certain ratio, and the ratio of the first glue solution to the second glue solution is controlled to control the amount of the reaction product. For example, the mass ratio of isocyanate to polyester polyol is 1:1 or 1:10 or 1:20 or 1:30 or 1:40 or 1:50 or 1:60 or 1:70 or 1:80 or 1:90 or 1: 100.
Specifically, the isocyanate contained in the first glue solution may include at least one of monoisocyanate, diisocyanate, and polyisocyanate. For example, the diisocyanate includes at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate. The polyether polyol contained in the second glue solution comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000 and PPG-2000; the polyester polyol contained in the second glue solution comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol. The second glue solution can comprise both polyether polyol and polyester polyol, and also can only contain polyether polyol or only contain polyester polyol. The present application is not limited thereto.
Secondly, mixing the first glue solution and the second glue solution and then adding perovskite quantum dots;
the perovskite quantum dot is PbCsBr3 quantum dot. Before adding the perovskite quantum dots, the perovskite quantum dots can be added after the first glue solution and the second glue solution react for a period of time, for example, 1 minute to 30 minutes, to form a part of liquid polyurethane glue solution. The perovskite quantum dots are generally dissolved in a toluene solvent, and when the perovskite quantum dots are added, the toluene solvent of the perovskite quantum dots is directly added into a mixed solution of the first glue and the second glue. The solvent for the perovskite quantum dots is not limited to toluene, but may be a chloroform solvent, a heptane solvent, or the like, and the present application is not limited thereto.
And secondly, performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
After the perovskite quantum dots are added, the mixed solution of the first glue solution and the second glue solution is kept stable for a certain time, for example, 1 hour to 12 hours, until a clear mixed solution is formed. At this time, urethane bonds (-NHCOO-) in the polyurethane provide lone pair electrons, and coordinate with the empty orbitals of the metal ions in the perovskite quantum dots to form a coordination compound. And forming a perovskite quantum dot-polyurethane coordination polymer along with the addition polymerization reaction of the first glue solution and the second glue solution, wherein the perovskite quantum dots are aggregated along with the polymerization of polyurethane, so that the luminescence red shift of the reaction product perovskite quantum dot composition is realized.
Through coordination of the perovskite quantum dots and the urethane bonds (-NHCOO-) and fixation of the perovskite quantum dots in polyurethane, the perovskite quantum dot-polyurethane coordination polymer can emit green light with large wavelength, and particularly the wavelength is within the range of 520-540 nm. Compared with the method for preparing the green light quantum dots with large wavelength by doping iodine elements in PbCsBr3, the preparation method of the application does not cause adverse effect on the stability of the perovskite quantum dots, and improves the stability of the perovskite quantum dots by inversely complexing the perovskite quantum dots with polyurethane.
And finally, solidifying the coordination polymer to form a film, and forming the perovskite quantum dot film.
The prepared perovskite quantum dot-polyurethane coordination polymer is coated on a substrate, for example, in one embodiment of the present application, the perovskite quantum dot-polyurethane coordination polymer is coated on a barrier film, and the coating thickness can be 10 μm to 500 μm. The present application is not limited thereto.
And after coating, forming a wet film, drying the wet film, evaporating the redundant toluene solvent, and finally curing to obtain the perovskite quantum dot film.
Further, in a specific embodiment of the present application, after the perovskite quantum dot film is formed, a barrier film is formed on the quantum dot film, so as to form a good water and oxygen barrier protection for the perovskite quantum dot film.
Further, in an embodiment of the present application, after the perovskite quantum dot film is formed, the quantum dot film may be subjected to a thermal curing process, for example, aging at 40 ℃ for 2 to 3 days; aging at 60 deg.C for 36 hr; aging was carried out at 80 ℃ for 12 hours.
The quantum dots in the perovskite quantum dot film are PbCsBr3 quantum dots, and the perovskite quantum dot film can emit green light with large wavelength, especially green light within the range of 520-540 nm, under the condition that iodine elements are not doped.
And the wavelength of green light emitted by the perovskite quantum dot film is controllable. Specifically, the green wavelength of the perovskite quantum dot film can be regulated and controlled by one factor or a combination of a plurality of factors in the ratio of the first glue to the second glue, the pre-reaction time of the first glue to the second glue or the time when the perovskite quantum dot is added into the mixed glue, and the reaction time after the perovskite quantum dot is added.
In a specific embodiment of the application, the regulation and control of the emission wavelength of the perovskite quantum dot film are realized by adjusting the ratio of the first glue to the second glue.
In a specific embodiment of the application, the regulation and control of the emission wavelength of the perovskite quantum dot film are realized by adjusting the reaction time of the first glue and the second glue.
In a specific embodiment of the present application, the perovskite quantum dot film emission wavelength is controlled by adjusting the time of adding the perovskite quantum dot.
In a specific embodiment of the present application, the adjustment and control of the emission wavelength of the perovskite quantum dot film are realized by adjusting the reaction time after the perovskite quantum dots are added.
The emission wavelength of the perovskite quantum dot film can be adjusted to be combined with the blue excitation light and the red light conversion layer, so that the finally generated white light color coordinate is adjusted, and the white light color coordinate meeting the requirement is achieved.
For example, the excitation light source is blue light, the blue light is firstly irradiated on the red light conversion layer, for example, the red light conversion layer is KSF fluorescent powder, product red light is generated, the product red light is then irradiated on the green perovskite quantum dot film, and finally the light emitted from the quantum dot film is white light.
If the wavelength of the blue light and the wavelength of the red light KSF fluorescent powder are fixed, the color coordinate of the finally generated white light can be adjusted by adjusting the emission wavelength of the green perovskite quantum dot film so as to achieve the white light required by customers.
Specifically, for example, the excitation light source may be a blue light emitting diode (light having a wavelength range of about 420nm to about 490 nm) that emits blue light. For example, the blue light wavelength is 447nm and the red converted by the red KSF phosphor is 630 nm. In some exemplary embodiments of the present application, the perovskite quantum dot film may absorb light emitted by the light source and emit light having a wavelength range different from that of the light source, i.e., the present application is not limited to light emitted by an excitation light source.
Hereinafter, embodiments of the present invention will be described in more detail with reference to examples. However, they are exemplary embodiments of the present invention, and the present invention is not limited thereto.
Preparation example:
3[Cs][Pb][Br]the preparation process of the quantum dot is as follows：
0.407g of Cs was weighed2CO315m of L octadecene and 1.25m of L oleic acid are weighed, nitrogen is introduced for degassing and protection, the temperature is heated to 120 ℃, the temperature is kept for 1 hour, and then a transparent Cs precursor solution is obtained and cooled for standby.
In a 50m L three-necked flask, 5m L of 1-octadecene and 0.069g of PbBr were taken2Degassing with nitrogen at 120 deg.C, stirring for 1 hr, and adding 0.5m L oilAmine and 0.5m of L oleic acid, then heating to 150 ℃, stirring for 1h, then quickly injecting 0.6m of L Cs precursor solution into the solution, stopping heating after reacting for 5s, cooling in ice water after 10s to obtain yellow-green condensed colloidal substances, and taking out and naturally cooling to room temperature.
Centrifuging the obtained yellow green liquid at 1000 r/min for 5min, collecting supernatant, centrifuging at 12000r/min for 10min, collecting bottom precipitate, adding 1.5m L toluene into the precipitate, and dispersing with ultrasonic wave to obtain [ Cs][Pb][Br]3And putting the toluene solution of the quantum dots into a glass bottle, and sealing and storing at room temperature.
The obtained [ Cs ]][Pb][Br]3The quantum dot emits light with a peak-to-peak wavelength of 516nm under the excitation of 447nm light, and the half-peak width is about 18 nm.
Example 1
The perovskite quantum dot film is prepared by the following steps:
taking 10 parts of polyether polyol PPG600 and 1 part of Toluene Diisocyanate (TDI), namely the mass ratio of PPG600 to TDI is 10:1, mixing the polyether polyol PPG600 and the Toluene Diisocyanate (TDI), stirring for 20 minutes, and then mixing [ Cs ] in the preparation example][Pb][Br]3And adding the toluene solution of the quantum dots into the mixed glue solution, and reacting for 12 hours to form clear mixed solution.
And (3) coating the mixed solution on a substrate in a rotating manner to form a wet film, drying the wet film, and finally curing to form the 10-micron perovskite quantum dot film.
The excitation light source is blue light with the wavelength of 447nm, and the blue light passes through the red KSF fluorescent powder (the wavelength of the converted red light is 630nm) and then passes through the perovskite quantum dot film to finally emit white light formed by mixing the blue light, the red light and the green light.
The perovskite quantum dot film was tested for fluorescence emission peak using PR655 photometer, and as shown in FIG. 3, the green light emission peak wavelength was 526nm compared to [ Cs ] in the preparation example][Pb][Br]3The wavelength of the quantum dot emission peak is 516nm, the red shift is 10nm, and the [ Cs ] is broken through][Pb][Br]3The green wavelength of the quantum dots is limited to 518nm at maximum.
Example 2
The perovskite quantum dot film is prepared by the following steps:
taking 20 parts of polyether polyol PPG600 and 1 part of Toluene Diisocyanate (TDI), namely the mass ratio of PPG600 to TDI is 20:1, mixing the polyether polyol PPG600 and the Toluene Diisocyanate (TDI), stirring for 20 minutes, and then mixing [ Cs ] in the preparation example][Pb][Br]3And adding the toluene solution of the quantum dots into the mixed glue solution, and reacting for 10 hours to form clear mixed solution.
And (3) coating the mixed solution on a substrate in a rotating manner to form a wet film, drying the wet film, and finally curing to form the perovskite quantum dot film with the thickness of 100 microns.
The excitation light source is blue light with the wavelength of 447nm, and the blue light passes through the red KSF fluorescent powder (the wavelength of the converted red light is 630nm) and then passes through the perovskite quantum dot film to finally emit white light formed by mixing the blue light, the red light and the green light.
The perovskite quantum dot film was tested for fluorescence emission peak using PR655 photometer, and as shown in FIG. 4, the emission peak wavelength of green light was 527nm, compared to [ Cs ] in the preparation example][Pb][Br]3The emission peak wavelength of the quantum dots is 516nm and is red-shifted by 11 nm.
Example 3
The perovskite quantum dot film is prepared by the following steps:
taking 30 parts of polyether polyol PPG600 and 1 part of Toluene Diisocyanate (TDI), namely the mass ratio of PPG600 to TDI is 30:1, mixing the polyether polyol PPG600 and the Toluene Diisocyanate (TDI), stirring for 20 minutes, and then mixing [ Cs ] in the preparation example][Pb][Br]3And adding the toluene solution of the quantum dots into the mixed glue solution, and reacting for 10 hours to form clear mixed solution.
And (3) coating the mixed solution on a substrate in a rotating manner to form a wet film, drying the wet film, and finally curing to form the perovskite quantum dot film with the thickness of 100 microns.
The excitation light source is blue light with the wavelength of 447nm, and the blue light passes through the red KSF fluorescent powder (the wavelength of the converted red light is 630nm) and then passes through the perovskite quantum dot film to finally emit white light formed by mixing the blue light, the red light and the green light.
The perovskite quantum dot film was tested for fluorescence emission peak using a PR655 photometer, as shown in FIG. 5The green light has an emission peak wavelength of 526nm, compared with [ Cs ] in the preparation example][Pb][Br]3The wavelength of the quantum dot emission peak is 516nm and is red-shifted by 10 nm.
Example 4
The perovskite quantum dot film is prepared by the following steps:
taking 40 parts of polyether polyol PPG600 and 1 part of Toluene Diisocyanate (TDI), namely the mass ratio of PPG600 to TDI is 40:1, mixing the polyether polyol PPG600 and the Toluene Diisocyanate (TDI), stirring for 20 minutes, and then mixing [ Cs ] in the preparation example][Pb][Br]3And adding the toluene solution of the quantum dots into the mixed glue solution, and reacting for 10 hours to form clear mixed solution.
And (3) coating the mixed solution on a substrate in a rotating manner to form a wet film, drying the wet film, and finally curing to form the perovskite quantum dot film with the thickness of 100 microns.
The excitation light source is blue light with the wavelength of 447nm, and the blue light passes through the red KSF fluorescent powder (the wavelength of the converted red light is 630nm) and then passes through the perovskite quantum dot film to finally emit white light formed by mixing the blue light, the red light and the green light.
The perovskite quantum dot film was tested for its fluorescence emission peak using a PR655 photometer, as shown in FIG. 6, and the emission peak wavelength of green light was 525nm, compared to [ Cs ] in the preparation example][Pb][Br]3The wavelength of the quantum dot emission peak is 516nm and is red-shifted by 9 nm.
Comparative example
The perovskite quantum dot film is prepared by the following steps:
the [ Cs ] in the preparation example][Pb][Br]3And adding the toluene solution of the quantum dots into the polyurethane glue solution to form a clear mixed solution.
And (3) coating the mixed solution on a substrate in a rotating manner to form a wet film, drying the wet film, and finally curing to form the perovskite quantum dot film with the thickness of 100 microns.
The excitation light source is blue light with the wavelength of 447nm, and the blue light passes through the red KSF fluorescent powder (the wavelength of the converted red light is 630nm) and then passes through the perovskite quantum dot film to finally emit white light formed by mixing the blue light, the red light and the green light.
Fluorescence of perovskite quantum dot films using a PR655 luminometerEmission peak was measured, and the emission peak wavelength of green light was 518nm, as compared with [ Cs ] in preparation example][Pb][Br]3The quantum dot emission peak wavelength is 516nm red-shifted by only 2 nm.
The results of the preparation examples, example 1, example 2, example 3, example 4 and comparative example are listed in the following table:
| wavelength of green light/nm | Red shift/nm | |
| Example 1 | 526 | 10 |
| Example 2 | 527 | 11 |
| Example 3 | 526 | 10 |
| Example 4 | 525 | 9 |
| Preparation example | 516 | 0 |
| Comparative example | 518 | 2 |
As can be seen from the table, the perovskite quantum dot films in examples 1 to 4 of the present application all have a very large red shift, and achieve emission of green light with a large wavelength. The perovskite quantum dot film in the comparative example has only red shift of 2nm, and the emission of green light with large wavelength is not realized yet. Therefore, the perovskite quantum dots are directly added during the preparation of polyurethane, so that the perovskite quantum dot-polyurethane coordination polymer emits light with red shift, and green light with large wavelength can be emitted, and particularly the wavelength is within the range of 520-540 nm.
Although the present disclosure has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent substitutions, will be apparent to those skilled in the art without departing from the spirit of the disclosure, and that no limitations to the present disclosure are intended or should be inferred therefrom.
Claims (10)
1. A preparation method of a perovskite quantum dot composition is characterized by comprising the following steps:
providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol;
mixing the first glue solution and the second glue solution;
adding perovskite quantum dots;
and performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
2. The preparation method according to claim 1, wherein the mass ratio of the first glue solution to the second glue solution is 1: 100-1: 1.
3. according to claim1, the preparation method is characterized in that the perovskite quantum dots comprise CsPbCl3、CsPbBr3Or CsPbI3At least one of (1).
4. The method of claim 1, wherein the isocyanate comprises at least one of a monoisocyanate, a diisocyanate, and a polyisocyanate.
5. The method according to claim 4, wherein the diisocyanate comprises at least one of toluene isocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate.
6. The method of claim 1, wherein the polyether polyol comprises at least one of PPG-200, PPG-400, PPG-600, PPG-1000, PPG-2000; and/or the polyester polyol comprises at least one of glycol, diethylene glycol, propylene glycol, dipropylene glycol, butanediol, neopentyl glycol and hexanediol.
7. A perovskite quantum dot composition, wherein the perovskite quantum dot composition is a perovskite quantum dot-polyurethane coordination polymer, and the coordination polymer comprises perovskite quantum dots and polyurethane coordinated with the perovskite quantum dots.
8. A preparation method of a perovskite quantum dot film is characterized by comprising the following steps:
providing a first glue solution and a second glue solution, wherein the first glue solution contains isocyanate, and the second glue solution contains polyether polyol and/or polyester polyol;
mixing the first glue solution and the second glue solution;
adding perovskite quantum dots;
and performing addition polymerization reaction on the first glue solution and the second glue solution to form the perovskite quantum dot-polyurethane coordination polymer.
And curing the coordination polymer to form a film, thereby forming the perovskite quantum dot film.
9. A perovskite quantum dot film, characterized in that it is obtained by the production method according to claim 8.
10. The perovskite quantum dot film of claim 9, wherein the perovskite quantum dot film comprises CsPbBr3The light emitted by the perovskite quantum dot film is green light with the wavelength of 520-540 nm; or
The perovskite quantum dot film contains CsPbCl3The light emitting wavelength of the perovskite quantum dot film is 460-480 nm; or
The perovskite quantum dot film contains CsPbI3And the light emitted by the perovskite quantum dot film is red light with the wavelength of 660-760 nm.
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