CN116001378A - Perovskite quantum dot composite film and preparation method thereof - Google Patents
Perovskite quantum dot composite film and preparation method thereof Download PDFInfo
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- CN116001378A CN116001378A CN202310141705.4A CN202310141705A CN116001378A CN 116001378 A CN116001378 A CN 116001378A CN 202310141705 A CN202310141705 A CN 202310141705A CN 116001378 A CN116001378 A CN 116001378A
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- perovskite quantum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The invention discloses a perovskite quantum dot composite film and a preparation method thereof. The perovskite quantum dot composite film comprises: the perovskite quantum dot layer is arranged on one surface of the first barrier layer, the perovskite quantum dot layer comprises perovskite quantum dots and a polymer matrix, and monomers for forming the polymer matrix comprise a water-blocking monomer and an adhesion promoting monomer; the second barrier layer is arranged on the surface of the perovskite quantum dot layer away from the first barrier layer, wherein the water-blocking monomer comprises a fluorine-containing acrylate monomer, and the adhesion promoting monomer comprises a group for combining with the first barrier layer and the second barrier layer to form a hydrogen bond. The perovskite quantum dot composite film not only has good bonding stability, water resistance, weather resistance, optical performance and high transparency, but also has a simple film structure and a convenient production process, and is beneficial to mass industrialized production.
Description
Technical Field
The invention belongs to the field of display, and particularly relates to a perovskite quantum dot composite film and a preparation method thereof.
Background
In recent years, quantum dot materials are increasingly used in the display field, and the color saturation of a display device can be remarkably improved due to the narrower emission spectrum. Compared with classical CdSe and InP quantum dots, the perovskite quantum dot has higher luminous efficiency, can be prepared by an in-situ method, has simple preparation process and lower preparation cost, does not contain heavy metal cadmium in the aspect of environmental protection, and accords with the European Union RoHS standard. At present, perovskite quantum dots become research hotspots of luminescent materials in the display field, and have huge market potential.
Disclosure of Invention
The present invention is mainly based on the following problems and findings:
because perovskite quantum dots are less stable and are susceptible to water oxygen during use, they generally need to be encapsulated with a barrier layer. In order to improve the stability of perovskite quantum dots and the adhesiveness between the perovskite quantum dot layer and the barrier layer, tetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), ethylene-tetrafluoroethylene copolymer (ETFE), polyvinyl fluoride (PVF) and the like are adopted as polymer matrixes to prepare the perovskite quantum dot composite film comprising the all-inorganic perovskite quantum dot layer, an upper water oxygen barrier layer, a pressure-sensitive adhesive layer and a lower water oxygen barrier layer, wherein the pressure-sensitive adhesive layer is used for bonding the all-inorganic perovskite quantum dot layer and the lower water oxygen barrier layer. For another example, it has been proposed to use PVDF, PMMA, polyacrylamide, bisphenol a epoxy acrylate, polyacrylonitrile, etc. as a polymer matrix, at least a portion of at least one surface of the formed perovskite quantum dot-polymer layer is coated with a transition layer, and then a layer of oily acrylate pressure-sensitive adhesive is coated on the transition layer, and then is compounded with a barrier layer. For another example, it is proposed to coat a PVDC source on the surface of the barrier layer to obtain a PVDC coated layer, so as to improve the binding force between the barrier layer and the perovskite quantum dot layer, but the PVDC source adopted in the method is PVDC emulsion, and an emulsifier in the PVDC emulsion may damage the perovskite quantum dot to affect the stability of the perovskite quantum dot. For another example, it has been proposed to use styrene-butadiene-styrene (SBS), styrene-ethylene/propylene-styrene (SEPS) and styrene-isoprene-styrene (SIS) as polymer substrates, mix with perovskite quantum dots and apply the mixture to a barrier layer to obtain a perovskite quantum dot composite film, but the styrene-based hot-melt pressure-sensitive adhesive resin adopted in the method is unfavorable for the growth of perovskite quantum dots in terms of molecular composition, and the method forms the composite film in a hot-press bonding manner, so that the hot-press temperature is high, damage to the quantum dots is likely to occur, and meanwhile, the preparation process needs to be subjected to vacuum drying treatment, which is unfavorable for industrial implementation.
The present invention aims to solve at least one of the technical problems in the related art to some extent. To this end, an object of the present invention is to propose a perovskite quantum dot composite film and a method for preparing the same. The perovskite quantum dot composite film not only has good bonding stability, water resistance, weather resistance, optical property and high transparency, but also has a simple film structure and a convenient production process, and is beneficial to mass industrialized production.
In one aspect of the invention, a perovskite quantum dot composite film is provided. According to an embodiment of the present invention, the composite film includes:
a first barrier layer;
the perovskite quantum dot layer is arranged on one surface of the first barrier layer, the perovskite quantum dot layer comprises perovskite quantum dots and a polymer matrix, and monomers forming the polymer matrix comprise a water-blocking monomer and an adhesion promoting monomer;
a second barrier layer disposed on a surface of the perovskite quantum dot layer remote from the first barrier layer,
wherein the water blocking monomer comprises a fluoroacrylate monomer and the adhesion promoting monomer comprises a group for forming hydrogen bonds with the first barrier layer and the second barrier layer.
The perovskite quantum dot composite film according to the embodiment of the invention has at least the following beneficial effects: 1) The fluorine-containing acrylic ester monomer is introduced into the polymer matrix of the perovskite quantum dot layer, so that the fluorine-containing acrylic ester polymer can be polymerized, and the fluorine-containing acrylic ester polymer has good optical performance and electrical performance due to the small atomic radius of fluorine atoms, small polarization rate, low refractive index and high electronegativity; on the other hand, as the fluorine-containing side chain groups in the polymer can be subjected to phase separation at the molecular level, the side chain fluorine-containing groups (such as fluorine-containing alkyl) extend outwards from the main chain of the polymer and are arranged in an oriented manner to form an ordered comb-shaped structure, and the electron cloud of fluorine atoms has a shielding protection effect on the main chain and internal molecules, so that the stability of the main chain is enhanced, the water resistance, weather resistance and chemical inertness of a polymer matrix in the perovskite quantum dot layer are improved, and the stability of the perovskite quantum dot composite film is enhanced; on the other hand, the fluorine-containing acrylate polymer is favorable for the growth of perovskite quantum dots, meanwhile, fluorine atoms can form stronger and uniform interaction with methylamine ions forming the perovskite quantum dots, and along with the polymerization of the fluorine-containing acrylate and the arrangement of polymer molecular chains, the fluorine-containing acrylate polymer is favorable for enhancing the dispersing effect of the perovskite quantum dots in a polymer matrix and promoting the uniform distribution of the perovskite quantum dots in a perovskite quantum dot layer; furthermore, the polyacrylate has better adhesiveness, so that the adhesive strength of the perovskite quantum dot layer and the barrier layer is also improved, and the protective effect on the perovskite quantum dot is enhanced; 2) By introducing the adhesion promoting monomer, the formed polymer matrix can contain groups capable of combining with the first barrier layer and the second barrier layer to form hydrogen bonds, and the perovskite quantum dot layer and the barrier layer form hydrogen bonds, so that the overall bonding strength of the perovskite quantum dot composite film is improved, and the service stability of the perovskite quantum dot composite film is further improved.
In addition, the perovskite quantum dot composite film according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, the water-blocking monomer is used in an amount of no less than 5wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the adhesion promoting monomer is used in an amount of no less than 45wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the adhesion promoting monomer comprises a hydroxyl-containing acrylate monomer and/or a furan ring-containing acrylate monomer.
In some embodiments of the invention, the water blocking monomer comprises at least one of trifluoroethyl acrylate, trifluoroethyl methacrylate, hexafluoroisopropyl acrylate, hexafluorobutyl methacrylate, octafluoropentyl acrylate, pentafluorophenyl acrylate, dodecafluoroheptyl acrylate, heptafluorobutyl acrylate, fluorooctyl ethyl acrylate, fluorooctyl methacrylate, fluorohexyl ethyl acrylate, perfluorohexyl methacrylate.
In some embodiments of the invention, the water-blocking monomer is used in an amount of 5 to 20wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the adhesion promoting monomer is used in an amount of 45 to 75wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the peel force of the perovskite quantum dot composite film is 5 to 25N/25mm.
In yet another aspect of the present invention, a method of preparing the perovskite quantum dot composite film described above is provided. According to an embodiment of the invention, the method comprises: (1) Mixing a water-blocking monomer, an adhesion promoting monomer, an initiator and a first solvent to obtain a first mixed solution, and carrying out polymerization reaction on the first mixed solution to obtain a polymer matrix solution; (2) Mixing a precursor and a ligand for forming perovskite quantum dots with a second solvent to obtain a second mixed solution; (3) Mixing the polymer matrix solution with the second mixed solution to obtain perovskite quantum dot layer coating solution; (4) Coating the perovskite quantum dot layer coating liquid on one surface of a first barrier layer so as to obtain a perovskite quantum dot layer; (5) Covering a second barrier layer on the surface of the perovskite quantum dot layer, which is far away from the first barrier layer, so as to obtain a perovskite quantum dot composite film; wherein the water blocking monomer comprises a fluoroacrylate monomer and the adhesion promoting monomer comprises a group for forming hydrogen bonds with the first barrier layer and the second barrier layer.
Compared with the prior art, the method is not only beneficial to improving the optical performance, the bonding stability, the water resistance, the weather resistance and the transparency of the perovskite quantum dot composite film, but also simple in preparation process and beneficial to realizing industrialized mass production.
In addition, the method for preparing the perovskite quantum dot composite film according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, in step (1), the mixing further comprises: the general acrylate monomer was added.
In some embodiments of the invention, the universal acrylate monomer is used in an amount of 15 to 45wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the initiator is used in an amount of 0.5 to 6wt% based on the total mass of monomers forming the polymer matrix.
In some embodiments of the invention, the first solvent is used in an amount of 65 to 85wt% based on the total mass of the first mixed liquor.
In some embodiments of the invention, the initiator comprises 2, 2-azobisisobutyronitrile and/or benzoyl peroxide.
In some embodiments of the invention, the first solvent comprises ethyl acetate.
In some embodiments of the present invention, in step (2), the precursor comprises a first precursor comprising a compound of formula PbX and a second precursor 2 A compound of the type wherein the second precursor comprises a metal halide of the formula AX, wherein A comprises CH 3 NH 2 、CH(NH)NH 2 At least one of Cs, X includes at least one of F, cl, br, I.
In some embodiments of the invention, the ligand comprises at least one of butylamine, n-octylamine, dodecylamine, oleylamine, oleic acid, 2-dicarboxydiphenyl, alkylphosphinic acid, 3-diphenylpropylamine, n-dodecylmercaptan, trioctylphosphine oxide.
In some embodiments of the invention, the second solvent comprises N, N-dimethylformamide.
In some embodiments of the invention, the first precursor is used in an amount of 2 to 20wt%, the second precursor is used in an amount of 2 to 5wt%, the ligand is used in an amount of 1 to 5wt%, and the second solvent is used in an amount of 70 to 95wt%, based on the total mass of the second mixture.
In some embodiments of the present invention, in step (3), the second mixed solution is contained in an amount of 0.1 to 5wt% based on the total mass of the perovskite quantum dot layer coating solution.
In still another aspect of the present invention, the present invention provides a display device, which is prepared by using the perovskite quantum dot composite film and/or the perovskite quantum dot composite film obtained by the method according to the embodiment of the present invention. Compared with the prior art, the display device has all technical characteristics and effects of the perovskite quantum dot composite film and the method for preparing the perovskite quantum dot composite film, and the description is omitted herein. In general, the display device has the advantages of simple preparation process, higher luminous efficiency, better use stability and lower cost.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of a perovskite quantum dot composite film according to one embodiment of the invention;
FIG. 2 is a flow chart of a method of preparing a perovskite quantum dot composite film according to one embodiment of the invention;
Fig. 3 is a graph of the emission spectrum of a perovskite quantum dot composite film according to example 2 of the invention.
Reference numerals:
10-a first barrier layer; 11-a side of the first barrier layer remote from the perovskite quantum dot layer; 12-one side of the first barrier layer contacted with the perovskite quantum dot layer; a 20-perovskite quantum dot layer; 21-perovskite quantum dots; 22-a polymer matrix; 30-a second barrier layer; 31-a side of the second barrier layer remote from the perovskite quantum dot layer; 32-the side of the second barrier layer in contact with the perovskite quantum dot layer.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention. In the description of the present invention, it should be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In one aspect of the invention, a perovskite quantum dot composite film is provided. As understood in connection with fig. 1, the composite membrane includes: a first barrier layer 10, a perovskite quantum dot layer 20, and a second barrier layer 30, the perovskite quantum dot layer 20 being provided on one surface of the first barrier layer 10, the perovskite quantum dot layer 20 including perovskite quantum dots 21 and a polymer matrix 22, monomers forming the polymer matrix 22 including a water blocking monomer and an adhesion promoting monomer; the second barrier layer 30 is provided on the surface of the perovskite quantum dot layer 20 remote from the first barrier layer 10, wherein the water-blocking monomer comprises a fluoroacrylate monomer and the adhesion promoting monomer comprises a group for forming hydrogen bonds with the first barrier layer and the second barrier layer.
The perovskite quantum dot composite film according to the embodiment of the invention has at least the following beneficial effects: 1) The fluorine-containing acrylic ester monomer is introduced into the polymer matrix of the perovskite quantum dot layer, so that the fluorine-containing acrylic ester polymer can be polymerized, and the fluorine-containing acrylic ester polymer has good optical performance and electrical performance due to the small atomic radius of fluorine atoms, small polarization rate, low refractive index and high electronegativity; on the other hand, as the fluorine-containing side chain groups in the polymer can be subjected to phase separation at the molecular level, the side chain fluorine-containing groups (such as fluorine-containing alkyl) extend outwards from the main chain of the polymer and are arranged in an oriented manner to form an ordered comb-shaped structure, and the electron cloud of fluorine atoms has a shielding protection effect on the main chain and internal molecules, so that the stability of the main chain is enhanced, the water resistance, weather resistance and chemical inertness of a polymer matrix in the perovskite quantum dot layer are improved, and the stability of the perovskite quantum dot composite film is enhanced; on the other hand, the fluorine-containing acrylate polymer is favorable for the growth of perovskite quantum dots, meanwhile, fluorine atoms can form stronger and uniform interaction with methylamine ions forming the perovskite quantum dots, and along with the polymerization of the fluorine-containing acrylate and the arrangement of polymer molecular chains, the fluorine-containing acrylate polymer is favorable for enhancing the dispersing effect of the perovskite quantum dots in a polymer matrix and promoting the uniform distribution of the perovskite quantum dots in a perovskite quantum dot layer; furthermore, the polyacrylate has better adhesiveness, so that the adhesive strength of the perovskite quantum dot layer and the barrier layer is also improved, and the protective effect on the perovskite quantum dot is enhanced; 2) By introducing the adhesion promoting monomer, the formed polymer matrix can contain groups capable of combining with the first barrier layer and the second barrier layer to form hydrogen bonds, and the perovskite quantum dot layer and the barrier layer form hydrogen bonds, so that the overall bonding strength of the perovskite quantum dot composite film is improved, and the service stability of the perovskite quantum dot composite film is further improved.
According to the embodiment of the invention, the amount of the water-blocking monomer may be not less than 5wt%, for example, may be 8wt%, 10wt%, 15wt%, 20wt%, 30wt%, 40wt%, 60wt%, or the like, based on the total mass of the monomers forming the polymer matrix, and the inventor finds that if the amount of the water-blocking monomer is too small, the formed polymer matrix has too small fluorine atom content, not only the growth and the dispersion effect of the perovskite quantum dots are affected, but also the water-blocking property, weather resistance and chemical inertness of the polymer matrix in the perovskite quantum dot layer are not improved, the protection effect of the polymer matrix on the perovskite quantum dot layer is not enhanced, and the stability of the perovskite quantum dot composite film is not improved. Further, according to some specific examples of the present invention, the amount of the water-blocking monomer may be 5 to 20wt%, for example, 6wt%, 9wt%, 12wt%, 16wt% or 18wt%, etc., based on the total mass of the monomers forming the polymer matrix, and the inventors found that if the amount of the water-blocking monomer is too large, it is difficult to further significantly improve the water-blocking property and weather resistance of the polymer matrix, and also cause an increase in production cost, and the present invention is advantageous not only in promoting the growth and dispersion of perovskite quantum dots, improving the stability of perovskite quantum dots, but also in further controlling the processing cost by controlling the amount of the water-blocking monomer within the above range. The specific type of the water-blocking monomer in the present invention is not particularly limited, and those skilled in the art can flexibly select the water-blocking monomer according to the actual situation, and for example, the water-blocking monomer may include at least one of trifluoroethyl acrylate, trifluoroethyl methacrylate, hexafluoroisopropyl acrylate, hexafluorobutyl methacrylate, octafluoropentyl acrylate, pentafluorophenyl acrylate, dodecafluoroheptyl acrylate, heptafluorobutyl acrylate, fluorooctyl ethyl acrylate, fluorooctyl methacrylate, fluorohexyl ethyl acrylate, and perfluorohexyl methacrylate.
According to the embodiment of the present invention, the amount of the adhesion promoting monomer may be not less than 45wt%, for example, 48wt%, 55wt%, 60wt%, 70wt%, 80wt%, or 90wt%, based on the total mass of the monomers forming the polymer matrix, and the inventors found that if the amount of the adhesion promoting monomer is too small, it is disadvantageous to improve the adhesive strength of the polymer matrix and the barrier layer, affecting the water-oxygen barrier effect of the barrier layer on the perovskite quantum dot layer. Further, according to some specific examples of the present invention, the adhesion promoting monomer may be used in an amount of 45 to 75wt%, for example, 50wt%, 58wt%, 65wt%, 72wt%, etc., based on the total mass of the monomers forming the polymer matrix, and the inventors found that if the adhesion promoting monomer is used in an excessive amount, it may result in a decrease in the amount of the water blocking monomer, which not only easily affects the growth of the perovskite quantum dots, but also adversely affects the water blocking, weather resistance, and chemical inertness of the polymer matrix in the perovskite quantum dot layer. The invention controls the dosage of the adhesion promoting monomer in the range, thereby being beneficial to considering the water resistance, weather resistance and bonding stability of the perovskite quantum dot composite film. The specific type of the adhesion promoting monomer is not particularly limited in the present invention, and those skilled in the art can flexibly select the monomer according to the actual situation, and preferably the monomer is an acrylate monomer containing hydroxyl groups and/or furan rings, and may include at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate, tetrahydrofuran methacrylate, 2-hydroxyethyl methacrylate phosphate, and 4-hydroxybutyl acrylate, thereby increasing the content of acrylate segments in the polymer matrix and further enhancing the bonding strength of the perovskite quantum dot layer and the barrier layer.
According to the embodiment of the invention, the monomer forming the polymer matrix can also comprise a general acrylate monomer, so that the chain segments formed by the water-blocking monomer and the adhesion promoting monomer are uniformly distributed in the total chain segments of the polymer matrix, the water-blocking property of the perovskite quantum dot layer and the adhesion with the barrier layer are improved, and the raw material cost can be reduced. Further, according to some specific examples of the present invention, the amount of the general acrylate monomer may be 15 to 45wt%, for example, 20wt%, 25wt%, 30wt%, 35wt%, 40wt%, etc., based on the total mass of the monomers forming the polymer matrix, and the inventors found that if the amount of the general acrylate is too small, the raw material cost increases; if the dosage of the general acrylic ester is too large, the water blocking and bonding stability of the perovskite quantum dot composite film can be affected. The invention is beneficial to considering the production cost and the use stability of the composite film by controlling the dosage of the universal acrylic ester monomer in the range. The specific type of the general acrylate monomer in the present invention is not particularly limited, and those skilled in the art can flexibly select the general acrylate monomer according to practical situations, and may include at least one of methyl acrylate, ethyl acrylate, butyl acrylate, and octyl acrylate, for example.
According to the embodiment of the invention, the perovskite quantum dot composite film is prepared into a polymer matrix by adding the water-blocking monomer, and the fluorine-containing acrylate polymer is introduced into the polymer matrix, so that the in-situ growth of the perovskite quantum dot in the polymer matrix is facilitated, the damage of water oxygen to the perovskite quantum dot is reduced, the use stability of the perovskite quantum dot composite film is enhanced, and the transparency of the composite film is also improved; on the other hand, the adhesion promoting monomer is introduced to prepare the polymer matrix, so that the adhesion strength of the perovskite quantum dot layer and the barrier layer is improved, the perovskite quantum dot layer can be directly attached to the barrier layer, the number of layers of the composite film can be reduced, surface treatment processes such as corona or under coating are not required for the barrier layer, the raw material and process cost can be reduced, the problem that the adhesion between the conventional perovskite quantum dot layer and the barrier layer is poor can be solved, specifically, the peeling force of the perovskite quantum dot composite film prepared by the method can be not lower than 5N/25mm, for example, can reach 5-25N/25 mm, and can be specifically 7N/25mm, 10N/25mm, 13N/25mm, 15N/25mm, 18N/25mm, 21N/25mm or 24N/25mm and the like, so that the adhesion requirement of the perovskite quantum dot layer and the barrier layer can be met, and the stability of the perovskite quantum dot is prevented or reduced.
In yet another aspect of the present invention, a method of preparing the perovskite quantum dot composite film described above is provided. As will be appreciated in connection with fig. 2, according to an embodiment of the invention, the method comprises:
s100: mixing a water-blocking monomer, an adhesion promoting monomer, an initiator and a first solvent to obtain a first mixed solution, and carrying out polymerization reaction on the first mixed solution to obtain a polymer matrix solution
According to the embodiment of the invention, the water-blocking monomer, the adhesion promoting monomer, the initiator and the first solvent are mixed, so that the water-blocking monomer and the adhesion promoting monomer can be dispersed in the solution, and simultaneously, the copolymerization reaction is carried out under the catalysis promoting effect of the initiator, so that the polymer comprising the fluorine-containing acrylate chain segment can be obtained, and meanwhile, the polymer contains groups capable of forming hydrogen bonds with the barrier layer, such as hydroxyl groups, furan rings and the like. The selection type, effect and amount of the water-blocking monomer and the adhesion promoting monomer in the present invention are described in detail in the foregoing sections, and are not repeated here. Furthermore, according to some specific examples of the present invention, the amount of the initiator may be 0.5 to 6wt%, for example, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, etc., based on the total mass of the monomers forming the polymer matrix, and the inventors found that if the amount of the initiator is too small, it may result in a slow polymerization reaction rate or even difficulty in complete reaction of the monomers; if the initiator is used in an excessive amount, the risk of reaction explosion increases. The invention is beneficial to controlling the polymerization reaction to be smoothly carried out by controlling the dosage of the initiator in the range. In addition, the amount of the first solvent may be 65 to 85wt% based on the total mass of the first mixed solution, for example, 70wt%, 75wt% or 80wt%, and the inventors found that if the amount of the first solvent is too small, the concentration of the monomer and the initiator in the first mixed solution is too high, explosion polymerization is easily initiated, and a safety hazard exists; if the amount of the first solvent is too large, on the one hand, the reaction efficiency is reduced, or even the reaction degree is insufficient, and on the other hand, resources are wasted. The present invention is also advantageous in controlling the rate and extent of the polymerization reaction by controlling the amount of the first solvent used in the above-mentioned range. It should be noted that, in the present invention, the specific types of the initiator and the first solvent are not particularly limited, and those skilled in the art can flexibly select according to practical situations, for example, the initiator may be 2, 2-azobisisobutyronitrile and/or benzoyl peroxide; the first solvent may include ethyl acetate and the like.
According to the embodiment of the present invention, a general acrylate monomer may be further added during the above mixing process, wherein the selection type, effect and amount of the acrylate are also described in detail in the foregoing sections, and are not described herein again.
According to the embodiment of the invention, the specific conditions of the mixing process and the polymerization process of the first mixed solution are not particularly limited, and a person skilled in the art can flexibly select according to practical situations, for example, a protective gas, for example, at least one of nitrogen, argon and helium, can be introduced into the reaction system (the first mixed solution) before the polymerization is performed, the flow rate of the protective gas can be controlled to be 1-10 mL/min, the temperature of the polymerization reaction can be 50-80 ℃ and the time can be 8-24 hours, so that the efficiency and the reaction degree of the polymerization reaction can be considered, and the polymer matrix with complete polymerization can be obtained.
S200: mixing the precursor and the ligand for forming the perovskite quantum dots with a second solvent to obtain a second mixed solution
According to an embodiment of the present invention, the second mixed solution, that is, the perovskite quantum dot precursor solution may be obtained by subjecting the precursor for forming the perovskite quantum dots, the ligand, to a mixing treatment in the second solvent. Wherein the precursor for forming the perovskite quantum dot may include a first precursor and a second precursor, the first precursor may include a compound having the formula PbX 2 A compound of the type, the second precursor may comprise a metal halide of the formula AX, wherein A may comprise CH 3 NH 2 、CH(NH)NH 2 At least one of Cs, X may include at least one of F, cl, br, I. In addition, the specific type of the ligand in the present invention is not particularly limited, and those skilled in the art can flexibly select the ligand according to the actual circumstances, and for example, the ligand may include butylamine, n-octylamine, dodecylamine, oleylamine, oleic acid, 2-dicarboxydiphenyl, alkylphosphinic acid, 3-diphenylpropylamine, n-dodecylmercaptan, trioctylphosphine,at least one of trioctylphosphine oxide. In addition, the specific type of the second solvent in the present invention is not particularly limited, and it is only required that the second solvent is miscible with the polymer matrix solution, for example, N-dimethylformamide or the like, so that the growth of perovskite quantum dots in the polymer matrix can be achieved in the same system.
According to an embodiment of the present invention, the amount of the first precursor may be 2 to 20wt%, for example, 5wt%, 12wt%, 15wt%, 18wt%, or the like, based on the total mass of the second mixed solution; the second precursor may be used in an amount of 2 to 5wt%, for example, 3wt%, 3.5wt%, 4wt%, 4.5wt%, or the like; the amount of the ligand may be 1 to 5wt%, for example, 1.5wt%, 2wt%, 3wt% or 4wt%, etc.; the second solvent may be used in an amount of 70 to 95wt%, for example, 75wt%, 80wt%, 85wt%, 90wt%, or the like. The inventor finds that if the first precursor is used too much or the second precursor is used too little, the excessive first precursor can be precipitated as solid in the film forming process of the subsequently formed perovskite quantum dot layer coating liquid; if the second precursor is excessively used or the first precursor is excessively used, excessive second precursor can be separated out as solid in the film forming process of the subsequently formed perovskite quantum dot layer coating liquid, and both the second precursor and the perovskite quantum dot layer coating liquid can influence the growth of the perovskite quantum dots and the stability of the perovskite quantum dot layer; in addition, the inventors found that if the amount of the second solvent is too small, incomplete dissolution of the precursor may be caused, and if the amount of the second solvent is too large, the film formation efficiency of the perovskite quantum dot layer may be hindered or slowed. The method is beneficial to promoting the growth stability of the perovskite quantum dots by controlling the dosage of the first precursor, the second precursor, the ligand and the second solvent in the range.
S300: mixing the polymer matrix solution with the second mixed solution to obtain perovskite quantum dot layer coating solution
According to the embodiment of the invention, the perovskite quantum dot coating liquid comprises a polymer matrix solution (comprising a polymer matrix and a first solvent) and a second mixed liquid (comprising a perovskite quantum dot precursor and a second solvent), the content of the second mixed liquid can be 0.1-5wt%, such as 0.5wt%, 1wt%, 2wt%, 3wt% or 4wt%, based on the total mass of the perovskite quantum dot layer coating liquid, and the inventor finds that when the dosage of the second mixed liquid is too small, the content of the perovskite quantum dots in the formed perovskite quantum dot layer is too small, and the effective luminous effect is difficult to realize; if the second mixed solution is used too much, the concentration of the precursor in the perovskite quantum dot layer coating solution is higher, agglomeration is easy to occur, and the growth of the perovskite quantum dots is influenced. The invention is beneficial to considering the growth and luminous effect of the perovskite quantum dots by controlling the dosage of the second mixed solution in the perovskite quantum dot layer coating solution in the range.
S400: coating a perovskite quantum dot layer coating liquid on one surface of the first barrier layer so as to obtain a perovskite quantum dot layer
According to the embodiment of the invention, after the perovskite quantum dot layer coating liquid is coated on one surface of the first barrier layer, the perovskite quantum dots can be crystallized and grown in the polymer matrix, specifically, the coated first barrier layer can be dried, as the solvent in the coating liquid volatilizes, due to hydrogen bonding action among precursor molecules of the perovskite quantum dots, when the critical nucleation concentration is reached, self-assembly can occur among the precursor molecules, inorganic metal cations can form coordination octahedron with halogen anions, organic amine cations can enter pores among adjacent octahedrons to form a hybridized perovskite structure, meanwhile, as the solvent is reduced, the chain segment movement of the polymer matrix is gradually limited, the surfaces of the formed perovskite particles are limited, the growth of the perovskite particles in the three-dimensional direction is limited, and the particle size is limited to the nanometer level, so that the perovskite quantum dot layer can be obtained. In the present invention, the coating method, the drying method, and the thickness of the perovskite quantum dot layer formed are not particularly limited, and those skilled in the art can flexibly select the coating method according to practical situations, for example, comma doctor blade coating, gravure coating, micro gravure coating, etc. can be used as the coating method; the coating speed can be 1-5 m/s; the drying temperature can be 25-80 ℃, and the drying mode can be that the first barrier layer coated with the perovskite quantum dot layer coating liquid is sequentially dried and solidified through drying channels in four temperature intervals; the thickness of the finally formed perovskite quantum dot layer may be 1 to 20 μm.
S500: covering a second barrier layer on the surface of the perovskite quantum dot layer far away from the first barrier layer so as to obtain the perovskite quantum dot composite film
According to the embodiment of the invention, after the second barrier layer is covered on the surface of the perovskite quantum dot layer far away from the first barrier layer, the perovskite quantum dot composite film can be obtained through lamination treatment, the specific conditions of the lamination treatment and the thickness of the perovskite quantum dot composite film after the lamination treatment are not particularly limited, and the perovskite quantum dot composite film can be flexibly selected by a person skilled in the art according to practical situations, for example, the lamination force can be 0.1-0.5 MPa, and the thickness of the composite film can be 101-420 mu m.
According to an embodiment of the present invention, as understood in conjunction with fig. 1, the side of the first barrier layer 10 and the second barrier layer 30 that is in contact with the perovskite quantum dot layer 20 may be the barrier side (as understood in conjunction with fig. 1, 12 and 32), and the side that is remote from the perovskite quantum dot layer may be the diffusion side (as understood in conjunction with fig. 1, 11 and 31). In addition, the specific material, thickness and water oxygen permeability of the barrier layer are not particularly limited in the present invention, and those skilled in the art can flexibly select according to practical situations, for example, the water vapor permeability of the first barrier layer and the second barrier layer can be respectively and independently (10 -2 ～10 -1 )g/m 2 The oxygen transmission rate per day can be (10) -2 ～10 -1 )mL/m 2 The day and the thickness can be respectively 50-200 μm, and the materials of the first barrier layer and the second barrier layer can respectively and independently comprise Al 2 O 3 、SiO 2 At least one of them.
In summary, according to the method for preparing the perovskite quantum dot composite film, compared with the prior art, the method is beneficial to improving the optical performance, the bonding stability, the water resistance, the weather resistance and the transparency of the perovskite quantum dot composite film, and is simple in preparation process and beneficial to realizing industrial mass production.
In still another aspect of the present invention, the present invention provides a display device, which is prepared by using the perovskite quantum dot composite film and/or the perovskite quantum dot composite film obtained by the method according to the embodiment of the present invention. Compared with the prior art, the display device has all technical characteristics and effects of the perovskite quantum dot composite film and the method for preparing the perovskite quantum dot composite film, and the description is omitted herein. In general, the display device has the advantages of simple preparation process, higher luminous efficiency, better use stability and lower cost.
Embodiments of the present invention are described in detail below. The following examples are illustrative only and are not to be construed as limiting the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
(1) Respectively carrying out reduced pressure distillation refining on raw materials of Butyl Acrylate (BA), hydroxyethyl acrylate (HEA) and hexafluoroisopropyl acrylate (HFIA) which are sold in the market, adding 84g of the refined Butyl Acrylate (BA), 226g of hydroxyethyl acrylate (HEA) and 40g of hexafluoroisopropyl acrylate (HFIA) into a reaction bottle, adding 4.5g of Azobisisobutyronitrile (AIBN) and 1200g of Ethyl Acetate (EA) into the reaction bottle, mechanically stirring at a rotating speed of 500r/min to obtain a first mixed solution, introducing nitrogen into the reaction bottle at a flow rate of 1mL/min, blowing residual air in a system, heating the first mixed solution to 58 ℃ for reaction after 2h, continuously reacting the first mixed solution to 60 ℃ after 4h, and discharging after 12h to obtain 1500g of polymer matrix solution;
(2) Mixing 14.2g of lead bromide, 3.6g of cesium bromide, 2.4g of methylamine bromide, 4.8g of 3, 3-diphenylpropylamine and 175g of N, N-dimethylformamide, and stirring at normal temperature to completely dissolve the solid to obtain 200g of a second mixed solution;
(3) Adding 15g of a second mixed solution into 1500g of the polymer matrix solution prepared in the step (1), and mechanically stirring at a rotating speed of 500r/min for 6 hours to obtain a perovskite quantum dot layer coating solution; coating the perovskite quantum dot layer coating liquid on the barrier surface of the first barrier layer in a comma coating mode, wherein the thickness of a wet film is 50 mu m, the coating speed is 5m/s, drying is carried out through drying channels with the temperature interval of 50 ℃,55 ℃,60 ℃ and 65 ℃, and then the perovskite quantum dot composite film with the thickness of 270 mu m is obtained by bonding the wound part and the barrier surface of the second barrier layer at the pressure of 0.2 MPa.
Example 2
The difference from example 1 is that: in the step (1), the amount of the refined butyl acrylate is 79g, the amount of the hydroxyethyl acrylate is 211g, and the amount of the hexafluoroisopropyl acrylate is 60g.
Example 3
The difference from example 1 is that: in the step (1), the amount of butyl acrylate after refining was 129g, the amount of hydroxyethyl acrylate was 170g, and the amount of hexafluoroisopropyl acrylate was 51g.
Example 4
The difference from example 1 is that: in the step (1), the amount of the refined butyl acrylate is 93g, the amount of the hydroxyethyl acrylate is 220g, and the amount of the hexafluoroisopropyl acrylate is 37g.
Example 5
The difference from example 1 is that: in the step (1), the amount of the refined butyl acrylate is 76g, the amount of the hydroxyethyl acrylate is 204g, and the amount of the hexafluoroisopropyl acrylate is 70g.
Example 6
The difference from example 1 is that: in the step (1), the amount of the refined butyl acrylate is 150g, the amount of the hydroxyethyl acrylate is 140g, and the amount of the hexafluoroisopropyl acrylate is 60g.
Comparative example 1
The difference from example 1 is that: the step (1) is as follows: 350g of polyvinylidene fluoride (PVDF) are dissolved in 1150g of DMF and mixed uniformly by mechanical stirring to obtain 1500g of polymer matrix solution.
Testing and analysis
Under the same conditions, the perovskite quantum dot composite films prepared in examples 1 to 6 and comparative example 1 were characterized by the following test methods, and the characterization contents include: peeling force of the perovskite quantum dot composite film, emission spectrum of the perovskite quantum dot composite film before and after aging, and failure edge of the perovskite quantum dot composite film after aging. The specific steps of the aging treatment for examples 1 to 6 and comparative example 1 are as follows: under the same conditions, perovskite quantum dot composite film samples prepared in the examples 1-6 and the comparative example 1 are cut into 10cm multiplied by 10cm sample pieces, and the sample pieces are placed at 60 ℃ and continuously aged for 500 hours in a constant temperature and humidity box with 90% RH.
Failure edge: taking out the aged perovskite quantum dot composite film, and measuring the failure edge of the perovskite quantum dot composite film by using a magnifying glass with scales;
cutting the perovskite quantum dot composite film into 200mm multiplied by 25mm, wherein the peeling speed is 300mm/min, and performing 180-degree peeling test by using a tensile machine to obtain the peeling force value.
The peel force of the perovskite quantum dot composite films prepared in examples 1 to 6 and comparative example 1 and the test results of the failure edge of the perovskite quantum dot composite film after aging are shown in table 1.
TABLE 1 stripping force and failure edge test results of perovskite Quantum dot composite films produced in examples 1 to 6 and comparative example 1
Results and discussion
The perovskite quantum dot composite films prepared in the examples and the comparative examples were subjected to aging analysis, and according to the emission spectra of the perovskite quantum dot composite films before and after aging, the perovskite quantum dot composite films prepared in the above examples of the present invention have good aging resistance stability. For example, taking the composite film prepared in example 2 as an example, two curves in fig. 3 are respectively an emission spectrum diagram before and after aging of the perovskite quantum dot composite film prepared in example 2, and as can be seen from fig. 3, the emission spectrum peak position of the composite film before aging is 525nm, the half-peak width is 24nm, and the half-peak width is narrower; the emission spectrum of the composite film after aging and the emission spectrum of the composite film before aging do not have obvious change, which indicates that the perovskite quantum dot composite film has better aging resistance stability.
In addition, as can be seen from the data in table 1, examples 1 to 6 can have higher peel strength by employing the perovskite quantum dot composite film of the above-described example of the invention without significantly increasing the failure edge after aging, as compared with comparative example 1. Further, as shown in table 1, as the amount of the water-blocking monomer (for example, HFIA) increases, the failure edge decreases, which indicates that the addition of the water-blocking monomer can effectively improve the long-term use stability of the perovskite quantum dot composite film; in addition, with the increase of the dosage of the adhesion promoting monomer (HEA for example), the peeling force is improved, and the addition of the surface adhesion promoting monomer can effectively enhance the bonding strength of the perovskite quantum dot composite film. The dosage of the water-blocking monomer and the adhesion promoting monomer in the polymer matrix can be flexibly adjusted according to actual needs by a person skilled in the art, so that the perovskite quantum dot composite film with better stripping force and/or failure edges is obtained.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. A perovskite quantum dot composite film, comprising:
a first barrier layer;
the perovskite quantum dot layer is arranged on one surface of the first barrier layer, the perovskite quantum dot layer comprises perovskite quantum dots and a polymer matrix, and monomers forming the polymer matrix comprise a water-blocking monomer and an adhesion promoting monomer;
a second barrier layer disposed on a surface of the perovskite quantum dot layer remote from the first barrier layer,
wherein the water blocking monomer comprises a fluoroacrylate monomer and the adhesion promoting monomer comprises a group for forming hydrogen bonds with the first barrier layer and the second barrier layer.
2. The perovskite quantum dot composite film according to claim 1, wherein the amount of the water-blocking monomer is not less than 5wt% based on the total mass of monomers forming the polymer matrix; and/or the adhesion promoting monomer is used in an amount of not less than 45wt%.
3. The perovskite quantum dot composite film according to claim 1, wherein the adhesion promoting monomer comprises a hydroxyl-containing acrylate monomer and/or a furan ring-containing acrylate monomer; and/or the number of the groups of groups,
the water-blocking monomer comprises at least one of trifluoroethyl acrylate, trifluoroethyl methacrylate, hexafluoroisopropyl acrylate, hexafluorobutyl methacrylate, octafluoropentyl acrylate, pentafluorophenyl acrylate, dodecafluoroheptyl acrylate, heptafluorobutyl acrylate, fluorooctyl ethyl acrylate, fluorooctyl methacrylate, fluorohexyl ethyl acrylate and perfluorohexyl methacrylate.
4. The perovskite quantum dot composite film according to claim 1, wherein the amount of the water-blocking monomer is 5 to 20wt% based on the total mass of monomers forming the polymer matrix; and/or the adhesion promoting monomer is used in an amount of 45 to 75wt%.
5. The perovskite quantum dot composite film according to any one of claims 1 to 4, wherein the peeling force of the perovskite quantum dot composite film is 5 to 25N/25mm.
6. A method of preparing the perovskite quantum dot composite film as claimed in any one of claims 1 to 5, comprising:
(1) Mixing a water-blocking monomer, an adhesion promoting monomer, an initiator and a first solvent to obtain a first mixed solution, and carrying out polymerization reaction on the first mixed solution to obtain a polymer matrix solution;
(2) Mixing a precursor and a ligand for forming perovskite quantum dots with a second solvent to obtain a second mixed solution;
(3) Mixing the polymer matrix solution with the second mixed solution to obtain perovskite quantum dot layer coating solution;
(4) Coating the perovskite quantum dot layer coating liquid on one surface of a first barrier layer so as to obtain a perovskite quantum dot layer;
(5) Covering a second barrier layer on the surface of the perovskite quantum dot layer, which is far away from the first barrier layer, so as to obtain a perovskite quantum dot composite film;
wherein the water blocking monomer comprises a fluoroacrylate monomer and the adhesion promoting monomer comprises a group for forming hydrogen bonds with the first barrier layer and the second barrier layer.
7. The method of claim 6, wherein in step (1), the mixing further comprises: adding a general acrylate monomer;
optionally, the universal acrylate monomer is used in an amount of 15 to 45wt%, based on the total mass of monomers forming the polymer matrix;
Optionally, the initiator is used in an amount of 0.5 to 6wt%, based on the total mass of monomers forming the polymer matrix;
optionally, the amount of the first solvent is 65 to 85wt% based on the total mass of the first mixed solution;
optionally, the initiator comprises 2, 2-azobisisobutyronitrile and/or benzoyl peroxide;
optionally, the first solvent comprises ethyl acetate.
8. The method of claim 6, in step (2), the precursor comprises a first precursor comprising a compound of formula PbX and a second precursor 2 A compound of the type wherein the second precursor comprises a metal halide of the formula AX, wherein A comprises CH 3 NH 2 、CH(NH)NH 2 At least one of Cs, X comprises at least one of F, cl, br, I;
optionally, the ligand comprises at least one of butylamine, n-octylamine, dodecylamine, oleylamine, oleic acid, 2-dicarboxyidiphenylamine, alkylphosphinic acid, 3-diphenylpropylamine, n-dodecylmercaptan, trioctylphosphine oxide;
optionally, the second solvent comprises N, N-dimethylformamide;
optionally, the amount of the first precursor is 2 to 20wt%, the amount of the second precursor is 2 to 5wt%, the amount of the ligand is 1 to 5wt%, and the amount of the second solvent is 70 to 95wt%, based on the total mass of the second mixed solution.
9. The method according to claim 6, wherein in the step (3), the content of the second mixed liquid is 0.1 to 5wt% based on the total mass of the perovskite quantum dot layer coating liquid.
10. A display device, characterized in that the perovskite quantum dot composite film according to any one of claims 1 to 5 and/or the perovskite quantum dot composite film obtained by the method according to any one of claims 7 to 9 is used.
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