CN110551304A - Cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film - Google Patents
Cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
the invention relates to a cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film, and belongs to the field of preparation of all-inorganic perovskite quantum dots. The preparation method of the composite film comprises the following steps: 1) dissolving lead halide, cesium halide and a surface ligand in a first solvent to prepare a precursor solution; 2) dropwise adding the precursor solution into the polymer solution under stirring to obtain a colloidal solution; preparing a film by using a colloidal solution; the polymer solution is prepared by dissolving a transparent polymer material in a second solvent, wherein the second solvent does not dissolve the cesium-lead halogen quantum dots. The cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film provided by the invention realizes the generation of quantum dots and the in-situ encapsulation of polymer resin, has the advantages of simple whole process flow, strong repeatability, small pollution in the production process, low energy consumption, wide raw material source, realization of batch production and good practical effect.
Description
Technical Field
The invention belongs to the field of preparation of all-inorganic perovskite quantum dots, and particularly relates to a cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film.
Background
3Quantum Dots (QDs) are nano materials defined in a zero-dimensional quantum system and are particles limited in three-dimensional directions, and the quantum effect is a quantum size effect, a quantum confinement effect and a surface effect, when the particle size is smaller than a certain value, an electron level near a fermi level is changed into a discontinuous energy level, a phenomenon that an energy gap is widened occurs, electrons are in a bound state, excitons are easily formed, the specific surface area of the quantum dots is large, the surface activity is high, and defects are easily generated.
Compared with the traditional semiconductor quantum dot, the CsPbX 3 quantum dot material has the following performance advantages that (1) the band gap width of a nanocrystal can be changed through halogen proportion adjustment, so that the luminescence of the nanocrystal can cover the whole visible light range, (2) the nanocrystal with different emission wavelengths can be excited by a single light source with the wavelength of 350-400 nm, (3) the color purity is high, the half-height width of an emission peak is only 12-42 nm and is much narrower than that of the traditional quantum dot and an organic dye, and (4) the defect tolerance is high, so that the fluorescence quantum yield can reach 100% under the condition of no passivation modification, the application foundation of the material in the fields of photoelectric devices, biomedicine and the like is laid.
The sensitivity of cesium-lead halide quantum dots to polar solvents directly affects its application. In a polar solvent (such as water) environment, the fluorescence characteristics of the quantum dots rapidly degrade for a short time until the fluorescence characteristics disappear. The solubility of the cesium-lead halogen perovskite in a polar solvent is high, and even a low dosage of the polar solvent can cause the decomposition of quantum dots, so that the structure of the quantum dots is damaged, and the luminescence of the quantum dots is influenced. Research shows that after the quantum dots are soaked in water for 3 hours, the fluorescence performance of the quantum dots is reduced by about 80%. In addition, when the perovskite quantum dots are in the air for a long time, the quantum dots are decomposed under the combined action of water and oxygen in the air, and the long-term stability of the perovskite quantum dots is seriously influenced.
The application publication number of CN108034391A of Chinese invention discloses a solar cell EVA (ethylene-vinyl acetate copolymer) packaging adhesive film material with a light conversion function and a preparation method thereof, wherein EVA is dissolved in dichloromethane to form a dichloromethane solution of EVA, cesium-lead halogen quantum dots are dispersed in an organic solvent to form a dispersion solution, the dispersion solution is added into the dichloromethane solution of EVA, a cross-linking agent is added for reaction, and then the reaction product is dried to form a film, so that the transparent light conversion adhesive film material is prepared.
The existing composite film material is prepared by mixing cesium-lead halide quantum dot dispersion liquid and EVA solution, in the preparation process, cesium-lead halide quantum dots undergo multiple stages of reaction generation, separation precipitation, redispersion and the like, the stability of the cesium-lead halide quantum dots is poor due to sensitivity of all-inorganic cesium-lead halide quantum dots to air, water and polar solvents, and the structures of the quantum dots are easy to damage in the multiple operation and transfer processes, so that the luminescence performance of a film product is poor.
Disclosure of Invention
The invention aims to provide a cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film to solve the problem that the luminescent performance of quantum dots is poor due to the fact that the quantum dot structure is easily damaged by an existing method.
In order to achieve the purpose, the technical scheme of the cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film is as follows:
A cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film is prepared by the following steps:
1) Dissolving lead halide, cesium halide and a surface ligand in a first solvent to prepare a precursor solution;
2) dropwise adding the precursor solution into the polymer solution under stirring to obtain a colloidal solution; preparing a film by using a colloidal solution; the polymer solution is prepared by dissolving a transparent polymer material in a second solvent, wherein the second solvent does not dissolve the cesium-lead halogen quantum dots.
According to the cesium-lead-halogen inorganic perovskite quantum dot/transparent polymer composite film provided by the invention, a supersaturated recrystallization method is utilized to crystallize and precipitate cesium-lead-halogen quantum dots in a second solvent, the quantum dots are positioned in a network structure of polymer resin while being synthesized, and the resin wraps the quantum dots after drying to form the composite film material. The quantum dots obtained by the method of supersaturated recrystallization have small and uniform particle size, good dispersibility and good luminous performance, and the method realizes the generation of the quantum dots and the in-situ encapsulation of the polymer resin, and has the advantages of simple whole process flow, strong repeatability, small pollution in the production process, less energy consumption, wide raw material source, realization of batch production and good practical effect.
In order to promote the formation of the cesium-lead halogen quantum dots with small particle size, good dispersion and avoidance of agglomeration, preferably, in the step 2), the volume ratio of the precursor solution to the polymer solution is (0.1-2): 10-20.
In order to accelerate the rapid synthesis of the cesium-lead halogen quantum dots and promote the precipitation of a fine crystal structure, it is preferable that the temperature of the polymer solution in the step 2) is 60-90 ℃.
In order to further optimize the crystallization effect of the precursor solution in the polymer solution, preferably, in the step 1), the concentration of the lead halide in the precursor solution is 0.01-0.05 mol/L; in the step 2), the concentration of the macromolecular solution is 0.01-1 g/mL.
In order to achieve better passivation and stabilization effects, it is preferable that in step 1), the surface ligands are oleic acid and oleylamine, the volume ratio of oleic acid to oleylamine is (1.5-2.5):1, and the molar ratio of oleic acid to lead halide is (7-9): 1.
The first solvent may be capable of dissolving the lead halide, cesium halide and the surface ligand, and is preferably N, N-dimethylformamide or dimethylsulfoxide in view of raw material cost. The second solvent is preferably selected such that the smaller the solubility of the cesium-lead halide quantum dots, the better, and in step 2), the second solvent is toluene or n-hexane.
the choice of the polymer matrix is not particularly limited, and in order to make the film material have the characteristics of good water resistance, transparency and high flexibility, preferably, the transparent polymer material is ethylene-vinyl acetate copolymer (EVA). The cesium-lead halogen perovskite quantum dots are wrapped by EVA, so that the quantum dots can be prevented from contacting water and oxygen molecules in the air, the stability of the quantum dot film is improved, and related products are expected to have good application in the fields of white light LEDs, flexible display and the like.
Drawings
FIG. 1 is a TEM (a), HRTEM (b) and a size distribution diagram (c) of cesium-lead halide inorganic perovskite quantum dots obtained in example 1 of the present invention;
FIG. 2 is an XRD pattern of thin film materials of examples of the present invention and comparative examples;
FIG. 3 is a FT-IR chart of film materials of examples of the invention and comparative examples;
FIG. 4 shows SEM (a) and EDS (EDS Spectroscopy) spectra of the surface of the CsPbBr 3/EVA film prepared in example 1, wherein the EDS spectra respectively show four elements, namely (b) C, (C) Cs, (d) Br and (e) Pb;
FIG. 5 is a Photoluminescence (PL) spectrum of thin film materials of examples of the present invention and comparative examples;
FIG. 6 is a full width at half maximum (FWHM) plot of thin film materials of examples and comparative examples of the present invention;
FIG. 7 is a PL spectrum of a composite film material of example 1 after different soaking times;
FIG. 8 is a graph of strength retention of the composite film material of example 1 of the present invention after various soaking times;
FIG. 9 is a PL spectrum of a composite thin film material of example 1 of the present invention after a long-term standing;
FIG. 10 is a graph showing the strength retention of the composite film material of example 1 of the present invention after a long-term storage.
Detailed Description
The following examples are provided to further illustrate the practice of the invention.
First, a specific embodiment of the cesium-lead halide inorganic perovskite quantum dot/transparent polymer composite film of the present invention
Example 1
The cesium-lead halide inorganic perovskite quantum dot/transparent polymer composite film is prepared by the following steps:
1) Weighing 0.0734g of PbBr 2 and 0.0425g of CsBr powder, dissolving in 5mL of N, N-Dimethylformamide (DMF), stirring for 30min (stirring speed is 200rpm) to fully dissolve, then dropwise adding 0.5mL (OA) of surface ligand oleic acid and 0.25mL (OAm) of oleylamine, stirring for 5min (stirring speed is 200rpm), and obtaining a precursor solution after complete dissolution;
2) Putting ethylene-vinyl acetate copolymer (EVA) resin particles and a polytetrafluoroethylene circular mold into absolute ethyl alcohol, performing ultrasonic treatment for 30min (ultrasonic power is 400W), and drying for later use, wherein the diameter of the mold is 1.5mm, and the groove depth is 0.5 mm; 1g of EVA resin particles was weighed and added to 10mL of toluene, and stirred at 70 ℃ for 30min (stirring speed of 200rpm) to be sufficiently dissolved, thereby obtaining an EVA solution.
3) 0.2mL of precursor solution is sucked by a dropper and is dripped into EVA at 70 ℃ and 200rpm, the solution is changed from a colorless transparent state to a yellow state, the reaction process is very quick, the reaction can be completed within a few seconds, and after the dripping is completed, the colloidal solution of the all-inorganic perovskite quantum dot (CsPbBr 3) can be obtained.
4) And (3) dropwise adding the colloidal solution obtained in the step 3) into a polytetrafluoroethylene mold groove, placing the polytetrafluoroethylene mold groove in a 70 ℃ oven for drying for 3 hours, and demolding to obtain the CsPbBr 3/EVA film composite material.
Examples 2 to 5
The difference between the cesium-lead halide inorganic perovskite quantum dot/transparent polymer composite thin film of the present example and the preparation method of example 1 is only that the drop amount of the precursor solution in step 3) is 0.1mL, 0.4mL, 0.6mL, and 0.8 mL.
Example 6
the difference between the cesium-lead halide inorganic perovskite quantum dot/transparent polymer composite film of the embodiment and the preparation method of the embodiment 1 is only that in the step 3), the stirring speed is 300 rpm; the temperature of the polymer solution was 80 ℃.
Second, comparative example
The film of the comparative example was prepared in a manner different from that of example 1 in that the amount of the precursor solution added in step 3) was 0 mL.
Third, Experimental example
Experimental example 1
this experimental example examined the TEM, HRTEM and size distribution of the cesium-lead halide inorganic perovskite quantum dots obtained in example 1, and the results are shown in fig. 1.
As can be seen from fig. 1, the size distribution of the CsPbBr 3 quantum dots prepared in the examples is very uniform, the specific size is uniformly distributed in the range of 8.5-11.5nm, the average size is 10nm, due to the quantum size effect, the increase or decrease of the quantum dot size causes the red shift or blue shift of the corresponding wavelength, and the increase of the size distribution range indicates the presence of quantum dots with too large or too small size, which causes the broadening of the wavelength and the increase of the FWHM.
Experimental example 2
In this example, XRD analysis and FT-IR analysis were performed on the thin film materials of examples and comparative examples, and the results are shown in FIGS. 2 and 3.
In fig. 2, characteristic peaks are shown in which broad diffraction peaks appearing at around 21 ° correspond to EVA, and diffraction peaks appearing at 15 °, 22 °, and 31 ° coincide with CsPbBr 3 in monoclinic phase.
in fig. 3, compared with the control group (pure EVA film), the infrared spectrogram of the CsPbBr 3/EVA film prepared by adding different content of precursor solution has no change basically, which indicates that the recombination of CsPbBr 3 quantum dots and EVA resin does not generate obvious damage to the structure of EVA resin.
As can be seen from the analysis results of fig. 2 and 3, the CsPbBr 3 quantum dots can be conveniently synthesized by the method of the embodiment.
Experimental example 3
In this experimental example, the CsPbBr 3/EVA film prepared in example 1 was subjected to surface SEM and EDS energy spectrum analysis, and the result is shown in fig. 4.
From fig. 4, it can be seen that the CsPbBr 3/EVA film prepared in example 1 has a rough surface, and Cs, Br, and Pb elements are uniformly distributed in the matrix, which indicates that the distribution of CsPbBr 3 quantum dots in EVA is very uniform.
Experimental example 4
This experimental example analyzes Photoluminescence (PL) spectra and full width at half maximum (FWHM) of thin film materials of examples and comparative examples, and the results are shown in fig. 5 and 6.
The ultraviolet light with the wavelength of 361nm is used for excitation, the luminous peak of the embodiment is located at 521nm, the full width at half maximum is 21nm, and the color purity is high and the full width at half maximum is narrow. As can be seen from the figure, when the amount of the precursor added is 0.2mL, the corresponding thin film material has the highest luminous intensity, and the luminous intensity tends to decrease with the increase of the amount of the precursor added, which has a certain relationship with the increase of the particle size of the generated quantum dot. When the added precursor liquid is less, perovskite crystals can be well dispersed and separated out in the precursor liquid to form perovskite quantum dots, and with the increase of the precursor liquid, the yield of the perovskite quantum dots is increased, and the luminescence is enhanced; when the volume of the dripped precursor liquid exceeds the dispersion carrying capacity of the quantitative toluene solution, the concentration of perovskite quantum dots precipitated in a certain space is increased, so that the distance between the quantum dots is reduced, the quantum dots continue to grow due to the self-welding effect, the nano crystals with larger sizes are formed, the nano crystals exceed the range of quantum dot zero-dimensional materials, and are further excited by laser to be converted into crystal luminescence, and the luminescence is weakened.
Experimental example 5
In this experimental example, the PL spectrum and the intensity retention rate of the composite thin film material of example 1 after different soaking times were analyzed, and the test conditions of the PL spectrum were the same as those of example 4, and the results are shown in fig. 7 and 8.
As can be seen from fig. 7 and 8, the fluorescence intensity retention rate of the composite film material prepared in example 1 after soaking in water for 5 hours is 99.0%, and the intensity retention rate of the composite film material after soaking in water for 15 hours is 81.1%.
experimental example 6
This example analyzes the long-term standing properties of the composite film material of example 1. The PL spectrum and the intensity retention of the film material of example 1 after being left in air for 3 months are shown in fig. 9 and 10.
As can be seen from fig. 9 and 10, the composite film material of example 1 has good long-term standing performance, and the retention rate of fluorescence intensity after standing for 30d is 67.4%, and the retention rate of fluorescence intensity after standing for 90d is 63.4%.
Claims (8)
1. the cesium-lead halogen inorganic perovskite quantum dot/transparent polymer composite film is characterized by being prepared by the method comprising the following steps:
1) Dissolving lead halide, cesium halide and a surface ligand in a first solvent to prepare a precursor solution;
2) Dropwise adding the precursor solution into the polymer solution under stirring to obtain a colloidal solution; preparing a film by using a colloidal solution; the polymer solution is prepared by dissolving a transparent polymer material in a second solvent, wherein the second solvent does not dissolve the cesium-lead halogen quantum dots.
2. The cesium-lead-halide inorganic perovskite quantum dot/transparent polymer composite thin film according to claim 1, wherein in the step 2), the volume ratio of the precursor solution to the polymer solution is (0.1-2) to (10-20).
3. The cesium-lead-halide inorganic perovskite quantum dot/transparent polymer composite film according to claim 1, wherein in the step 2), the temperature of the polymer solution is 60-90 ℃.
4. The cesium-lead-halide inorganic perovskite quantum dot/transparent polymer composite thin film according to claim 1, wherein in the step 1), the concentration of lead halide in the precursor solution is 0.01-0.05 mol/L; in the step 2), the concentration of the macromolecular solution is 0.01-1 g/mL.
5. The cesium lead halide inorganic perovskite quantum dot/transparent polymer composite film according to any one of claims 1 to 4, wherein in the step 1), the surface ligands are oleic acid and oleylamine, the volume ratio of the oleic acid to the oleylamine is (1.5-2.5):1, and the molar ratio of the oleic acid to the lead halide is (7-9): 1.
6. The cesium lead halide inorganic perovskite quantum dot/transparent polymer composite thin film according to any one of claims 1 to 4, wherein in step 1), the first solvent is N, N-dimethylformamide or dimethyl sulfoxide.
7. The cesium-lead-halide inorganic perovskite quantum dot/transparent polymer composite thin film according to any one of claims 1 to 4, wherein in the step 2), the second solvent is toluene or n-hexane.
8. The cesium-lead-halide inorganic perovskite quantum dot/transparent polymer composite thin film according to any one of claims 1 to 4, wherein in the step 2), the transparent polymer material is an ethylene-vinyl acetate copolymer.
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| CN112457597A (en) * | 2020-12-04 | 2021-03-09 | 中国矿业大学 | Perovskite metal nonmetal compound core-shell quantum dot polymer film and preparation method and application thereof |
| CN113061313A (en) * | 2021-03-31 | 2021-07-02 | 华中科技大学 | Flexible perovskite scintillator thick film and preparation method thereof |
| CN113402865A (en) * | 2021-06-03 | 2021-09-17 | 西安建筑科技大学 | 3D printing material with photoluminescence, 3D printing wire and preparation method |
| CN113493383A (en) * | 2020-04-08 | 2021-10-12 | 丰田自动车株式会社 | Method for manufacturing methyl ammonium lead halide perovskite quantum dots |
| CN113773571A (en) * | 2021-08-12 | 2021-12-10 | 温州大学 | Ethylene-vinyl acetate copolymer coated Cs4PbBr6 nanocrystalline composite film |
| CN113817456A (en) * | 2021-08-12 | 2021-12-21 | 温州大学 | Ethylene-vinyl acetate copolymer coated CsPbX3 nanocrystalline composite film |
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| CN113493383A (en) * | 2020-04-08 | 2021-10-12 | 丰田自动车株式会社 | Method for manufacturing methyl ammonium lead halide perovskite quantum dots |
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| CN113061313A (en) * | 2021-03-31 | 2021-07-02 | 华中科技大学 | Flexible perovskite scintillator thick film and preparation method thereof |
| CN113402865A (en) * | 2021-06-03 | 2021-09-17 | 西安建筑科技大学 | 3D printing material with photoluminescence, 3D printing wire and preparation method |
| CN113773571A (en) * | 2021-08-12 | 2021-12-10 | 温州大学 | Ethylene-vinyl acetate copolymer coated Cs4PbBr6 nanocrystalline composite film |
| CN113817456A (en) * | 2021-08-12 | 2021-12-21 | 温州大学 | Ethylene-vinyl acetate copolymer coated CsPbX3 nanocrystalline composite film |
| CN114842736A (en) * | 2022-05-12 | 2022-08-02 | 重庆大学 | Quantum dot material-based encoding label and packaging method thereof |
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