CN113046063B - Hybrid perovskite luminescent material and preparation method and application thereof - Google Patents
Hybrid perovskite luminescent material and preparation method and application thereof Download PDFInfo
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Abstract
The application belongs to the technical field of perovskite materials. The application provides a hybrid perovskite luminescent material and a preparation method thereof. The organic matter and the lead-containing compound are regulated and controlled in proportion, the brightness of the material is gradually enhanced along with the replacement of the halogen element, the material has the characteristic of adjustable emission, and can generate a large Stokes broadband under the excitation of ultraviolet light and emit green light; the organic matter is cheap and easy to obtain and is nontoxic, the hybrid perovskite luminescent material plays a good role in protection, the luminescent performance of the material is enhanced, and the stability is greatly improved. The hybrid perovskite luminescent material has great application prospect in biological imaging and luminescent solar concentrators. The preparation method has the advantages of simple and easily-operated process flow, easily-realized and controllable synthesis conditions, and suitability for large-scale production.
Description
Technical Field
The application belongs to the technical field of perovskite materials, and particularly relates to a hybrid perovskite luminescent material, and a preparation method and application thereof.
Background
The organic-inorganic hybrid perovskite is a novel molecular composite material, which is formed by self-assembly of organic molecules and inorganic molecules, the structure of the perovskite takes inorganic parts as the basis, organic cations and inorganic layers are mutually connected through hydrogen bond interaction, and finally, a long-range ordered single crystal sample with alternately stacked organic components and inorganic components is formed. The hybrid material combines the advantages of organic and inorganic components, and has high structure adjustability and abundant physical properties. On one hand, the inorganic framework provides opportunities for semiconductor behaviors and broadband band gaps, so that the material has the characteristics of good photoelectric characteristics, electron mobility and the like. On the other hand, the organic phase offers structural diversity and the possibility of kinetic behavior for the crystals.
In recent decades, organic-inorganic hybrid perovskite materials have been developed greatly and have been applied to many fields such as photodetectors, field effect transistors, ferroelectric memories, light emitting diodes, solar cells, and the like. These materials have many specific properties, such as ferroelectric properties, optical properties, nonlinear optical properties, etc., and new materials are being synthesized due to the diversity and complexity of organic molecules. However, most of organic and inorganic hybrid materials have the problems of poor stability and short solution synthesis and storage time.
Disclosure of Invention
In view of the above, the present application provides a hybrid perovskite luminescent material, and a preparation method and an application thereof, which not only enhance the luminescent performance of the material, but also greatly improve the stability.
The specific technical scheme of the application is as follows:
the application provides a hybrid perovskite luminescent material, wherein the chemical expression of the hybrid perovskite luminescent material is as follows:
[[CH 3 (CH 2 ) n ] m NH 4-m ] 2 PbBr 4-x Cl x wherein x is more than or equal to 0 and less than or equal to 2,n is a positive integer, and m is an integer of 1-4.
According to the application, the organic matter and the lead-containing compound are regulated and controlled in proportion, the brightness of the material is gradually enhanced along with the replacement of halogen elements, the material has the characteristic of adjustable emission, and can generate a large Stokes broadband under the excitation of ultraviolet light and emit green light; the organic matter is cheap and easy to obtain and is nontoxic, the hybrid perovskite luminescent material plays a good role in protection, the luminescent performance of the material is enhanced, and the stability is greatly improved.
Preferably, n is 7,m is 4.
Preferably, the Stokes shift of the hybrid perovskite luminescent material is 165-235 nm, and the full width at half maximum is 50-71 nm.
In this application, hybridization perovskite luminescent material has bigger stokes displacement, can reduce the autofluorescence quenching of material, and the displacement is big more, and energy loss is few, and fluorescence efficiency is high, and the background interference is low, and is little to biological sample damage, and sample penetrability is strong, and monitoring sensitivity is high for the hybridization perovskite luminescent material of this application all has very big application prospect in biological imaging and the spotlight ware of luminous solar energy.
Preferably, the hybrid perovskite luminescent material is a zero-dimensional perovskite.
In the application, the organic matter and the lead-containing compound are regulated, the connectivity of the metal halide polyhedron can be regulated, strong lattice distortion is generated, the metal halide octahedron is completely isolated by the wide-band-gap organic ligand, the interaction between the metal halide octahedrons is inhibited, the broadband emission with large Stokes displacement is realized, and the stability is good.
The application also provides two preparation methods of the hybrid perovskite luminescent material, namely a solid phase method and a liquid phase method.
The solid phase method comprises the following steps:
and weighing organic matters and lead-containing compounds according to the stoichiometric ratio, mixing, grinding, firing and cooling to obtain the hybrid perovskite luminescent material.
In the application, the solid-phase method is adopted to prepare the hybrid perovskite luminescent material, the preparation is simple and easy to realize, conditions such as high temperature and high pressure are not needed, and the cost is greatly reduced.
Preferably, the firing temperature is 70-100 ℃, and the time is 3-5 h;
the temperature of the cooling is room temperature.
The liquid phase method comprises the following steps:
weighing organic matters and lead-containing compounds according to the stoichiometric ratio, dissolving the organic matters and the lead-containing compounds in an organic solvent, stirring for reaction, and performing ultrasonic treatment to obtain the hybrid perovskite luminescent material.
In the application, the liquid phase method is adopted to prepare the hybrid perovskite luminescent material, the problem that the product structure rigidity limits the structural recombination can be effectively solved, and larger Stokes displacement can be obtained.
Preferably, the temperature of the stirring reaction is room temperature, and the time is 30-60 min;
the frequency of the ultrasonic wave is 80-100W, and the time is 5-10 min.
Preferably, the organic solvent is dimethylformamide, and the dosage ratio of the organic matter to the organic solvent is 1094mg:5ml.
Preferably, the organic substance is tetra-n-octyl ammonium bromide, and the lead-containing compound is chloride and/or bromide of a lead-containing element.
Preferably, the molar ratio of the organic substance, the chloride and the bromide is 4.
In summary, the present application provides a hybrid perovskite luminescent material and a preparation method thereof. The chemical expression of the hybrid perovskite luminescent material is as follows: [ [ CH ] 3 (CH 2 ) n ] m NH 4-m ] 2 PbBr 4-x Cl x Wherein x is more than or equal to 0 and less than or equal to 2,n is a positive integer, and m is an integer of 1-4. The organic matter and the lead-containing compound are regulated and controlled in proportion, the brightness of the material is gradually enhanced along with the replacement of the halogen element, the material has the characteristic of adjustable emission, and can generate a large Stokes broadband under the excitation of ultraviolet light and emit green light; the organic matter is cheap and easy to obtain and is nontoxic, the hybrid perovskite luminescent material plays a good role in protection, the luminescent performance of the material is enhanced, and the stability is greatly improved. The hybrid perovskite luminescent material has great application prospect in biological imaging and luminescent solar concentrators. The preparation method has the advantages of simple and easily-operated process flow, easily-realized and controllable synthesis conditions, and suitability for large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 shows the excitation and emission spectra of the product obtained in example 1 of the present application;
FIG. 2 shows the excitation and emission spectra of the product obtained in example 2 of the present application;
FIG. 3 shows excitation and emission spectra of the product obtained in example 3 of the present application;
FIG. 4 shows excitation and emission spectra of the product obtained in example 4 of the present application;
FIG. 5 shows excitation and emission spectra of the product obtained in example 5 of the present application;
FIG. 6 is a graph showing the excitation and emission spectra of the product obtained in example 6 of the present application;
FIG. 7 shows excitation and emission spectra of the product obtained in example 7 of the present application;
FIG. 8 shows excitation and emission spectra of the product obtained in example 8 of the present application;
FIG. 9 is an XRD pattern of the product obtained in example 4 of the present application;
FIG. 10 is an XRD pattern of the product obtained in example 5 of the present application;
FIG. 11 is an XRD pattern of the product obtained in example 6 of the present application.
Detailed Description
In order to make the objects, features and advantages of the present application more obvious and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is obvious that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The starting materials and reagents used in the examples of the present application are commercially available.
Example 1
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 4 Respectively weighing lead bromide and tetra-n-octyl ammonium bromide, fully mixing and grinding until the mixture is uniform, putting the obtained mixture into a corundum crucible, putting the corundum crucible into an oven, heating to 70 ℃ under the air atmosphere, preserving the temperature for 3 hours, and taking out the mixture after the mixture is naturally cooled to room temperature to obtain a product. FIG. 1 shows the excitation and emission spectra of the product obtained in example 1 of the present application.
Example 2
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 3 Respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromide, fully mixing and grindingAnd after the mixture is uniform, putting the mixture into a corundum crucible, putting the corundum crucible into an oven, raising the temperature to 70 ℃ in the air atmosphere, preserving the heat for 3 hours, and taking out the corundum crucible after the mixture is naturally cooled to room temperature to obtain a product. FIG. 2 shows the excitation and emission spectra of the product obtained in example 2 of the present application.
Example 3
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 2 Cl 2 Respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromide, fully mixing and grinding until uniform, putting the obtained mixture into a corundum crucible, putting the corundum crucible into an oven, heating to 70 ℃ under air atmosphere, preserving heat for 3 hours, and taking out after naturally cooling to room temperature to obtain a product. FIG. 3 shows the excitation and emission spectra of the product obtained in example 3 of the present application.
Example 4
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 4 Respectively weighing lead bromide and tetra-n-octyl ammonium bromide, dissolving the lead bromide and the tetra-n-octyl ammonium bromide into a beaker filled with dimethylformamide with a certain volume, placing the beaker on a magnetic stirrer, violently stirring the solution for 30 minutes, and then transferring the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5 minutes to obtain a product. FIG. 4 shows the excitation and emission spectra of the product obtained in example 4 of the present application. Figure 9 is an XRD pattern of the product obtained in example 4 of the present application.
Example 5
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 3 And (4) respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromide, dissolving the lead bromide, the lead chloride and the tetra-n-octylammonium bromide into a beaker filled with a certain volume of dimethylformamide, placing the beaker on a magnetic stirrer, violently stirring the solution for 30 minutes, and then transferring the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5 minutes to obtain a product. FIG. 5 shows the excitation and emission spectra of the product obtained in example 5 of the present application. FIG. 10 is an XRD pattern of the product obtained in example 5 of the present application.
Example 6
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 2 Cl 2 Respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromideDissolving the mixture into a beaker filled with a certain volume of dimethylformamide, placing the beaker on a magnetic stirrer to stir vigorously for 30 minutes, and then transferring the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5 minutes to obtain a product. FIG. 6 shows the excitation and emission spectra of the product obtained in example 6 of the present application. FIG. 11 is an XRD pattern of the product obtained in example 6 of the present application.
Example 7
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 3.5 Cl 0.5 Respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromide, dissolving the lead bromide, the lead chloride and the tetra-n-octylammonium bromide into a beaker filled with a certain volume of dimethylformamide, placing the beaker on a magnetic stirrer, violently stirring the mixture for 30 minutes, and then transferring the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5 minutes to obtain a product. FIG. 7 shows the excitation and emission spectra of the product obtained in example 7 of the present application.
Example 8
According to the following stoichiometric ratio: (C) 32 H 68 N) 2 PbBr 0.5 Cl 3.5 Respectively weighing lead bromide, lead chloride and tetra-n-octylammonium bromide, dissolving the lead bromide, the lead chloride and the tetra-n-octylammonium bromide into a beaker filled with a certain volume of dimethylformamide, placing the beaker on a magnetic stirrer, violently stirring the mixture for 30 minutes, and then transferring the beaker into an ultrasonic cleaning machine to carry out ultrasonic treatment for 5 minutes to obtain a product. FIG. 8 shows the excitation and emission spectra of the product obtained in example 8 of the present application.
FIGS. 1 to 11 show that the products prepared by the examples of the present application can generate large Stokes broadband under the excitation of ultraviolet light, and the maximum Stokes broadband can be reached (235 nm), and the full width at half maximum FEHM =71nm. In addition, the Stokes shift and the half-height width of the product prepared by the liquid phase method are larger, and the excitation and emission peaks of the product prepared by the solid phase method are partially overlapped, because the large Stokes shift is caused by obvious structural distortion of an excited state, and the structural recombination of the product is limited by the solid rigidity.
The emission spectrum relative intensity ratios of the following products prepared by the liquid phase method are shown in table 1, and the results show that the emission intensity of the products prepared by the liquid phase method can be gradually enhanced along with the increase of Cl element, and the products have the characteristic of adjustable emission.
TABLE 1 comparison of relative intensities of emission spectra of products prepared by the liquid phase method of the present application
Table 2 shows the relative emission intensities at different temperatures of the products obtained in examples 1 to 3 of the present application. The result shows that the emission intensity of the product prepared by the embodiment of the application has good stability under the temperature change, can still maintain certain emission intensity at high temperature, and has the advantages of strong thermal stability and high wet stability.
Table 3 shows the relative emission intensity 203 days after the products obtained in examples 5 to 6 of the present application were left. The results show that the products prepared in the examples can still maintain high emission intensity after being placed for 203 days and can be stored for a long time.
Table 2 relative emission intensities at different temperatures of the products obtained in examples 1 to 3
| 293K | 313K | 333K | 353K | 373K | 393K | |
| (C 32 H 68 N) 2 PbBr 4 | 543972 | 354838 | 119524 | 47368 | 43633 | 37011 |
| (C 32 H 68 N) 2 PbBr 3 Cl 1 | 983588 | 921052 | 844086 | 719015 | 237691 | 88568 |
| (C 32 H 68 N) 2 PbBr 2 Cl 2 | 2121561 | 787492 | 268930 | 152518 | 78450 | 78438 |
TABLE 3 relative emission intensity 203 days after the products from examples 5 to 6 were left
| Initial value | After 203 days of standing | |
| (C 32 H 68 N) 2 PbBr 3 Cl 1 | 379165 | 236063 |
| (C 32 H 68 N) 2 PbBr 2 Cl 2 | 607696 | 420712 |
Comparative example
Prepared in stoichiometric proportions by the method of preparation of example 1 (C) 13 H 19 N 4 ) 2 PbBr 4 Compounds and the excitation and emission spectra of the products were obtained and compared to the properties of the products obtained in example 1 of the present application, and the stokes shifts and full widths at half maximum of the products obtained in example 1 and comparative example are shown in table 4 below. The results show that the hybrid perovskite luminescent material of the application can generate larger Stokes shift, mainly in a green light wave band. Compared with zero dimension (C) 13 H 19 N 4 ) 2 PbBr 4 The Stokes shift of the compound is obviously improved, 64nm is increased, and the compound is converted from a blue light waveband to a green light waveband. In addition, compare (C) 4 H 9 NH 3 ) 2 PbBr 4 The Stokes shift of the compound is increased by 30nm. Compared with typical Pb-based 3D perovskite CH 3 NH 3 PbBr 3 The full width at half maximum is increased by 50nm.
TABLE 4 Stokes shift and half-height Width of the products obtained in example 1 and comparative example
| Full width at half maximum (FWHM) | Stokes shift | |
| (C 32 H 68 N) 2 PbBr 4 | 71nm | 175nm |
| (C 13 H 19 N 4 ) 2 PbBr 4 | 66nm | 111nm |
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (8)
1. A hybrid perovskite luminescent material, wherein the chemical expression of the hybrid perovskite luminescent material is as follows:
[[CH 3 (CH 2 ) 7 ] 4 N] 2 PbBr 4-x Cl x wherein, 0<x≤2。
2. The hybrid perovskite luminescent material as claimed in claim 1, wherein the Stokes shift of the hybrid perovskite luminescent material is 165-235 nm, and the full width at half maximum is 50-71 nm.
3. The method for preparing hybrid perovskite luminescent material as claimed in claim 1, which comprises the following steps:
weighing organic matters and lead-containing compounds according to the stoichiometric ratio, mixing, grinding, firing and cooling to obtain the hybrid perovskite luminescent material;
the lead-containing compound is chloride and bromide of lead-containing elements.
4. The preparation method according to claim 3, wherein the firing is carried out at a temperature of 70 to 100 ℃ for 3 to 5 hours;
the temperature of the cooling is room temperature.
5. The method for preparing hybrid perovskite luminescent material as claimed in claim 1, which comprises the following steps:
weighing organic matters and lead-containing compounds according to the stoichiometric ratio, dissolving the organic matters and the lead-containing compounds in an organic solvent, stirring for reaction, and performing ultrasonic treatment to obtain the hybrid perovskite luminescent material.
6. The preparation method according to claim 5, wherein the temperature of the stirring reaction is room temperature, and the time is 30-60 min;
the frequency of the ultrasonic wave is 80-100W, and the time is 5-10 min.
7. The method according to claim 5, wherein the organic substance is tetra-n-octylammonium bromide.
8. Use of the hybrid perovskite luminescent material as defined in any one of claims 1 to 2 in a concentrator for bioimaging or luminescent solar energy.
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