CN110950375B - CsPb2Br5Middle doped CsPbBr3Composite perovskite material and preparation method and application thereof - Google Patents
CsPb2Br5Middle doped CsPbBr3Composite perovskite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a CsPb2Br5Middle doped CsPbBr3The doped perovskite material is CsPb2Br5The material is doped with a small amount of CsPbBr3Composition is carried out; the preparation method is ingenious in design, firstly utilizes the trimesic acid ligand and lead ions to synthesize the metal organic framework Pb-MOF with lead as the framework, then cesium bromide aqueous solution and the Pb-MOF are reacted under the ultrasonic condition in an alcohol solution, and the Pb-MOF is dissociated in the reaction to obtain CsPb Pb and Pb2Br5Middle doped with small amount of CsPbBr3The composite of (a); the synthesis process has few steps, is easy to implement, does not need heating or inert gas protection, and saves energy; and the used synthetic solvents are only pure water and ethanol, so that the method is green and environment-friendly and has little pollution to the environment.
Description
Technical Field
The invention relates to the technical field of perovskite, in particular to CsPb2Br5Middle doped CsPbBr3The composite perovskite material and the preparation method and the application thereof.
Background
Recently, all-inorganic perovskite quantum dot material (CsPbX)3PQD) is gaining more and more attention due to its ultra-high photoluminescence efficiency, flexible and tunable emission wavelength and narrow-band emission, and this material has a wide range of applications and can be used in the fields of light emitting diodes, lasers, solar cells, photodetectors and visible light communications. However, the structural characteristics of the pure perovskite quantum dot material make the perovskite quantum dot material sensitive to humidity, light and temperature, the chemical stability is poor under general environmental conditions, the crystal structure is easily destroyed due to hydrolysis, and the calcium is greatly limitedThe application of the titanium ore quantum dot material; in order to solve the problem of poor stability of the perovskite quantum dot, organic ligands or polymers such as titanium butoxide and tri-n-octylphosphine are generally adopted for surface modification, or inorganic materials such as silicon dioxide and aluminum oxide are adopted to improve the stability of the perovskite quantum dot, but the measures are difficult to improve the stability and enhance the optical performance of the perovskite quantum dot.
The metal organic framework material MOF has the advantages of traditional inorganic and organic luminescent materials, a composite material is formed by introducing object molecules or ions into holes of the MOF material, and the enhancement of optical performance is realized through the interaction between a host and an object, but the size of perovskite quantum dots is large (about 10 nm), the pores of MOF crystals are small (0.78nm), so that the perovskite quantum dots are difficult to enter the MOF crystals, the effect of increasing the stability of the perovskite quantum dots cannot be achieved, and the application of the metal organic framework material MOF is limited.
How to solve the problem that the existing perovskite quantum dot material stably exists and has excellent optical performance is the problem to be solved urgently by the existing perovskite.
Disclosure of Invention
In order to solve the problem that the excellent optical property and stability of the perovskite quantum dot material in the prior art cannot be simultaneously achieved, the invention aims to provide CsPb2Br5Middle doped CsPbBr3The doped perovskite material and the preparation method and the application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
CsPb2Br5Middle doped CsPbBr3The composite perovskite material is prepared in CsPb2Br5The material is doped with a small amount of CsPbBr3And (4) forming.
The invention also includes CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution and a trimesic acid aqueous solution, carrying out ultrasonic oscillation, carrying out suction filtration, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder;
dissolving cesium bromide in ultrapure water to obtain a cesium bromide aqueous solution;
dispersing Pb-MOF powder in ethanol under ultrasonic oscillation, dripping cesium bromide aqueous solution into the ethanol, and carrying out ultrasonic oscillation, filtration, washing and freeze drying on the cesium bromide aqueous solution to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Preferably, the concentration of the lead nitrate solution is 0.01-0.1 mol/L, the concentration of the trimesic acid aqueous solution is 0.01-0.1 mol/L, and the molar ratio of the lead nitrate to the trimesic acid is 1-2: 1.
preferably, the concentration of the cesium bromide aqueous solution is 200-400 mg/ml.
Preferably, when the Pb-MOF powder is dispersed in ethanol, the mass-volume ratio of the Pb-MOF powder to the ethanol is 20-40 mg/ml.
Preferably, in the third step, Pb-MOF powder is dispersed in ethanol, and cesium bromide aqueous solution is dropwise added into the ethanol, wherein the mass ratio of cesium bromide to Pb-MOF powder is 5-15: 1.
preferably, the step (c) is washed with ultrapure water.
Preferably, the preparation method of the doped perovskite material with CsPbBr3 doped in CsPb2Br5 comprises the step three, wherein the temperature of freeze drying is-10 to-30 ℃ and the time is 10 to 15 hours.
The invention also includes CsPb2Br5Middle doped CsPbBr3The doped perovskite material is used for detecting the concentration of iron ions and potassium ions in a solution.
Compared with the prior art, the invention has the following advantages:
CsPb of the present invention2Br5Middle doped with small amount of CsPbBr3And conventional CsPbBr, and3the quantum dot is different from the Pb-MOF composite luminescent material, and the structure is CsPb2Br5/CsPbBr3The composite material has excellent fluorescence intensity, stable structure, good water resistance and high thermal stability, and can stably exist in water;
CsPb of the invention2Br5Middle doped with small amount of CsPbBr3The preparation method of the composite perovskite material is ingenious in design, firstly, the trimesic acid ligand and lead ions are utilized to synthesize the metal organic framework Pb-MOF with lead as a framework, then, the cesium bromide aqueous solution and the Pb-MOF are reacted under the ultrasonic condition in an alcohol solution, and the Pb-MOF is dissociated in the reaction to obtain CsPb Pb2Br5Middle doped with small amount of CsPbBr3The composite of (a);
CsPb of the invention2Br5Middle doped with small amount of CsPbBr3The preparation method of the composite perovskite material has the advantages of few synthesis process steps, easy process implementation, no need of heating and no need of inert gas protection, and energy conservation; and the used synthetic solvents are only pure water and ethanol, so that the method is green and environment-friendly and has little pollution to the environment.
CsPb of the invention2Br5Middle doped with small amount of CsPbBr3The composite perovskite material can be used for detecting the concentration of iron ions and potassium ions in a solution; and can also be used for photoelectric devices such as solar cells, light-emitting diodes and the like.
Drawings
FIG. 1 shows CsPb2Br5/CsPbBr3Composite and reference synthesis of CsPb2Br5A fluorescence spectrum of the material;
FIG. 2 shows CsPb2Br5/CsPbBr3XRD pattern of the composite;
FIG. 3 shows CsPb2Br5/CsPbBr3XPS plot of composite material;
FIG. 4 shows a portion CsPb2Br5/CsPbBr3High power transmission electron microscopy (HTEM) images of the composite material;
FIG. 5 shows a portion CsPb2Br5/CsPbBr3High power transmission electron microscopy (HTEM) images of the composite material;
FIG. 6 shows CsPb2Br5/CsPbBr3Scanning electron microscope SEM picture of the composite material;
FIG. 7 shows CsPb2Br5/CsPbBr3Photoluminescence intensity of composite material at different temperaturesA degree schematic diagram;
FIG. 8 shows CsPb2Br5/CsPbBr3The reversibility result of the composite material at 30-70 ℃ is shown in a schematic diagram;
FIG. 9 shows CsPb2Br5/CsPbBr3A graph of the fluorescence intensity of the composite material in water at different times;
FIG. 10 is a bar graph of fluorescence intensity at different times;
FIG. 11 shows different concentrations of Fe3+The following graph of the fluorescence intensity is shown,
FIG. 12 is Fe3+Schematic diagram of the standard curve of (1);
FIG. 13 shows different concentrations of K+The following graph of the fluorescence intensity is shown,
FIG. 14 is K+Schematic diagram of the standard curve of (1);
reference numerals: 1CsPb2Br5/CsPbBr3Composite material, 2CsPb2Br5Material, 3 Pb-MOF.
Detailed Description
The invention aims to provide CsPb2Br5Middle doped CsPbBr3The composite perovskite material and the preparation method and the application thereof are realized by the following technical scheme:
CsPb2Br5Middle doped CsPbBr3The composite perovskite material is prepared in CsPb2Br5The material is doped with a small amount of CsPbBr3And (4) forming.
The invention also includes CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution and a trimesic acid aqueous solution, carrying out ultrasonic oscillation, carrying out suction filtration, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder;
dissolving cesium bromide in ultrapure water to obtain a cesium bromide aqueous solution;
dispersing Pb-MOF powder in ethanol under ultrasonic oscillation, dripping cesium bromide aqueous solution into the ethanol, performing ultrasonic oscillation and filtering,washing, freezing and drying to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
The concentration of the lead nitrate solution is 0.01-0.1 mol/L, the concentration of the trimesic acid aqueous solution is 0.01-0.1 mol/L, and the molar ratio of the lead nitrate to the trimesic acid is 1-2: 1.
the concentration of the cesium bromide aqueous solution is 200-400 mg/ml.
When the Pb-MOF powder is dispersed in ethanol, the mass-to-volume ratio of the Pb-MOF powder to the ethanol is 20-40 mg/ml.
Dispersing Pb-MOF powder into ethanol, and dropwise adding a cesium bromide aqueous solution into the ethanol, wherein the mass ratio of cesium bromide to Pb-MOF powder is 5-15: 1.
and step three, washing with ultrapure water.
The preparation method of the doped perovskite material with CsPbBr3 doped in CsPb2Br5 comprises the step three, wherein the temperature of freeze drying is-10 ℃ to-30 ℃ and the time is 10-15 hours.
Firstly, synthesizing a metal organic framework Pb-MOF (metal organic framework) with lead as a framework by adopting a trimesic acid ligand and lead ions, then reacting cesium bromide aqueous solution and the Pb-MOF under an ultrasonic condition, and dissociating the Pb-MOF in the reaction to obtain Cspb (lead-doped metallothionein) Pb-MOF2Br5Middle doped with small amount of CsPbBr3The composite of (a); the obtained material has good water resistance and high-temperature stability, and excellent fluorescence performance.
The invention also includes CsPb2Br5Middle doped CsPbBr3The composite perovskite material is used for detecting the concentration of iron ions and potassium ions in a solution.
The invention is further described with reference to specific examples.
Example 1
CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution with the concentration of 0.01mol/L and a trimesic acid aqueous solution with the concentration of 0.01mol/L, ultrasonically oscillating, filtering, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder; the volume ratio of the lead nitrate solution to the trimesic acid solution is 2: 1;
dissolving cesium bromide in ultrapure water to prepare a cesium bromide aqueous solution with the concentration of 200 mg/ml;
dispersing the 1gPb-MOF powder obtained in the step I in 50ml of ethanol under ultrasonic oscillation, dropwise adding 25ml of cesium bromide aqueous solution with the concentration of 200mg/ml, and obtaining CsPb by ultrasonic oscillation, filtration, washing and freeze drying2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Example 2
CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution with the concentration of 0.1mol/L and a trimesic acid solution with the concentration of 0.1mol/L, ultrasonically oscillating, filtering, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder; the volume ratio of the lead nitrate solution to the trimesic acid solution is 1: 1;
dissolving cesium bromide in ultrapure water to prepare a cesium bromide aqueous solution with the concentration of 400 mg/ml;
dispersing 1g of Pb-MOF powder obtained in the step I in ethanol under ultrasonic oscillation, dropwise adding 37.5ml of cesium bromide aqueous solution with the concentration of 400mg/ml, and carrying out ultrasonic oscillation, filtration, washing and freeze drying to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Example 3
CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution with the concentration of 0.3mol/L and a trimesic acid solution with the concentration of 0.3mol/L, ultrasonically oscillating, filtering, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder; the volume ratio of the lead nitrate solution to the trimesic acid solution is 1.6: 1;
dissolving cesium bromide in ultrapure water to prepare a cesium bromide aqueous solution with the concentration of 250 mg/ml;
dispersing 1gPb-MOF powder in ethanol under ultrasonic oscillation, dripping 40ml of 250mg/ml cesium bromide aqueous solution, ultrasonic oscillation, filtering, washing with ethanol, and freeze-drying at-10 ℃ for 10 hours to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Example 4
CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution with the concentration of 0.8mol/L and a trimesic acid solution with the concentration of 0.8mol/L, ultrasonically oscillating, filtering, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder; the volume ratio of the lead nitrate solution to the trimesic acid solution is 1.2: 1;
dissolving cesium bromide in ultrapure water to prepare a cesium bromide aqueous solution with the concentration of 250 mg/ml;
dispersing 1gPb-MOF powder in ethanol under ultrasonic oscillation, dripping 48ml of 250mg/ml cesium bromide aqueous solution, ultrasonic oscillation, filtering, washing with ultrapure water, and freeze-drying at-30 ℃ for 15 hours to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Example 5
CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material comprises the following steps:
mixing a lead nitrate solution with the concentration of 0.5mol/L and a trimesic acid solution with the concentration of 0.5mol/L, ultrasonically oscillating, filtering, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder; the volume ratio of the lead nitrate solution to the trimesic acid solution is 1.5: 1;
dissolving cesium bromide in ultrapure water to prepare a cesium bromide aqueous solution with the concentration of 300 mg/ml;
dispersing 1gPb-MOF powder in B under ultrasonic vibrationAdding 30ml of 300mg/ml cesium bromide aqueous solution dropwise into alcohol, ultrasonically oscillating, filtering, washing with ultrapure water, and freeze-drying at-20 deg.C for 12 hr to obtain CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (1).
Composite perovskite material (namely CsPb) doped with CsPbBr3 in CsPb2Br5 obtained in example 52Br5/CsPbBr3Composite material) for detection of fluorescent ultraviolet spectrum.
Compared CsPb2Br5/CsPbBr3Composite materials and literature-synthesized CsPb2Br5Solid fluorescence ultraviolet spectrum of the material, as shown in FIG. 1, it can be seen that both materials have a fluorescence peak at 520nm, and CsPb2Br5/CsPbBr3Composite materials and literature-synthesized CsPb2Br5Compared with the material, the fluorescence is obviously enhanced, and as can be seen from ultraviolet absorption spectrum, the main contribution source of the fluorescence is a wide absorption band of 420-520 nm, and the corresponding band gap is 2.3Ev, namely the fluorescence in the composite material is formed by CsPb2Br5Medium doped with small amount of CsPbBr3And (4) causing.
For the determination of CsPb2Br5/CsPbBr3Structure of composite Material, we tested the Pb-MOF powder and the product (CsPb) obtained in the first step of example five2Br5Middle doped CsPbBr3Doped perovskite material) and X-ray electron spectroscopy XPS, the XRD image of fig. 2 shows that the crystal structure of the Pb-MOF powder is similar to that described in the literature, but the product is identical to Pb-MOF and to CsPb2Br5The standard cards are completely matched, namely the product of the application destroys the crystal structure of Pb-MOF and generates CsPb2Br5However, CsPbBr3The peak of (A) is not detected, and CsPbBr can be obtained3The amount of (A) is very small or in CsPb2Br5Deep layer, surface layer can not be detected;
as can be seen from the XPS plot of FIG. 3, not only Cs, Pb, Br but also a large amount of C and O are detected, i.e., Pb-MOF is CsPb2Br5/CsPbBr3CompoundingThe material provides trimesic acid as a ligand so as to improve the stability of the material;
to further validate CsPb2Br5Middle doped CsPbBr3CsPbBr in doped perovskite material3We performed high power transmission electron microscopy HTEM and scanning electron microscopy SEM examinations, as shown in fig. 4, which shows a partial high power transmission electron microscopy HTEM map in which the 3.68A lattice fringes correspond to CsPbBr3The (110) crystal plane of FIG. 5 is a partial high power transmission electron microscope HTEM image, and the lattice fringe of 7.59A corresponds to CsPb2Br5(002) Crystal face, the synthesized material is proved to be CsPb2Br5Middle doped CsPbBr3The doped perovskite material of (a); as can be seen from the SEM image of FIG. 6, CsPb2Br5Middle doped CsPbBr3The doped perovskite material is in a shape of a sheet with uniform size, and the size of the doped perovskite material is about 1 micron.
CsPb obtained in example 52Br5Middle doped CsPbBr3The thermal stability of the doped perovskite material is detected by the following steps: for 2mg/ml CsPb2Br5Middle doped CsPbBr3The fluorescence intensity of the doped perovskite material is respectively detected within the range of 20-80 ℃, the result is shown in figure 7, CsPb2Br5Middle doped CsPbBr3The doped perovskite material has good linear relation within the test temperature range of 30-70 ℃, and the correlation coefficient R2Is 0.99 and the photoluminescent intensity of the composite material increases again as the temperature decreases from 70 ℃ to 30 ℃, indicating that the photoluminescent intensity of the material is a reversible process dependent on the heating and cooling temperatures.
The reversibility of the composite material is further evaluated, as shown in FIG. 8, five cycles of cyclic detection are carried out in the temperature range of 30-70 ℃, and the emission intensity of each cycle is found to be almost unchanged at different temperatures, which indicates the good reversibility of the system.
CsPb obtained in example 52Br5Middle doped CsPbBr3The composite perovskite material of (a) was subjected to water resistance test by directly exposing the resulting material to water (at a concentration of 5mg/ml) for 1 day, 5 days, 10 days,the fluorescence intensity (365nm) of 15 days, 20 days and 30 days is detected, the result is shown in figure 9, weak fluorescence still exists after 30 days, the fluorescence intensity of each time is shown in figure 10, the fluorescence intensity is reduced to half of that of 1 day from day 5, the fluorescence intensity is basically kept unchanged from day 5 to day 15 until the intensity is reduced again from day 20 to day 30, the fluorescence intensity is greatly attenuated, and the weak fluorescence still exists, so that the material disclosed by the invention has good water resistance.
CsPb obtained in example 5 was used2Br5Middle doped CsPbBr3Of composite perovskite material to Fe3+And K+And (3) carrying out concentration detection, and comprising the following steps:
(ii) reacting CsPb2Br5Middle doped CsPbBr3The composite perovskite material is dispersed into a standard solution of metal ions to be detected, and is subjected to ultrasonic treatment for 5-10 minutes to be fully dispersed, wherein the metal ions to be detected are Fe3+And K+；
Testing the change of the fluorescence intensity of the solution, and drawing a standard curve by taking the fluorescence intensity and the concentration of ions to be tested as coordinates;
③ CsPb of the same phase mass2Br5Middle doped CsPbBr3The composite perovskite material is dispersed into a sample solution to be detected, and the concentration of metal ions in the sample is calculated by combining the detected fluorescence intensity with the standard curve of the step II.
With Fe3+For example, 2mgCsPb2Br5Middle doped CsPbBr3The composite perovskite material is dispersed in 1ml containing Fe3+In the aqueous solution of (5), the results are shown in FIG. 11 for different concentrations of Fe3+FIG. 12Fe and fluorescence intensity diagram3+Is shown in the graph of the standard curve of (1), at 10-4～10-3Has good linear relation (r) in the range of M concentration2＝0.99174)；
And K+For CsPb2Br5Middle doped CsPbBr3The composite perovskite material has obvious enhancement effect, enhances the stability of the composite material, leads the luminous intensity of the composite material to be enhanced in aqueous solution, and the result is shown in figure 13 that Fe with different concentrations3+FIG. 14 shows fluorescence intensity of Fe3+Is shown in the graph of the standard curve of (1), at 10-9～10-7Has good linear relation (r) in the range of M concentration2＝0.99292)。
Claims (6)
1.CsPb2Br5Middle doped CsPbBr3The preparation method of the composite perovskite material is characterized by comprising the following steps: the method comprises the following steps:
mixing a lead nitrate solution and a trimesic acid aqueous solution, carrying out ultrasonic oscillation, carrying out suction filtration, washing with absolute ethyl alcohol, and drying to obtain Pb-MOF powder;
dissolving cesium bromide in ultrapure water to obtain a cesium bromide aqueous solution;
dispersing Pb-MOF powder in ethanol under ultrasonic oscillation, dripping cesium bromide aqueous solution into the ethanol, and carrying out ultrasonic oscillation, filtration, washing and freeze drying on the cesium bromide aqueous solution to obtain CsPb2Br5Middle doped CsPbBr3The composite perovskite material of (a);
the concentration of the cesium bromide aqueous solution is 200-400 mg/ml; when the Pb-MOF powder is dispersed in ethanol, the mass-to-volume ratio of the Pb-MOF powder to the ethanol is 20-40 mg/ml.
2. The CsPb of claim 12Br5Middle doped CsPbBr3The preparation method of the composite perovskite material is characterized by comprising the following steps: the concentration of the lead nitrate solution is 0.01-0.1 mol/L, the concentration of the trimesic acid aqueous solution is 0.01-0.1 mol/L, and the molar ratio of the lead nitrate to the trimesic acid is 1-2: 1.
3. the CsPb of claim 12Br5Middle doped CsPbBr3The preparation method of the composite perovskite material is characterized by comprising the following steps: dispersing Pb-MOF powder into ethanol, and dropwise adding a cesium bromide aqueous solution into the ethanol, wherein the mass ratio of cesium bromide to Pb-MOF powder is 5-15: 1.
4. the CsPb of claim 12Br5Middle doped CsPbBr3The preparation method of the composite perovskite material is characterized by comprising the following steps: and step three, washing with ultrapure water.
5. The CsPb of claim 12Br5Middle doped CsPbBr3The preparation method of the composite perovskite material is characterized by comprising the following steps: and step three, the temperature of freeze drying is-10 to-30 ℃, and the time is 10 to 15 hours.
6. CsPb obtained according to claim 12Br5Middle doped CsPbBr3The use of a composite perovskite material of (a), characterized in that: the method is used for detecting the concentration of iron ions and potassium ions in the solution.
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| CN115212902B (en) * | 2022-05-11 | 2024-04-05 | 山东大学 | All-inorganic halide perovskite composite material and preparation method and application thereof |
| CN116496781A (en) * | 2022-06-07 | 2023-07-28 | 广东聚华印刷显示技术有限公司 | Perovskite composite material, preparation method thereof and electroluminescent device |
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