CN110846715A - Large size zero dimension Cs4PbBr6/CsPbBr3Perovskite scintillation crystal and preparation method thereof - Google Patents
Large size zero dimension Cs4PbBr6/CsPbBr3Perovskite scintillation crystal and preparation method thereof Download PDFInfo
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- G01T1/20—Measuring radiation intensity with scintillation detectors
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Abstract
The invention discloses a large-size zero-dimensional Cs4PbBr6/CsPbBr3The method can realize zero-dimensional perovskite scintillation crystal required by radiation field detection, and successfully synthesize large-size Cs in batch by using a solution method in an organic solvent and adjusting parameters such as reactant proportion, growth temperature and time4PbBr6/CsPbBr3The size of the perovskite crystal can reach 9 mm. The method comprises the following steps: taking solution obtained by mixing and reacting organic solvents N, N-Dimethylformamide (DMF) and hydrobromic acid (HBr) as a solvent, and CsBr and PbBr2Is prepared from solute through preparing solution of precursor, filtering, and crystallizing in saturated solutionAnd preparing large-size pure inorganic perovskite crystals in a solution at the temperature of 30-60 ℃. The pure inorganic perovskite scintillator nuclear radiation detector prepared by the invention has the advantages of good stability and higher scintillation luminescence performance.
Description
Technical Field
The invention belongs to the field of scintillator nuclear radiation detection, and particularly relates to a large-size zero-dimensional Cs4PbBr6/CsPbBr3Perovskite scintillation crystal and a preparation method thereof.
Background
The scintillator nuclear radiation detector is widely applied to the fields of medical imaging, safety inspection, scientific research and the like as a common nuclear radiation detector at present. At present, the materials used for nuclear radiation detectors mainly comprise scintillator materials, which are bulk materials. Although research on the use of a scintillator material based on a micro-nano material for a nuclear radiation detector also exists, compared with a scintillator material of a body material, the taking is inconvenient, and the scintillator material of the body material is more beneficial to the detection of high-energy rays.
Commonly used scintillator materials for making body materials for nuclear radiation detectors are known to include thallium-activated sodium iodide (nai (tl)), cesium iodide (CsI), Bismuth Germanate (BGO), cerium doped gadolinium orthosilicate (GSO). These scintillator materials all have their own unique scintillation characteristics, such as high light yield, fast response speed, short decay time, good stability, etc.
However, the above scintillator materials also have respective disadvantages when used for manufacturing a nuclear radiation detector, for example, sodium iodide and cesium iodide are very deliquescent and have poor stability; the bismuth germanate and cerium-doped gadolinium orthosilicate are complex in growth process, high in cost, low in energy resolution, low in quantum efficiency and low in light yield. In order to overcome the above shortcomings of inorganic pure inorganic scintillator materials, other materials with better overall performance and lower cost for nuclear radiation detection need to be found.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, a large-size zero-dimensional Cs is provided4PbBr6/CsPbBr3A perovskite scintillation crystal and a preparation method thereof.
The technical scheme is as follows: large-size zero-dimensional Cs of the invention4PbBr6/CsPbBr3The perovskite scintillation crystal and the preparation method thereof comprise the following steps:
(1) mixing N, N-dimethylformamide and hydrobromic acid at the temperature of 40-60 ℃;
(2) adding lead bromide and cesium bromide in a molar ratio of 1: 3-1: 6 into the mixed solution, and rotationally stirring at the temperature of 40-70 ℃ to obtain a supersaturated precursor solution;
(3) filtering the prepared supersaturated precursor solution for multiple times, and putting the supersaturated precursor solution into a crystal growth bottle;
(4) placing the growth bottle filled with the filtered supersaturated precursor solution on a heating table, and heating to 60-80 ℃ until the bottle becomes clear so as to completely dissolve tiny particles in the solution;
(5) and controlling the temperature of the growth bottle to gradually decrease to 30-60 ℃ for crystal growth.
Further, in the step (1), the volume ratio of the N, N-dimethylformamide to the hydrobromic acid is 2: 3-3: 2.
Further, in the step (2), the rotation speed of the rotary stirring is (500-2500) rpm, and the time is 6-15 hours.
Further, in the step (3), a sand core funnel with the aperture of 2-5 microns is adopted to filter the supersaturated precursor solution, and the filtering times are 2-4 times.
Further, in the step (5), the temperature of the growth bottle is decreased at a rate of 0.1-2.5 ℃/h.
Has the advantages that: compared with the prior art, the method can realize the growth of the large-size zero-dimensional Cs4PbBr6/CsPbBr3 perovskite scintillation crystal material by the solution method through the adjustment of the growth conditions. The method is simple, strong in controllability, good in repeatability, high in quality of grown crystals, regular in appearance, good in transparency, good in stability and high in quantum luminous efficiency (up to 98.3%), and can be used for detecting nuclear radiation fields (alpha particles, X rays and gamma rays). Meanwhile, compared with a melting method, the solution method is lower in cost in growth, and large-scale industrial production can be realized. In addition, the Cs grown by the present invention4PbBr6/CsPbBr3The size of the perovskite crystal can reach centimeter magnitude at most, and the perovskite crystal has good application prospect.
Drawings
FIG. 1 shows Cs prepared in example 54PbBr6/CsPbBr3XRD patterns of perovskite scintillation crystals;
FIG. 2 shows Cs prepared in example 54PbBr6/CsPbBr3A transmission spectrum of the perovskite scintillation crystal;
FIG. 3 shows Cs prepared in example 54PbBr6/CsPbBr3Scanning electron micrographs of perovskite scintillating crystals;
FIG. 4 shows Cs prepared in example 54PbBr6/CsPbBr3A transmission electron microscope photograph of the perovskite scintillation crystal;
FIG. 5 shows Cs prepared in example 54PbBr6/CsPbBr3A fluorescence spectrum of the perovskite scintillation crystal;
FIG. 6 shows Cs prepared in example 54PbBr6/CsPbBr3Luminescence quantum efficiency map of perovskite crystal.
Detailed Description
The present invention is further described with reference to the following examples, which are carried out on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to these examples.
Example 1
(1) 20mL of N, N-Dimethylformamide (DMF) and 30mL of hydrobromic acid (HBr) of HBr were mixed at a temperature of 40 ℃;
(2) adding lead bromide and cesium bromide with a molar ratio of 1:3 into the mixed solution obtained in the step (1), and rotationally stirring for 15 hours at the temperature of 70 ℃, wherein the rotational speed is 500rpm, so as to obtain a supersaturated precursor solution;
(3) filtering the supersaturated precursor solution prepared in the step (2) for 2 times by using a 2-micron funnel, and putting the filtered supersaturated precursor solution into a crystal growth bottle;
(4) placing the growth bottle filled with the filtered saturated precursor solution on a heating table, and heating to 70 ℃ to completely dissolve the tiny particles in the solution;
(5) the temperature of the growth bottle is controlled to be reduced at the speed of 0.1 ℃/h until the temperature is reduced to 60 ℃, and crystal growth is carried out.
Example 2
(1) 22mL of N, N-Dimethylformamide (DMF) and 28mL of hydrobromic acid (HBr) are mixed at a temperature of 45 ℃;
(2) adding lead bromide and cesium bromide with a molar ratio of 1:4 into the mixed solution obtained in the step (1), and rotationally stirring for 9 hours at a temperature of 60 ℃, wherein the rotational speed is 1000rpm, so as to obtain a supersaturated precursor solution;
(3) filtering the supersaturated precursor solution prepared in the step (2) for 3 times by using a 2.5-micron funnel, and putting the filtered supersaturated precursor solution into a crystal growth bottle;
(4) placing the growth bottle filled with the filtered saturated precursor solution on a heating table, and heating to 65 ℃ to completely dissolve the tiny particles in the solution;
(5) the temperature of the growth bottle is controlled to be reduced at the speed of 2.5 ℃/h until the temperature is reduced to 30 ℃, and crystal growth is carried out.
Example 3
(1) 24mL of N, N-Dimethylformamide (DMF) and 26mL of hydrobromic acid (HBr) were mixed at a temperature of 50 ℃;
(2) adding lead bromide and cesium bromide with a molar ratio of 1:5 into the mixed solution obtained in the step (1), and rotationally stirring for 12 hours at a temperature of 60 ℃, wherein the rotational speed is 2000rpm, so as to obtain a supersaturated precursor solution;
(3) filtering the supersaturated precursor solution prepared in the step (2) for 4 times by using a 5-micron funnel, and putting the supersaturated precursor solution into a crystal growth bottle;
(4) the growth flask containing the filtered saturated precursor solution was placed on a heating table and heated to 60 ℃ to completely dissolve the fine particles in the solution.
(5) The temperature of the growth bottle is controlled to be reduced at the speed of 2 ℃/h until the temperature is reduced to 35 ℃, and crystals are grown.
Example 4
(1) 26mL of N, N-Dimethylformamide (DMF) and 24mL of hydrobromic acid (HBr) were mixed at a temperature of 60 ℃;
(2) adding lead bromide and cesium bromide with a molar ratio of 1:6 into the mixed solution obtained in the step (1), and rotationally stirring for 15 hours at a temperature of 50 ℃, wherein the rotational speed is 2500rpm, so as to obtain a supersaturated precursor solution;
(3) filtering the supersaturated precursor solution prepared in the step (2) for 3 times by using a 4-micron funnel, and putting the filtered supersaturated precursor solution into a crystal growth bottle;
(4) the growth flask containing the filtered saturated precursor solution was placed on a heating table and heated to 80 ℃ to completely dissolve the fine particles in the solution.
(5) The temperature of the growth bottle is controlled to be reduced at the speed of 1 ℃/h until the temperature is reduced to 50 ℃, and crystals are grown.
Example 5
(1) Mixing 30mL of N, N-Dimethylformamide (DMF) and 20mL of hydrobromic acid (HBr) at a temperature of 50 ℃;
(2) adding lead bromide and cesium bromide with a molar ratio of 1:4 into the mixed solution obtained in the step (1), and rotationally stirring for 12 hours at the temperature of 40 ℃, wherein the rotational speed is 1500rpm, so as to obtain a supersaturated precursor solution;
(3) filtering the supersaturated precursor solution prepared in the step (2) for 3 times by using a 2.5-micron funnel, and putting the filtered supersaturated precursor solution into a crystal growth bottle;
(4) placing the growth bottle filled with the filtered saturated precursor solution on a heating table, and heating to 70 ℃ to completely dissolve the tiny particles in the solution;
(5) the temperature of the growth bottle is controlled to be reduced at the speed of 1 ℃/h until the temperature is reduced to 40 ℃, and crystals are grown.
According to the experimental results, Cs can be prepared in any of the above examples 1 to 54PbBr6/CsPbBr3Perovskite crystals. Wherein, the crystal prepared in the example 5 has the highest transparency and regular crystal shape, and is in a parallelepiped shape, as shown in fig. 2 and 3; other examples the crystals prepared in example 5 were inferior in transparency and regularity of appearance. Meanwhile, as can be seen from the scanning electron microscope image in fig. 3, the crystal prepared in example 5 has a size of 9mm, which is close to a centimeter level, and is suitable for the preparation of a detector, and the crystal prepared in other examples has a size of about 1-2 mm. It should be noted that, since the diameter of the growth flask used in the above examples is slightly larger than 1 cm, the size of the crystals to be produced is likely to be limited by the growth flask, and it is reasonable toIt is believed that the replacement of the growth flask enables the growth of Cs of larger size4PbBr6/CsPbBr3Perovskite centimeter crystals. From the transmission electron micrograph of fig. 4, the lattice spacing of the prepared crystal can be determined, and it can also be found that the minimum constituent unit of the crystal comprises two different lattice spacings, and the two lattice spacings respectively correspond to the crystal orientations specific to the two substances, which means that the minimum constituent unit of the crystal consists of Cs4PbBr6And CsPbBr3Are formed together. In FIG. 5 we can see that the position of the luminescence peak when excited with 365nm is around 520nm, which coincides with the absorption edge in the transmission spectrum in FIG. 2. From FIG. 2 we can see that the absorption edge on the left corresponds to Cs4PbBr6On the right side is CsPbBr3The calculation shows that Cs4PbBr6Has a forbidden band width of about 3.6ev and CsPbBr3The forbidden band width of (A) is about 2.4eV, and from FIG. 1, it can be seen that Cs4PbBr6The corresponding peak value is stronger, CsPbBr3The corresponding characteristic peak is very weak, so that the doping of the low-energy CsPbBr3 can enhance the luminescence of the whole material and simultaneously keep a larger forbidden bandwidth. The luminescence quantum efficiencies of the crystals prepared in examples 1 to 4 were 43.6%, 61.0%, 55.2% and 49.8%, respectively, and the luminescence quantum efficiency of example 5 was even as high as 98.3%, as shown in fig. 6, which reflects to some extent that the detector prepared from the material can have a better detection efficiency. The analysis on the attached drawings is combined, so that the prepared material has better comprehensive performance for nuclear radiation detection.
In addition, the solution method is adopted for preparation, and compared with a melting method which needs to be carried out at high temperature, the temperature is greatly reduced, so that the cost is greatly reduced.
Meanwhile, experiments prove that the zero-dimensional Cs prepared by the preparation method of the invention4PbBr6/CsPbBr3The perovskite scintillation crystal has good controllability and repeatability.
Therefore, the invention can prepare the zero-dimensional Cs with better comprehensive performance (higher quantum efficiency and good quality morphology) at lower growth cost4PbBr6/CsPbBr3PerovskiteThe crystal is scintillated to provide the nuclear radiation detector with higher detection efficiency.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. Large-size zero-dimensional Cs4PbBr6/CsPbBr3The preparation method of the perovskite scintillation crystal is characterized by comprising the following steps:
(1) mixing N, N-dimethylformamide and hydrobromic acid at the temperature of 40-60 ℃;
(2) adding lead bromide and cesium bromide in a molar ratio of 1: 3-1: 6 into the mixed solution, and rotationally stirring at the temperature of 40-70 ℃ to obtain a supersaturated precursor solution;
(3) filtering the prepared supersaturated precursor solution for multiple times, and putting the supersaturated precursor solution into a crystal growth bottle;
(4) placing the growth bottle filled with the filtered supersaturated precursor solution on a heating table, and heating to 60-80 ℃ until the bottle becomes clear so as to completely dissolve tiny particles in the solution;
(5) and controlling the temperature of the growth bottle to gradually decrease to 30-60 ℃ for crystal growth.
2. The large-size zero-dimensional Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite scintillation crystal is characterized by comprising the following steps: in the step (1), the volume ratio of the N, N-dimethylformamide to the hydrobromic acid is 2: 3-3: 2.
3. The large-size zero-dimensional Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite scintillation crystal is characterized by comprising the following steps: in the step (2), the rotating speed for rotating and stirring is 500-2500 rpm, and the time is 6-15 hours.
4. The large-size zero-dimensional Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite scintillation crystal is characterized by comprising the following steps: and (3) filtering the supersaturated precursor solution by adopting a sand core funnel with the aperture of 2-5 microns for 2-4 times.
5. The large-size zero-dimensional Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite scintillation crystal is characterized by comprising the following steps: in the step (5), the temperature of the growth bottle is reduced at a speed of 0.1-2.5 ℃/h.
6. Large-size zero-dimensional Cs prepared by the preparation method according to any one of claims 1 to 54PbBr6/CsPbBr3A perovskite scintillation crystal.
7. The large-size zero-dimensional Cs of claim 64PbBr6/CsPbBr3Use of a perovskite scintillation crystal for nuclear radiation detection.
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Cited By (6)
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| CN111960461A (en) * | 2020-07-20 | 2020-11-20 | 齐鲁工业大学 | Zero-dimensional perovskite Cs capable of regulating and controlling laser performance4PbBr6Micron crystal and preparation method thereof |
| CN112048764A (en) * | 2020-08-17 | 2020-12-08 | 南京航空航天大学 | Zero-dimensional Cs3Cu2I5Perovskite scintillation crystal and application thereof |
| CN112064115A (en) * | 2020-08-11 | 2020-12-11 | 南京航空航天大学 | Cs (volatile organic Compounds)4PbI6Perovskite crystal, preparation method and application |
| CN112876084A (en) * | 2020-12-25 | 2021-06-01 | 温州大学 | Quantum dot glass ceramics and preparation method thereof and method for preparing quantum dot glass ceramics product by applying 3D printing technology |
| CN115198361A (en) * | 2022-06-14 | 2022-10-18 | 山东大学 | High-quality and large-size Cs for aqueous solution growth 3 Cu 2 I 5 Method and application of fast scintillation response monocrystal |
| CN115703967A (en) * | 2021-08-14 | 2023-02-17 | 兰州大学 | Preparation method of perovskite nanocrystalline luminescent material |
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Cited By (8)
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| CN111960461A (en) * | 2020-07-20 | 2020-11-20 | 齐鲁工业大学 | Zero-dimensional perovskite Cs capable of regulating and controlling laser performance4PbBr6Micron crystal and preparation method thereof |
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| CN112048764B (en) * | 2020-08-17 | 2021-12-07 | 南京航空航天大学 | Zero-dimensional Cs3Cu2I5Perovskite scintillation crystal and application thereof |
| CN112876084A (en) * | 2020-12-25 | 2021-06-01 | 温州大学 | Quantum dot glass ceramics and preparation method thereof and method for preparing quantum dot glass ceramics product by applying 3D printing technology |
| CN112876084B (en) * | 2020-12-25 | 2022-12-09 | 温州大学 | Quantum dot glass ceramics and preparation method thereof and method for preparing quantum dot glass ceramics product by applying 3D printing technology |
| CN115703967A (en) * | 2021-08-14 | 2023-02-17 | 兰州大学 | Preparation method of perovskite nanocrystalline luminescent material |
| CN115198361A (en) * | 2022-06-14 | 2022-10-18 | 山东大学 | High-quality and large-size Cs for aqueous solution growth 3 Cu 2 I 5 Method and application of fast scintillation response monocrystal |
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