CN110734765A - Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillation powder and preparation method thereof - Google Patents
Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillation powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Cs4PbBr6/CsPbBr3The method can realize zero-dimensional perovskite nanocrystalline scintillation powder required by radiation field detection, and successfully synthesize Cs in batches by using a solvothermal method and adjusting parameters such as reactant proportion, reaction temperature, reaction time and the like in an organic solvent4PbBr6/CsPbBr3The perovskite nanocrystalline scintillation powder method comprises the following steps: taking an organic solvent dimethyl sulfoxide as a solvent, and CsBr and PbBr2The yellow-green sample synthesized by the solute at the constant temperature of is washed, filtered and driedEqual series process to obtain bright green product, namely Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillating powders. The preparation method is simple, low in cost and strong in controllability, and can be used for mass production, and the Cs prepared by the method4PbBr6/CsPbBr3The perovskite has excellent quantum luminous efficiency, good stability and good heat recovery characteristic.
Description
Technical Field
The invention belongs to the technical field of inorganic nano material preparation, and particularly relates to Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillation powder and a preparation method thereof.
Background
Recently, scintillator materials based on micro-nano materials have been developed to a great extent due to the defects of difficult preparation, high growth cost and the like of scintillator materials of traditional body materials, high-light-yield and low-cost micro-nano scintillation material powders are used in the field of nuclear radiation detection, particularly in the field of X-ray imaging, which are generalized by , and include Pb-based nanocrystals (e.g., PbS, PbSe, PbTe) and inorganic perovskite nanocrystals (e.g., CsPbBr)3) A material.
The nano-crystalline of PbS, PbSe and PbTe has been studied by due to obvious quantum confinement effect, and has achieved success in the field of radiographic detection, however, because the forbidden bandwidth from the material to the nano-crystalline material is small, the material is easily affected by the environmental temperature, and the of limiting the material in degree of limitation is advanced3The nanocrystalline material is applied to the X-ray scintillation imaging field due to the characteristics of low preparation cost, high light yield, fast response time, large forbidden bandwidth and the like, and obtains higher spatial resolution and imaging graph, however, further researches show that CsPbBr3The nanocrystalline material is easy to deliquesce in air due to large surface area, has poor stability, and cannot collect the energy spectrum of the emission signal due to limited material thickness and insufficient energy deposition, so that nanocrystalline scintillating materials with high detection efficiency, good stability and high light yield are needed in the field.
Disclosure of Invention
Object of the invention to solve the above problems of the prior art, nuclear radiation signals are providedDetected Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillation powder and a preparation method thereof. The method has the advantages of low preparation cost, high synthesis efficiency, high luminescence quantum efficiency of products prepared in a large scale, good stability, good response to X-ray detection, and capability of being used for detecting nuclear radiation signals.
The technical scheme is as follows: the invention provides Cs for nuclear radiation signal detection4PbBr6/CsPbBr3The preparation method of the perovskite nanocrystalline scintillating powder comprises the following steps: (1) placing dimethyl sulfoxide solution into a bottle, adding CsBr and PbBr2Obtaining mixed solution by powder; (2) heating the mixed solution at a preset ambient temperature and rotating for a preset time, and then adding CsBr and PbBr again2Continuously heating and rotating the new mixed solution at the preset environmental temperature until the color of the new mixed solution becomes orange, then transferring to the room temperature for standing for periods until the color of the new mixed solution appears yellow-green, (4) putting the standing solution into a funnel for filtering, repeatedly washing and filtering, and drying the finally filtered solution to obtain the Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillating powders.
step, CsBr and PbBr added in step (1)2The molar ratio of the powder is 1 (0.8-2.5).
, in the step (2), the preset environment temperature is 70-90 ℃, the rotating speed is 500-2500 rpm, and the rotating time is 20-120 minutes.
, standing at 20-30 deg.C for 0.5-2.5 h.
, in the step (4), a sand core funnel with the aperture of 2-5 mu m is adopted for filtering or re-filtering, the total filtering times are 2-5 times, or the sand core funnel is placed on a conical flask and is tightly plugged by a rubber plug during filtering, and the conical flask is connected with a vacuum pump for suction filtration.
Further , in step (4), washing with dimethyl sulfoxide is carried out.
, in the step (4), the drying treatment of the final filtered solution includes drying in a vacuum drying oven at 50-70 deg.C for 6-12 hours.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) can prepare Cs4PbBr6/CsPbBr3The perovskite nanocrystalline scintillating powder has the energy gap of about 3.6ev, which is higher than the PbS, PbSe, PbTe and CsPbBr for nuclear radiation signal detection3Etc. the forbidden band width of the material. The material is less affected by the ambient temperature due to the large forbidden band width, and the ambient thermal noise is reduced.
(2) The Cs prepared by experimental determination4PbBr6/CsPbBr3The perovskite nanocrystalline scintillating powder has excellent quantum luminous efficiency (up to 51.3%), good stability, can be stored in air for at least 45 days without change, has good heat recovery characteristic, and can be used for detecting nuclear radiation fields (alpha particles, X rays and gamma rays).
(3) By adding CsBr and PbBr in two portions2The powder is added into the solvent, so that the two can be reacted fully and uniformly; meanwhile, the solute proportion, the reaction temperature, the washing times and the washing solution are elaborately set, so that the high-quality Cs can be grown by the solution thermal method4PbBr6/CsPbBr3Perovskite nanocrystalline scintillating powder; the preparation method is simple, low in cost, strong in controllability and capable of being manufactured in large batch.
Drawings
FIG. 1 shows Cs prepared in example 14PbBr6/CsPbBr3XRD pattern of perovskite nanocrystals;
FIG. 2 shows Cs prepared in example 14PbBr6/CsPbBr3TEM photograph of perovskite nanocrystal;
FIG. 3 shows Cs prepared in example 24PbBr6/CsPbBr3Temperature change PL profile of perovskite nanocrystal;
FIG. 4 shows Cs prepared in example 34PbBr6/CsPbBr3X-ray excitation spectrum photo of perovskite nanocrystalline;
FIG. 5 shows Cs prepared in example 44PbBr6/CsPbBr3A steady state fluorescence lifetime map of the perovskite nanocrystals;
FIG. 6 shows Cs prepared in example 54PbBr6/CsPbBr3A luminescence quantum efficiency map of the perovskite nanocrystals;
FIG. 7 shows Cs prepared in example 64PbBr6/CsPbBr3Luminescence quantum efficiency map of perovskite nanocrystal.
Detailed Description
The following is a detailed description of the present invention with reference to the accompanying drawings. The present embodiment is performed on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to these embodiments.
Example 1
(1) 25ml of dimethyl sulfoxide was added to a vessel, CsBr and PbBr were added2Mixing the powder into the solution according to the proportion of 1mol to 1 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 80 ℃, the rotating speed is 500rpm, and the rotating time is 30 minutes;
(3) adding the powder added last time (namely CsBr and PbBr mixed according to the proportion of 1mol:1 mol) into the solution prepared in the step (2)2Powder) and continued heating and spinning until the solution turned orange at high temperature;
(4) standing the solution prepared in the step (3) at room temperature of 20 ℃ for 30 minutes to turn into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 2 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) washing the powder filtered in the step (5) with dimethyl sulfoxide for 2 times, and repeating the suction filtration operation in the step (5) after each washing;
(7) drying the powder obtained in the step (6) in a vacuum drying oven at 50 ℃ for 6 hours to obtain the targetProduct of bright green Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
Example 2
(1) 25ml of dimethyl sulfoxide was added to a vessel, CsBr and PbBr were added2Mixing the powder into the solution according to the proportion of 1mol:1.5 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 70 ℃, the rotating speed of the rotation is 1000rpm, and the rotating time is 30 minutes;
(3) adding the last added powder (namely CsBr and PbBr mixed according to the proportion of 1mol:1.5 mol) into the solution prepared in the step (2)2Powder) and continued heating and spinning until the solution turned orange at high temperature;
(4) standing the solution prepared in the step (3) at room temperature of 22 ℃ for 45 minutes to turn into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 2.5 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) washing the powder filtered in the step (5) for 3 times by using dimethyl sulfoxide, and continuously repeating the suction filtration operation in the step (5) after washing each time;
(7) drying the powder obtained in the step (6) in a vacuum drying oven at 55 ℃ for 9 hours to obtain the target product of bright green Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
Example 3
(1) 25ml of dimethyl sulfoxide was added to a vessel, CsBr and PbBr were added2Mixing the powder into the solution according to the proportion of 1mol:0.8 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 75 ℃, the rotating speed is 1500rpm, and the rotating time is 30 minutes;
(3) adding the last added powder (namely CsBr and PbBr mixed according to the proportion of 1mol:0.8 mol) into the solution prepared in the step (2)2Powder) repeating step (2) until the solution turns orange at elevated temperature;
(4) standing the solution prepared in the step (3) at room temperature of 24 ℃ for 1h to change the solution into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 2.5 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) washing the powder filtered in the step (5) with dimethyl sulfoxide for 4 times, and continuously repeating the suction filtration operation in the step (5) after each washing;
(7) drying the powder obtained in the step (6) in a vacuum drying oven at 70 ℃ for 12 hours to obtain a target product Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
Example 4
(1) 25ml of dimethyl sulfoxide was added to a vessel, CsBr and PbBr were added2Mixing the powder into the solution according to the proportion of 1mol to 2 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 90 ℃, the rotating speed is 2500rpm, and the rotating time is 50 minutes;
(3) adding the powder added last time (namely CsBr and PbBr mixed according to the proportion of 1mol:2 mol) into the solution prepared in the step (2)2Powder) repeating step (2) until the solution turns orange at elevated temperature;
(4) standing the solution prepared in the step (3) at room temperature of 26 ℃ for 1.5h to turn into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 5 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) washing the powder filtered in the step (5) with dimethyl sulfoxide for 5 times, and continuously repeating the suction filtration operation in the step (5) after each washing;
(7) drying the powder obtained in the step (6) in a vacuum drying oven at 70 ℃ for 15 hours to obtain a target product Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
Example 5
(1) Adding 25ml of dimethyl sulfoxide into a container, and addingCsBr and PbBr2Mixing the powder into the solution according to the proportion of 1mol:2.5 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 90 ℃, the rotating speed is 2000rpm, and the rotating time is 30 minutes;
(3) adding the powder added last time (namely CsBr and PbBr mixed according to the proportion of 1mol:2.5 mol) into the solution prepared in the step (2)2Powder) repeating step (2) until the solution turns orange at elevated temperature;
(4) standing the solution prepared in the step (3) at room temperature of 30 ℃ for 2h to change the solution into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 2.5 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) washing the powder filtered in the step (5) for 3 times by using dimethyl sulfoxide, and continuously repeating the suction filtration operation in the step (5) after washing each time;
(7) drying the powder obtained in the step (6) in a vacuum drying oven at 60 ℃ for 12 hours to obtain a target product Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
Example 6
(1) 25ml of dimethyl sulfoxide was added to a vessel, CsBr and PbBr were added2Mixing the powder into the solution according to the proportion of 1mol to 1 mol;
(2) putting the solution obtained in the step (1) into an oil bath pot for heating and rotating, wherein the heating temperature is set at 80 ℃, the rotating speed is 2000rpm, and the rotating time is 30 minutes;
(3) adding the powder added last time (namely CsBr and PbBr mixed according to the proportion of 1mol:1 mol) into the solution prepared in the step (2)2Powder) repeating step (2) until the solution turns orange at elevated temperature;
(4) standing the solution prepared in the step (3) at room temperature of 30 ℃ for 2.5h to turn into yellow green;
(5) placing the solution prepared in the step (4) on a conical flask by using a sand core funnel with the aperture of 2.5 mu m, and plugging the conical flask by using a rubber plug, wherein the conical flask is connected with a vacuum pump for suction filtration;
(6) drying the powder filtered in the step (5) in a vacuum drying oven at 60 ℃ for 12 hours to obtain a target product Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder.
In the above example, CsBr and PbBr were added in two portions2The powder is added into the solvent, so that the reaction of the powder and the solvent is more fully and uniformly. Meanwhile, due to the careful arrangement of the solute proportion, the reaction temperature, the washing times and the washing solution, the prepared material has better quality and performance.
From the analysis of FIG. 1, it can be seen that the powder thus prepared was Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder. Two luminescence peaks appear in FIG. 3, the left luminescence peak corresponding to Cs4PbBr6And the right luminescence peak corresponds to CsPbBr3And Cs is calculated4PbBr6The corresponding forbidden band width is 3.6 eV. The forbidden band width is larger than the aforementioned PbS, PbSe, PbTe and CsPbBr3Etc. the forbidden band width of the material. A larger forbidden band width can reduce the influence of ambient thermal noise. Small amount of CsPbBr with low forbidden band width3Can be added to make the Cs4PbBr6/CsPbBr3Perovskite nanocrystalline powder overall vs. pure Cs4PbBr6The light emission is enhanced while maintaining a large forbidden bandwidth. As shown in fig. 4, the full width at half maximum of the X-ray excitation spectrum of the prepared powder is 27.78 nm, which indicates that the powder has higher resolution for X-rays and has better application prospect in the field of X-ray nuclear radiation detection. As shown in fig. 6, the luminescence quantum efficiency of the powder prepared in example 5 is as high as 51.3%, and the luminescence quantum efficiency of the powder prepared in other examples is between 16% and 40%, respectively, which indicates that the material has excellent detection performance. The difference in luminescence quantum efficiency in FIGS. 6 and 7 shows the effect of washing on the increase in luminescence quantum efficiency, the purpose of washing being to remove the Cs from the wash4PbBr6Bound excess CsPbBr3The content of the powder is high, the purpose of improving the luminous quantum efficiency is achieved, and the CsPbBr is pure3The luminescence quantum efficiency of (A) is less than 1%, and perovskite luminescence can be caused if the perovskite is not subjected to washing filtrationThe light efficiency is obviously reduced, and the perovskite Cs4PbBr6Has a forbidden band width larger than CsPbBr3The transition to low energy level when excited, increases radiative recombination and reduces non-radiative coincidence, so that the luminescent quantum efficiency of the perovskite is significantly enhanced, and the stability in air is tested and can be preserved for at least 45 days without change, mainly because of Cs4PbBr6Doped with points CsPbBr3And then becomes more stable.
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 (9)
1, Cs4PbBr6/CsPbBr3The preparation method of the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps:
(1) placing dimethyl sulfoxide solution into a bottle, adding CsBr and PbBr2Obtaining mixed solution by powder;
(2) heating the mixed solution at a preset ambient temperature and rotating for a preset time, and then adding CsBr and PbBr again2Powder to obtain a new mixed solution;
(3) continuing to heat and rotate the new mixed solution at the predetermined ambient temperature until the color of the new mixed solution becomes orange, and then transferring to room temperature for hours until the new mixed solution appears bright green;
(4) putting the solution after standing into a funnel for filtering, repeatedly washing and filtering, and drying the finally filtered solution to obtain the Cs4PbBr6/CsPbBr3Perovskite nanocrystalline scintillating powders.
2. The Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps: in the step (1), addingCsBr and PbBr incorporated2The molar ratio of the powder is 1 (0.8-2.5).
3. The Cs of claim 14PbBr6/CsPbBr3The method for preparing the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps: in the step (2), the preset environmental temperature is 70-90 ℃, the rotating speed is 500-2500 rpm, and the rotating time is 20-120 minutes.
4. The Cs of claim 14PbBr6/CsPbBr3The preparation method of the nanocrystalline scintillation powder is characterized by comprising the following steps: and (4) standing for 0.5-2.5 h at the room temperature of 20-30 ℃ in the step (3).
5. The Cs of claim 14PbBr6/CsPbBr3The method for preparing the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps: and (4) filtering or re-filtering by adopting a sand core funnel with the aperture of 2-5 mu m for 2-5 times, wherein the sand core funnel is tightly plugged by a rubber stopper on a conical flask during filtering, and the conical flask is connected with a vacuum pump for suction filtration.
6. The Cs of claim 14PbBr6/CsPbBr3The method for preparing the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps: in the step (4), dimethyl sulfoxide is adopted for washing.
7. The Cs of claim 14PbBr6/CsPbBr3The preparation method of the perovskite nanocrystalline scintillation powder is characterized by comprising the following steps: in the step (4), the drying treatment of the final filtered solution comprises: drying the mixture in a vacuum drying oven at 50-70 ℃ for 6-12 hours.
8, Cs prepared according to the method of any of claims 1-74PbBr6/CsPbBr3Perovskite nanocrystalline scintillating powders.
9, Cs according to claim 84PbBr6/CsPbBr3The perovskite nanocrystalline scintillating powder is applied to nuclear radiation signal detection.
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| CN111348675A (en) * | 2020-02-25 | 2020-06-30 | 华中科技大学 | Application of non-self-absorption nanocrystalline as scintillator and preparation method thereof |
| CN111909696A (en) * | 2020-06-24 | 2020-11-10 | 华南理工大学 | Organic-inorganic hybrid zero-dimensional non-lead perovskite material and synthetic method thereof |
| CN113325462A (en) * | 2021-04-25 | 2021-08-31 | 上海大学 | Preparation method of perovskite nanocrystal-based gamma ray scintillation conversion screen |
| WO2023047144A1 (en) | 2021-09-22 | 2023-03-30 | Szegedi Tudományegyetem | Dopant-free copper-based perovskite-analogue inorganic thin-film scintillator for charged particle detection |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110643360A (en) * | 2019-08-29 | 2020-01-03 | 广东工业大学 | Water-resistant and heat-resistant perovskite nanocrystalline and preparation method and application thereof |
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| CN111348675A (en) * | 2020-02-25 | 2020-06-30 | 华中科技大学 | Application of non-self-absorption nanocrystalline as scintillator and preparation method thereof |
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| CN111909696B (en) * | 2020-06-24 | 2022-10-25 | 华南理工大学 | Organic-inorganic hybrid zero-dimensional non-lead perovskite material and synthetic method thereof |
| CN113325462A (en) * | 2021-04-25 | 2021-08-31 | 上海大学 | Preparation method of perovskite nanocrystal-based gamma ray scintillation conversion screen |
| WO2023047144A1 (en) | 2021-09-22 | 2023-03-30 | Szegedi Tudományegyetem | Dopant-free copper-based perovskite-analogue inorganic thin-film scintillator for charged particle detection |
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