CN113136203A - Thallium-doped Cs with high luminous yield3Cu2I5Nanocrystalline scintillator - Google Patents

Thallium-doped Cs with high luminous yield3Cu2I5Nanocrystalline scintillator Download PDF

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CN113136203A
CN113136203A CN202110325995.9A CN202110325995A CN113136203A CN 113136203 A CN113136203 A CN 113136203A CN 202110325995 A CN202110325995 A CN 202110325995A CN 113136203 A CN113136203 A CN 113136203A
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李晓明
胡旭东
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Nanjing University of Science and Technology
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Abstract

The invention discloses thallium-doped Cs with high light yield3Cu2I5The nanocrystalline scintillator comprises the following steps: combining thallium acetylacetonate with Cs2CO3Heating the mixed solution of oleic acid and octadecene to a first temperature under the protection of argon, and carrying out heat preservation, heating to a second temperature, and carrying out heat preservation to obtain a first precursor solution; mixing CuI and ZnI2Heating the mixed solution of oleic acid, oleylamine and octadecene to a third temperature under the protection of inert gas, and then heating to a fourth temperature for heat preservation to obtain a second precursor solution; quickly injecting the first precursor solution into the second precursor solution, and quickly stirring and cooling to room temperature after reacting for a certain time; washed with ethyl acetate. Cs prepared by the present invention3Cu2I5:Tl+The nanocrystalline scintillator has the characteristics of higher radiation absorption coefficient, high light yield, solution-soluble processing and the like, and has better application prospect in the fields of high-resolution flexible X-ray imaging, radiation detection and the like.

Description

Thallium-doped Cs with high luminous yield3Cu2I5Nanocrystalline scintillator
Technical Field
The invention belongs to the technical field of inorganic semiconductor luminescent materials, and particularly relates to thallium-doped Cs with high light yield and high radiation absorption coefficient3Cu2I5A nanocrystalline scintillator and a method for making the same.
Background
Among the scintillators, metal halides have become the most widely used scintillator material due to their high radiation luminous efficiency. However, although conventional metal halide scintillators such as CsI: Tl and NaI: Tl have high light yield, they have long afterglow and cannot realize flexible detection imaging by a solution processing method. In addition, because the transition mode is fixed, the tunable spectrum can not be realized (J Phy D, 2015, 118 (21), 213106; Ieee T Nucl Sci, 1998). In another aspect, rare earth doped halides such as LaX3: Ce（J Phy D, 2006. 99 (12), 123520; Appl. Phys. Lett.2001, 79 (10), 1573-1575) has the advantages of high light yield, short decay time, high energy resolution, etc. However, due to rare earth element resource scarcity and high production cost, there is still a need to find a rare earth ion-free scintillator material. To date, metal halide perovskites are considered to be scintillator materials with application prospects due to the advantages of high quantum yield, tunable light-emitting wavelength, simple preparation, low cost and the likeNature, 2018, 561 (7721), 88-93; ACS Nano, 2019, 13 (2), 2520-2525). However, the low light yield resulting from the severe self-absorption effect severely limits its practical applications. Tin-based halides, e.g. two-dimensional layers (C)8H17NH3)2SnBr4Scintillator, Bmpip2SnBr4Scintillator (A)ACS Appl. Mater. Interfaces., 2020, 12 (17), 19797-19804；J. Am. Chem. Soc.2019, 141 (25), 9764-9768) and the like have high quantum yield, but Sn2+Easily oxidized to Sn in the air4+And is not suitable for commercial application. Copper-based halide Cs3Cu2I5Scintillator (A)Adv. Sci2020, 7 (11), 2000195) has better stability than the above materials, but lower radiation luminescence intensity.
Therefore, there is an urgent need to develop a nano-crystal scintillator with high radiation absorption coefficient, high light yield, high stability and short afterglow, and provide a scintillator material for low-cost, high-resolution, flexible X-ray medical imaging and radiation detection technologies.
Disclosure of Invention
The invention aims to provide Cs with high radiation absorption coefficient, high light yield, high stability and short afterglow3Cu2I5: Tl+A nanocrystalline scintillator and a method for making the same.
The invention adopts the following technical scheme:
thallium-doped Cs with high radiant luminous intensity3Cu2I5Halide nanocrystal scintillator, wherein ions Tl are doped+The atomic ratio of (A) is 0.5-10%.
Above thallium doped Cs3Cu2I5The preparation method of the nanocrystalline scintillator comprises the following steps:
(1) combining thallium acetylacetonate with Cs2CO3Heating the mixed solution of oleic acid and octadecene to a first temperature under the protection of argon, and preserving heat, and then heating to a second temperature and preserving heat until the mixed solution fully reacts to form a brown clear transparent liquid;
(2) mixing CuI and ZnI2Heating the mixed solution of oleic acid, oleylamine and octadecene to a third temperature under the protection of inert gas, and then heating to a fourth temperature for heat preservation until the mixed solution becomes yellow clear transparent liquid;
(3) quickly injecting the precursor solution obtained in the step (1) into the solution obtained in the step (2) by using a needle tube, and quickly stirring and cooling to room temperature after reacting for a certain time;
(4) washing the solution cooled in the step (3) by using ethyl acetate, and obtaining thallium-doped Cs3Cu2I5And re-dispersing the nano-crystal scintillator in an organic solvent for storage.
Preferably, in the step (1), the mixture is heated to a first temperature and kept at the first temperature for 10 min, and then heated to a second temperature and kept at the second temperature for 10 min, wherein the first temperature is 120 ℃ and the second temperature is 150 ℃.
Preferably, in the step (2), the mixture is heated to a third temperature and kept for 10 min, and then heated to a fourth temperature and kept for 10 min, wherein the third temperature is 120 ℃ and the fourth temperature is 160 ℃.
Preferably, in step (3), the reaction time is 30 s.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method adopted by the invention can successfully prepare Tl+Incorporation of Cs3Cu2I5The crystal lattice is combined to replace the Cs bit to form the thallium doped Cs3Cu2I5A nanocrystalline scintillator and the scintillator has a higher light yield than existing similar materials.
(2) Cs prepared by the invention3Cu2I5: Tl+The nanocrystalline scintillator has uniform size, high radiation absorption coefficient, high energy resolution, short afterglow and high stability, so the nanocrystalline scintillator can be applied to the fields of high-resolution flexible X-ray medical imaging equipment, high-energy particle radiation detection and the like.
Drawings
FIG. 1 shows Cs synthesized under the conditions shown in example 3 of the present invention3Cu2I5: Tl+(dopant ion Tl)+Atomic ratio of 1%) scintillator samples with nanocrystals dispersed in three organic solvents were photographed for luminescence under 254 nm uv irradiation.
FIG. 2 shows the preparation of Cs in example 3 of the present invention3Cu2I5: Tl+X-ray diffraction (XRD) pattern of the nanocrystalline sample.
FIG. 3 shows the preparation of Cs in example 3 of the present invention3Cu2I5: Tl+Transmission Electron Microscope (TEM) pictures of nanocrystalline samples.
FIG. 4 shows Cs prepared in examples 1 and 3 of the present invention3Cu2I5Nanocrystal and Cs3Cu2I5: Tl+Schematic representation of Photoluminescence (PL) of nanocrystalline samples under 254 nm excitation.
FIG. 5 shows Cs prepared in examples 1 and 3 of the present invention3Cu2I5Nanocrystal and Cs3Cu2I5: Tl+Schematic representation of photoluminescence (RL) of nanocrystalline samples under X-ray excitation.
Detailed Description
The present invention is further illustrated by the following description taken in conjunction with the accompanying drawings and the specific embodiments, it is to be understood that these embodiments are merely illustrative of the invention and are not intended to limit the scope of the invention, which is defined by the appended claims, and that various equivalent modifications thereof will occur to those skilled in the art upon reading the present invention
Thallium-doped Cs of the invention3Cu2I5The preparation method of the nanocrystalline scintillator comprises the following steps:
(1) combining thallium acetylacetonate with Cs2CO3Heating the mixed solution of oleic acid and octadecene to a certain temperature under the protection of argon gas for heat preservation, and then heating to a high temperature until the mixed solution is fully reacted to form a brown clear transparent liquid;
(2) storing the solution obtained in the step (1) as a precursor in a reagent bottle for later use;
(3) mixing CuI and ZnI2Heating the mixed solution of oleic acid, oleylamine and octadecene to a certain temperature under the protection of inert gas for heat preservation, and then heating to a high temperature until reactants are fully dissolved and the solution becomes yellow clear transparent liquid;
(4) taking a proper amount of the precursor solution collected in the step (2) by using a disposable needle tube, quickly injecting the precursor solution into the clear transparent liquid in the step (3), quickly transferring the precursor solution into a water tank after reacting for a specific time, and stirring and cooling the precursor solution to room temperature by using an ice water bath;
(5) washing the cooled original solution in the step (4) with ethyl acetate according to a specific ratio, and obtaining thallium-doped Cs3Cu2I5Re-dispersing the nano-crystal scintillator in organic solvent to obtain Cs3Cu2I5Dispersing in organic solvent through centrifugation can screen out nanometer level size particle first, and can disperse the storage of nanometer crystal better.
Example 1
According to the formula Cs3Cu2I5The stoichiometric ratio of each element in the ion Tl+Cs with a doping ratio of 0%3Cu2I5Sample of nanocrystalline scintillator, 5 mmol of Cs2CO3Adding 5 mL of oleic acid and 20 mL of octadecylene into a 100 mL three-necked flask, heating to 120 ℃ under the protection of argon, preserving heat for 10 min, heating to 150 ℃, preserving heat for 10 min, then cooling to 80 ℃, collecting in a reagent bottle while the solution is hot, and storing for later use as a precursor solution.
According to the formula Cs3Cu2I5The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL of oleic acid, 0.8 mL of oleylamine and 15 mL of octadecene were added to a 100 mL three-necked flask and heated to 120 ℃ under argon shield, held for 10 min, and heated to 160 ℃ until the solution became a yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Example 2
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the ion Tl+Cs with a doping ratio of 0.5%3Cu2I5A nanocrystalline scintillator sample, 0.0498 mmol of thallium acetylacetonate and 4.9551 mmol of Cs2CO3Adding 5 mL of oleic acid and 20 mL of octadecylene into a 100 mL three-necked flask, heating to 120 ℃ under the protection of argon, preserving heat for 10 min, heating to 150 ℃, preserving heat for 10 min, then cooling to 80 ℃, collecting in a reagent bottle while the solution is hot, and storing for later use as a precursor solution.
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL ofOleic acid, 0.8 mL oleylamine, and 15 mL octadecene were added to a 100 mL three-necked flask and heated to 120 ℃ under argon shield, held for 10 min, and heated to 160 ℃ until the solution turned to a yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5: Tl+And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Example 3
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the ion Tl+Cs with doping ratio of 1%3Cu2I5A nanocrystalline scintillator sample, 0.0990 mmol of thallium acetylacetonate and 4.9010 mmol of Cs2CO3Adding 5 mL of oleic acid and 20 mL of octadecylene into a 100 mL three-necked flask, heating to 120 ℃ under the protection of argon, preserving heat for 10 min, heating to 150 ℃, preserving heat for 10 min, then cooling to 80 ℃, collecting in a reagent bottle while the solution is hot, and storing for later use as a precursor solution.
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL of oleic acid, 0.8 mL of oleylamine and 15 mL of octadecene were added to a 100 mL three-necked flask and heated to 120 ℃ under argon shield, held for 10 min, and heated to 160 ℃ until the solution became a yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5: Tl+And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Example 4
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the ion Tl+Cs with a doping ratio of 2%3Cu2I5A nanocrystalline scintillator sample, 0.1960 mmol of thallium acetylacetonate and 4.8039 mmol of Cs2CO3Adding 5 mL of oleic acid and 20 mL of octadecylene into a 100 mL three-necked flask, heating to 120 ℃ under the protection of argon, preserving heat for 10 min, heating to 150 ℃, preserving heat for 10 min, then cooling to 80 ℃, collecting in a reagent bottle while the solution is hot, and storing for later use as a precursor solution.
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL of oleic acid, 0.8 mL of oleylamine and 15 mL of octadecene were added to a 100 mL three-necked flask and heated to 120 ℃ under argon shield, held for 10 min, and heated to 160 ℃ until the solution became a yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5: Tl+And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Example 5
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the ion Tl+Cs with a doping ratio of 5%3Cu2I5A nanocrystalline scintillator sample, 0.4762 mmol of thallium acetylacetonate and 4.5238 mmol of Cs2CO35 mL of oleic acid, 20 mL of octadecanolAdding alkene into a 100 mL three-neck flask, heating to 120 ℃ under the protection of argon, preserving heat for 10 min, heating to 150 ℃, preserving heat for 10 min, then enabling the solution to become colorless clear transparent liquid, cooling to 80 ℃, collecting in a reagent bottle while the solution is hot, and storing for later use as a precursor.
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL of oleic acid, 0.8 mL of oleylamine and 15 mL of octadecene were added to a 100 mL three-necked flask and heated to 120 ℃ under argon shield, held for 10 min, and heated to 160 ℃ until the solution became a yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5: Tl+And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Example 6
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the ion Tl+Cs with a doping ratio of 10%3Cu2I5A nanocrystalline scintillator sample, 0.9091 mmol of thallium acetylacetonate and 4.0909 mmol of Cs2CO3And 5 mL of oleic acid and 20 mL of octadecene are added into a 100 mL three-necked flask, the flask is heated to 120 ℃ under the protection of argon, the temperature is kept for 10 min, the flask is heated to 150 ℃ and kept for 10 min, at the moment, the solution becomes colorless clear transparent liquid, the solution is cooled to 80 ℃ and collected in a reagent bottle while the solution is hot, and the solution is used as a precursor solution to be stored for later use.
According to the formula Cs3Cu2I5: Tl+The stoichiometric ratio of each element in the mixture is 0.8 mmol of CuI and 1.2 mmol of ZnI20.8 mL of oleic acid, 0.8 mL of oleylamine, and 15 mL of octadecene were added to 100Heating to 120 ℃ under the protection of argon in a mL three-neck flask, preserving the temperature for 10 min, and heating to 160 ℃ until the solution becomes yellow clear transparent liquid.
At the moment, 2 mL of the precursor solution is extracted and quickly injected into yellow clear transparent liquid at the temperature, the mixture is moved to a water tank after reacting for 30 s, the mixture is stirred and cooled to room temperature by adopting an ice water bath, 45 mL of ethyl acetate solution is added into the obtained milky turbid liquid, the milky turbid liquid is centrifugally washed at 9000 rpm for 5 min, the washing is repeated for 1-2 times, and the obtained Cs is3Cu2I5: Tl+And re-dispersing the nano-crystals in 2 mL of cyclohexane solution.
Fig. 1 is a photograph showing the luminescence of the nanocrystal sample obtained in example 3 when dispersed in three different organic solvents and excited by 254 nm ultraviolet light, and it is shown in fig. 1 that the nanocrystal dispersion of cyclohexane is the best.
FIG. 2 is the XRD pattern of the nanocrystal sample obtained in example 3, from FIG. 2, the Cs3Cu2I5: Tl+The nanocrystalline sample belongs to a pure orthogonal phase, and doping of Tl does not introduce new impurities or other phases.
FIG. 3 is a TEM photograph of the sample obtained in example 3, and it is clear from FIG. 3 that the obtained nanocrystals are long rods and have a relatively uniform size distribution.
FIG. 4 is a PL comparison graph of the nanocrystal samples obtained in example 1 and example 3 under excitation of 254 nm UV light, and FIG. 5 shows that the undoped Cs3Cu2I5The PL spectrum of the nanocrystal has a luminescence center at 445 nm and Cs3Cu2I5: Tl+The PL spectrum of the nanocrystal has an emission center at 454 nm, and the intensity is superior to that of the PL spectrum.
FIG. 5 is a schematic diagram showing RL comparison of the nanocrystalline samples obtained in examples 1 and 3 under X-ray excitation, and it is shown in FIG. 5 that Cs3Cu2I5: Tl+The radiation luminescence intensity of the nanocrystalline scintillator is greater than that of undoped Cs3Cu2I5The nano-crystal scintillator is as much as six times higher.

Claims (5)

1. AThallium-doped Cs3Cu2I5The halide nanocrystalline scintillator is characterized in that the atomic proportion of thallium doping is 0.5-10%.
2. The thallium-doped Cs of claim 13Cu2I5The preparation method of the nanocrystalline scintillator is characterized by comprising the following steps:
combining thallium acetylacetonate with Cs2CO3Heating the mixed solution of oleic acid and octadecene to a first temperature under the protection of argon, and carrying out heat preservation, heating to a second temperature, and carrying out heat preservation to obtain a first precursor solution;
mixing CuI and ZnI2Heating the mixed solution of oleic acid, oleylamine and octadecene to a third temperature under the protection of inert gas, and then heating to a fourth temperature for heat preservation to obtain a second precursor solution;
quickly injecting the first precursor solution into the second precursor solution, and quickly stirring and cooling to room temperature after reacting for a certain time;
washing the cooled solution of the step (3) by using ethyl acetate.
3. The method of claim 2, wherein in step (1), the heating is carried out to a first temperature for 10 min, and then to a second temperature for 10 min, the first temperature being 120 ℃ and the second temperature being 150 ℃.
4. The method of claim 2, wherein in step (2), the heating is carried out to a third temperature for 10 min, and then to a fourth temperature for 10 min, the third temperature being 120 ℃ and the fourth temperature being 160 ℃.
5. The method of claim 2, wherein in step (3), the reaction time is 30 s.
CN202110325995.9A 2021-03-26 2021-03-26 Thallium-doped Cs with high luminous yield3Cu2I5Nanocrystalline scintillator Pending CN113136203A (en)

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CN114276802B (en) * 2021-12-27 2023-10-13 南京理工大学 Preparation method of thallium-doped cesium-copper-iodine scintillator film for inhibiting oxidation precipitation of iodide ions
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WO2023132607A1 (en) * 2022-01-05 2023-07-13 주식회사 한솔케미칼 Method for manufacturing non-lead-based perovskite particles
KR102602279B1 (en) * 2022-01-05 2023-11-14 주식회사 한솔케미칼 Preparation method of lead-free perovskite nanocrystalline particles
CN115678546A (en) * 2022-10-28 2023-02-03 南京理工大学 Thallium-doped Cs 3 Cu 2 I 5 Scintillator microcrystalline powder and preparation method and application thereof
CN115678546B (en) * 2022-10-28 2023-12-15 南京理工大学 Thallium doped Cs 3 Cu 2 I 5 Scintillator microcrystalline powder and preparation method and application thereof
CN117552106A (en) * 2024-01-10 2024-02-13 江苏先进无机材料研究院 Rare earth-based zero-dimensional perovskite halide scintillation monocrystal as well as preparation method and application thereof
CN117552106B (en) * 2024-01-10 2024-04-05 江苏先进无机材料研究院 Rare earth-based zero-dimensional perovskite halide scintillation monocrystal as well as preparation method and application thereof

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