CN114276802A - Preparation method of thallium-doped cesium-copper-iodine scintillator film for inhibiting oxidation and precipitation of iodide ions - Google Patents
Preparation method of thallium-doped cesium-copper-iodine scintillator film for inhibiting oxidation and precipitation of iodide ions Download PDFInfo
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Abstract
The invention discloses thallium-doped Cs for inhibiting the oxidation precipitation of iodide ions3Cu2I5A method for preparing a scintillator film. The method comprises the steps of mixing and reacting cuprous iodide, cesium iodide, thallium iodide, PMMA, dimethylformamide, hypophosphorous acid and Tween80 to form a precursor solution, vacuumizing to remove bubbles, uniformly coating the precursor solution on a glass substrate, and then heating and annealing to obtain thallium-doped Cs3Cu2I5A scintillator film. The invention introduces strong reducing acid H3PO2So as to inhibit the oxidation precipitation of iodide ions in the formation stage of the precursor solution, and in addition, ether bonds contained in the Tween80 can also inhibit the oxidation precipitation of iodide ions after film formation, so that the prepared Cs3Cu2I5：Tl+The scintillator film has the advantages of high radiation absorption coefficient, larger light yield, no afterglow caused by extremely short service life and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic semiconductor scintillator materials, and relates to thallium-doped cesium copper iodide (Cs) for inhibiting oxidation and precipitation of iodide ions3Cu2I5:Tl+) A method for preparing a scintillator film.
Background
The metal halide has high radiation luminous efficiency and is a scintillator material with the most extensive application. However, the current commercial metal halide scintillators such as CsI: Tl and NaI: Tl have high light yield, but generally have long afterglow, and cannot realize simplification of a synthesis process through a convenient processing method, so that the current method still adopts a crucible growth method; in addition, due to the defect problem of larger crystal, flexible detection and high-resolution imaging are difficult to realize (IeeeSensors Journal,2009,9(9),1154 and 1156, Astroparticle Phys,2019,108(6), 50-56); meanwhile, the tunable spectrum can not be realized because the transition mode is fixed (J Phy D,2015,118(21), 213106; Ieee TNucl Sci, 1998).
Rare earth doped halides such as LaX3Ce (J Phy D,2006.99(12), 123520; appl. Phys. Lett.,2001,79(10), 1573-. 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.
The metal halide perovskite has the advantages of high quantum yield, tunable luminescence wavelength, simple preparation, low cost and the like, and is considered to be a scintillator material with application prospect (Nature,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. Copper-based halide Cs3Cu2I5Scintillators (adv.sci.,2020,7(11),2000195) have better stability than the above materials, but have lower light yield, so it is highly desirable to introduce dopant ions to increase the radiant luminous intensity to increase the light yield (Nuclear instrument and Methods in Physics Research, a991(2021)164963, adv.optical mater.2021, 2100460).
In addition, the conventional method for realizing flexible X-ray imaging is to mix the scintillator material into the polymer matrix to form a film, which causes poor compatibility of the scintillator material in the film, resulting in poor resolution of the finished film, complex process, long film manufacturing time and high cost.
Therefore, it is urgently needed to develop a new product for the technologies of low cost, high resolution, flexible X-ray medical imaging, radiation detection and the like by in-situ preparing a nanocrystalline scintillator film with the characteristics of high radiation absorption coefficient, high light yield, high stability, short afterglow and the like in a polymer matrix.
Disclosure of Invention
The invention provides thallium-doped Cs for inhibiting the oxidation and precipitation of iodide ions3Cu2I5A method for preparing a scintillator film.
The technical scheme of the invention is as follows:
thallium-doped Cs for inhibiting iodide ion oxidation and precipitation3Cu2I5The preparation method of the scintillator film comprises the following steps:
(1) mixing copper iodide (CuI), cesium iodide (CsI), thallium iodide (TlI), polymethyl methacrylate (PMMA), Dimethylformamide (DMF), hypophosphorous acid (H)3PO2) Mixing with an additive sorbitan monooleate polyoxyethylene ether (Tween80), stirring and dissolving at 40-100 ℃, cooling to room temperature after the reaction is completed to obtain a clear transparent liquid, and vacuumizing to remove bubbles in the solution to obtain a precursor solution;
(2) uniformly coating the precursor solution on a clean glass substrate;
(3) after coating is finished, annealing the wet film and the glass substrate at 60-80 ℃, and obtaining thallium-doped Cs after the solvent is completely volatilized3Cu2I5(Cs3Cu2I5:Tl+) A scintillator film.
Preferably, in the step (1), the molar amount of thallium iodide is 0.06-0.1% of the molar amount of cesium iodide.
Preferably, in the step (1), the stirring temperature is 60-80 ℃.
Preferably, in step (1), the stirring time is 4 ± 0.5 hours.
Preferably, in step (3), the film thickness is 200 ± 20 microns.
Preferably, in step (3), thallium-doped Cs3Cu2I5In the scintillator, Tl+The atomic ratio of (A) is 0.06% -0.1%.
Compared with the prior art, the invention has the following advantages:
(1) the invention successfully converts Tl+Incorporation of Cs3Cu2I5In crystal lattice and realize Cs3Cu2I5：Tl+In situ synthesis of nanocrystals in a polymer matrix versus undoped Cs3Cu2I5The yield of the radiation light of the scintillator film is greatly improved, and the scintillator film with a larger area can be prepared.
(2) The invention introduces strong reducing acid H in the process of preparing precursor solution3PO2So as to inhibit the oxidation and precipitation of iodide ions in the formation stage of the precursor solution. Secondly, ether bond contained in Tween80 successfully inhibits the oxidative precipitation of iodide ions after film formation, and further improves Cs3Cu2I5Stability of scintillator films.
(3) Cs prepared by the invention3Cu2I5：Tl+The scintillator film has the advantages of high radiation absorption coefficient, large light yield, no afterglow caused by extremely short service life and the like, and 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 is Cs synthesized in example 23Cu2I5:0.1％Tl+The luminescence patterns of the scintillator film sample under the irradiation of 254nm and 365nm ultraviolet light, and the left luminescence pattern under 254nm UV light; the right is the luminescence under 365nm UV light.
FIG. 2 shows Cs prepared in comparative example 2 without Tween803Cu2I5:0.1％Tl+Color change profile of the scintillator film sample before and after 30 days.
FIG. 3 is a schematic representation of large-area films prepared in comparative examples 5, 6 and 7 using 18-crown-6 as an additive.
FIG. 4 is Cs prepared in comparative example 63Cu2I5:0.1％Tl+TEM images of nanocrystalline samples.
FIG. 5 shows the Cs obtained in comparative example 2 without thallium doping3Cu2I5Cs of the thin film and the Cs prepared in examples 1 and 2 under different doping amounts3Cu2I5:Tl+XRD pattern of scintillator film sample.
FIG. 6 shows the Cs obtained in comparative example 1 without thallium doping3Cu2I5Films and Cs prepared in examples 1 and 23Cu2I5: absorption coefficient of Tl scintillator films is plotted against percent attenuation at X-ray energies of 50 keV.
FIG. 7 is Cs of various thicknesses prepared by the preparation method of example 23Cu2I5:0.1％Tl+RL intensity plot of scintillator films.
FIG. 8 shows Cs before and after doping prepared in comparative example 1 and example 23Cu2I5:Tl+Graph comparing the radiant luminescence to the light yield for a scintillator film sample.
FIG. 9 shows Cs prepared in example3Cu2I5:0.1％Tl+TEM images of nanocrystalline samples.
FIG. 10 shows Cs prepared in example3Cu2I5:0.1％Tl+Resolution test pattern under X-ray imaging of scintillator films.
FIG. 11 is a graph showing fluorescence lifetimes of samples of films prepared in comparative example 1, and examples 1 and 2.
Detailed Description
The present invention is further illustrated by the following figures and specific examples, which are to be understood as illustrative only and not as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
Example 1
According to the formula Cs3Cu2I5：0.06％Tl+The stoichiometric ratio of the elements is 11.993mmol CsI, 8mmol CuI, 0.0072mmol TlI, 6g PMMA, 20ml DMF, 100uLH3PO2And 0.5g of Tween80, heating and stirring the mixed solution at 60 ℃ for 4 hours, and cooling the solution to obtain a precursor solution after the reaction is completed and the solution becomes a light yellow clear transparent liquid.
And putting the precursor solution into a vacuum drying oven, and pumping out bubbles of the solution to be used as the precursor solution to be blade-coated. Wiping the glass substrate with alcohol, adjusting a screw micrometer on a scraper, setting the thickness of the film to be 200 micrometers, and placing the scraper on an automatic coating machine after the setting is finished. The precursor solution to be knife coated was removed with a dropper and coating was started at a rate of 15 mm/s. After coating, transferring the wet film and the glass substrate to a heating table, annealing at 70 ℃ to promote solvent evaporation, and obtaining Cs with thallium ion doping amount of 0.06% after the solvent is completely volatilized3Cu2I5：0.06％Tl+A scintillator film.
Example 2
According to the formula Cs3Cu2I5：0.1％Tl+The stoichiometric ratio of the elements is 11.988mmolCsI, 8mmolCuI, 0.012mmolTlI, 6gPMMA, 20mLDMF and 100uLH3PO2And 0.5g of Tween80, heating and stirring the mixed solution at 60 ℃ for 4 hours, and cooling the solution to obtain a precursor solution after the reaction is completed and the solution becomes a light yellow clear transparent liquid.
And putting the precursor solution into a vacuum drying oven, and pumping out bubbles of the solution to be used as the precursor solution to be blade-coated. Wiping the glass substrate with alcohol, adjusting a screw micrometer on a scraper, setting the thickness of the film to be 200 micrometers, and placing the scraper on an automatic coating machine after the setting is finished. The precursor solution to be knife coated was removed with a dropper and coating was started at a rate of 15 mm/s. After coating, transferring the wet film and the glass substrate to a heating table, annealing at 70 ℃ to promote solvent evaporation, and obtaining Cs with 0.1% thallium ion doping amount after the solvent is completely volatilized3Cu2I5：0.1％Tl+A scintillator film. As can be seen from fig. 1 and 7, the flatness of the film at 200 μm is good, and the obtained film has high radiant luminous intensity.
Example 3
This example is essentially the same as example 2, except that the stirring temperature of the mixed solution was 40 ℃.
Example 4
This example is essentially the same as example 2, except that the stirring temperature of the mixed solution was 100 ℃.
Cs prepared in examples 3 and 43Cu2I5：Tl+The performance of the scintillator film is similar to that of the scintillator film in the embodiment 1-2, and the stirring temperature only affects the time for completing the preparation of the precursor solution and does not affect the performance of subsequent products.
Example 5
This example is essentially the same as example 2, except that the annealing temperature is 60 ℃.
Example 6
This example is essentially the same as example 2, except that the annealing temperature is 80 ℃.
Cs prepared in examples 5 and 63Cu2I5：Tl+The performance of the scintillator film is similar to that of the scintillator film in examples 1-2, and the annealing temperature only affects the forming speed of the crystal film and does not affect the final film forming quality.
Comparative example 1
According to the formula Cs3Cu2I5The stoichiometric ratio of each element is 12mmolCsI, 8mmolCuI, 6gPMMA, 20mLDMF and 100uLH3PO2And 0.5g of Tween80, heating and stirring the mixed solution at 60 ℃ for 4 hours, and cooling the solution to obtain a precursor solution after the reaction is completed and the solution becomes colorless clear transparent liquid.
And putting the precursor solution into a vacuum drying oven, and pumping out bubbles of the solution to be used as the precursor solution to be blade-coated. And adjusting a screw micrometer on the scraper, setting the thickness of the film to be 200 micrometers, and placing the scraper on an automatic coating machine after the setting is finished. The precursor solution to be knife coated was removed with a dropper and coating was started at a rate of 15 mm/s. After coating, transferring the wet film and the glass substrate to a heating table, annealing at 70 ℃ to promote solvent evaporation, and obtaining the Cs without thallium doping after the solvent is completely volatilized3Cu2I5A film.
Comparative example 2
The only difference between this comparative example and example 2 is that no Tween80 was added. As can be seen from FIG. 2, if Tween80 is not added, the subsequent film will gradually turn yellow due to the oxidation and precipitation of iodide ions.
Comparative example 3
This comparative example is essentially the same as example 2, except that Tween80 was added in an amount of 0.02 g.
Comparative example 4
This comparative example is essentially the same as example 2, except that Tween80 was added in an amount of 0.1 g.
In combination with example 2, the effect of inhibiting the extraction of iodide ions is not obvious when the amount of Tween80 is too small, and the situation is similar to that of comparative example 2, only difference is that the time for which the film resists the extraction of iodide ions is slightly longer; when the amount of Tween80 is too large, the film-forming property is not greatly affected.
Comparative example 5
According to the formula Cs3Cu2I5：0.06％Tl+The stoichiometric ratio of the elements is 11.993mmol CsI, 8mmol CuI, 0.0072mmol TlI, 6g PMMA, 20ml DMF, 100uLH3PO2And 0.08g of 18-crown-6 mixed solution is heated and stirred for 4 hours at the temperature of 60 ℃, and when the reaction is completed, the solution becomes light yellow clear transparent liquid, and the precursor solution is obtained after cooling.
And putting the precursor solution into a vacuum drying oven, and pumping out bubbles of the solution to be used as the precursor solution to be blade-coated. Wiping the glass substrate with alcohol, adjusting a screw micrometer on a scraper, setting the thickness of the film to be 200 micrometers, and placing the scraper on an automatic coating machine after the setting is finished. The precursor solution to be knife coated was removed with a dropper and coating was started at a rate of 15 mm/s. After coating, transferring the wet film and the glass substrate to a heating table, annealing at 70 ℃ to promote solvent evaporation, and obtaining Cs with thallium ion doping amount of 0.06% after the solvent is completely volatilized3Cu2I5：0.06％Tl+A scintillator film.
Comparative example 6
According to the formula Cs3Cu2I5：0.1％Tl+The stoichiometric ratio of the elements is 11.988mmolCsI, 8mmolCuI, 0.012mmolTlI, 6gPMMA, 20mLDMF and 100uLH3PO2、008g of 18-crown-6 mixed solution is heated and stirred at 60 ℃ for 4 hours until the reaction is completed and the solution becomes light yellow clear transparent liquid, and the solution is cooled to obtain precursor solution.
And putting the precursor solution into a vacuum drying oven, and pumping out bubbles of the solution to be used as the precursor solution to be blade-coated. Wiping the glass substrate with alcohol, adjusting a screw micrometer on a scraper, setting the thickness of the film to be 200 micrometers, and placing the scraper on an automatic coating machine after the setting is finished. The precursor solution to be knife coated was removed with a dropper and coating was started at a rate of 15 mm/s. After coating, transferring the wet film and the glass substrate to a heating table, annealing at 70 ℃ to promote solvent evaporation, and obtaining Cs with 0.1% thallium ion doping amount after the solvent is completely volatilized3Cu2I5：0.1％Tl+A scintillator film.
Comparative example 7
This comparative example is essentially the same as comparative example 6, except that 18-crown-6 was added in an amount of 0.04 g.
Comparative example 8
This comparative example is essentially the same as comparative example 6, except that 18-crown-6 was added in an amount of 0.12 g.
It should be noted that, through experiments, it was found that 18-crown-6, regardless of the amount of added, can generate CsCu2I3Accordingly, the addition amount of 18-crown-6 is high or low to obtain a poor film state as shown in FIG. 2.
FIG. 1 is Cs synthesized in example 23Cu2I5:0.1％Tl+The luminescence patterns of the scintillator film sample under the irradiation of 254nm and 365nm ultraviolet light, and the left luminescence pattern under 254nm UV light; the right is the luminescence under 365nm UV light.
FIG. 2 shows Cs prepared in comparative example 2 without Tween803Cu2I5:0.1％Tl+The color change of the scintillator film sample before and after 30 days, it can be seen that the sample has turned yellow due to the oxidative precipitation of iodide ions.
FIG. 3 is a diagram showing a large-area film obtained by using 18-crown-6 as an additive in comparative examples 5, 6 and 7, and it can be seen that 18-crown-6 is used as an additiveThe prepared film has obvious granular feeling on the surface, and the granules are impure phase CsCu2I3The light emission of (1).
FIG. 4 is Cs prepared in comparative example 63Cu2I5:0.1％Tl+The TEM images of the nanocrystalline samples revealed that the crystal morphology was mostly amorphous.
FIG. 5 shows the Cs obtained in comparative example 2 without thallium doping3Cu2I5Cs of the thin film and the Cs prepared in examples 1 and 2 under different doping amounts3Cu2I5:Tl+X-ray diffraction pattern of scintillator thin film samples. It can be seen that the crystal structure remains unchanged before and after doping, and the diffraction peak does not shift significantly due to the very small doping amount, demonstrating that Cs is synthesized3Cu2I5The pure phase crystal structure of (3).
FIG. 6 shows the Cs obtained in comparative example 1 without thallium doping3Cu2I5Films and Cs prepared in examples 1 and 23Cu2I5: plot of absorption coefficient of Tl scintillator film versus percent attenuation at X-ray energies of 50keV, it can be seen that to completely absorb the X-rays at such energies, the thickness of the crystalline film should be at least greater than 200 um.
FIG. 7 is Cs of various thicknesses prepared by the preparation method of example 23Cu2I5:0.1％Tl+The RL intensity of the scintillator film shows that the actual thickness is preferably 200 μm at this doping level.
FIG. 8 shows Cs before and after doping prepared in comparative example 1 and example 23Cu2I5:Tl+Graph comparing the radiant luminescence to the light yield for a scintillator film sample.
FIG. 9 shows Cs prepared in example3Cu2I5:0.1％Tl+According to a TEM image of a nanocrystalline sample, the crystal size distribution can be seen to be about 20nm, and the crystal size distribution has a definite shape, which indicates that the prepared scintillator film has better resolution to a certain extent.
FIG. 10 shows Cs prepared in example3Cu2I5:0.1％Tl+FlashingAccording to a resolution test chart under X-ray imaging of the thin film, three lines under the spatial resolution of 10lp/mm can be seen clearly, and the resolution capability is high.
FIG. 11 is a graph of the fluorescence lifetimes of the film samples prepared in comparative example 1, examples 1 and 2, as determined by lifetime fitting, that the lifetimes of all three samples are very short, only a few microseconds, and are within the capability of being identified by a commercial detector, so that afterglow is completely negligible.
Claims (6)
1. Thallium-doped Cs for inhibiting iodide ion oxidation and precipitation3Cu2I5The method for preparing the scintillator film is characterized by comprising the following steps:
(1) mixing cuprous iodide, cesium iodide, thallium iodide, polymethyl methacrylate, dimethylformamide, hypophosphorous acid and additive sorbitan monooleate polyoxyethylene ether, stirring and dissolving at 40-100 ℃, cooling to room temperature after the reaction is completed to obtain a clear transparent liquid, and vacuumizing to remove bubbles in the solution to obtain a precursor solution;
(2) uniformly coating the precursor solution on a clean glass substrate;
(3) after coating is finished, annealing the wet film and the glass substrate at 60-80 ℃, and obtaining thallium-doped Cs after the solvent is completely volatilized3Cu2I5A scintillator film.
2. The production method according to claim 1, wherein in the step (1), the molar amount of thallium iodide is from 0.06% to 0.1% of the molar amount of cesium iodide.
3. The method according to claim 1, wherein the stirring temperature in the step (1) is 60 to 80 ℃.
4. The method according to claim 1, wherein the stirring time in the step (1) is 4 ± 0.5 hours.
5. The method according to claim 1, wherein in the step (3), the film has a thickness of 200 ± 20 μm.
6. The method according to claim 1, wherein in the step (3), thallium-doped Cs3Cu2I5In the scintillator, Tl+The atomic ratio of (A) is 0.06% -0.1%.
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| 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 |
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| CN115323323A (en) * | 2021-04-25 | 2022-11-11 | 中国科学院上海硅酸盐研究所 | Thallium-doped low-dimensional perovskite structure microcrystalline scintillation film and preparation method and application thereof |
| CN115323323B (en) * | 2021-04-25 | 2024-04-12 | 中国科学院上海硅酸盐研究所 | Thallium-doped low-dimensional perovskite structure microcrystalline scintillation film and preparation method and application thereof |
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| 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 |
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