CN114276802B - Preparation method of thallium-doped cesium-copper-iodine scintillator film for inhibiting oxidation precipitation of iodide ions - Google Patents
Preparation method of thallium-doped cesium-copper-iodine scintillator film for inhibiting oxidation precipitation of iodide ions Download PDFInfo
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Abstract
The application discloses thallium doped Cs for inhibiting oxidation precipitation of iodide ions 3 Cu 2 I 5 A method for producing a scintillator film. The method comprises the steps of mixing cuprous iodide, cesium iodide, thallium iodide, PMMA, dimethylformamide, hypophosphorous acid and Tween80 for reaction 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 Cs 3 Cu 2 I 5 A scintillator film. The application is realized by introducing the acid H with strong reducibility 3 PO 2 To inhibit the oxidation precipitation of iodide ions in the precursor solution formation stage, and the ether bond contained in Tween80 can inhibit the oxidation precipitation of iodide ions after film formation, thus obtaining Cs 3 Cu 2 I 5 ：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.
Description
Technical Field
The application belongs to the technical field of preparation of inorganic semiconductor scintillator materials, and relates to thallium doped cesium copper iodine (Cs) for inhibiting oxidation precipitation of iodide ions 3 Cu 2 I 5 :Tl + ) A method for producing a scintillator film.
Background
The metal halide has higher radiation luminous efficiency and is a scintillator material which is most widely used. However, currently commercial metal halide scintillators such as CsI: tl and NaI: tl have high light yield but generally have long afterglow, and can not achieve simplification of the synthesis process by a convenient processing method, and still use a crucible growth method at present; in addition, due to the defect problems existing in the large crystals, flexible detection and high-resolution imaging (IeeeSensors Journal,2009,9 (9), 1154-1156,Astroparticle Phys,2019,108 (6), 50-56) are difficult to realize; meanwhile, because the transition mode is fixed, the spectrum tuning can not be realized (J Phy D,2015,118 (21), 213106;Ieee TNucl Sci,1998).
Rare earth doped halides such as LaX 3 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, because rare earth elements are scarce and costly to produce, there is still a need to find scintillator materials free of rare earth ions.
The metal halide perovskite has the advantages of high quantum yield, tunable luminescence wavelength, simple preparation, low cost and the like, and is considered as a scintillator material with application prospect (Nature, 2018,561 (7721), 88-93;ACS Nano,2019,13 (2), 2520-2525). However, the low light yield caused by the severe self-absorption effect severely limits its practical application. Copper-based halide Cs 3 Cu 2 I 5 The scintillator (adv. Sci.,2020,7 (11), 2000195) is more stable than the above materials, but has a lower light yield, so that it is highly desirable to introduce dopant ions to increase its radiant emission intensity to increase its light yield (Nuclear inst. And Methods in Physics Research, a991 (2021) 164963,Adv.Optical Mater.2021,2100460).
In addition, the traditional method for realizing flexible X-ray imaging is to mix the scintillator material into the polymer matrix for film formation, which leads to 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, there is an urgent need to develop an in-situ preparation method for a nanocrystalline scintillator film with high radiation absorption coefficient, high light yield, high stability, short afterglow and other characteristics in a polymer matrix, and a new product is provided for low-cost, high-resolution, flexible X-ray medical imaging, radiation detection and other technologies.
Disclosure of Invention
The application provides thallium doped Cs for inhibiting oxidation precipitation of iodide ions 3 Cu 2 I 5 A method for producing a scintillator film.
The technical scheme of the application is as follows:
thallium doped Cs for inhibiting oxidation precipitation of iodide ions 3 Cu 2 I 5 A method of preparing a scintillator film comprising the steps of:
(1) Cuprous iodide (CuI), cesium iodide (CsI), thallium iodide (TlI), polymethyl methacrylate (PMMA), dimethylformamide (DMF), hypophosphorous acid (H) 3 PO 2 ) Mixing with an additive sorbitan monooleate polyoxyethylene ether (Tween 80), stirring and dissolving at 40-100 ℃, cooling to room temperature after the reaction is completed to clear and transparent liquid, and vacuumizing to remove solution bubbles to obtain a precursor solution;
(2) Uniformly coating the precursor solution on a clean glass substrate;
(3) After the coating is finished, the wet film and the glass substrate are annealed at 60-80 ℃ until the solvent volatilizes completely, thus obtaining thallium doped Cs 3 Cu 2 I 5 (Cs 3 Cu 2 I 5 :Tl + ) A scintillator film.
Preferably, in step (1), the molar amount of thallium iodide is 0.06% to 0.1% of the molar amount of cesium iodide.
Preferably, in step (1), the stirring temperature is 60 to 80 ℃.
Preferably, in step (1), the stirring time is 4.+ -. 0.5 hours.
Preferably, in step (3), the film thickness is 200.+ -.20. Mu.m.
Preferably, in step (3), thallium doped Cs 3 Cu 2 I 5 Tl in scintillator + The atomic ratio of (2) is 0.06% -0.1%.
Compared with the prior art, the application has the following advantages:
(1) The application successfully uses Tl + Incorporation of Cs 3 Cu 2 I 5 Among the crystal lattices, and realize Cs 3 Cu 2 I 5 ：Tl + In situ synthesis of nanocrystals in a polymer matrix, relative to undoped Cs 3 Cu 2 I 5 Scintillator films having a high radiant light yieldThe width is improved, and a scintillator film with a larger area can be prepared.
(2) The method introduces the strong reducing acid H in the preparation process of the precursor solution 3 PO 2 To inhibit the oxidation precipitation of iodide ions in the precursor solution formation stage. Secondly, the ether bond contained in Tween80 successfully inhibits the oxidation precipitation of iodide ions after film formation, and further improves Cs 3 Cu 2 I 5 Stability of scintillator films.
(3) Cs prepared by the application 3 Cu 2 I 5 ：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 a sample of Cs synthesized in example 2 3 Cu 2 I 5 :0.1％Tl + Luminescence patterns of the scintillator film sample under 254nm and 365nm ultraviolet light irradiation, and luminescence patterns under 254nm UV light are left; the right is a luminescence plot under 365nm UV light.
FIG. 2 is a sample of Cs obtained in comparative example 2 without Tween80 3 Cu 2 I 5 :0.1％Tl + Color change plot of samples before and after 30 days of scintillator film samples.
FIG. 3 is a graphic 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 6 3 Cu 2 I 5 :0.1％Tl + TEM image of nanocrystalline samples.
FIG. 5 is a thallium-free doped Cs prepared in comparative example 2 3 Cu 2 I 5 Cs at different doping levels of the films prepared in examples 1 and 2 3 Cu 2 I 5 :Tl + XRD pattern of scintillator film samples.
FIG. 6 is a thallium-free doped Cs prepared in comparative example 1 3 Cu 2 I 5 Films and Cs prepared in examples 1 and 2 3 Cu 2 I 5 : absorption coefficient of Tl scintillator film and X-ray energy at 50keVThe following decay percentage graph.
FIG. 7 is a graph of Cs of varying thickness prepared by the preparation method of example 2 3 Cu 2 I 5 :0.1％Tl + RL intensity plot of scintillator film.
FIG. 8 is Cs before and after doping prepared in comparative example 1 and example 2 3 Cu 2 I 5 :Tl + Radiation luminescence versus light yield for scintillator film samples.
FIG. 9 is a sample of Cs prepared in the examples 3 Cu 2 I 5 :0.1％Tl + TEM image of nanocrystalline samples.
FIG. 10 is a sample of Cs prepared in the examples 3 Cu 2 I 5 :0.1％Tl + Resolution test chart under X-ray imaging of scintillator films.
FIG. 11 is a graph of fluorescence lifetime of film samples prepared in comparative example 1, examples 1 and 2.
Detailed Description
The present application is further illustrated in the accompanying drawings and detailed description which are to be understood as being merely illustrative of the application and not limiting of its scope, and various modifications of the application, which are equivalent to those skilled in the art upon reading the application, will fall within the scope of the application as defined in the appended claims.
Example 1
According to chemical formula Cs 3 Cu 2 I 5 ：0.06％Tl + The stoichiometric ratio of each element is 11.993mmolCsI, 8mmolCuI, 0.0072mmolTlI, 6gPMMA, 20mLDMF, 100uLH 3 PO 2 The mixed solution of 0.5g Tween80 is heated and stirred for 4 hours at 60 ℃, and after the reaction is complete, the solution becomes light yellow clear transparent liquid and is cooled to obtain precursor solution.
And placing the precursor solution into a vacuum drying oven, and pumping out solution bubbles to serve as the precursor solution to be scraped. The glass substrate was wiped with alcohol, the screw micrometer on the doctor blade was adjusted, the film thickness was set to 200 μm, and the doctor blade was placed on an automatic coater after the setting was completed. The precursor solution to be scraped is removed by a dropper at 15mm/sThe speed starts the coating. 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 solvent evaporation is complete 3 Cu 2 I 5 ：0.06％Tl + A scintillator film.
Example 2
According to chemical formula Cs 3 Cu 2 I 5 ：0.1％Tl + The stoichiometric ratio of each element is 11.988mmolCsI, 8mmolCuI, 0.012mmolTlI, 6gPMMA, 20mLDMF, 100uLH 3 PO 2 The mixed solution of 0.5g Tween80 is heated and stirred for 4 hours at 60 ℃, and after the reaction is complete, the solution becomes light yellow clear transparent liquid and is cooled to obtain precursor solution.
And placing the precursor solution into a vacuum drying oven, and pumping out solution bubbles to serve as the precursor solution to be scraped. The glass substrate was wiped with alcohol, the screw micrometer on the doctor blade was adjusted, the film thickness was set to 200 μm, and the doctor blade was placed on an automatic coater after the setting was completed. The precursor solution to be scraped is removed with a dropper and the application is started at a speed of 15 mm/s. After the coating is finished, 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 0.1% after the solvent is completely volatilized 3 Cu 2 I 5 ：0.1％Tl + A scintillator film. As can be seen by combining fig. 1 and fig. 7, the flatness of the film at 200 micrometers is good, and the obtained film has higher radiation luminous intensity.
Example 3
This example is essentially the same as example 2, except that the temperature of agitation of the mixed solution is 40 ℃.
Example 4
This example is essentially the same as example 2, except that the temperature of stirring of the mixed solution is 100 ℃.
Cs prepared in examples 3 and 4 3 Cu 2 I 5 ：Tl + The scintillator film performance is similar to examples 1-2, and the stirring temperature only affects the time for preparing the precursor solution, and does not affect the laterProduct performance.
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 6 3 Cu 2 I 5 ：Tl + The scintillator film performance is similar to examples 1-2, and the annealing temperature only affects the crystal film formation rate and does not affect the final film formation quality.
Comparative example 1
According to chemical formula Cs 3 Cu 2 I 5 The stoichiometric ratio of each element is 12mmolCsI, 8mmolCuI, 6gPMMA, 20mLDMF, 100uLH 3 PO 2 And heating and stirring the mixed solution of 0.5g Tween80 at 60 ℃ for 4 hours, changing the solution into colorless clear transparent liquid after the reaction is complete, and cooling to obtain a precursor solution.
And placing the precursor solution into a vacuum drying oven, and pumping out solution bubbles to serve as the precursor solution to be scraped. And (3) adjusting a spiral 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 scraped is removed with a dropper and the application is started at a speed 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 without thallium doping after solvent evaporation is complete 3 Cu 2 I 5 A film.
Comparative example 2
The only difference between this comparative example and example 2 is that no Tween80 was added. It can be seen in connection with FIG. 2 that without the addition of Tween80, the subsequent film will gradually yellow due to the oxidation precipitation of iodide ions.
Comparative example 3
This comparative example is essentially the same as example 2, except that Tween80 is added in an amount of 0.02g.
Comparative example 4
This comparative example is essentially the same as example 2, except that Tween80 is added in an amount of 0.1g.
In combination with example 2, too small an amount of tween80 had no remarkable effect of inhibiting the precipitation of iodide ions, and the case was similar to comparative example 2, except that the time for which the film was resistant to the precipitation of iodide ions was slightly longer; too much Tween80 has little effect on film forming properties.
Comparative example 5
According to chemical formula Cs 3 Cu 2 I 5 ：0.06％Tl + The stoichiometric ratio of each element is 11.993mmolCsI, 8mmolCuI, 0.0072mmolTlI, 6gPMMA, 20mLDMF, 100uLH 3 PO 2 And heating and stirring the mixed solution of 0.08g of 18-crown-6 at 60 ℃ for 4 hours, changing the solution into light yellow clear transparent liquid after the reaction is complete, and cooling to obtain a precursor solution.
And placing the precursor solution into a vacuum drying oven, and pumping out solution bubbles to serve as the precursor solution to be scraped. The glass substrate was wiped with alcohol, the screw micrometer on the doctor blade was adjusted, the film thickness was set to 200 μm, and the doctor blade was placed on an automatic coater after the setting was completed. The precursor solution to be scraped is removed with a dropper and the application is started at a speed 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 solvent evaporation is complete 3 Cu 2 I 5 ：0.06％Tl + A scintillator film.
Comparative example 6
According to chemical formula Cs 3 Cu 2 I 5 ：0.1％Tl + The stoichiometric ratio of each element is 11.988mmolCsI, 8mmolCuI, 0.012mmolTlI, 6gPMMA, 20mLDMF, 100uLH 3 PO 2 And heating and stirring the mixed solution of 0.08g of 18-crown-6 at 60 ℃ for 4 hours, changing the solution into light yellow clear transparent liquid after the reaction is complete, and cooling to obtain a precursor solution.
And placing the precursor solution into a vacuum drying oven, and pumping out solution bubbles to serve as the precursor solution to be scraped. Wiping the glass substrate with alcohol, and adjusting the doctor bladeThe thickness of the film was set to 200. Mu.m, and after the completion of the setting, a doctor blade was placed on an automatic coater. The precursor solution to be scraped is removed with a dropper and the application is started at a speed of 15 mm/s. After the coating is finished, 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 0.1% after the solvent is completely volatilized 3 Cu 2 I 5 ：0.1％Tl + A scintillator film.
Comparative example 7
This comparative example was substantially the same as comparative example 6, except that 18-crown-6 was added in an amount of 0.04g.
Comparative example 8
This comparative example was substantially the same as comparative example 6, except that 18-crown-6 was added in an amount of 0.12g.
It is noted that, it was found through experiments that 18-crown-6, regardless of the amount added, produced CsCu 2 I 3 The phase, therefore, was either higher or lower than the 18-crown-6 addition, and a poor film state was obtained as shown in FIG. 2.
FIG. 1 is a sample of Cs synthesized in example 2 3 Cu 2 I 5 :0.1％Tl + Luminescence patterns of the scintillator film sample under 254nm and 365nm ultraviolet light irradiation, and luminescence patterns under 254nm UV light are left; the right is a luminescence plot under 365nm UV light.
FIG. 2 is a sample of Cs obtained in comparative example 2 without Tween80 3 Cu 2 I 5 :0.1％Tl + The color change pattern of the samples before and after 30 days of the scintillator film samples, it can be seen that the samples had turned yellow due to oxidation of iodide ions.
FIG. 3 is a graphic representation of large area films prepared in comparative examples 5, 6 and 7 using 18-crown-6 as an additive, it can be seen that the films prepared using 18-crown-6 as an additive have a pronounced grainy surface and that the particles are heterogeneous CsCu 2 I 3 Is provided.
FIG. 4 is Cs prepared in comparative example 6 3 Cu 2 I 5 :0.1％Tl + The TEM images of nanocrystalline samples revealed mostly amorphous crystal morphology.
FIG. 5 is a thallium-free doped Cs prepared in comparative example 2 3 Cu 2 I 5 Cs at different doping levels of the films prepared in examples 1 and 2 3 Cu 2 I 5 :Tl + X-ray diffraction pattern of scintillator film samples. It can be seen that the crystal structure remains unchanged before and after doping, and that the diffraction peaks have no significant shift due to the very small doping amount, proving that Cs is synthesized 3 Cu 2 I 5 Is a pure phase crystal structure of (c).
FIG. 6 is a thallium-free doped Cs prepared in comparative example 1 3 Cu 2 I 5 Films and Cs prepared in examples 1 and 2 3 Cu 2 I 5 : the absorption coefficient of Tl scintillator films versus the percentage decay at 50keV X-ray energy is a graph showing that to fully absorb X-rays at such energies, the thickness of the crystalline film should be at least greater than 200um.
FIG. 7 is a graph of Cs of varying thickness prepared by the preparation method of example 2 3 Cu 2 I 5 :0.1％Tl + As can be seen from the RL intensity map of the scintillator film, the actual thickness is preferably 200um at this doping level.
FIG. 8 is Cs before and after doping prepared in comparative example 1 and example 2 3 Cu 2 I 5 :Tl + Radiation luminescence versus light yield for scintillator film samples.
FIG. 9 is a sample of Cs prepared in the examples 3 Cu 2 I 5 :0.1％Tl + TEM image of nanocrystalline sample can see that crystal size distribution is about 20nm, and has definite shape, which shows that the prepared scintillator film has better resolution.
FIG. 10 is a sample of Cs prepared in the examples 3 Cu 2 I 5 :0.1％Tl + The resolution test chart under X-ray imaging of the scintillator film shows that three line pairs under the spatial resolution of 10lp/mm can be seen clearly, which shows that the resolution capability is high.
FIG. 11 is a graph of fluorescence lifetime for the film samples prepared in comparative example 1, examples 1 and 2, and by lifetime fitting, it was determined that the lifetime of all three samples was very short, only a few microseconds, and was well within the capability of commercial detectors, so that afterglow was completely negligible.
Claims (6)
1. Thallium doped Cs for inhibiting oxidation precipitation of iodide ions 3 Cu 2 I 5 The preparation method of the scintillator film is characterized by comprising the following steps:
(1) Mixing cuprous iodide, cesium iodide, thallium iodide, polymethyl methacrylate, dimethylformamide, hypophosphorous acid and an additive sorbitan monooleate polyoxyethylene ether, stirring and dissolving at 40-100 ℃, cooling to room temperature after the reaction is completed to clear and transparent liquid, and vacuumizing to remove solution bubbles to obtain a precursor solution;
(2) Uniformly coating the precursor solution on a clean glass substrate;
(3) After the coating is finished, the wet film and the glass substrate are annealed at 60-80 ℃ until the solvent volatilizes completely, thus obtaining thallium doped Cs 3 Cu 2 I 5 A scintillator film.
2. The method according to claim 1, wherein the molar amount of thallium iodide in the step (1) is 0.06% to 0.1% of the molar amount of cesium iodide.
3. The process according to claim 1, wherein in the step (1), the stirring temperature is 60 to 80 ℃.
4. The method according to claim 1, wherein in the step (1), the stirring time is 4.+ -. 0.5 hours.
5. The method according to claim 1, wherein in the step (3), the film thickness is 200.+ -.20. Mu.m.
6. The method of claim 1 wherein in step (3) thallium doped Cs 3 Cu 2 I 5 FlashingIn the body, tl + The atomic ratio of (2) is 0.06% -0.1%.
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| 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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