CN116804150A - X-ray scintillator material, and preparation method and application thereof - Google Patents
X-ray scintillator material, and preparation method and application thereof Download PDFInfo
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- CN116804150A CN116804150A CN202310538012.9A CN202310538012A CN116804150A CN 116804150 A CN116804150 A CN 116804150A CN 202310538012 A CN202310538012 A CN 202310538012A CN 116804150 A CN116804150 A CN 116804150A
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- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000003384 imaging method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 229910052714 tellurium Inorganic materials 0.000 claims description 13
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 12
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims 1
- 239000004814 polyurethane Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 description 8
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 5
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000004528 spin coating Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 239000002775 capsule Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 description 3
- 241000287828 Gallus gallus Species 0.000 description 2
- 238000012984 biological imaging Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
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- 239000002243 precursor Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ANDNPYOOQLLLIU-UHFFFAOYSA-N [Y].[Lu] Chemical compound [Y].[Lu] ANDNPYOOQLLLIU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
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- 230000005284 excitation Effects 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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Abstract
The invention provides an X-ray scintillator material, a preparation method and application thereof, wherein the chemical formula of the X-ray scintillator material is Cs 2 SnCl 6 :Te 4+ . The X-ray scintillator material can be made into an X-ray scintillator film and the like for X-ray imaging. Cs of the invention 2 SnCl 6 :Te 4+ Scintillator materialThe scintillator film prepared by the method has the advantages of good optical performance, excellent stability, environmental friendliness and the like, and is nontoxic and simple in preparation method. As a novel scintillator material, the material has great potential in the fields of X-ray imaging and X-ray detection.
Description
Technical Field
The invention relates to the field of scintillator materials and X-ray imaging, in particular to an X-ray scintillator material, a preparation method and application thereof.
Background
An X-ray scintillator is a type of converting absorbed high energy particles to lowPhoton-capable materials. X-ray scintillator materials find wide application in a variety of fields such as biological imaging and nuclear detection. Conventional scintillator materials are made of plastic scintillators or iodides (NaI, csI: TI, srI) 2 :Eu 2+ ) Single crystals and partial oxide single crystals (LuAG, YAG, etc.) are mainly used, but single crystals are expensive to prepare; the absorption cross section of the plastic scintillator is small.
In recent years, lead halide perovskite materials have received a great deal of attention for use in X-ray imaging. However, the defects of poor stability, strong lead toxicity, strong light self-absorption and the like exist, so that the development and the application of the fluorescent dye in the field of X-ray imaging are limited.
In addition, the currently mainstream commercial product Lutetium Yttrium Silicate (LYSO) has the advantages of high light yield, high energy resolution and the like, but has complex preparation process and poor scintillation property controllability. The complex preparation process greatly increases the production cost of large area scintillation screens, and the bulk crystal of LYSO prepared at high temperature is highly fragile and unsuitable for application in flexible X-ray imaging such as in stomatology, complex non-planar objects, and the like.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides an X-ray scintillator material, and a preparation method and application thereof. The X-ray scintillator material has the advantages of good optical performance, no toxicity, stability, simple preparation method, low preparation cost and the like.
In a first aspect, the present invention provides an X-ray scintillator material having the formula Cs 2 SnCl 6 :Te 4+ 。
The invention has found that Cs 2 SnCl 6 The double perovskite material has greatly improved environmental stability and completely avoids Pb toxicity. Te (Te) 4+ Doping Cs 2 SnCl 6 (CST) in an excited state, self-trapping excitons (STEs) may be formed, thereby achieving scintillation properties of the material under X-rays. In addition, the material shows large Stokes shift, can well avoid the light self-absorption of the material, has atomic numbers of Cs, sn and Te of more than 50, has a larger action cross section with X rays, and can become high excited by the X raysAnd (3) an effective luminescent material.
In a second aspect, the present invention also provides a method for preparing the above X-ray scintillator material.
The preparation method provided by the invention comprises the step of carrying out mixed reaction on tellurium oxide solution, cesium carbonate solution and tin tetrachloride solution.
In some embodiments of the invention, the molar ratio of tellurium oxide, tin tetrachloride, cesium carbonate is x (1-x): 1,0< x <1. In a preferred embodiment of the invention, x=0.014.
In some embodiments of the invention, the reaction is carried out at a temperature of 70-90 ℃ for a time of 30-60 minutes.
In some preferred embodiments of the invention, the reaction temperature is 80℃and the reaction time is 30 minutes.
In some embodiments of the invention, the tellurium oxide solution, cesium carbonate solution and tin tetrachloride solution are all hydrochloric acid solutions.
In a specific operation, tellurium oxide, cesium carbonate and tin tetrachloride pentahydrate can be respectively dissolved in concentrated hydrochloric acid to obtain corresponding precursor solutions.
Further, tellurium oxide solution and cesium carbonate solution are added into tin tetrachloride solution in sequence.
Further, after the reaction is finished, washing the material for the target X-ray scintillator material Cs by absolute ethyl alcohol for a plurality of times, and performing solid-liquid separation to obtain solid and dry the solid 2 SnCl 6 :Te 4+ 。
The solid-liquid separation may be carried out by solid-liquid separation means commonly used in the art, such as centrifugation. In some embodiments of the invention, centrifugation is used at a speed of about 7000rpm/min for about 5 minutes. The temperature at which the separated solids dry was selected to be around 70 ℃.
In a third aspect, the present invention provides an X-ray scintillator film comprising a carrier film and an X-ray scintillator material wrapped inside the carrier film.
In some embodiments of the invention, the carrier film is polydimethylsiloxane and the X-ray scintillator material Cs 2 SnCl 6 :Te 4+ The particle size of (2) is in the order of micrometers.
The invention fully utilizes the small-size characteristic of the microcrystal, and can prepare a large-area flexible scintillation screen/film (such as 10 x 10 cm) by combining with the PDMS transparent film 2 ) The film has excellent X-ray imaging performance and can be used in the X-ray imaging fields of medical imaging, security inspection equipment and the like.
In some embodiments of the invention, the X-ray scintillator material Cs 2 SnCl 6 :Te 4+ The mass ratio of the polymer to the polydimethylsiloxane is (0.5-4): 10, preferably 1:10.
In some embodiments of the present invention, the preparation of the X-ray scintillator film includes a step of coating a carrier film material after mixing with the X-ray scintillator material, adjusting the size of the resulting film area according to the size of the coated substrate, and adjusting the resulting film thickness according to the coating thickness.
In some embodiments of the present invention, the preparation of the X-ray scintillator film includes the steps of: cs is processed by 2 SnCl 6 :Te 4+ Mixing the powder, PDMS prepolymer and curing agent, stirring and pumping simultaneously, spin-coating the obtained mixture on a glass liner at a certain rotating speed, curing the glass liner on a heating table at 120 ℃ for 20 minutes after spin-coating, and finally stripping the film from the glass liner to obtain the scintillator film with a certain thickness.
Wherein the mass ratio of the PDMS prepolymer to the curing agent is 9:1. Stirring and pumping for 30-50 min.
In a fourth aspect, the present invention also provides the use of the above-described X-ray scintillator material or X-ray scintillator film in the field of X-ray imaging.
The invention provides an X-ray scintillator material, a preparation method and application thereof, and Cs of the invention 2 SnCl 6 :Te 4 + The scintillator material and the scintillator film prepared by the same have the advantages of good optical performance, excellent stability, environmental friendliness and the like, and are nontoxic and simple in preparation method. As a novel scintillator material, the material has the following properties in the field of X-ray imaging and X-ray detectionGreat potential.
Drawings
FIG. 1 shows Cs obtained in example 1 2 SnCl 6 :Te 4+ Comparing the XRD spectrogram of the powder with a PDF standard card;
FIG. 2 shows Cs obtained in example 1 2 SnCl 6 :Te 4+ Is a graph of the absorption coefficient of (2);
FIG. 3 shows Cs obtained in example 1 2 SnCl 6 :Te 4+ A spectrogram under X-ray irradiation;
FIG. 4 is a pictorial view of a flexible scintillator film of different thickness, illuminated by an ultraviolet lamp;
FIG. 5 is an X-ray imaging application of the flexible scintillator film obtained in example 2;
fig. 6 is an X-ray bioimaging application of the flexible scintillator film obtained in example 2.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless specifically indicated, the technical means used in the embodiments of the present invention are conventional means well known to those skilled in the art.
In the examples below, materials and reagents used were obtained from regular commercial sources unless otherwise specified.
Example 1
The present embodiment provides a Cs 2 SnCl 6 :Te 4+ The preparation method of the microcrystalline scintillator material comprises the following steps:
step 1: 0.986 mmole of tin tetrachloride pentahydrate was dissolved in concentrated hydrochloric acid, 0.014 mmole of tellurium oxide was dissolved in concentrated hydrochloric acid, and 1 mmole of cesium carbonate was dissolved in concentrated hydrochloric acid, respectively.
Step 2: and adding the tellurium oxide solution and the cesium carbonate solution which are fully dissolved into the tin tetrachloride solution in sequence for reaction, wherein the reaction temperature is 80 ℃ and the reaction time is 30 minutes.
Step 3: after the reaction, 5 ml of absolute ethanol was added.
Step 4: the cooled product was transferred to a centrifuge tube and centrifuged at 7000rpm/min for 5 minutes, and the supernatant was removed.
Step 5: 10 ml of absolute ethanol was added to the precipitate, the precipitate was sufficiently dispersed, and the precipitate was centrifuged at 7000rpm/min for 5 minutes, and the supernatant was removed. The process needs to be repeated once again to ensure that the product is cleaned.
Step 6: placing the precipitate obtained in the step 5 in a 70 ℃ oven for 24 hours, and completely drying to obtain Cs 2 SnCl 6 :Te 4+ And (3) powder. The particle size is 3-5 microns.
FIG. 1 shows Cs obtained in this example 2 SnCl 6 :Te 4+ Comparing the XRD spectrogram of the powder with a PDF standard card; as can be seen from the figure, the Cs prepared by coprecipitation 2 SnCl 6 :Te 4+ The product has high purity, no impurity generation and good crystallinity.
FIG. 2 shows Cs obtained in this example 2 SnCl 6 :Te 4+ Is a graph of the absorption coefficient of (2); the high atomic numbers of Cs, sn and Te in the material composition elements are beneficial to lead Cs 2 SnCl 6 :Te 4+ The double perovskite scintillator material has a high absorption coefficient comparable to that of the mainstream LYSO scintillator material.
FIG. 3 shows Cs obtained in this example 2 SnCl 6 :Te 4+ Spectral diagram under X-ray irradiation.
Example 2
The present embodiment provides a Cs 2 SnCl 6 :Te 4+ The preparation method of the @ PDMS scintillator film is as follows:
PDMS prepolymer and curing agent were added to the reactor in a mass ratio of 9:1, and then Cs obtained in example 1 was added 2 SnCl 6 :Te 4+ Powder (1:10 mass ratio of PDMS) was added to the reactor, which was then filled with the powderStirring and air-extracting for 30 minutes, and spin-coating the obtained mixed precursor on a glass liner at a rotating speed of 2000r/min for 15 seconds. After spin coating was completed, the glass liner was transferred to a hot plate at 120 ℃ until the coating was completely cured, and finally the coating was peeled off the glass liner to obtain a scintillator film having a thickness of about 340 μm.
In other embodiments, the film dimensions can be adjusted by controlling the glass liner size and the film thickness can be adjusted by controlling the number of spin-on layers.
Fig. 4 is a physical image of flexible scintillator films with different thicknesses and a light-emitting photograph under irradiation of an ultraviolet lamp, and it can be seen that the physical image of the flexible scintillator film is pale yellow under normal light, and can emit uniform yellow light under irradiation of the ultraviolet lamp. It should be noted that, in order to submit a satisfactory application document, the yellow color image is not seen after the adjustment.
Fig. 5 shows the application of the flexible scintillator film obtained in this embodiment in X-ray imaging (the capsule is placed between the X-ray source and the scintillator film, and the capsule is made of plastic), and it can be seen that the metal spring inside the capsule can be clearly observed under X-rays by using the flexible scintillator film.
Fig. 6 shows the application of the flexible scintillator film obtained in this example in X-ray biological imaging (chicken feet are placed between the X-ray source and the scintillator film), and the flexible scintillator film can be used to clearly observe the bones of the chicken feet (the black part of the middle of the picture is the bones) under the X-ray, which proves that the flexible scintillator film has better application performance in X-ray imaging.
The photographing camera used in this example was a simple camera (Sony. Alpha.7) with a spatial resolution of 6LP/mm. In other words, if a camera with higher resolution is used for photographing, the obtained X-ray imaging map will be clearer.
Comparative example 1
This comparative example provides a Cs 2 SnCl 6 :Bi 3+ The preparation method of the microcrystalline scintillator material comprises the following steps:
step 1: 0.92 mmole of tin tetrachloride pentahydrate was dissolved in concentrated hydrochloric acid, 0.08 mmole of bismuth chloride was dissolved in concentrated hydrochloric acid, and 1 mmole of cesium carbonate was dissolved in concentrated hydrochloric acid, respectively.
Step 2: and adding the fully dissolved bismuth chloride solution and cesium carbonate solution into the tin tetrachloride solution in sequence for reaction, wherein the reaction temperature is 80 ℃ and the reaction time is 30 minutes.
Step 3: after the reaction, 5 ml of absolute ethanol was added.
Step 4: the cooled product was transferred to a centrifuge tube and centrifuged at 7000rpm/min for 5 minutes, and the supernatant was removed.
Step 5: 10 ml of absolute ethanol was added to the precipitate, the precipitate was sufficiently dispersed, and the precipitate was centrifuged at 7000rpm/min for 5 minutes, and the supernatant was removed. The process needs to be repeated once again to ensure that the product is cleaned.
Step 6: placing the precipitate obtained in the step 5 in a 70 ℃ oven for 24 hours, and completely drying to obtain Cs 2 SnCl 6 :8％Bi 3+ And (3) powder.
By X-ray excitation, cs 2 SnCl 6 :8％Bi 3+ The scintillator has blue emission around 455nm, but its scintillation performance is much lower than Cs 2 SnCl 6 :1.4％Te 4+ A scintillator.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. An X-ray scintillator material, characterized in that the chemical formula is Cs 2 SnCl 6 :Te 4+ 。
2. The method for producing an X-ray scintillator material according to claim 1, comprising a step of mixing a tellurium oxide solution, a cesium carbonate solution and a tin tetrachloride solution for reaction.
3. The method for preparing the X-ray scintillator material according to claim 2, wherein the molar ratio of tellurium oxide, tin tetrachloride and cesium carbonate is X (1-X): 1,0< X <1.
4. The method of producing an X-ray scintillator material according to claim 2, wherein the reaction is carried out at a temperature of 70 to 90 ℃ for a time of 30 to 60 minutes.
5. The method for producing an X-ray scintillator material according to any one of claims 2 to 4, wherein the tellurium oxide solution, the cesium carbonate solution and the tin tetrachloride solution are hydrochloric acid solutions.
6. An X-ray scintillator film comprising a carrier film and the X-ray scintillator material of claim 1 encased within the carrier film.
7. The X-ray scintillator film according to claim 6, wherein the carrier film is polydimethylsiloxane and the X-ray scintillator material Cs 2 SnCl 6 :Te 4+ The particle size of (2) is in the order of micrometers.
8. The X-ray scintillator film of claim 7, wherein the X-ray scintillator material Cs 2 SnCl 6 :Te 4+ The mass ratio of the modified polyurethane to the polydimethylsiloxane is (0.5-4): 10.
9. The X-ray scintillator film according to any one of claims 6 to 8, wherein the preparation of the X-ray scintillator film includes a step of coating after mixing a carrier film material with the X-ray scintillator material, the size of the resulting film area being adjusted according to the size of a coated substrate, and the resulting film thickness being adjusted according to the coating thickness.
10. Use of the X-ray scintillator material of claim 1 or the X-ray scintillator film of any of claims 6-9 in the field of X-ray imaging.
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| CN202310538012.9A CN116804150A (en) | 2023-05-12 | 2023-05-12 | X-ray scintillator material, and preparation method and application thereof |
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| CN202310538012.9A CN116804150A (en) | 2023-05-12 | 2023-05-12 | X-ray scintillator material, and preparation method and application thereof |
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| CN202310538012.9A Pending CN116804150A (en) | 2023-05-12 | 2023-05-12 | X-ray scintillator material, and preparation method and application thereof |
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- 2023-05-12 CN CN202310538012.9A patent/CN116804150A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| FEI ZHANG ET AL.: "Thermally Activated Delayed Fluorescence Zirconium-Based Perovskites for Large-Area and Ultraflexible X-ray Scintillator Screens", 《ADV. MATER.》, vol. 34, 23 September 2022 (2022-09-23), pages 1 - 12 * |
| XIAOFEI QING ET AL.: "Efficient Near-Infrared Luminescence Based on Double Perovskite Cs2SnCl6", 《MOLECULES》, vol. 28, 20 April 2023 (2023-04-20), pages 1 - 9 * |
| ZHIFANG TAN ET AL.: "Tailoring the electron and hole dimensionality to achieve efficient and stable metal halide perovskite scintillators", 《NANOPHOTONICS》, vol. 10, no. 8, 17 February 2021 (2021-02-17), pages 2249 - 2256 * |
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