CN113970779A - Microstructure scintillation screen formed by perovskite filled microporous panel and preparation method - Google Patents
Microstructure scintillation screen formed by perovskite filled microporous panel and preparation method Download PDFInfo
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- CN113970779A CN113970779A CN202111185786.5A CN202111185786A CN113970779A CN 113970779 A CN113970779 A CN 113970779A CN 202111185786 A CN202111185786 A CN 202111185786A CN 113970779 A CN113970779 A CN 113970779A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000011049 filling Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000031700 light absorption Effects 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims description 53
- 150000001875 compounds Chemical class 0.000 claims description 43
- 239000011521 glass Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 20
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 16
- -1 cesium ions Chemical class 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 11
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 10
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 claims description 10
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- ZSUXOVNWDZTCFN-UHFFFAOYSA-L tin(ii) bromide Chemical compound Br[Sn]Br ZSUXOVNWDZTCFN-UHFFFAOYSA-L 0.000 claims description 10
- QWANGZFTSGZRPZ-UHFFFAOYSA-N aminomethylideneazanium;bromide Chemical compound Br.NC=N QWANGZFTSGZRPZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 7
- GIDDQKKGAYONOU-UHFFFAOYSA-N octylazanium;bromide Chemical compound Br.CCCCCCCCN GIDDQKKGAYONOU-UHFFFAOYSA-N 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 5
- 229940117803 phenethylamine Drugs 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- VJHDVMPJLLGYBL-UHFFFAOYSA-N tetrabromogermane Chemical compound Br[Ge](Br)(Br)Br VJHDVMPJLLGYBL-UHFFFAOYSA-N 0.000 claims description 5
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 4
- VVZBFOKBSDGVGZ-UHFFFAOYSA-N BENZALKONIUM Chemical compound CCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 VVZBFOKBSDGVGZ-UHFFFAOYSA-N 0.000 claims description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-O Methylammonium ion Chemical compound [NH3+]C BAVYZALUXZFZLV-UHFFFAOYSA-O 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- ISWNAMNOYHCTSB-UHFFFAOYSA-N methanamine;hydrobromide Chemical compound [Br-].[NH3+]C ISWNAMNOYHCTSB-UHFFFAOYSA-N 0.000 claims description 2
- QLCPTARABILRDA-UHFFFAOYSA-N n-bromo-2-methylpropan-2-amine Chemical compound CC(C)(C)NBr QLCPTARABILRDA-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- BHHGXPLMPWCGHP-UHFFFAOYSA-O 2-phenylethanaminium Chemical compound [NH3+]CCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-O 0.000 claims 1
- 150000001768 cations Chemical class 0.000 claims 1
- 238000003384 imaging method Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 230000008859 change Effects 0.000 abstract description 5
- 238000002493 microarray Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000012229 microporous material Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 9
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000005043 ethylene-methyl acrylate Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- CQKAPARXKPTKBK-UHFFFAOYSA-N tert-butylazanium;bromide Chemical compound Br.CC(C)(C)N CQKAPARXKPTKBK-UHFFFAOYSA-N 0.000 description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- ZYCMDWDFIQDPLP-UHFFFAOYSA-N hbr bromine Chemical compound Br.Br ZYCMDWDFIQDPLP-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- IRAGENYJMTVCCV-UHFFFAOYSA-N 2-phenylethanamine;hydrobromide Chemical compound [Br-].[NH3+]CCC1=CC=CC=C1 IRAGENYJMTVCCV-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 1
- 229940075613 gadolinium oxide Drugs 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 150000003956 methylamines Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
- G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
- G01T1/2023—Selection of materials
Abstract
The invention relates to a microstructure scintillation screen for filling a scintillator of perovskite material into a microporous panel and a preparation method thereof. The invention can prepare the microstructure scintillation screen with the advantages of regular microarray structure, higher scintillation light-emitting performance, good beam performance, higher X-ray imaging resolution ratio and the like. The microstructure perovskite scintillation screen prepared by the method can obviously improve the luminous uniformity of X-ray converted visible light; meanwhile, the micropore structure panel with the reflecting layer and the light absorption layer has a light restriction effect, so that the crosstalk of light among micropores can be reduced, and the spatial resolution of X-ray imaging is improved. In addition, the size of the microstructure perovskite scintillation screen prepared by the invention can be changed along with the change of the size of the micropore panel, and a large-size scintillation screen can be conveniently manufactured; moreover, the special microporous material adopted in the invention ensures that the prepared perovskite scintillation screen has good environmental adaptability.
Description
Technical Field
The invention belongs to the field of nuclear radiation detection, and relates to a microstructure scintillation screen formed by a perovskite-filled microporous panel and a preparation method thereof.
Background
Since the discovery of X-rays by william conradjen, X-ray detectors have been widely usedIn the medical and industrial fields. X-ray detection is classified into a semiconductor detector for direct detection and a scintillator detector for indirect detection. The scintillator detector plays an important role in the field of X-ray imaging, and common scintillator materials include thallium-doped cesium iodide (CsI: Tl) and terbium-doped gadolinium oxide sulfide (Gd)2O2Tb, GOS), bismuth orthogermanate doped with cerium (BGO), etc. The scintillator material plays an important role in the X-ray imaging field by depending on the characteristics of high light yield, high response speed, short decay time, good stability and the like. However, the conventional scintillator material is fragile, easy to wet, and harsh in manufacturing process, and cannot meet wide requirements.
In recent years, perovskite nuclear radiation detection materials have become a hot research point in the field of X-ray imaging. The advantages of perovskite scintillator materials over traditional scintillator materials are apparent. The perovskite material has extremely high application prospect in the field of X-ray imaging due to the advantages of adjustable optical band gap, high luminescent quantum yield, low synthesis cost and the like. However, at present, no good solution is available for preparing the perovskite scintillator screen with the high-position-resolution microstructure, and further the industrial application of the perovskite scintillator screen in the field of high-spatial-resolution X-ray imaging is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an X-ray high-position-resolution microstructure scintillation screen formed by filling a perovskite scintillator into a microporous structure panel and a preparation method thereof, so as to develop a microstructure scintillation screen with a regular microarray structure, higher scintillation light-emitting performance and good light-emitting performance and a preparation method thereof, and achieve the purposes of improving the uniformity of X-ray conversion visible light emission and improving the X-ray imaging spatial resolution.
In order to achieve the purpose, the invention provides a microstructure scintillation screen formed by a perovskite-filled microporous panel, which comprises a microporous panel and a scintillator made of perovskite material; wherein:
the micropore panel has a regular micropore array structure, the inner part of the micropore wall comprises a light absorption layer, and the inner wall of the micropore plays a role of a reflecting layer;
each micropore is uniformly filled with a scintillator of the perovskite material.
Further, the scintillators of the perovskite materials include, but are not limited to, perovskites of the following classes: three-dimensional perovskite ABX3Two-dimensional perovskite A2B'B"X6One-dimensional perovskite A3BX5And zero-dimensional perovskite A4BX6(ii) a Wherein A is selected from cesium ions Cs+Formamidine cation FA+Methylammonium cation MA+N-octylammonium cation OA+Phenethylammonium cation PEA+Benzalkonium cation PMA+One or more of tert-butylammonium cation; b is selected from Pb2+、Sn2+B' is selected from Ag+、Na+、Cu+One or more of the above; b' is selected from Bi3+、Sb3+、In3+One or more of the above; x is selected from I-、Br-、Cl-One or more of them.
The invention also provides a preparation method of the microstructure scintillation screen formed by the perovskite filled microporous panel, which comprises the following steps:
(1) preparing a perovskite material: dissolving an E compound and an F compound which can be matched to form a perovskite material in a G solvent, and continuously stirring and heating the obtained perovskite precursor solution to obtain a clear supersaturated perovskite precursor solution; the mass ratio of the E compound to the F compound is more than or equal to 1;
(2) filling the microporous panel: completely immersing the prepared dust-free microporous panel into the supersaturated perovskite precursor solution which is continuously stirred and heated by adopting a clamp, so that each micropore in the microporous panel is fully filled with the perovskite precursor solution;
(3) drying and surface treatment: controlling the speed of perovskite crystal precipitation growth by controlling the temperature gradient of the oil bath pan until each micropore in the micropore panel is filled; and taking out the microporous panel, drying, and wiping off redundant crystals on two sides to obtain the microstructure scintillation screen formed by filling the perovskite into the microporous panel.
Further, the E compounds include, but are not limited to, one or more of the following: cesium bromide, methylamine bromide, n-octylamine hydrobromide, formamidine hydrobromide, phenethyl amine bromide, benzyl amine bromide, tert-butylamino hydrobromide;
such F compounds include, but are not limited to, one or more of the following: lead bromide powder, lead chloride powder, lead iodide powder, stannous bromide and germanium bromide;
the G solvent includes, but is not limited to, one or more of the following compounds: dimethyl sulfoxide, N-dimethylformamide and gamma-butyrolactone.
Further, in the step (1), the condition of continuous stirring and heating is that the perovskite precursor solution is placed in an oil bath pan at the temperature of 80-125 ℃ under the stirring action of a magnetic stirrer with the rotating speed of 1500-2000 rpm, and the continuous stirring and heating time is 3-24 hours.
Further, in the step (2), a magnetic stirrer is adopted to continuously stir the supersaturated perovskite precursor solution, the rotating speed is 120-160 rpm, the time is 1h, and the magnetic rotor is ensured not to be in contact with the microporous panel.
Further, in the step (2), the clamp is a glass clamp, and the glass clamp should not react with the precursor solution and ensure that the microporous panel does not directly contact the bottom and the side wall of the beaker containing the perovskite precursor solution.
Further, the temperature reduction gradient of the oil bath kettle is 10-15 ℃/h; the drying condition of the microporous panel is drying for 1h in a vacuum drying oven at 120 ℃.
Further, the mass ratio of the E compound to the F compound is 1-2: 1.
Further, the method comprises the steps of:
filling the perovskite to fill the microstructure scintillation screen formed by the microporous panel and drying: placing the microstructure scintillation screen formed by the perovskite filling microporous panel obtained in the step (3) on the surface of a sand core funnel, and dripping the clarified supersaturated perovskite precursor solution on the microstructure scintillation screen formed by the perovskite filling microporous panel at the speed of 2 drops/s by using a glass dropper under the condition of continuously vacuumizing the other end of the sand core funnel until the surface is fully paved with white precipitates; then putting the microstructure scintillation screen filled with the perovskite material again into a vacuum drying oven at 120 ℃ for drying for 1 h; and then wiping off redundant crystals on two sides by using acetone.
The invention has the beneficial effects that the microstructure scintillation screen formed by the perovskite filled microporous panel and the preparation method thereof can be used for preparing the microstructure scintillation screen with the advantages of regular microarray structure, higher scintillation light-emitting performance, good beam property, higher X-ray imaging resolution ratio and the like. The microstructure perovskite scintillation screen prepared by the method provided by the invention can obviously improve the luminous uniformity of X-ray converted visible light; meanwhile, the micropore structure panel with the reflecting layer and the light absorption layer has a light restriction effect, so that the crosstalk of light among micropores can be reduced, and the spatial resolution of X-ray imaging is improved. In addition, the size of the microstructure perovskite scintillation screen prepared by the invention can be changed along with the change of the size of the micropore panel, and a large-size scintillation screen can be conveniently manufactured; moreover, the special microporous material adopted in the invention ensures that the prepared microstructure perovskite scintillation screen has good environmental adaptability.
Drawings
FIG. 1 is a schematic view of the structure of a dust-free cellular panel used in example 1 of the present invention.
Fig. 2 is an SEM image of a microstructure scintillator screen formed by a perovskite scintillator filled microporous panel in example 1 of the present invention.
FIG. 3 is a schematic diagram of the light beam effect of a microstructure scintillation screen formed by a perovskite-filled microporous panel prepared according to an embodiment of the present invention.
FIG. 4 is a graph of the resolution and pixel value analysis of a 10lp/mm micro-structured scintillation screen formed by a perovskite-filled micro-porous panel prepared in example 3 of the present invention.
FIG. 5 is a flow chart of a method for preparing a microstructure scintillation screen formed by a perovskite-filled microporous panel provided by the invention.
Detailed Description
In order to make the technical problems solved, the technical solutions adopted, and the technical effects achieved by the present invention clearer, the technical solutions of the embodiments of the present invention will be further described in detail with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
As shown in fig. 1 to 3, the present embodiment provides a microstructure scintillation screen formed by a perovskite-filled microporous panel and a preparation method thereof, where the microstructure scintillation screen includes a microporous panel and a scintillator made of perovskite material; the adopted micropore panel is a dust-free micropore panel with a regular micropore array structure, as shown in figure 1, the pore size of the micropore 2 is 2-10 mu m, and Al contained in the inner wall of the micropore 22O3The equal components can play a role in reflection; the light absorbing layer in the pore walls 1 between adjacent micropores 2 has a function of absorbing light. In the micropore panel, a reflecting layer formed on the inner wall of each micropore 2 and a light absorption layer in the pore wall 1 between the micropores have a constraint effect on light, so that the crosstalk of the light between the micropores 2 can be reduced, and the spatial resolution of X-ray imaging can be improved.
Scintillators of the perovskite materials include, but are not limited to, perovskites of the following classes: three-dimensional perovskite ABX3Two-dimensional perovskite A2B'B"X6One-dimensional perovskite A3BX5And zero-dimensional perovskite A4BX6(ii) a Wherein A is selected from cesium ions Cs+Formamidine cation FA+(i.e. the
) Methylammonium cation MA+(i.e. the
) N-octylammonium cation OA+(i.e. the
) Phenethylammonium cation PEA+(i.e. the
) Benzalkonium cation PMA+(i.e. the
) Tert-butylammonium cation (i.e.
) One or more of the following; b is selected from Pb2+、Sn2+And B' is selected from Ag+、Na+、Cu+One or more of the following; b' is selected from Bi3+、Sb3+、In3+One or more of the following; x is selected from I-、Br-、Cl-One or more of them. In the present embodiment, the scintillator of the perovskite material uniformly filled in the micropores is perovskite (OA)2PbBr4The uniformity of the luminescence of the X-ray converted into the visible light can be obviously improved. The light beam effect of the micro-structured scintillation screen formed by the perovskite-filled micro-porous panel is schematically shown in fig. 3.
As shown in FIG. 5, composed of (OA)2PbBr4The preparation method of the microstructure scintillation screen formed by filling the microporous panel with the scintillator of the perovskite material comprises the following steps:
(1) preparing a dust-free microporous panel: preparing a clean dust-free microporous panel with a regular microporous array structure, wherein the dust-free microporous panel is prepared by compounding, melting and pressing core glass, skin glass matched with the core glass and light absorption layer glass (the main component is ethylene-methyl acrylate glass, namely EMA glass) for multiple times to form a panel, and then performing acid etching to remove the core and cleaning and decontaminating treatment;
(2) preparing a perovskite material: dissolving an E compound and an F compound which can be matched to form a perovskite material in a G solvent to obtain a precursor solution, wherein the mass ratio of the E compound to the F compound is more than or equal to 1; stirring conditions of a magnetic stirrer with the rotating speed of 1500-2000 rpmAnd then, placing the precursor solution in an oil bath kettle at the temperature of 80-125 ℃ and continuously stirring until a clear supersaturated perovskite precursor solution is obtained. Wherein, the E compound includes but is not limited to one or more of the following compounds: bromide of methylamine (CH)3NH3Br), n-octylamine hydrobromide (C)8H20BrN), formamidine hydrobromide (CH)5BrN2) Phenethyl amine bromide (C)8H12BrN), benzyl amine bromide (C)8H12BrN), tert-butylamine hydrobromide (C)4H12BrN), etc.; such F compounds include, but are not limited to, one or more of the following: lead bromide powder (PbBr)2) Lead chloride powder (PbCl)2) Lead iodide powder (PbI)2) Stannous bromide (SnBr)2) Germanium bromide (GeBr)2) Etc.; the G solvent includes, but is not limited to, one or more of the following compounds: dimethyl sulfoxide, N-dimethylformamide, gamma-butyrolactone, etc.
In this example, a beaker containing 10mL of 47% by mass hydrobromic acid (HBr) was placed in an ice-water coexisting environment, and 2mL of n-octylamine (n-C) having a purity of 99% was added under continuous stirring8H17NH2OA) dropwise added to hydrobromic acid (HBr) and after reacting sufficiently for about 2 hours, transparent n-octylamine hydrobromide (C) was obtained8H17NH3Br, OABr) precursor solution. Dissolving 10mmol of lead oxide (PbO) in a beaker containing 10mL of hydrobromic acid (HBr), heating in an oil bath at 80 ℃ and continuously stirring for reaction to obtain transparent PbBr2And (3) precursor solution. Mixing the two precursor solutions in a beaker under the stirring condition of a magnetic stirrer with the rotation speed of 1500rpm, placing the mixture in an oil bath kettle with the temperature of 115 ℃, and continuously heating and stirring for 6 hours to obtain clear and transparent supersaturation (OA)2PbBr4The molar concentration of the perovskite precursor solution is 0.16 mol/L.
(3) Filling the microporous panel: and (3) completely immersing the dust-free microporous panel into the supersaturated perovskite precursor solution prepared in the step (2) by using a glass clamp, wherein the glass clamp does not react with the precursor solution, and the microporous panel is ensured not to be in direct contact with the bottom and the side wall of the beaker containing the perovskite precursor solution. Continuously stirring the perovskite precursor solution by using a magnetic stirrer at the rotating speed of 120rpm for 1h to fully fill each micropore 2 in the micropore panel with the perovskite precursor solution; at the same time, it is ensured that the magnetic rotor cannot come into contact with the microporous panel.
(4) Drying and surface treatment: gradually reducing the temperature of the oil bath pot, and controlling the temperature reduction gradient to be 10 ℃/h; the change of the perovskite solubility in the perovskite precursor solution is controlled by controlling the temperature gradient of the oil bath pan, and further the speed of the perovskite crystal gradually separating out and growing in the transverse direction and the longitudinal direction in the micropores 2 is controlled until each micropore 2 in the micropore panel is filled. Taking out the microporous panel, putting into a vacuum drying oven, and drying at 120 deg.C for 1 h; then wiping off the excess crystals on both sides with acetone to Obtain (OA)2PbBr4The scintillator of perovskite material fills the microstructure scintillation screen formed by the microporous panel.
The scanning electron microscope images of the microstructure scintillation screen formed by the perovskite scintillator filling microporous panel prepared by the embodiment magnified 2000 times and 500 times are shown in fig. 2, and it can be seen from fig. 2 that the perovskite scintillator material is uniformly filled in the microporous panel with a regular array structure.
Example 2
As shown in fig. 1 to 3, the present embodiment provides a microstructure scintillation screen formed by a perovskite-filled microporous panel and a preparation method thereof, where the microstructure scintillation screen includes a microporous panel and a scintillator made of perovskite material. The adopted micropore panel is a dust-free micropore panel with a regular micropore array structure, as shown in figure 1, the pore size of the micropore 2 is 2-10 mu m, and Al contained in the inner wall of the micropore 22O3The equal components can play a role in reflection; the light absorbing layer in the pore walls 1 between adjacent micropores 2 has a function of absorbing light. In the micropore panel, a reflecting layer formed on the inner wall of each micropore 2 and a light absorption layer in the pore wall 1 between the micropores have a constraint effect on light, so that the crosstalk of the light between the micropores 2 can be reduced, and the spatial resolution of X-ray imaging can be improved.
The scintillator of perovskite material comprisesThe perovskite species were as in example 1. In this embodiment, the scintillator in which the perovskite material is uniformly filled in the micropores 2 is perovskite Cs4PbBr6The uniformity of the luminescence of the X-ray converted into the visible light can be obviously improved. The light beam effect of the micro-structured scintillation screen formed by the perovskite-filled micro-porous panel is schematically shown in fig. 3.
As shown in FIG. 5, from Cs4PbBr6The preparation method of the microstructure scintillation screen formed by filling the microporous panel with the scintillator of the perovskite material comprises the following steps:
(1) preparing a dust-free microporous panel: preparing a clean dust-free microporous panel with a regular microporous array structure, wherein the dust-free microporous panel is prepared by compounding, melting and pressing core glass, skin glass matched with the core glass and light absorption layer glass (the main component is ethylene-methyl acrylate glass, namely EMA glass) for multiple times to form a panel, and then performing acid etching to remove the core and cleaning and decontaminating treatment;
(2) preparing a perovskite material: dissolving an E compound and an F compound in a G solvent to obtain a precursor solution, wherein the mass ratio of the E compound to the F compound is more than or equal to 1; and under the stirring condition of a magnetic stirrer with the rotating speed of 1500-2000 rpm, placing the precursor solution in an oil bath kettle at the temperature of 80-125 ℃ for continuous stirring until a clear supersaturated perovskite precursor solution is obtained. Wherein, the E compound includes but is not limited to one or more of the following compounds: bromometamine (CH)3NH3Br), n-octylamine hydrobromide (C)8H20BrN), formamidine hydrobromide (CH)5BrN2) Phenethyl amine bromide (C)8H12BrN), benzyl amine bromide (C)8H12BrN), tert-butylamine hydrobromide (C)4H12BrN), etc.; compounds F include, but are not limited to, one or more of the following: lead bromide powder (PbBr)2) Lead chloride powder (PbCl)2) Lead iodide powder (PbI)2) Stannous bromide (SnBr)2) Germanium bromide (GeBr)2) Etc.; g solvents include, but are not limited to, one or more of the following compounds: dimethyl sulfoxide, N-dimethylformamide, gamma-butyrolactone, etc.
In this example, cesium bromide (CsBr) and lead bromide (PbBr) were added in amounts greater than 2:12) Dissolving in a beaker containing N, N-Dimethylformamide (DMF), and stirring in 90 deg.C oil bath for 60min to obtain transparent solution and Cs4PbBr6And (4) precipitating. Mixing Cs4PbBr6The precipitate was washed in ethyl acetate, and the washed Cs was then4PbBr6Dissolving the powder in a mixed organic solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF); then, Cs dissolved in the mixed organic solution was stirred continuously by a magnetic stirrer at 2000rpm4PbBr6Placing in an oil bath kettle at 90 deg.C, and continuously stirring for 3 hr to obtain clear and transparent supersaturated Cs4PbBr6A perovskite precursor solution.
(3) Filling the microporous panel: and (3) completely immersing the dust-free microporous panel into the perovskite precursor solution prepared in the step (2) by using a glass clamp, wherein the glass clamp does not react with the precursor solution, and the microporous panel is ensured not to be in direct contact with the bottom and the side wall of the beaker containing the perovskite precursor solution. Continuously stirring the perovskite precursor solution by using a magnetic stirrer at the rotating speed of 160rpm for 1h to fully fill each micropore 2 in the micropore panel with the perovskite precursor solution; at the same time, it is ensured that the magnetic rotor cannot come into contact with the microporous panel.
(4) Drying and surface treatment: gradually reducing the temperature of the oil bath pot, and controlling the temperature reduction gradient to be 15 ℃/h; the change of the perovskite solubility in the perovskite precursor solution is controlled by controlling the temperature gradient of the oil bath pan, and further the speed of the perovskite crystal gradually separating out and growing in the transverse direction and the longitudinal direction in the micropores 2 is controlled until each micropore 2 in the micropore panel is filled. Taking out the microporous panel, putting into a vacuum drying oven, and drying at 120 deg.C for 1 h; then wiping off the redundant crystals on the two sides with acetone to obtain Cs4PbBr6The scintillator of perovskite material fills the microstructure scintillation screen formed by the microporous panel.
Example 3
As shown in FIGS. 1-3, the present example provides a perovskite-filled microporous panelThe microstructure scintillation screen comprises a micropore panel and a scintillator made of perovskite materials. The adopted micropore panel is a dust-free micropore panel with a regular micropore array structure, as shown in figure 1, the pore size of the micropore 2 is 2-10 mu m, and Al contained in the inner wall of the micropore 22O3The equal components can play a role in reflection; the light absorbing layer in the pore walls 1 between adjacent micropores 2 has a function of absorbing light. In the micropore panel, a reflecting layer formed on the inner wall of each micropore 2 and a light absorption layer in the pore wall 1 between the micropores have a constraint effect on light, so that the crosstalk of the light between the micropores 2 can be reduced, and the spatial resolution of X-ray imaging can be improved.
The scintillator of the perovskite material comprises perovskite species as in example 1. In the present embodiment, the scintillator in which the perovskite material is uniformly filled in the micropores 2 is Perovskite (PEA)2PbBr4The uniformity of the luminescence of the X-ray converted into the visible light can be obviously improved. The light beam effect of the micro-structured scintillation screen formed by the perovskite-filled micro-porous panel is schematically shown in fig. 3.
As shown in FIG. 5, composed of (PEA)2PbBr4The preparation method of the microstructure scintillation screen formed by filling the microporous panel with the scintillator of the perovskite material comprises the following steps:
(1) preparing a dust-free microporous panel: preparing a clean dust-free microporous panel with a regular microporous array structure, wherein the dust-free microporous panel is prepared by compounding, melting and pressing core glass, skin glass matched with the core glass and light absorption layer glass (the main component is ethylene-methyl acrylate glass, namely EMA glass) for multiple times to form a panel, and then performing acid etching to remove the core and cleaning and decontaminating treatment;
(2) preparing a perovskite material: dissolving an E compound and an F compound in a G solvent to obtain a precursor solution, wherein the mass ratio of the E compound to the F compound is more than or equal to 1; and under the stirring condition of a magnetic stirrer with the rotating speed of 1500-2000 rpm, placing the precursor solution in an oil bath kettle at the temperature of 80-125 ℃ for continuous stirring until a clear supersaturated perovskite precursor solution is obtained. Wherein, the E compound includes but is not limited to one or more of the following compounds: bromomethylated methylAmine (CH)3NH3Br), n-octylamine hydrobromide (C)8H20BrN), formamidine hydrobromide (CH)5BrN2) Phenethyl amine bromide (C)8H12BrN), benzyl amine bromide (C)8H12BrN), tert-butylamine hydrobromide (C)4H12BrN), etc.; compounds F include, but are not limited to, one or more of the following: lead bromide powder (PbBr)2) Lead chloride powder (PbCl)2) Lead iodide powder (PbI)2) Stannous bromide (SnBr)2) Germanium bromide (GeBr)2) Etc.; g solvents include, but are not limited to, one or more of the following compounds: dimethyl sulfoxide, N-dimethylformamide, gamma-butyrolactone, etc.
In this example, equal amounts of phenethyl ammonium bromide PEABr and lead bromide PbBr were added2Dissolving in a mixed organic solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF) in N2Continuously stirring and heating to 100 ℃ under the atmosphere, and reacting for 2h to obtain the (PEA) with the concentration of 1.00mol/L2PbBr4A perovskite solution; then placing the prepared perovskite solution in an oil bath pan with the temperature of 115 ℃ for continuous stirring for 24 hours under the condition of continuous stirring of a magnetic stirrer with the rotating speed of 1500rpm to obtain clear and transparent supersaturation (PEA)2PbBr4A perovskite precursor solution.
(3) Filling the microporous panel: and (3) completely immersing the dust-free microporous panel into the perovskite precursor solution prepared in the step (2) by using a glass clamp, wherein the glass clamp does not react with the precursor solution, and the microporous panel is ensured not to be in direct contact with the bottom and the side wall of the beaker containing the perovskite precursor solution. Continuously stirring the perovskite precursor solution by using a magnetic stirrer at the rotating speed of 150rpm for 1h to fully fill each micropore 2 in the micropore panel with the perovskite precursor solution; at the same time, it is ensured that the magnetic rotor cannot come into contact with the microporous panel.
(4) Drying and surface treatment: gradually reducing the temperature of the oil bath pot, and controlling the temperature reduction gradient to be 15 ℃/h; the change of the perovskite solubility in the perovskite precursor solution is controlled by controlling the temperature gradient of the oil bath panWhile controlling the rate at which perovskite crystals gradually precipitate and grow in both the transverse and longitudinal directions in the micropores 2 until each micropore 2 in the microporous panel is filled. Taking out the microporous panel, putting into a vacuum drying oven, and drying at 120 deg.C for 1 h; then wiping off the excess crystals on both sides with acetone to obtain (PEA)2PbBr4The scintillator of perovskite material fills the microstructure scintillation screen formed by the microporous panel.
(5) Filling a microstructure scintillation screen: the (PEA) in the step (4)2PbBr4A microstructure scintillation screen formed by filling a microporous panel with a scintillator of perovskite material is placed on the surface of the sand core funnel, the other end of the sand core funnel is continuously vacuumized, and the supersaturated Phase (PEA) at 120 ℃ is treated by a glass dropper2PbBr4The perovskite precursor solution is dripped on the (PEA) at the speed of 2 drops/s2PbBr4Filling the scintillator of the perovskite material on a microstructure scintillation screen formed by the microporous panel, and continuing until the surface is fully paved with white precipitates.
(6) Drying again and performing surface treatment: refilling supersaturation (PEA) in step (5)2PbBr4Placing the microstructure scintillation screen obtained after the perovskite precursor solution into a vacuum drying oven at 120 ℃ for drying for 1 h; then wiping off the excess crystals on both sides with acetone to obtain (PEA)2PbBr4And filling the scintillator made of the perovskite material into the microstructure scintillation screen formed by the microporous panel again.
Prepared by this example (PEA)2PbBr4The resolution and pixel value analysis graph of a microstructure scintillation screen formed by a perovskite material scintillator-filled microporous panel for 10lp/mm is shown in fig. 4.
The above-described embodiments are merely illustrative of the present invention, and those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A microstructure scintillation screen formed by a perovskite-filled microporous panel is characterized by comprising a microporous panel and a scintillator made of perovskite material; wherein:
the micropore panel has a regular micropore array structure, the wall of each micropore hole comprises a light absorption layer, and the inner wall of each micropore is a light reflection layer;
each micropore is uniformly filled with a scintillator of the perovskite material.
2. A perovskite-filled microporous panel forming a microstructured scintillation screen according to claim 1, wherein said perovskite material scintillators include, but are not limited to, perovskites of the following species: three-dimensional perovskite ABX3Two-dimensional perovskite A2B'B"X6One-dimensional perovskite A3BX5And zero-dimensional perovskite A4BX6(ii) a Wherein A is selected from cesium ions Cs+Formamidine cation FA+Methylammonium cation MA+N-octylammonium cation OA+Phenethylammonium cation PEA+Benzalkonium cation PMA+One or more of tert-butylammonium cation; b is selected from Pb2+、Sn2+B' is selected from Ag+、Na+、Cu+One or more of the above; b' is selected from Bi3+、Sb3+、In3+One or more of the above; x is selected from I-、Br-、Cl-One or more of them.
3. A method of making a microstructured scintillation screen formed from a perovskite-filled microporous panel according to claim 1 or 2, comprising the steps of:
(1) preparing a perovskite material: dissolving an E compound and an F compound which can be matched to form a perovskite material in a G solvent, and continuously stirring and heating the obtained perovskite precursor solution to obtain a clear supersaturated perovskite precursor solution; the mass ratio of the E compound to the F compound is more than or equal to 1;
(2) filling the microporous panel: completely immersing the prepared dust-free microporous panel into the supersaturated perovskite precursor solution which is continuously stirred and heated by adopting a clamp, so that each micropore in the microporous panel is fully filled with the perovskite precursor solution;
(3) drying and surface treatment: controlling the speed of perovskite crystal precipitation growth by controlling the temperature gradient of the oil bath pan until each micropore in the micropore panel is filled; and taking out the microporous panel, drying, and wiping off redundant crystals on two sides to obtain the microstructure scintillation screen formed by filling the perovskite into the microporous panel.
4. The method of claim 3, wherein the E compound includes but is not limited to one or more of the following compounds: cesium bromide, methylamine bromide, n-octylamine hydrobromide, formamidine hydrobromide, phenethyl amine bromide, benzyl amine bromide, tert-butylamino hydrobromide;
such F compounds include, but are not limited to, one or more of the following: lead bromide powder, lead chloride powder, lead iodide powder, stannous bromide and germanium bromide;
the G solvent includes, but is not limited to, one or more of the following compounds: dimethyl sulfoxide, N-dimethylformamide and gamma-butyrolactone.
5. The method for preparing a microstructure scintillation screen formed by a perovskite-filled microporous panel according to claim 4, wherein in the step (1), the perovskite precursor solution is placed in an oil bath kettle at 80-125 ℃ under the stirring action of a magnetic stirrer with the rotation speed of 1500-2000 rpm, and the continuous stirring and heating time is 3-24 hours.
6. The method for preparing a microstructure scintillation screen formed by a perovskite-filled microporous panel according to claim 5, wherein in the step (2), a magnetic stirrer is used for continuously stirring the supersaturated perovskite precursor solution, the rotating speed is 120-160 rpm, and the time is 1h, and the magnetic rotor is ensured not to contact with the microporous panel.
7. The method according to claim 5, wherein in step (2), the fixture is a glass fixture, and the glass fixture is not reactive with the precursor solution and ensures that the microporous panel does not directly contact the bottom and the side walls of the beaker containing the perovskite precursor solution.
8. The preparation method of the microstructure scintillation screen formed by the perovskite-filled microporous panel according to claim 5, wherein the temperature reduction gradient of the oil bath pan is 10-15 ℃/h; the drying condition of the microporous panel is drying for 1h in a vacuum drying oven at 120 ℃.
9. The method for preparing a microstructure scintillation screen formed by a perovskite-filled microporous panel according to claim 5, wherein the mass ratio of the E compound to the F compound is 1-2: 1.
10. The method for preparing a microstructure scintillation screen formed by a perovskite-filled microporous panel according to claim 5, wherein the method comprises the following steps:
filling the perovskite to fill the microstructure scintillation screen formed by the microporous panel and drying: placing the microstructure scintillation screen formed by the perovskite filling microporous panel obtained in the step (3) on the surface of a sand core funnel, and dripping the clarified supersaturated perovskite precursor solution on the microstructure scintillation screen formed by the perovskite filling microporous panel at the speed of 2 drops/s by using a glass dropper under the condition of continuously vacuumizing the other end of the sand core funnel until the surface is fully paved with white precipitates; then putting the microstructure scintillation screen filled with the perovskite material again into a vacuum drying oven at 120 ℃ for drying for 1 h; and then wiping off redundant crystals on two sides by using acetone.
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