CN116948629A - Perovskite scintillator material and preparation method of indirect X-ray detector thereof - Google Patents
Perovskite scintillator material and preparation method of indirect X-ray detector thereof Download PDFInfo
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- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
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Classifications
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
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- 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
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Abstract
The present disclosure provides a method of preparing a perovskite scintillator material, the method comprising: s11, spin-coating a bottom perovskite nanocrystalline layer, and depositing a bottom polymer film layer; s12, sequentially spin-coating a perovskite nanocrystalline layer and a polymer film layer on the upper surface of the bottom polymer film layer, wherein the perovskite nanocrystalline layer and the polymer film layer form a composite structure layer; wherein the composite structure layer is at least two layers; the uppermost layer of the composite structure layer comprises a top perovskite nanocrystalline layer; wherein, from bottom perovskite nanocrystalline layer to top perovskite nanocrystalline layer from bottom up, the band gap of perovskite nanocrystalline layer reduces by layer. Another aspect of the present disclosure provides a method of making an indirect X-ray detector using a perovskite scintillator material. The present disclosure solves the self-absorption problem by introducing a multilayer film of varying perovskite nanocrystalline band gap gradients, increasing perovskite scintillator material stability with polymer films, and fitting perovskite scintillator sections with high responsivity photodetectors.
Description
Technical Field
The disclosure provides a perovskite scintillator material and a preparation method of an indirect X-ray detector thereof, belongs to the field of sensors, and particularly relates to the field of ray detectors.
Background
X-rays are widely applied to the fields of industry, security inspection, medicine, scientific research and the like, and the X-rays have strong penetrating capacity and can realize nondestructive detection of internal information of substances. The absorption capacity of different substances to X-rays is different, so that the intensity distribution information of the X-rays after penetrating through the object can reflect the distribution of the substances inside the object. Ionizing radiation of X-rays damages genetic material and increases the risk to the person being irradiated, so high-sensitivity and low-dose detection is the main direction of research on X-ray detection. At present, the X-ray imaging mode mainly comprises two modes of direct detection imaging and indirect detection imaging, wherein the indirect detection imaging mainly relies on a scintillator to carry out imaging, and is the most mainstream scheme. The common scintillator materials mainly comprise cesium iodide doped thallium, sodium iodide doped thallium, lutetium yttrium silicate doped cerium and the like, and the traditional scintillator materials have higher luminous efficiency and shorter decay time, but the radiation luminescence of the traditional scintillator materials is difficult to adjust in the visible spectrum. Moreover, these scintillator materials generally need to be synthesized by crystallization at high temperature, and have the defects of complex preparation process and long preparation time. The development of high performance and low cost X-ray detection materials is a major direction of development of X-ray detectors.
In recent years, halide perovskite has been considered as a very competitive class of X-ray detection materials due to its strong X-ray absorbing capability, as well as low cost solution preparation methods. The inorganic lead halide perovskite nanocrystalline material has the advantages of simple preparation, high response speed, good spatial resolution and the like, and is an excellent scintillator material. However, perovskite materials have a very serious self-absorption phenomenon and low stability, which greatly limit their application in the X-ray field. In addition, compared with the conventional commercial scintillator, the light conversion efficiency is lower, namely the same X-ray irradiation generates fewer visible light photons, and in order to effectively detect fewer photons, a high-sensitivity photoelectric detector sensitive to fewer photons needs to be developed.
Disclosure of Invention
First, the technical problem to be solved
In view of the above, the present disclosure provides a perovskite scintillator material and a method for preparing an indirect X-ray detector thereof, so as to solve the technical problems of self-absorption of the scintillator material, improvement of stability of the scintillator material, improvement of sensitivity of the X-ray detector, and the like.
(II) technical scheme
To achieve the above object, the present disclosure provides, in one aspect, a perovskite scintillator material preparation method including: s11, spin-coating a bottom perovskite nanocrystalline layer, and depositing a bottom polymer film layer; s12, sequentially spin-coating a perovskite nanocrystalline layer and a polymer film layer on the upper surface of the bottom polymer film layer, wherein the perovskite nanocrystalline layer and the polymer film layer form a composite structure layer; wherein the composite structure layer is at least two layers; the uppermost layer of the composite structure layer comprises a top perovskite nanocrystalline layer; wherein, from bottom perovskite nanocrystalline layer to top perovskite nanocrystalline layer from bottom up, the band gap of perovskite nanocrystalline layer reduces by layer.
According to an embodiment of the present disclosure, the spin-on perovskite nanocrystalline layer further includes: the perovskite nanocrystalline is mixed with PMMA solution and then spin-coated.
According to embodiments of the present disclosure, the polymer film includes at least parylene.
According to embodiments of the present disclosure, the band gap of the perovskite nanocrystalline layer is adjusted by adjusting the quantum dot size, the halogen element species and the content.
According to embodiments of the present disclosure, the perovskite scintillator material preparation environment is an anhydrous oxygen-free environment.
The second aspect of the present disclosure provides a perovskite scintillator material obtained by the above-described method for producing a perovskite scintillator material, for use in an indirect X-ray detector with a photodetector.
A third aspect of the present disclosure provides a method of manufacturing an indirect X-ray detector using the perovskite scintillator material described above, comprising: s21, forming an electrode embedded in the substrate on the surface of the substrate with the silicon oxide layer; s22, transferring graphene to the surface of the silicon oxide layer, and patterning the graphene; s23, spin-coating semiconductor quantum dots, and depositing a polymer film; s24, preparing a perovskite scintillator part, wherein the perovskite scintillator part is prepared according to the preparation method of the perovskite scintillator material; s25, depositing an aluminum film to cover the perovskite scintillator part, and patterning the aluminum film; s26, etching the perovskite scintillator part and the aluminum film; s27, depositing an aluminum film to cover the side wall of the scintillator part, and obtaining the indirect X-ray detector.
According to an embodiment of the present disclosure, the upper surface of the electrode in S21 is on the same plane as the upper surface of the silicon oxide layer; the electrode is connected with the signal processing circuit.
According to an embodiment of the present disclosure, the scintillator portion etched out is square, and the side length of the square is 10 to 100 μm.
A fourth aspect of the present disclosure provides an indirect-type X-ray detector obtained by the above method for preparing an indirect-type X-ray detector using a perovskite scintillator material, for use in a single X-ray detector or an array of X-ray detectors, to achieve X-ray imaging.
(III) beneficial effects
The stability of the perovskite scintillator material is increased by depositing the polymer film on the upper surface of each layer of perovskite nanocrystalline; by introducing the inorganic perovskite nanocrystalline multilayer film structure with the gradient change of the band gap, the self-absorption problem of the perovskite scintillator material is solved; the problem of low X-ray detection sensitivity is solved by using the high-responsivity graphene photoelectric detector as the light detector of the indirect X-ray detector.
Drawings
For a clearer description of the technical solutions in the embodiments of the present disclosure, the drawings that are needed in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present disclosure, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art;
FIG. 1 schematically illustrates a flow chart of a method of preparing a perovskite scintillator material provided by embodiments of the present disclosure;
FIG. 2 schematically illustrates a flow chart of a perovskite scintillator material preparation indirect-type X-ray detector provided by an embodiment of the present disclosure;
FIG. 3 schematically illustrates a block diagram of an indirect-type X-ray detector provided by an embodiment of the present disclosure;
[ reference numerals description ]
1-perovskite nanocrystalline layers with gradually decreasing band gaps from bottom layer to top layer; 2-polymer film; 3-a substrate; 4-electrode; a 5-silicon oxide layer; 6-graphene; 7-semiconductor quantum dots; 8-aluminum film.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
First, technical terms described herein are explained and illustrated as follows.
Band gap: the forbidden bandwidth refers to a band width, also called bandgap, in electron volts (eV). To become free electrons, the electrons bound in the valence band must acquire enough energy to transition to the conduction band, and the energy required for an electron to reach the bottom of the conduction band from the top of the valence band (Ev) is the band gap.
Parylene: parylene, is a common designation for a unique series of polymers. The polymer of paraxylene can be divided into N type, C type, D type, F type, HT type and other types according to different molecular structures.
A first aspect of embodiments of the present disclosure provides a method for preparing a perovskite scintillator material, please refer to fig. 1, including steps S11 to S12.
In step S11, an underlying perovskite nanocrystalline layer is spin-coated and an underlying polymer film layer is deposited.
In step S12, a perovskite nanocrystalline layer and a polymer film layer are sequentially spin-coated on the upper surface of the bottom polymer film layer, and a composite structural layer is formed by the perovskite nanocrystalline layer and the polymer film layer; wherein the composite structure layer is at least two layers; the uppermost layer of the composite structure layer comprises a top perovskite nanocrystalline layer; wherein, from bottom perovskite nanocrystalline layer to top perovskite nanocrystalline layer from bottom up, the band gap of perovskite nanocrystalline layer reduces by layer.
In this example, the thickness of the 1 composite structural layer is 10 to 33 μm.
According to the embodiment of the disclosure, the band gap of the perovskite nanocrystalline layer is reduced from the bottom perovskite nanocrystalline layer to the top perovskite nanocrystalline layer by layer, and as the electrons of the perovskite nanocrystalline with the wide band gap are more required to reach the bottom band from the valence band and are not easy to excite, the perovskite nanocrystalline on the lower layer cannot absorb the light generated by the upper layer, so that the self-absorption problem of the perovskite scintillator material is solved; at the same time, the stability of the perovskite scintillator material is increased by the polymer film.
On the basis of the above embodiment, the perovskite nanocrystalline layer further includes: the perovskite nanocrystalline is mixed with PMMA solution and then spin-coated.
In this example, the ratio of PMMA solution to perovskite nanocrystals mass is 1:1 to 100:1.
in another embodiment, a perovskite nanocrystalline layer includes: and directly spin-coating perovskite nanocrystalline.
Through the embodiment of the disclosure, the PMMA solution has good transparency and optical characteristics, and the perovskite nanocrystalline film is coated, so that the stability of the perovskite nanocrystalline film is improved while the optical property of the perovskite nanocrystalline is not influenced.
Based on the above embodiments, the polymer film includes at least parylene.
In this example, the polymer film is a Parylene film layer, and the thickness of the Parylene film is 10-50 nm.
According to the embodiment of the disclosure, the polymer film is prepared by a unique vacuum vapor deposition process, and a completely conforma polymer film coating is grown on the surface of the perovskite nanocrystalline by using active small molecules, so that the 10-50 nm film coating prepared by room temperature deposition has the advantages of uniform thickness, compactness, no pinholes, transparency, no stress, no auxiliary agent, no damage to a workpiece, excellent electrical insulation and protection, is an effective moisture-proof, mildew-proof, corrosion-proof and salt mist-proof coating material, and is beneficial to improving the stability of the perovskite scintillator material.
Based on the above embodiments, the band gap of the perovskite nanocrystals is adjusted by adjusting the quantum dot size, the kind and the content of the halogen element.
In this example, csPbCl 3 The band gap is widest, csPbI 3 The band gap is narrowest, the size range of the perovskite nanocrystalline quantum dot is 2-10 nm, the total number of layers of the bottom layer, the middle layer and the top layer is 3-10 layers, and the band gap is reduced from the bottom layer to the middle layer to the top layer at equal intervals.
According to the embodiment of the disclosure, the band gap of the perovskite nanocrystalline is reduced layer by adjusting the size of the quantum dot, the type and the content of the halogen element, so that the light generated by the upper layer is not absorbed by the lower layer.
Based on the above embodiments, the perovskite scintillator material preparation environment is an anhydrous and anaerobic environment.
In this example, the perovskite scintillator material was prepared in a glove box.
By the embodiment of the disclosure, water and oxygen are isolated, the preparation environment of the perovskite scintillator material is ensured, and the quality of the water and oxygen perovskite scintillator material is prevented.
The second aspect of the disclosed embodiments provides a perovskite scintillator material obtained by the above-mentioned perovskite scintillator material preparation method, which is used for forming an indirect type X-ray detector with a photoelectric detector.
By the embodiment of the disclosure, the self-absorption problem of the perovskite scintillator material is solved, the stability of the perovskite scintillator material is improved, and the application of the perovskite scintillator material in the X-ray field is optimized.
Referring to fig. 2, a third aspect of the disclosed embodiments provides a method for manufacturing an indirect X-ray detector using the perovskite scintillator material described above, comprising: s21, forming an electrode embedded in the substrate on the surface of the substrate with the silicon oxide layer; s22, transferring graphene to the surface of the silicon oxide layer, and patterning the graphene; s23, spin-coating semiconductor quantum dots, and depositing a polymer film; s24, preparing a perovskite scintillator part, wherein the perovskite scintillator part is prepared according to the preparation method of the perovskite scintillator material; s25, depositing an aluminum film to cover the perovskite scintillator part, and patterning the aluminum film; s26, etching the perovskite scintillator part and the aluminum film; s27, depositing an aluminum film to cover the side wall of the scintillator part, and obtaining the indirect X-ray detector.
In this embodiment, the substrate is optionally a CMOS chip; the thickness of the aluminum film is 100-1000 nm.
With the embodiments of the present disclosure, since the perovskite scintillator material has lower light conversion efficiency than the conventional scintillator, fewer visible light photons are generated, and in order to solve the above-mentioned problems, the graphene photodetector is creatively applied to the indirect X-ray detector, and fewer photons are effectively detected.
On the basis of the above embodiment, the upper surface of the electrode in S21 is on the same plane as the upper surface of the silicon oxide layer; the electrode is connected with the signal processing circuit.
According to the embodiment of the disclosure, the generated optical signals are processed by the signal processing circuit connected with the electrodes, and the optical signals are output in the form of digital signals, so that the processing and the reading of X-ray data are completed.
On the basis of the above embodiment, the scintillator portion etched out is square, and the side length of the square is 10 to 100 μm.
The square structure and the two-dimensional coordinates have high fitting degree, can be directly used as a minimum unit to process optical signals, and are convenient to form an X-ray detector device array to finish X-ray detection.
A fourth aspect of the disclosed embodiments provides an indirect-type X-ray detector obtained by the above method for manufacturing an indirect-type X-ray detector using a perovskite scintillator material, which is used for a single X-ray detector or an X-ray detector array to implement X-ray imaging.
Referring to fig. 3, the indirect X-ray detector sequentially includes, from bottom to top: the semiconductor device comprises a substrate 3, a silicon oxide layer 5 on the upper surface of the substrate, electrodes 5 embedded in the silicon oxide layer, graphene 6, semiconductor quantum dots 7, a polymer film 2, a perovskite nanocrystalline layer 1 with gradually decreasing band gaps from bottom layer to top layer, a polymer film 2 and an aluminum film 8 on the upper surface of each perovskite nanocrystalline layer.
According to the embodiment of the disclosure, the perovskite nanocrystalline material which is simple to prepare, high in response speed and good in spatial resolution is applied to the scintillator part, and the graphene photoelectric detector with high responsivity is correspondingly applied to the detector part, so that the preparation difficulty of the X-ray detector is reduced, and the response speed and the spatial resolution of the X-ray detector are improved.
It should be noted that the indirect X-ray detector provided by the embodiments of the present disclosure further has at least one of the following effects and advantages:
(1) The self-absorption problem is solved, an inorganic perovskite nanocrystalline multilayer film structure with the band gap gradient change is introduced, the band gap of the film is gradually reduced from the bottom layer to the top layer, and the light generated by the upper layer is ensured not to be absorbed by the perovskite nanocrystalline of the lower layer.
(2) The problem of stability is solved, PMMA and Parylene are used for coating the perovskite nanocrystalline, the PMMA and Parylene can not influence the optical property of the perovskite nanocrystalline, meanwhile, the perovskite scintillator material has excellent protection performance, and the stability of the perovskite scintillator material is improved.
(3) The problem of low X-ray detection sensitivity is solved, and because compared with a traditional commercial scintillator, the perovskite scintillator has lower light conversion efficiency, namely the same X-ray irradiation, fewer visible light photons are generated, and a graphene photoelectric detector with high responsivity is used as a light detector for effectively detecting fewer photons.
While the foregoing embodiments have been described in some detail for purposes of clarity of understanding, it will be understood that the foregoing embodiments are merely illustrative of the invention and are not intended to limit the invention, and that any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the present disclosure are intended to be included within the scope of the present disclosure.
Claims (10)
1. A method of preparing a perovskite scintillator material, comprising:
s11, spin-coating a bottom perovskite nanocrystalline layer, and depositing a bottom polymer film layer;
s12, sequentially spin-coating a perovskite nanocrystalline layer and a polymer film layer on the upper surface of the bottom polymer film layer, wherein the perovskite nanocrystalline layer and the polymer film layer form a composite structure layer; wherein the composite structure layer is at least two layers; the uppermost layer of the composite structure layer comprises a top perovskite nanocrystalline layer;
wherein, from bottom to top from the bottom perovskite nanocrystalline layer to the top perovskite nanocrystalline layer, the band gap of perovskite nanocrystalline layer decreases layer by layer.
2. The method of producing a perovskite scintillator material according to claim 1, wherein the spin-on perovskite nanocrystalline layer further comprises: and mixing the perovskite nanocrystalline with a PMMA solution and spin-coating.
3. The method of producing a perovskite scintillator material according to claim 1, wherein the polymer film includes at least parylene.
4. The method for producing a perovskite scintillator material according to claim 1, wherein the band gap of the perovskite nanocrystalline layer is adjusted by adjusting the quantum dot size, the kind and the content of the halogen element.
5. The method of producing a perovskite scintillator material according to claim 1, wherein the perovskite scintillator material production environment is an anhydrous oxygen-free environment.
6. A perovskite scintillator material obtained by the method for producing a perovskite scintillator material according to any one of claims 1 to 5, for use in an indirect X-ray detector with a photodetector.
7. A method of making an indirect X-ray detector using a perovskite scintillator material, comprising:
s21, forming an electrode embedded in the substrate on the surface of the substrate with the silicon oxide layer;
s22, transferring graphene to the surface of a silicon oxide layer, and patterning the graphene;
s23, spin-coating semiconductor quantum dots, and depositing a polymer film;
s24, preparing a perovskite scintillator portion, wherein the perovskite scintillator portion is prepared according to the perovskite scintillator material preparation method of any one of claims 1 to 5;
s25, depositing an aluminum film to cover the perovskite scintillator part, and patterning the aluminum film;
s26, etching the perovskite scintillator part and the aluminum film;
and S27, coating the side wall of the scintillator part by a deposited aluminum film to obtain the indirect X-ray detector.
8. The method for manufacturing an indirect X-ray detector using perovskite scintillator material according to claim 7, wherein the upper surface of the electrode in S21 is on the same plane as the upper surface of the silicon oxide layer; the electrode is connected with a signal processing circuit.
9. The method of manufacturing an indirect X-ray detector using perovskite scintillator material according to claim 7, wherein the etched-out scintillator portion is square, and the side length of the square is 10-100 μm.
10. An indirect-type X-ray detector obtained by the method for manufacturing an indirect-type X-ray detector using a perovskite scintillator material according to any one of claims 7 to 9, for use in a single X-ray detector or an array of X-ray detectors, for effecting X-ray imaging.
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| CN117651465A (en) * | 2024-01-29 | 2024-03-05 | 西安电子科技大学 | Multi-step tabletting perovskite heterogeneous crystallization circle X-ray detector and preparation method thereof |
| WO2024085893A3 (en) * | 2021-10-11 | 2024-05-30 | University Of Kansas | High energy radiation detectors |
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| WO2024085893A3 (en) * | 2021-10-11 | 2024-05-30 | University Of Kansas | High energy radiation detectors |
| CN117651465A (en) * | 2024-01-29 | 2024-03-05 | 西安电子科技大学 | Multi-step tabletting perovskite heterogeneous crystallization circle X-ray detector and preparation method thereof |
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