CN117913112A - Integrated scintillator detector prepared from metal halides - Google Patents
Integrated scintillator detector prepared from metal halides Download PDFInfo
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- CN117913112A CN117913112A CN202311583283.2A CN202311583283A CN117913112A CN 117913112 A CN117913112 A CN 117913112A CN 202311583283 A CN202311583283 A CN 202311583283A CN 117913112 A CN117913112 A CN 117913112A
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- film
- ray detector
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- metal halide
- scintillator
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- 229910001507 metal halide Inorganic materials 0.000 title claims abstract description 14
- 150000005309 metal halides Chemical class 0.000 title claims abstract description 14
- 238000003384 imaging method Methods 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000011268 mixed slurry Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 24
- 229920000642 polymer Polymers 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 5
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 229940045803 cuprous chloride Drugs 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- -1 Polydimethylsiloxane Polymers 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
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Abstract
The invention belongs to an integrated scintillator detector, and particularly discloses an integrated metal halide perovskite X-ray detector, which is characterized in that Cs 5Cu3Cl6I2 mixed slurry is directly coated on a CMOS substrate to obtain an imaging device with a Cs 5Cu3Cl6I2 film and the CMOS substrate being completely coupled, and in the integrated Cs 5Cu3Cl6I2 X-ray detector, an optical signal emitted by a Cs 5Cu3Cl6I2 scintillator can be better collected by a detector array, and the process of converting the optical signal into an electric signal can be better completed, so that the definition of an imaging image of the integrated device is obviously higher than that of an un-integrated device, the influence of optical crosstalk is reduced, and the imaging quality is improved.
Description
Technical Field
The invention belongs to an integrated scintillator detector, and particularly relates to an integrated metal halide perovskite X-ray detector.
Background
X-ray imaging techniques are widely used in a variety of fields including medicine, industry and security inspection to enable detailed visualization of internal structures that are not visible to the naked eye. Scintillation x-ray flat panel detectors are one application that uses scintillator materials to convert x-rays into visible light, which is then combined with photodetectors to achieve x-ray detection. The most widespread scintillator detectors such as the CsI: tl scintillator detector, the GOS: tb scintillator detector, and the NaI scintillator detector have found commercial use in medical and industrial imaging devices. However, these scintillator detectors also have the problems of complex manufacturing process, deliquescence, toxicity, poor irradiation resistance and the like, and require further optimization. In the studies on non-commercialized scintillators, there is little integration of the scintillator directly on the imaging device, which makes optical crosstalk serious, and imaging performance is limited. Therefore, there is an urgent need to develop scintillator detectors that are low in optical crosstalk, inexpensive, stable, and nontoxic.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an integrated metal halide perovskite X-ray detector, which reduces the influence of optical crosstalk and improves imaging quality.
The aim of the invention is realized by the following technical scheme: an integrated metal halide perovskite X-ray detector directly coats Cs 5Cu3Cl6I2 mixed slurry on a CMOS substrate in one step to obtain an imaging device with a Cs 5Cu3Cl6I2 film fully coupled with the CMOS substrate.
As one example, the thickness of the Cs 5Cu3Cl6I2 film is 200-600 μm.
As an embodiment, the preparation method of the Cs 5Cu3Cl6I2 film includes the following steps:
S1, respectively weighing cuprous chloride, cesium chloride and cesium iodide in a glass sample bottle, adding a solvent into the bottle, heating and stirring, and reacting to obtain Cs 5Cu3Cl6I2 white powder;
S2, air-drying the obtained Cs 5Cu3Cl6I2 white powder at room temperature;
S3, sieving the dried Cs 5Cu3Cl6I2 white powder to obtain fine and uniform powder for later use;
s4, weighing Cs 5Cu3Cl6I2 powder and polymer slurry, grinding in an agate mortar to obtain mixed slurry of Cs 5Cu3Cl6I2 and polymer, and placing in vacuum to remove internal bubbles;
s5, coating mixed slurry obtained by Cs 5Cu3Cl6I2 and the polymer on the CMOS substrate.
As one of the possible embodiments, the solvent is acetonitrile and the polymer is an epoxy resin, such as Polydimethylsiloxane (PDMS).
As one of the possible embodiments, the reaction temperature in the step S1 is 20-50 ℃, the stirring speed is 500-1000r/min, and the reaction time is 12-36 h.
As one example, the film forming temperature in step S5 is 100℃and the average grain size of the film is 3. Mu.m.
The beneficial effects of the invention are as follows: the Cs 5Cu3Cl6I2 scintillator film is directly prepared on the CMOS detector, the scintillator is better coupled with the detector array to obtain the integrated Cs 5Cu3Cl6I2 scintillator detector, the optical signals emitted by the scintillator can be better collected by the detector array, the process of converting the optical signals into electric signals is better completed, the definition of an imaging image of an integrated device is obviously higher than that of an unintegrated device, the influence of optical crosstalk is reduced, the imaging quality is improved, and the technology is favorable for the application of an x-ray imaging technology in a plurality of fields such as medicine, industry, safety inspection and the like.
Drawings
FIG. 1 is a graph of fluorescence quantum yield vs;
FIG. 2 is a graph of photoluminescence intensity vs;
FIG. 3 is a resolution diagram of a detector;
FIG. 4 is a diagram of an example of 200 μmCs 5Cu3Cl6I2 scintillator detector imaging;
FIG. 5 is a graph of scintillator luminescence intensity versus temperature;
FIG. 6 is a graph of imaging contrast for different scintillators having a thickness of 400 μm;
FIG. 7 is a graph of 10 line-to-card imaging effects for scintillators of different thicknesses;
FIG. 8 is a graph of 30 line pair card imaging effects for scintillators of different thicknesses;
Description of the drawings: m1: a sample prepared by a solution method; m2: samples prepared by milling.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.
In one embodiment of the present application, an integrated metal halide perovskite X-ray detector that coats Cs 5Cu3Cl6I2 mixed slurry on a CMOS substrate to provide an imaging device with a Cs 5Cu3Cl6I2 film fully coupled to the CMOS substrate. The thickness of the Cs 5Cu3Cl6I2 film is 200 μm. The preparation method of the Cs 5Cu3Cl6I2 film comprises the following steps:
S1, respectively weighing cuprous chloride, cesium chloride and cesium iodide in a glass sample bottle, adding a solvent into the bottle, heating to 20-50 ℃, stirring, and reacting to obtain Cs 5Cu3Cl6I2 white powder;
S2, air-drying the obtained Cs 5Cu3Cl6I2 white powder at room temperature;
S3, sieving the dried Cs 5Cu3Cl6I2 white powder to obtain fine and uniform powder for later use;
s4, weighing Cs 5Cu3Cl6I2 powder and polymer slurry, grinding in an agate mortar to obtain mixed slurry of Cs 5Cu3Cl6I2 and polymer, and placing in vacuum to remove internal bubbles;
s5, coating mixed slurry obtained by Cs 5Cu3Cl6I2 and the polymer on the CMOS substrate.
In the existing scintillator preparation process, a scintillator film is mostly made on a glass substrate for imaging by a spin coating or knife coating mode, or a film is pulled off the glass substrate and is attached to an imaging device, so that light scattering is caused, an imaging effect is poor, the scintillator is attached again, and the attached adhesion is unstable and possibly falls off; the scintillator is also integrated on the imaging device by high temperature vapor deposition, but it is also required to be stabilized by encapsulation, which is costly and cumbersome. In the application, cs 5Cu3Cl6I2 is prepared by adopting a solution method, in the preparation process, each process step and process flow are strictly controlled, the Cs 5Cu3Cl6I2 film can be directly integrated on an imaging device according to any shape, size and specification, and a proper scintillator film is prepared according to the specification of a detector, so that the preparation method is more practical, the preparation process is simple, and optical crosstalk is effectively avoided.
Example 1
An integrated metal halide perovskite X-ray detector, the method of making comprising the steps of:
S1, respectively weighing 0.2376g of cuprous chloride, 0.4041g of cesium chloride and 0.4157g of cesium iodide in a glass sample bottle, adding 10mL of acetonitrile into the bottle, and reacting for 12-36h at 20-50 ℃ under the condition of stirring at the speed of 500-1000r/min to obtain Cs 5Cu3Cl6I2 white powder;
S2, air-drying the obtained Cs 5Cu3Cl6I2 white powder for 24 hours at room temperature;
S3, sieving the dried Cs 5Cu3Cl6I2 white powder to obtain fine and uniform powder for later use;
S4, weighing 0.5gCs 5Cu3Cl6I2 powder and 1g of polydimethylsiloxane slurry, grinding for 20min in an agate mortar to obtain mixed slurry of Cs 5Cu3Cl6I2 and polymer, and placing in vacuum for 15min to remove internal bubbles;
S5, coating the mixed slurry obtained by Cs 5Cu3Cl6I2 and polydimethylsiloxane on a CMOS substrate, and forming a 200 mu m film at 100 ℃.
Example 2
The film thickness was 400. Mu.m, compared with example 1.
Example 3
The film thickness was 600. Mu.m, compared with example 1.
Comparative example 1
An integrated metal halide perovskite X-ray detector, the method of making comprising the steps of:
s1, respectively weighing 0.2376g of cuprous chloride, 0.4041g of cesium chloride and 0.4157g of cesium iodide in an agate mortar, and grinding for 15min to obtain Cs 5Cu3Cl6I2 white powder;
s2, sieving Cs 5Cu3Cl6I2 white powder to obtain fine and uniform powder for later use;
S3, weighing 0.5gCs 5Cu3Cl6I2 powder and 1g of polydimethylsiloxane slurry, grinding for 20min in an agate mortar to obtain mixed slurry of Cs 5Cu3Cl6I2 and polymer, and placing in vacuum for 15min to remove internal bubbles;
S4, coating the mixed slurry obtained by Cs 5Cu3Cl6I2 and polydimethylsiloxane on a CMOS substrate, and forming a 200 mu m film at the temperature of 100 ℃.
Comparative example 2
And adopting a GOS ceramic scintillator to replace a Cs 5Cu3Cl6I2 film to prepare the scintillator detector.
Comparative example 3
The scintillator detector was prepared using LYSO scintillator instead of Cs 5Cu3Cl6I2 film.
Performance measurements were performed on the scintillator detectors prepared in examples and comparative examples, and the measurement results are shown in FIGS. 1 to 8.
As can be seen from fig. 4, the optical signals emitted by the scintillator prepared by the present invention can be better collected by the detector array, the process of converting the optical signals into electrical signals can be better completed, and the obtained image effect is better; the spring in the pen and the wire and the chip in the card can be clearly seen, and the practical imaging effect of the scintillator detector prepared by the invention is proved to be excellent. Under the same fluorescence effect, the higher the quantum yield means higher light output and stronger the luminescence, and as can be seen from fig. 1, the PLQY of M1 is obviously higher than that of M2, which indicates that the scintillator detector prepared by the method has higher light output performance and stronger luminescence. The luminous intensity directly influences the actual application of the material in the detection field, the high luminous intensity means that the detected object can be seen more clearly under the same radiation dose, and as shown in fig. 2, the luminous intensity of M1 is obviously higher than that of M2, so that the Cs 5Cu3Cl6I2 film prepared by the invention can be applied to a scintillator detector to see the detected object more clearly. 3, the resolution ratio of the detector prepared by the invention is 10 lp/mm, which proves that the scintillator detector prepared by the invention has excellent resolution ratio; as can be seen from fig. 5, the luminescence intensity of the scintillator detector is higher than that at 100 ℃ and 180 ℃ at 20 ℃. As can be seen in fig. 6, the imaging of the integrated Cs 5Cu3Cl6I2 device was much clearer than those of LYSO and CsI at a thickness of 400 μm. FIGS. 7-8 show that the imaging effect of the 10-wire pair card can be seen clearly, the imaging of the 200um film is the clearest, and the thicker film has more serious light scattering, so that the imaging effect is affected; the imaging effect of the 30-wire pair card is the clearer of the 200um film imaging, and the thicker film is more serious in light scattering, so that the imaging effect is affected.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (5)
1. An integrated metal halide perovskite X-ray detector, characterized by: the Cs 5Cu3Cl6I2 slurry is directly coated on the CMOS substrate, so that an imaging device with a Cs 5Cu3Cl6I2 film and the CMOS substrate completely coupled is obtained.
2. An integrated metal halide perovskite X-ray detector as claimed in claim 1, wherein: the thickness of the Cs 5Cu3Cl6I2 film is 200-600 mu m.
3. The integrated metal halide perovskite X-ray detector of claim 1, wherein the Cs 5Cu3Cl6I2 film is prepared by a process comprising the steps of:
S1, respectively weighing cuprous chloride, cesium chloride and cesium iodide in a glass sample bottle, adding a solvent into the bottle, heating and stirring, and reacting to obtain Cs 5Cu3Cl6I2 white powder;
S2, air-drying the obtained Cs 5Cu3Cl6I2 white powder at room temperature;
S3, sieving the dried Cs 5Cu3Cl6I2 white powder to obtain fine and uniform powder for later use;
s4, weighing Cs 5Cu3Cl6I2 powder and polymer slurry, grinding in an agate mortar to obtain mixed slurry of Cs 5Cu3Cl6I2 and polymer, and placing in vacuum to remove internal bubbles;
S5, coating the mixed slurry obtained by the Cs 5Cu3Cl6I2 and the polymer on the CMOS substrate in one step.
4. An integrated metal halide perovskite X-ray detector as claimed in claim 3, wherein: the solvent is acetonitrile.
5. An integrated metal halide perovskite X-ray detector as claimed in claim 3, wherein: in the step S1, the reaction temperature is 20-50 ℃, the stirring speed is 500-1000r/min, and the reaction time is 12-36h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311583283.2A CN117913112A (en) | 2023-11-24 | 2023-11-24 | Integrated scintillator detector prepared from metal halides |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311583283.2A CN117913112A (en) | 2023-11-24 | 2023-11-24 | Integrated scintillator detector prepared from metal halides |
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| CN117913112A true CN117913112A (en) | 2024-04-19 |
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| CN202311583283.2A Pending CN117913112A (en) | 2023-11-24 | 2023-11-24 | Integrated scintillator detector prepared from metal halides |
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- 2023-11-24 CN CN202311583283.2A patent/CN117913112A/en active Pending
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