CN112456537B - Beta-phase Cs 3 Cu 2 Cl 5 Preparation method of rapid scintillator and X-ray detection application - Google Patents
Beta-phase Cs 3 Cu 2 Cl 5 Preparation method of rapid scintillator and X-ray detection application Download PDFInfo
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Abstract
The invention discloses a beta-phase Cs 3 Cu 2 Cl 5 The preparation method of the rapid scintillator and the application of X-ray detection comprise the following synthesis steps of thermally injecting cesium oleate into a specific cuprous chloride solution at a certain temperature, stirring nitrogen atmosphere for reaction, and then purifying and post-treating to obtain beta-phase Cs 3 Cu 2 Cl 5 The crystal and XRD result show that the phase is consistent with the target product. beta-Cs 3 Cu 2 Cl 5 Dissolving in toluene solution, and dripping to obtain film with large area and adjustable thickness 3 Cu 2 Cl 5 The film has the characteristics of lead-free environment friendliness, larger Stokes displacement and weak self-absorption, and has excellent optical characteristics of high luminous efficiency, extremely short transient service life and the like; in addition, the fluorescent powder has bright fluorescence and higher light yield under the irradiation of X rays, and the high-spatial resolution imaging result can be obtained by applying the fluorescent powder to X-ray imaging, and the results show that the beta-Cs prepared by the method 3 Cu 2 Cl 5 Can be used as a high-performance fast scintillator.
Description
Technical Field
The invention belongs to the technical field of application of all-inorganic copper-based halide luminescent materials, and in particular relates to beta-Cs 3 Cu 2 Cl 5 Is used as scintillator for high-performance X-ray detection and imaging.
Background
Scintillator materials can convert high-energy photons, such as X-rays, into visible photons for easy detection, and are currently widely used as core components of indirect X-ray imaging detectors in industrial, medical, public safety, and other fields. The conventional scintillator materials such as CsI: tl crystals require 1700 ℃ high temperature and vacuum conditions during growth, resulting in higher cost, and in addition, longer decay lifetime, resulting in imaging afterglow, GOS scintillators, while being cheaper, have limited spatial resolution and imaging quality, and longer decay lifetime.
In recent years, perovskite materials show very excellent photoelectric properties, and researchers apply all-inorganic perovskite nanocrystalline materials as scintillators to X-ray detection and imaging (Nature 561,88-93 (2018); adv. Mater.2018,1801743; ACS nano,2019,13 (2), 2520-2525), and have great application potential, mainly due to simple process, low preparation cost, short decay life, low detection limit, adjustable emission wavelength and higher imaging spatial resolution. However, the light yield is not high due to the toxicity of lead element, obvious self-absorption effect caused by small Stokes displacement and other factors, so that the large-scale further application of the lead element is limited. While copper-based halide luminescent materials are lead-free, have higher photoluminescence quantum yield (PLQY), larger Stokes shift and weak self-absorption effect, and have potential for application as high-performance scintillator materials, such as Rb 2 CuBr 3 Columnar crystals (advmate, 2019,31 (44), 1904711) were found to have extremely high photon yield and stability, however, such columnar crystals with diameters of around 0.2mm are relatively difficult to prepare as uniform films and to use in X-ray imaging. In addition alpha-Cs 3 Cu 2 I 5 Nanocrystalline materials also exhibit higher photon yields as scintillators (Advanced Science 2020,7 (11), 2000195.). However, the decay lifetime is very important for scintillator dynamic imaging, long decay lifetime can lead to afterglow and afterimage phenomena during imaging, degrading the quality of imaging, especially in medical fields such as CT, while Rb 2 CuBr 3 Columnar Crystal (41.4. Mu.s) and alpha-Cs 3 Cu 2 I 5 Nanocrystalline Material (1.92 μs) and alpha-Cs 3 Cu 2 Cl 5 The decay life of the nanocrystalline material (95.79 mu s) is longer than that of a fast scintillator<100 ns) long, while also being longer than commercial CsI: tl scintillators (-1 mus).
Therefore, for dynamic imaging and rapid detection of X-rays, development of a novel lead-free scintillator material with short decay lifetime, high solid film PLQY, high photon yield, good working stability and large stokes shift is needed.
Disclosure of Invention
The object of the present invention is therefore to provide a beta-phase copper-based halide beta-Cs 3 Cu 2 Cl 5 Use of such beta-Cs as scintillators 3 Cu 2 Cl 5 The solid film has better crystallinity, very short decay life, very high PLQY luminous efficiency, weak self-absorption effect, and can obtain higher photon yield, good linear response and lower detection lower limit, and simultaneously has good working stability, and a clearer photo and high spatial resolution are obtained by self-made X-ray imaging system.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
beta-phase Cs 3 Cu 2 Cl 5 A method of preparing a fast scintillator, the method comprising:
s1, preparing cesium oleate (Cs-OA); cesium carbonate (1.5-3 g), 40-60mL of Octadecene (ODE) and 9-12 mL of Oleic Acid (OA) are mixed in a 250 mL three-neck flask, the three-neck flask is vacuumized, the oil bath is heated to 115-125 ℃ and reacts for 20-40min, and then nitrogen protection and cooling are carried out, so that cesium oleate (Cs-OA) is obtained.
S2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the Adding 0.18-0.22 g CuCl, 9-12 mL ODE and 1-2.5 mL OA into a 100mL three-neck flask, transferring to an oil bath table, adding 1-2 mL OLAM (oleylamine), quickly sealing and starting vacuumizing while heating in the oil bath, heating to 115-125 ℃ and staying for 10-30 min, keeping the solution in a completely dissolved state and turning into yellowish green, starting introducing nitrogen, heating to 130-150 ℃, keeping the solution to be yellowish, taking 6-18 mL of cesium oleate preheated at 100-120 ℃ by using a syringe, quickly injecting the cesium oleate into the CuCl solution at 130-150 ℃ for stirring reaction for 20-120 s, then carrying out ice water bath for 2-5 min, wherein the adopted hot injection temperature is lower than that of the ordinary reaction, and the cesium oleate is obviously more used, thus being beneficial to controlling the crystal of the productThe regularity, size and CuCl of the body are such that they are nearly fully reacted. Taking out the product solution, centrifuging for 5-10 minutes at 7000-10000 rpm, pouring out the supernatant, washing twice with cyclohexane for three times, adding cyclohexane for ultrasonic dissolution, centrifuging for 4-6 minutes at 2000-6000 rpm, taking out the product solution, washing with cyclohexane, adding toluene solution for mixing and dissolving, and carrying out the next characterization and film forming, wherein the XRD result of the synthetic film is shown in figure 1, and the target product of the synthetic method is relatively pure.
S3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Is dissolved in toluene mainly due to the discovery that toluene is specific to beta-Cs 3 Cu 2 Cl 5 Better solubility. Can control beta-Cs 3 Cu 2 Cl 5 The concentration of the solution is regulated in 10-100 mg/mL, after being uniformly dispersed by ultrasonic vibration, the solution is directly dripped on clean substrates such as glass or quartz with the side length ranging from 1 cm to 5cm, and the substrate is naturally air-dried in a fume hood, thus obtaining the beta-Cs with controllable size and thickness and stable performance 3 Cu 2 Cl 5 Membranes, such as those that exhibit bright green fluorescence under X-ray irradiation (FIG. 3), can be prepared by modulating beta-Cs 3 Cu 2 Cl 5 The toluene solution concentration and the number of dropping times were used to adjust the thickness of the coating film.
S4X-ray detection and imaging
beta-Cs based on autonomous building as shown in figure 9 3 Cu 2 Cl 5 The membrane X-ray imaging system is provided with an X-ray source at the top for providing X-ray signals required for imaging. The film with the side length of 3-10 cm is placed on two split right-angle prisms with the side length of 5-10 cm, and the film faces upwards and the substrate faces downwards, so that X-ray signals with different intensities in different areas can be absorbed and then radiation-induced fluorescence with different intensities can be emitted. Then the relevant imaging objects can be placed on the upper part of the film, and the absorption degree of the X-ray signals is different in different areas of the imaging objects, so that the penetrated X-ray signals have information with different intensities, thereby exciting the beta-Cs 3 Cu 2 Cl 5 The film generates fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of the fluorescent signals are redundantIs filtered out, the fluorescent signal is captured and imaged by a horizontally placed camera, and high spatial resolution and high quality beta-Cs are obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging of the film (fig. 10).
Compared with the prior art, the traditional rapid scintillator needs to be synthesized under the high-temperature vacuum condition exceeding 1700 ℃ and generally needs to be doped with rare earth, and the cost is high. The invention has the advantages that the rapid scintillator with high luminous efficiency (figure 5) is synthesized by liquid phase synthesis under the conditions of reduced temperature (lower than 160 ℃) and no need of rare earth doping, and the obtained beta-Cs 3 Cu 2 Cl 5 The crystal grain size is more uniform, the crystallization is regular (figure 2), the attenuation life is very short (figure 6), the afterglow and the ghost effect in medical imaging are greatly reduced, and the time resolution and the dynamic imaging quality are improved. Toluene solution beta-Cs used by us 3 Cu 2 Cl 5 The method for forming the film by dripping is simple and convenient to operate, can control the thickness and the size of the film, has stable performance, and is favorable for further popularization and application to the film formation of other materials. In addition, we independently build beta-Cs-based 3 Cu 2 Cl 5 The film X-ray imaging system (figure 9) is different from the prior art in that two split right angle prisms are introduced to realize beta-Cs 3 Cu 2 Cl 5 The film can be well attached in parallel, so that not only can the phenomenon that redundant transmitted X-ray photons strike on a photosensitive element of a camera to generate noise signals be avoided, but also the imaging cannot be distorted and distorted due to the right-angle complete reflection mode, the imaging quality cannot be reduced, and a high-quality X-ray imaging effect is obtained (figure 10).
Drawings
FIG. 1 is beta-Cs 3 Cu 2 Cl 5 Experimental testing of the synthetic product XRD spectrum and the simulated spectrum according to the crystal phase structure, it can be deduced from figure 1 that the experimental result and the simulated result are well matchedBy usingThe product obtained by the liquid phase synthesis method is beta-Cs of purer phase 3 Cu 2 Cl 5 。
FIG. 2 is beta-Cs 3 Cu 2 Cl 5 As can be seen from the scanning electron micrograph of the synthesized product, the synthesized product is in the shape of cubes, the particle size varies from hundreds of nanometers to 1-2 micrometers, and the crystallinity is good.
FIG. 3 shows beta-Cs prepared by the drop coating method 3 Cu 2 Cl 5 The film produces a photograph of fluorescence under X-ray irradiation, wherein the central bright spot area is the X-ray spot area, as can be demonstrated by fig. 3 for beta-Cs 3 Cu 2 Cl 5 The film exhibits good radiation luminescence properties and is a relatively good scintillator material.
FIG. 4 is beta-Cs 3 Cu 2 Cl 5 As can be seen from FIG. 4, the relative intensity of photoluminescence of films of different thicknesses increases with increasing film thickness, mainly due to increasing emission peak intensity as a result of increasing absorption of ultraviolet light, the film thicknessBig size AboutAfter exceeding 60 μm, the luminescence peak intensity shows a weak decrease, mainly due to an increase in roughness caused by an increase in thickness, and thus light scattering loss increases. In addition, this result also demonstrates beta-Cs 3 Cu 2 Cl 5 The film has weak self-absorption effect, and is favorable for preparing thick films to absorb high-energy rays such as X-rays.
FIG. 5 is beta-Cs 3 Cu 2 Cl 5 The photoluminescence quantum yield (PLQY) of the film, beta-Cs, can be seen from FIG. 5 3 Cu 2 Cl 5 The films have a PLQY close to 100%, exhibiting very high luminous efficiency and good scintillator potential.
FIG. 6 is beta-Cs 3 Cu 2 Cl 5 As can be seen from FIG. 6, the transient lifetime test results of the film show that the transient lifetime is very short, the average lifetime is only 1.03ns, and the film is much faster than that of a commercial scintillator such as CsI: tl (1000 ns), and has very high theoretical time resolution and low afterglow high quality dynamic potential of a fast scintillator.
FIG. 7 is beta-Cs 3 Cu 2 Cl 5 The radiation-induced luminescence (RL) spectrum of the film, as can be seen from FIG. 7, is compared to the commercial scintillator YAG: ce, beta-Cs 3 Cu 2 Cl 5 Has higher radiation-induced luminescence intensity, and beta-Cs 3 Cu 2 Cl 5 Of filmsThe light yield reached a higher level of about 34500 photons/MeV.
FIG. 8 is beta-Cs 3 Cu 2 Cl 5 The radiation-induced luminescence spectrum of the film at different X-ray dose rates gradually increases from bottom to top. From FIG. 8, it can be seen that β -Cs 3 Cu 2 Cl 5 The film has good response to X-rays with different intensities, and the luminescence peak position is kept stable.
FIG. 9 is based on beta-Cs 3 Cu 2 Cl 5 The film's X-ray imaging system is schematic in that the right angle prism eliminates unwanted X-ray photon interference with the imaging quality while maintaining sharpness.
FIG. 10 is beta-Cs 3 Cu 2 Cl 5 As a result of film imaging of the object and radiograph, the left is the object and the right is the radiograph. From FIG. 10, it can be seen that β -Cs 3 Cu 2 Cl 5 The film imaging photograph is very clear, exhibiting very high X-ray detection and imaging performance.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
Please properly enumerate the following examples.
The present invention will be further described with reference to the following specific embodiments, but the scope of the present invention is not limited to the following embodiments.
Example 1
S1, cesium oleate (Cs-OA) is prepared, 1.629g of cesium carbonate, 50mL of Octadecene (ODE) and 10mL of Oleic Acid (OA) are mixed in a 250 mL three-neck flask, the three-neck flask is vacuumized, an oil bath is heated to 120 ℃ and reacted for 30min, and then nitrogen protection and cooling are carried out, so that cesium oleate (Cs-OA) is obtained.
S2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the 0.2g CuCl,10mL ODE,2mL OA adding into 100mL three-neck flask, transferring to oil bath table, adding 1mL OLAM (oleylamine), rapidly sealing, vacuumizing while heating in oil bath, heating to 120deg.C, standing for 10min, keeping the solution in completely dissolved state and turning to yellow green, introducing nitrogen, heating to 130deg.C, turning the solution to light yellow, and taking 100 deg.C strips with syringe6 ml of preheated cesium oleate is quickly injected into a CuCl solution at 130 ℃ for stirring reaction for 20s, then the ice-water bath is carried out for 5min, the product solution is taken out for centrifugation by a centrifuge at 7000rpm for 8 min, then the supernatant is poured off, the supernatant is washed twice and three times by cyclohexane, the cyclohexane is added for ultrasonic dissolution and then the centrifugation is carried out for 5min at 5000rpm, the mixture is taken out, the cyclohexane is washed and then the toluene solution is added for mixing dissolution, and the next characterization and film forming are carried out.
S3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Dissolved in toluene. Can control beta-Cs 3 Cu 2 Cl 5 The solution concentration is 10mg/mL, after being uniformly dispersed by ultrasonic vibration, the solution is directly dripped on clean substrates such as glass or quartz with the side length of 5cm, and the like, and naturally air-dried in a fume hood, thus obtaining the beta-Cs with controllable size and thickness and stable performance 3 Cu 2 Cl 5 The film exhibits fluorescence, such as under X-ray irradiation.
S4X-ray detection and imaging
A film with a side length of 5cm is placed on two split rectangular prisms with a side length of 5cm, and the film faces upwards and the substrate faces downwards. Then the relevant imaging objects can be placed on the upper part of the film, and the absorption degree of the X-ray signals is different in different areas of the imaging objects, so that the penetrated X-ray signals have information with different intensities, thereby exciting the beta-Cs 3 Cu 2 Cl 5 The film can generate fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of redundant X-ray photons are filtered, the fluorescent signals are captured and imaged by a camera arranged in the horizontal direction, and meanwhile, beta-Cs is obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging of the film.
Example two
S1, cesium oleate (Cs-OA) is prepared, 1.629g of cesium carbonate, 50mL of Octadecene (ODE) and 10mL of Oleic Acid (OA) are mixed in a 250 mL three-neck flask, the three-neck flask is vacuumized, an oil bath is heated to 120 ℃ and reacted for 30min, and then nitrogen protection and cooling are carried out, so that cesium oleate (Cs-OA) is obtained.
S2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the 0.2g CuCl,10mL ODE,2mL OA is added into a 100mL three-neck flask, after transferring to an oil bath table, 2mL OLAM (oleylamine) is added, then sealing is rapidly carried out, vacuumizing is started, meanwhile, oil bath heating is carried out, the temperature is kept for 20min, the solution is in a completely dissolved state and turns into yellow green, nitrogen is started to be introduced, then heating is carried out, after the temperature is kept at 140 ℃, the solution becomes light yellow, 18 mL of cesium oleate preheated at 100 ℃ is taken out by a syringe, is rapidly injected into 140 ℃ CuCl solution, stirring reaction is carried out for 90s, then ice water bath is carried out for 3 min, the product solution is taken out, centrifugal is carried out by a centrifugal machine at 8000rpm for 8 min, then supernatant is poured out, washing is carried out for three times by cyclohexane, ultrasonic dissolution is carried out by adding cyclohexane for secondary centrifugal, centrifugal at 5000rpm for 5min, toluene solution is added for mixed dissolution after washing by cyclohexane, and the product solution is taken out, and the next characterization and film forming are carried out.
S3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Dissolved in toluene. Can control beta-Cs 3 Cu 2 Cl 5 The concentration of the solution is 20mg/mL, the solution is uniformly dispersed through ultrasonic vibration, and then the solution is directly dripped on clean substrates such as glass or quartz with the side length of 5cm, and the substrate is naturally air-dried in a fume hood, thus obtaining the beta-Cs with controllable size and thickness and stable performance 3 Cu 2 Cl 5 The film exhibits fluorescence, such as under X-ray irradiation.
S4X-ray detection and imaging
A film with a side length of 5cm is placed on two split rectangular prisms with a side length of 5cm, and the film faces upwards and the substrate faces downwards. Then the relevant imaging objects can be placed on the upper part of the film, and the absorption degree of the X-ray signals is different in different areas of the imaging objects, so that the penetrated X-ray signals have information with different intensities, thereby exciting the beta-Cs 3 Cu 2 Cl 5 The film can generate fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of redundant X-ray photons are filtered, the fluorescent signals are captured and imaged by a camera arranged in the horizontal direction, and meanwhile, beta-Cs is obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging junction of filmAnd (5) fruits.
Example III
S1, cesium oleate (Cs-OA) is prepared, 1.629g of cesium carbonate, 50mL of Octadecene (ODE) and 10mL of Oleic Acid (OA) are mixed in a 250 mL three-neck flask, the three-neck flask is vacuumized, an oil bath is heated to 120 ℃ and reacted for 30min, and then nitrogen protection and cooling are carried out, so that cesium oleate (Cs-OA) is obtained.
S2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the 0.2g CuCl,10mL ODE,2mL OA is added into a 100mL three-neck flask, after transferring to an oil bath table, 2mL OLAM (oleylamine) is added, then sealing is rapidly carried out, vacuumizing is started, meanwhile, oil bath heating is carried out, after heating to 120 ℃, the solution stays for 15min, the solution is in a completely dissolved state and turns into yellow green, nitrogen is started to be introduced, then heating to 150 ℃, after the solution turns into light yellow, 18 mL of cesium oleate preheated at 100 ℃ is taken out by a syringe, the cesium oleate preheated at 150 ℃ is rapidly injected into a CuCl solution, stirring is carried out for 120s, then ice-water bath is carried out for 3 min, the product solution is taken out, centrifugal is carried out by a centrifugal machine at 8000rpm for 8 min, then supernatant is poured out, washing is carried out for three times by cyclohexane, ultrasonic dissolution is carried out by adding cyclohexane, centrifugal speed is 5000rpm for 5min, toluene solution is added for mixed dissolution after washing by cyclohexane, and the product solution is taken out for further characterization and film formation.
S3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Dissolved in toluene. Can control beta-Cs 3 Cu 2 Cl 5 The concentration of the solution is 20mg/mL, the solution is uniformly dispersed through ultrasonic vibration, and then the solution is directly dripped on clean substrates such as glass or quartz with the side length of 5cm, and the substrate is naturally air-dried in a fume hood, thus obtaining the beta-Cs with controllable size and thickness and stable performance 3 Cu 2 Cl 5 The film exhibits fluorescence, such as under X-ray irradiation.
S4X-ray detection and imaging
A film with a side length of 5cm is placed on two split rectangular prisms with a side length of 5cm, and the film faces upwards and the substrate faces downwards. Then the relevant imaging objects can be placed on the upper part of the film, and the absorption degree of the X-ray signals is different in different areas of the imaging objects, so that the penetrated X-ray signals have information with different intensities, therebyTo excite beta-Cs 3 Cu 2 Cl 5 The film can generate fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of redundant X-ray photons are filtered, the fluorescent signals are captured and imaged by a camera arranged in the horizontal direction, and meanwhile, beta-Cs is obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging of the film.
Example IV
S1, cesium oleate (Cs-OA) is prepared, 1.629g of cesium carbonate, 50mL of Octadecene (ODE) and 10mL of Oleic Acid (OA) are mixed in a 250 mL three-neck flask, the three-neck flask is vacuumized, an oil bath is heated to 120 ℃ and reacted for 30min, and then nitrogen protection and cooling are carried out, so that cesium oleate (Cs-OA) is obtained.
S2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the 0.2g CuCl,10mL ODE,2mL OA is added into a 100mL three-neck flask, after transferring to an oil bath table, 2mL OLAM (oleylamine) is added, then sealing is rapidly carried out, vacuumizing is started, meanwhile, oil bath heating is carried out, the temperature is kept for 20min, the solution is in a completely dissolved state and turns into yellow green, nitrogen is started to be introduced, then heating is carried out, after the temperature is kept at 140 ℃, the solution becomes light yellow, 16 mL of cesium oleate preheated at 100 ℃ is taken out by a syringe, is rapidly injected into 140 ℃ CuCl solution, stirring reaction is carried out for 90s, then ice water bath is carried out for 3 min, the product solution is taken out, centrifugal is carried out by a centrifugal machine at 8000rpm for 8 min, then supernatant is poured out, washing is carried out for three times by cyclohexane, ultrasonic dissolution is carried out by adding cyclohexane for secondary centrifugal, centrifugal speed is 3000rpm for 5min, toluene solution is added for mixed dissolution after washing by cyclohexane, and the product solution is taken out, and the next characterization and film forming are carried out.
S3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Dissolved in toluene. Can control beta-Cs 3 Cu 2 Cl 5 The concentration of the solution is 20mg/mL, the solution is uniformly dispersed through ultrasonic vibration, and then the solution is directly dripped on clean substrates such as glass or quartz with the side length of 5cm, and the substrate is naturally air-dried in a fume hood, thus obtaining the beta-Cs with controllable size and thickness and stable performance 3 Cu 2 Cl 5 Films, e.g. appearing under X-ray irradiationFluorescence.
S4X-ray detection and imaging
A film with a side length of 5cm is placed on two split rectangular prisms with a side length of 5cm, and the film faces upwards and the substrate faces downwards. Then the relevant imaging objects can be placed on the upper part of the film, and the absorption degree of the X-ray signals is different in different areas of the imaging objects, so that the penetrated X-ray signals have information with different intensities, thereby exciting the beta-Cs 3 Cu 2 Cl 5 The film can generate fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of redundant X-ray photons are filtered, the fluorescent signals are captured and imaged by a camera arranged in the horizontal direction, and meanwhile, beta-Cs is obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging of the film.
Claims (2)
1. The method comprises the following steps ofβPhase Cs 3 Cu 2 Cl 5 The preparation method of the rapid scintillator is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing cesium oleate; mixing 1.5-3 g of cesium carbonate, 40-60mL of octadecene and 9-12 mL of oleic acid in a 250 mL three-neck flask, vacuumizing, heating to 115-125 ℃ in an oil bath, reacting for 20-40min, and then introducing nitrogen for protection and cooling to obtain cesium oleate;
s2 synthesis of beta-Cs 3 Cu 2 Cl 5 The method comprises the steps of carrying out a first treatment on the surface of the Adding 0.18-0.22 g of CuCl, 9-12 mL of octadecene and 1-2.5 mL of oleic acid into a 100mL three-neck flask, transferring to an oil bath table, adding 1-2 mL of oleylamine, quickly sealing and starting vacuumizing while heating in an oil bath, heating to 115-125 ℃ and staying for 10-30 min, waiting for the solution to be in a completely dissolved state and turn into a yellowish green state, starting introducing nitrogen, heating to 130-150 ℃, waiting for the solution to become yellowish, taking 6-18 mL of cesium oleate preheated at 100-120 ℃ by using a syringe, quickly injecting into the CuCl solution at 130-150 ℃ and stirring for reacting for 20-120 s, and then carrying out an ice-water bath for 2-5 min; taking out the product solution, centrifuging with a centrifuge at 7000-10000 rpm for 5-10 min, pouring out supernatant, washing with cyclohexane twice and three times, and dissolving with cyclohexane by ultrasonicCentrifuging for 4-6 minutes at 2000-6000 rpm, taking out, cleaning with cyclohexane, adding toluene solution, mixing and dissolving, and carrying out characterization and film forming;
s3, dripping and coating to form a film; beta-Cs 3 Cu 2 Cl 5 Dissolving in toluene to control beta-Cs 3 Cu 2 Cl 5 The concentration of the solution is regulated in 10-100 mg/mL, after being uniformly dispersed through ultrasonic vibration, the solution is directly dripped on a glass or quartz substrate with the side length ranging from 1 cm to 5cm, and the solution is naturally air-dried in a fume hood, so that the beta-Cs with controllable size and thickness and stable performance can be obtained 3 Cu 2 Cl 5 A membrane;
construction based on beta-Cs 3 Cu 2 Cl 5 A film X-ray imaging system, the uppermost end is an X-ray source for providing X-ray signals required by imaging; placing a film with the side length of 3-10 cm on two split rectangular prisms with the side length of 5-10 cm, and enabling the film to face upwards and downwards to absorb X-ray signals with different intensities in different areas and then emit radiation-induced fluorescence with different intensities; then, the relevant imaging objects are placed on the upper part of the film, and the absorption degree of X-ray signals is different in different areas of the imaging objects, so that the transmitted X-ray signals have information with different intensities, thereby exciting beta-Cs 3 Cu 2 Cl 5 The film generates fluorescent signals with different intensities, and finally, after the radiation green fluorescent signals are reflected by the right-angle prism, a part of redundant X-ray photons are filtered, the fluorescent signals are captured and imaged by a camera arranged in the horizontal direction, and high spatial resolution and high quality beta-Cs are obtained by adjusting camera parameters 3 Cu 2 Cl 5 X-ray imaging of the film.
2. A kind of according to claim 1βPhase Cs 3 Cu 2 Cl 5 The preparation method of the rapid scintillator is characterized by comprising the following steps: s2, rapidly vacuumizing after adding oleylamine to avoid excessive oxidation of CuCl, and controlling the temperature of a hot injection reaction to obtain grains with adjustable size; in S3, beta-Cs 3 Cu 2 Cl 5 Dissolved in toluene and controlling the concentration of the solution and the number of dropsThe thickness of the coating film is regulated, and the coating film is applied to a series of different substrates with different sizes, and has easy operability and easy popularization.
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