CN112851985A - matrix-PQD scintillator film, and preparation method and application thereof - Google Patents
matrix-PQD scintillator film, and preparation method and application thereof Download PDFInfo
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- G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
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Abstract
The invention discloses a substrate-PQD scintillator film and a preparation method and application thereof, wherein the method comprises the following steps: firstly, mixing a matrix material precursor solution with a material containing PQD so as to obtain a matrix-PQD precursor solution; and injecting the matrix-PQD precursor solution into a mold, defoaming, and curing to obtain the matrix-PQD scintillator film. The method for preparing the substrate-PQD scintillator film can improve the water-oxygen barrier property of the substrate-PQD scintillator film, limit the self-absorption effect of PQD, avoid the problems of uneven film layer, local enrichment or cracking and the like in the process of preparing a PQD thick film by a traditional solution method, is beneficial to the visible light transmission of the scintillator and the visible light acquisition of a visible light detector, and meanwhile, the prepared substrate-PQD scintillator film has good mechanical property and flexibility and is easy to remove and replace in the later period.
Description
Technical Field
The invention belongs to the technical field of high-energy ray detection, and particularly relates to a substrate-PQD scintillator film, and a preparation method and application thereof.
Background
The scintillator is a material that can absorb energy of high-energy photons and release visible photons when irradiated with high-energy photons such as X-rays and gamma-rays. The scintillator is combined with a visible light detector and a TFT array to manufacture a high-energy photon detector, and the high-energy photon detector has wide application in the fields of medical diagnosis, industrial flaw detection, material analysis and the like. In order to obtain a good radiation luminous effect and to block absorption of high-energy photons to a certain extent, the scintillator material needs to have properties of higher density, high radiation photon yield, strong radiation resistance and the like. Traditionally used scintillator materials include thallium-doped cesium iodide crystals (CsI: Tl), bismuth germanate crystals (Bi)4Ge3O12) Cadmium tungstate crystal (CdWO)4) And the like, although having good radiation luminescence performance, have the disadvantages of high price, complicated manufacturing process, slow response time, high toxicity and the like.
In recent years, Perovskite Quantum Dots (PQD) are an emerging scintillator material. PQD is a nanocrystal with the size of about 10nm, and because the PQD contains Cs and Pb elements with high atomic numbers, the PQD material has high density and strong interaction with high-energy photons; meanwhile, PQD is a luminescent material with excellent performance and has the advantages of high fluorescence quantum yield, pure luminescence peak, short fluorescence response time and the like; compared with the traditional scintillator prepared by a high-temperature evaporation method (1000 ℃), the PQD can be synthesized by a room-temperature solution method and then coated to form a film by methods such as drop coating, blade coating, slit coating and the like, so that the cost is greatly reduced. Thus, PQD is considered to be a highly potential scintillator material.
However, the currently available methods for preparing scintillator films using PQD have the following significant drawbacks: (1) in order to convert the high-energy photons as far as possible into visible photons, while preventing the high-energy photons from escaping to the environment, the scintillator material needs to be of a larger thickness. Academic studies indicate that the ideal thickness of the PQD film needs to be more than 400 microns for X-rays with 100Kev energy, and the existing solution method film coating technology, such as drop coating, blade coating, slit coating and the like, is not sufficient; (2) volatilization of a solvent in the process of preparing the scintillator membrane by a solution method is difficult to effectively control, so that the thickness of the membrane is uneven, the surface flatness is poor, and even phenomena such as local enrichment of PQD or membrane cracking can occur; (3) the Stokes displacement of the PQD material is small (the absorption band edge is close to an emission peak, and the absorption and the emission spectrum are partially overlapped), the phenomenon of self-absorption is serious after the PQD material is coated into a scintillator thick film, a large amount of visible photons generated in the film layer are absorbed by the PQD material and are difficult to emit out of the film layer to be received by a visible light detector, so that the actual irradiated photon yield of the scintillator is far lower than a theoretical value; (4) after the PQD scintillator is coated on a visible light detector, the film layers are stacked together only by the self gravity of the PQD, and the film layers are connected only by the Van der Waals force of the surface of the PQD, so that the film layers have poor mechanical properties and cannot be bent, and once the PQD fails, the film layers are difficult to remove and replace; (5) PQD has poor resistance to water and oxygen and must be packaged to ensure stability in use.
Therefore, the existing technique for preparing PQD scintillator films is in need of improvement.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, one object of the present invention is to provide a substrate-PQD scintillator film, a preparation method and an application thereof, wherein the method for preparing the substrate-PQD scintillator film can improve the water and oxygen barrier properties of the scintillator film, limit the self-absorption effect of PQD, avoid the problems of non-uniformity, local enrichment or cracking of the film layer during the preparation of a PQD thick film by a conventional solution method, facilitate the visible light transmission of the scintillator and the visible light acquisition of a visible light detector, and simultaneously, the prepared substrate-PQD scintillator film has good mechanical properties and flexibility and is easy to remove and replace at a later stage.
In one aspect of the present invention, a method of preparing a matrix-PQD scintillator film is provided. According to an embodiment of the invention, the method comprises:
(1) mixing a substrate material precursor solution with a PQD-containing material to obtain a substrate-PQD precursor solution;
(2) and injecting the matrix-PQD precursor solution into a mold, defoaming, and curing to obtain the matrix-PQD scintillator film.
According to the method for preparing the matrix-PQD scintillator film, the matrix-PQD precursor solution can be obtained by mixing the matrix material precursor solution with a PQD-containing material; and injecting the substrate-PQD precursor solution into a mold, defoaming, curing, carrying out in-situ polymerization/reaction on the PQD-loaded substrate material precursor solution, and carrying out in-situ initiation curing to form a film so as to obtain the substrate-PQD scintillator film. The method of the present application for preparing PQD scintillator films has the following advantages over the prior art: (1) the substrate material is used for coating the PQD, so that water vapor can be isolated, the water oxygen barrier property is improved, the water oxygen tight packaging is not required to be blocked, and the stability of the PQD is improved; (2) the introduction of the matrix material can solve the problem of poor mechanical properties of the PQD; (3) the film forming process assisted by the matrix material does not involve solvent volatilization, overcomes the problems of nonuniform film layer, local enrichment or cracking and the like in the process of preparing the PQD thick film by the traditional solution method, and has simple film forming process without special equipment or fine process; (4) the matrix material can help the PQDs to be separated from each other in space, so that the PQDs are prevented from generating obvious self-absorption effect due to mutual agglomeration, and the irradiation photon yield of the scintillator film layer can be improved; (5) the scintillator film layer which can be stretched and bent can be obtained by using a substrate material with certain flexibility and can be adapted to a flexible device; (6) the substrate-PQD scintillator film can be made into a device only by attaching the substrate-PQD scintillator film to the surface of the detector, the process is simple and convenient, and the substrate-PQD scintillator film can be easily replaced according to the requirement; (7) the matrix material adopted by the application has high visible light transmittance and medium refractive index after being cured, namely the matrix material is favorable for the visible light of the scintillator to be transmitted and the visible light detector to collect the visible light. Therefore, the method for preparing the substrate-PQD scintillator film can improve the water-oxygen barrier property of the scintillator film, limit the self-absorption effect of PQD, avoid the problems of uneven film layer, local enrichment or cracking and the like in the process of preparing a PQD thick film by a traditional solution method, is beneficial to the visible light transmission of the scintillator and the visible light acquisition of a visible light detector, and meanwhile, the prepared substrate-PQD scintillator film has good mechanical property and flexibility and is easy to remove and replace in the later period.
In addition, the method of preparing the matrix-PQD scintillator film according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the present invention, in step (1), the matrix material precursor solution and PQD are mixed in a mass ratio of matrix material to PQD of (1-10): 1, mixing. Therefore, on one hand, the matrix-PQD scintillator film can have good mechanical properties; on the other hand, the response of the matrix-PQD scintillator film to irradiation with high-energy photons can be enhanced.
In some embodiments of the present invention, in step (1), the PQD-containing material is a PQD dispersion or a PQD powder.
In some embodiments of the present invention, in step (1), the matrix material comprises at least one of silicone polymer, silicon oxide, glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, linear aliphatic type epoxy resin, alicyclic type epoxy resin, isocyanate, two-component silicone containing silicone and siloxane, two-component inorganic silicon containing silicon oxide and auxiliaries, two-component epoxy resin containing epoxy curing agent and epoxy adhesive, and two-component polyurethane containing polyisocyanate and polyether alcohol.
In some embodiments of the invention, in step (1), the PQD has the chemical formula ABX3Wherein A is cesium, methylamine or formamidine, B is lead or tin, and X is chlorine, bromine or iodine.
In some embodiments of the invention, in step (1), the matrix material precursor solution is mixed with the PQD dispersion, and the solvent of the PQD dispersion is removed during the mixing process. Therefore, the solvent can assist PQD to be rapidly dispersed in the matrix material precursor solution, and the solvent can be removed in the mixing process, so that various negative effects caused by solvent volatilization in the film forming process can be avoided.
In some embodiments of the present invention, in step (1), the PQD is surface ligand-modified PQD or core-shell structure method-modified PQD or organic polymer-coated PQD, metallorganic framework-coated PQD, metal oxide-coated PQD, microporous material-coated PQD.
In some embodiments of the present invention, in step (1), the matrix material precursor solution is mixed with the PQD-containing material and an auxiliary agent, wherein the auxiliary agent includes at least one of a plasticizer, a leveling agent, an age resistor, an antioxidant, and a crosslinking agent. Therefore, the mechanical property of the matrix-PQD scintillator film can be improved, and the light emitting effect and the service life of the PQD scintillator can be improved.
In a second aspect of the invention, a host-PQD scintillator film is provided. According to an embodiment of the present invention, the matrix-PQD scintillator film is prepared by the method for preparing the matrix-PQD scintillator film as described above. Therefore, the substrate-PQD scintillator film does not need to be tightly packaged by blocking water and oxygen, has uniform thickness, smooth surface, uniform PQD distribution, good mechanical property and flexibility and higher irradiation photon yield, is beneficial to the visible light of the scintillator to be transmitted out and the visible light detector to collect the visible light, and is easy to remove and replace at the later stage.
In some embodiments of the invention, the thickness of the matrix-PQD scintillator film is 0.1mm to 5 mm. Thus, a higher conversion of high-energy photons to visible light can be achieved, while at the same time high-energy photons can be absorbed and prevented from escaping to the environment.
In a third aspect of the invention, a high energy photon detection device is presented. According to an embodiment of the invention, the high-energy photon detection device comprises a TFT array, a photodetector and a scintillator film layer, wherein the scintillator film layer is arranged on the surface of the photodetector, and the scintillator film layer is the substrate-PQD scintillator film or the substrate-PQD scintillator film prepared by the method. Therefore, the high-energy photon detection device has good integrity and longer service life, has excellent response performance to high-energy photon irradiation, can absorb high-energy photons to prevent the high-energy photons from escaping to the environment, can be designed and manufactured into a flexible device capable of being bent in an extending way, can be manufactured into a device only by attaching the substrate-PQD scintillator film on the surface of the photodetector, and is easy to remove and replace the substrate-PQD scintillator film at the later stage according to the requirement.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic flow diagram of a method for preparing a matrix-PQD scintillator film according to one embodiment of the present invention;
FIG. 2 is a schematic flow diagram of a method for preparing a matrix-PQD scintillator film according to yet another embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a high energy photon detection device according to one embodiment of the present invention;
FIG. 4 is an X-ray excitation spectrum of a PQD scintillator in the matrix-PQD scintillator film prepared in example 1;
FIG. 5 is an X-ray excitation spectrum of a PQD scintillator in the matrix-PQD scintillator film prepared in example 2;
fig. 6 shows an X-ray excitation spectrum of a PQD scintillator in the matrix-PQD scintillator film prepared in example 3.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In a first aspect of the present invention, a method of preparing a matrix-PQD scintillator film is provided. According to an embodiment of the invention, with reference to fig. 1, the method comprises:
s100: mixing the matrix material precursor solution with PQD-containing material
In this step, the matrix material precursor solution and the PQD dispersion liquid or the PQD powder are stirred (without limitation, the stirring method) and mixed to obtain a matrix-PQD precursor solution. The PQD dispersion liquid is a mixed solution formed by uniformly dispersing PQD powder in a solvent, the solvent can assist PQD to be rapidly dispersed in the matrix material precursor liquid, and the solvent is removed in the mixing process, so that various negative effects caused by solvent volatilization in the film forming process can be avoided. It should be noted that the specific type and removal method of the above solvent are not particularly limited, and those skilled in the art can select the solvent according to actual needs, for example, the solvent may be at least one of n-hexane and toluene; the removal method may be volatilization removal or removal under reduced pressure. Meanwhile, the amount of the solvent to be added may be selected by those skilled in the art according to actual needs, as long as the dispersion of PQD in the matrix material precursor solution can be assisted and the subsequent removal of the solvent is less burdensome.
Further, the matrix material precursor solution and the material containing PQD are mixed according to the mass ratio of the matrix material to the PQD of (1-10): 1, specifically 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, or 10: 1. The inventors found that if the mass ratio of the matrix material to PQD is too large, the prepared matrix-PQD scintillator film responds too poorly to high-energy photon irradiation; on the other hand, if the mass ratio of the host material to PQD is too small, a film layer having sufficient mechanical properties cannot be formed. Therefore, by adopting the mass ratio of the application, on one hand, the matrix-PQD scintillator film can have good mechanical properties; on the other hand, the response of the matrix-PQD scintillator film to irradiation with high-energy photons can be enhanced.
It should be noted that the specific type of the matrix material can be selected by those skilled in the art according to actual needs, for example, the matrix material includes at least one of silicone polymer, silicon oxide, glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin, alicyclic epoxy resin, isocyanate, two-component silicone containing silicone and siloxane, two-component inorganic silicone containing silicon oxide and auxiliaries, two-component epoxy resin containing epoxy curing agent and epoxy adhesive, and two-component polyurethane containing polyisocyanate and polyether alcohol. The matrix material that this application adopted has high visible light transmittance and medium refractive index after the solidification wherein, the luminousness is 60% ~ 100%, the refractive index is 1.3 ~ 1.6, if the luminousness crosses low then influences the efflux of scintillator visible light, reduce the work efficiency of device, in addition, the refractive index crosses low or too high and all can form the total reflection mirror surface with visible light detector, influence the collection of visible light, the matrix material who adopts this application from this is favorable to the transmission of scintillator visible light and visible light detector to the collection of visible light.
Further, the chemical formula of PQD is ABX3Wherein A is cesium, methylamine or formamidine, B is lead or tin, and X is chlorine, bromine or iodine. The method for producing PQD is not particularly limited, and those skilled in the art can select the method according to actual needs, and for example, PQD can be produced by methods such as an oil phase hot-injection method, a room temperature ligand-assisted precipitation method, an ultrasonic method, a microwave method, a solvothermal method, and a sintering method. Meanwhile, the PQD is PQD modified by a surface ligand modification method or a PQD modified by a core-shell structure method or organic polymer-coated PQD, PQD coated by a metal organic framework, PQD coated by a metal oxide, and PQD coated by a microporous material, and the surface ligand modification method, the modification method, and the surface coating method performed on PQD are conventional technical means in the art, and are not described herein again.
Further, referring to fig. 2, in this step, the above-mentioned matrix material precursor solution is mixed with a material containing PQD and an auxiliary agent, wherein the auxiliary agent includes at least one of a plasticizer, a leveling agent, an anti-aging agent, an antioxidant, and a crosslinking agent. The inventor finds that the addition of the auxiliary agent can improve the mechanical property of the matrix-PQD scintillator film, and improve the light emitting effect and the service life of the PQD scintillator. It should be noted that the mixing ratio of the matrix material precursor solution, PQD and each auxiliary agent and the specific type of each auxiliary agent are conventional technical means in the art, and are not described herein again.
S200: injecting the matrix-PQD precursor solution into a mold, defoaming and curing
In the step, the matrix-PQD scintillator film is obtained by injecting the matrix-PQD precursor liquid into a mold, then defoaming for 25-35 min, preferably 30min, then curing, carrying out in-situ polymerization/reaction on the matrix material precursor liquid loaded with PQD, carrying out in-situ initiated curing to form a film, then demoulding and edge cleaning. Preferably, the defoaming process is vacuum defoaming in a vacuum oven. It should be noted that, the skilled person can select the specific type and curing manner of the mold material according to the actual needs, for example, the mold material includes at least one of stainless steel, teflon plastic, glass and ceramic; the curing mode can be UV light curing, thermal curing or room temperature curing.
The inventors have found that a substrate-PQD precursor solution can be obtained by mixing a substrate material precursor solution with a material containing PQD; and injecting the substrate-PQD precursor solution into a mold, defoaming, curing, carrying out in-situ polymerization/reaction on the PQD-loaded substrate material precursor solution, and carrying out in-situ initiation curing to form a film so as to obtain the substrate-PQD scintillator film. The method of the present application for preparing PQD scintillator films has the following advantages over the prior art: (1) the substrate material is used for coating the PQD, so that water vapor can be isolated, the water oxygen barrier property is improved, the water oxygen tight packaging is not required to be blocked, and the stability of the PQD is improved; (2) the use of a matrix material having a certain strength can solve the problem of poor mechanical properties of the PQD; (3) the film forming process assisted by the matrix material does not involve solvent volatilization, overcomes the problems of nonuniform film layer, local enrichment or cracking and the like in the process of preparing the PQD thick film by the traditional solution method, and has simple film forming process without special equipment or fine process; (4) the matrix material can help the PQDs to be separated from each other in space, so that the PQDs are prevented from generating obvious self-absorption effect due to mutual agglomeration, and the irradiation photon yield of the scintillator film layer can be improved; (5) the scintillator film layer which can be stretched and bent can be obtained by using a substrate material with certain flexibility and can be adapted to a flexible device; (6) the substrate-PQD scintillator film can be made into a device only by attaching the substrate-PQD scintillator film to the surface of the detector, the process is simple and convenient, and the substrate-PQD scintillator film can be easily replaced according to the requirement; (7) the matrix material that this application adopted has high visible light transmission and medium refractive index after the solidification, wherein, the luminousness is 60% ~ 100%, if the luminousness crosses low then influences the efflux of scintillator visible light, reduce the work efficiency of device, in addition, the refracting index crosses low or too high all can form the total reflection mirror surface with visible light detector, influences the collection of visible light, from this, adopt the matrix material of this application to be favorable to the seeing through of scintillator visible light and visible light detector to the collection of visible light.
In a second aspect of the invention, a host-PQD scintillator film is provided. According to an embodiment of the present invention, the matrix-PQD scintillator film is prepared by the above-described method for preparing a matrix-PQD scintillator film. Therefore, the substrate-PQD scintillator film does not need to be tightly packaged by blocking water and oxygen, has uniform thickness, smooth surface, uniform PQD distribution, good mechanical property and flexibility and higher irradiation photon yield, is beneficial to the visible light of the scintillator to be transmitted out and the visible light detector to collect the visible light, and is easy to remove and replace at the later stage.
The thickness of the matrix-PQD scintillator film is 0.1mm to 5mm, and specifically, may be 0.1mm, 0.5mm, 1.0mm, 1.5mm, 2.0mm, 2.5mm, 3.0mm, 3.5mm, 4.0mm, 4.5mm, or 5.0 mm. The inventors found that if the thickness of the matrix-PQD scintillator film is too small, sufficient mechanical strength cannot be secured; if the thickness is too large, the emission of visible light is affected, and the integration with the device is difficult. Therefore, by adopting the thickness of the application, on one hand, the matrix-PQD scintillator film can have good mechanical strength; on the other hand, the prepared high-energy photon detector has excellent response performance to high-energy photon irradiation and good integrity.
It should be noted that the features and advantages described above with respect to the method of preparing the matrix-PQD scintillator film are also applicable to the matrix-PQD scintillator film, and will not be described herein again.
In a third aspect of the invention, a high energy photon detection device is presented. According to an embodiment of the present invention, referring to fig. 3, the high-energy photon detection device includes a TFT array 100, a photodetector 200, and a scintillator film 300, wherein the scintillator film 300 is disposed on a surface of the photodetector 200, and the scintillator film 300 is the above-mentioned matrix-PQD scintillator film or the matrix-PQD scintillator film prepared by the above-mentioned method. Therefore, the high-energy photon detection device has good integrity and longer service life, has excellent response performance to high-energy photon irradiation, can absorb high-energy photons to prevent the high-energy photons from escaping to the environment, can be designed and manufactured into a flexible device capable of being bent in an extending way, can be manufactured into a device only by attaching the substrate-PQD scintillator film on the surface of the photodetector, and is easy to remove and replace the substrate-PQD scintillator film at the later stage according to the requirement. It should be noted that the features and advantages described above for the matrix-PQD scintillator film and the method for fabricating the same are also applicable to the high-energy photon detection device, and are not described herein again.
The following embodiments of the present invention are described in detail, and it should be noted that the following embodiments are exemplary only, and are not to be construed as limiting the present invention. In addition, all reagents used in the following examples are commercially available or can be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
Example 1
Step 1: weighing 10g of a commercial polyester resin-based UV curing adhesive precursor solution (the mass ratio of the matrix material to the PQD is 10: 1) in a beaker, and adding 10ml of CsPbBr3PQD dispersion (solvent n-hexane, concentration 100mg/ml, emission 530nm), mechanically stirring until fully mixed to obtain matrix-PQD precursor solution;
step 2: transferring the substrate-PQD precursor solution to a stainless steel mold, placing the stainless steel mold into a vacuum oven for vacuum defoamation for 30 minutes, transferring the stainless steel mold to a UV curing box, curing the substrate-PQD precursor solution for 30 minutes by using UV light with the wavelength of 365nm and the power of 400w to finish film layer curing, and then demolding and edge cleaning the scintillator film layer to obtain the substrate-PQD scintillator film with a smooth surface, uniform thickness and uniform PQD distribution. The X-ray excitation spectrum of the PQD scintillator in the obtained matrix-PQD scintillator film is shown in fig. 4, and it can be observed that the emission peak of the obtained PQD scintillator irradiation spectrum is about 530nm and the half-width is about 20nm when excited with 100kv X-ray.
And step 3: and attaching the substrate-PQD scintillator film layer to one side surface of the visible light detector (the other side surface of the visible light detector is provided with a TFT array) to manufacture the high-energy photon detection device.
Example 2
Step 1: 10g of a component A silicone prepolymer precursor solution of a commercially available AB-type silicone gum (mass ratio of A matrix material to PQD 5: 1) was weighed into a beaker, and 2g of CsPbI was added3PQD powder (emitting light of 680nm) is mechanically stirred and premixed, 1g B parts of siloxane precursor solution (the mass ratio of the B matrix material to the PQD is 0.5: 1) is added, and the mixture is fully and uniformly stirred to obtain matrix-PQD precursor solution;
step 2: transferring the substrate-PQD precursor solution to a polytetrafluoroethylene plastic mould, placing the polytetrafluoroethylene plastic mould into a vacuum oven for vacuum defoamation for 30 minutes, standing for 12 hours, completing solidification, and then demoulding and edge cleaning the scintillator film layer to obtain the substrate-PQD scintillator film with smooth surface, uniform thickness and uniform PQD distribution. The X-ray excitation spectrum of the PQD scintillator in the obtained matrix-PQD scintillator film is shown in fig. 5, and it can be observed that the emission peak of the obtained PQD scintillator irradiation spectrum is about 680nm and the half-peak width is about 38nm when the obtained PQD scintillator is excited by 100Kv X-ray;
and step 3: and attaching the substrate-PQD scintillator film layer to one side surface of the visible light detector (the other side surface of the visible light detector is provided with a TFT array) to manufacture the high-energy photon detection device.
Example 3
Step 1: 5g of A component polyether alcohol precursor solution (the mass ratio of A matrix material to PQD is 5: 1) of commercially available AB adhesive type polyurethane thermal curing adhesive is weighed in a beaker, and 10ml of FAPBI is added3Mixing PQD dispersion (solvent n-hexane, concentration 100mg/ml, emission light 780nm), mechanically stirring and premixing, adding 5g B components of polyisocyanate precursor solution (mass ratio of B matrix material to PQD is 5: 1), and stirring thoroughly to obtain matrix-PQD precursor solution;
step 2: transferring the substrate-PQD precursor solution to a glass surface dish, placing the glass surface dish into a vacuum oven for vacuum defoamation for 30 minutes, then placing the glass surface dish into the oven for curing at 70 ℃ for 2 hours to finish curing, and then demolding and edge cleaning the scintillator film layer to obtain the substrate-PQD scintillator film with smooth surface, uniform thickness and uniform PQD distribution. The X-ray excitation spectrum of the PQD scintillator in the obtained matrix-PQD scintillator film is shown in fig. 6, and it can be observed that the emission peak of the obtained PQD scintillator irradiation spectrum is about 780nm and the half-peak width is about 50nm when the obtained PQD scintillator is excited by 100Kv X-ray;
and step 3: and attaching the substrate-PQD scintillator film layer to one side surface of the visible light detector (the other side surface of the visible light detector is provided with a TFT array) to manufacture the high-energy photon detection device.
Example 4
Step 1: 10g of commercially available glycidyl ether epoxy resin-based UV curing adhesive precursor solution (mass ratio of matrix material to PQD is 10: 1) is weighed in a beaker, and 10ml of CsPb (ClBr) is added3PQD dispersion (solvent toluene, concentration 100mg/ml, emission 470nm), mechanically stirring until well mixed to obtain matrix-PQD precursor;
step 2: and transferring the substrate-PQD precursor solution to a ceramic mold, placing the ceramic mold in a vacuum oven for vacuum defoamation for 30 minutes, transferring the ceramic mold to a UV curing box, curing the ceramic mold for 30 minutes by using UV light with 365nm wavelength and 400w power to complete film layer curing, and then demolding and edge cleaning the scintillator film layer to obtain the substrate-PQD scintillator film with smooth surface, uniform thickness and uniform PQD distribution. From the X-ray excitation spectrum of the PQD scintillator in the obtained matrix-PQD scintillator film, it was observed that the emission peak of the obtained PQD scintillator irradiation spectrum was about 470nm and the half-width was about 12nm when excited with 100kv X-ray.
And step 3: and attaching the substrate-PQD scintillator film layer to one side surface of the visible light detector (the other side surface of the visible light detector is provided with a TFT array) to manufacture the high-energy photon detection device.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method of making a matrix-PQD scintillator film, comprising:
(1) mixing a substrate material precursor solution with a PQD-containing material to obtain a substrate-PQD precursor solution;
(2) and injecting the matrix-PQD precursor solution into a mold, defoaming, and curing to obtain the matrix-PQD scintillator film.
2. The method according to claim 1, wherein in step (1), the matrix material precursor solution and PQD are mixed in a mass ratio of matrix material to PQD of (1-10): 1, mixing.
3. The method according to claim 1 or 2, wherein the PQD-containing material is PQD dispersion or PQD powder in step (1).
4. The method according to claim 2, wherein in step (1), the matrix material comprises at least one of silicone polymer, silicon oxide, glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin, alicyclic epoxy resin, isocyanate, two-component silicone containing silicone and siloxane, two-component inorganic silicone containing silicon oxide and auxiliaries, two-component epoxy resin containing epoxy curing agent and epoxy binder, and two-component polyurethane containing polyisocyanate and polyether alcohol.
5. The method of claim 2, wherein the chemical formula of the PQD is ABX in step (1)3Wherein A is cesium, methylamine or formamidine, B is lead or tin, and X is chlorine, bromine or iodine.
6. The method according to claim 3, wherein in step (1), the matrix material precursor solution is mixed with the PQD dispersion and the solvent of the PQD dispersion is removed during the mixing.
7. The method according to claim 1, wherein in step (1), the PQD is surface ligand-modified PQD, core-shell structure method-modified PQD, organic polymer-coated PQD, metallorganic framework-coated PQD, metal oxide-coated PQD, microporous material-coated PQD.
8. The method of claim 1, wherein in step (1), the matrix material precursor solution is mixed with the PQD-containing material and an auxiliary agent, wherein the auxiliary agent comprises at least one of a plasticizer, a leveling agent, an anti-aging agent, an antioxidant, and a crosslinking agent.
9. A matrix-PQD scintillator film, which is produced by the method according to any one of claims 1 to 8;
optionally, the thickness of the matrix-PQD scintillator film is 0.1mm to 5 mm.
10. A high-energy photon detection device is characterized by comprising a TFT array, a light detector and a scintillator film layer, wherein the scintillator film layer is arranged on the surface of the light detector,
wherein the scintillator film layer is a matrix-PQD scintillator film obtained by the method according to any one of claims 1 to 8 or a matrix-PQD scintillator film according to claim 9.
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