Preparation method of perovskite thick film and x-ray flat panel detector

CN118450779BActive Publication Date: 2026-08-07SUN YAT SEN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
SUN YAT SEN UNIV
Filing Date
2024-05-14
Publication Date
2026-08-07

AI Technical Summary

Technical Problem

但是,浆料刮涂法得到钙钛矿厚膜存在孔隙多、内部不均匀的问题,且机械强度差,容易开裂或脱落

Benefits of technology

[0025] In summary, compared with the prior art, the beneficial effects of the technical solution provided in this application include at least the following: In the preparation process of the perovskite thick film, the vibration-assisted casting process enables the high-viscosity perovskite slurry to be uniformly distributed on the array pixel electrode substrate, forming a flat film layer. Simultaneously, it eliminates air bubbles and pores in the slurry, improving the density and uniformity of the perovskite thick film. Adding polymer monomers to the perovskite slurry allows for in-situ polymerization and cross-linking during the perovskite thick film annealing process, forming a three-dimensional network structure. This improves the mechanical strength of the perovskite thick film and simultaneously passivates grain boundary defects, reduces dark current, and enhances device stability. Furthermore, this preparation method is simple, adaptable to backplanes of different sizes, and easily scalable. When this perovskite thick film is applied to X-ray detectors, the high density and uniformity of the perovskite thick film effectively improves detection sensitivity and enhances device performance.

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Abstract

The application discloses a preparation method of a perovskite thick film and an X-ray flat panel detector. A polymer shielding film is covered on an array pixel electrode substrate except for a detection active area, so that the detection active area is exposed; an interface connecting layer is coated on the detection active area; a perovskite slurry containing a polymer monomer additive is prepared, and the perovskite slurry is cast on the detection active area coated with the interface connecting layer; the array pixel electrode substrate is transferred to a vibration table, and vibration is started, so that the perovskite slurry forms a perovskite thick film on the array pixel electrode substrate in the vibration process; the array pixel electrode substrate and the perovskite thick film after vibration are placed on a heating table, the perovskite thick film is dried by heating at a first temperature, and then the temperature is adjusted to a second temperature for heating, so that the polymer monomer in the perovskite thick film is polymerized and crosslinked, and a final perovskite thick film is formed. The compactness, uniformity and mechanical strength of the perovskite thick film can be effectively improved.
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Description

Technical Field

[0001] This application relates to the field of optoelectronic materials technology, and in particular to a method for preparing a perovskite thick film and an X-ray flat panel detector. Background Technology

[0002] Metal halide perovskite materials are considered promising new X-ray direct detection materials due to their large atomic numbers, good radiation resistance, excellent charge transport properties, and low preparation costs. In recent years, the performance of X-ray detectors based on lead halide perovskite single crystals has developed rapidly. However, preparing perovskite single crystals with sufficiently large areas is very difficult. Furthermore, the preparation of metal halide perovskite single crystals faces insurmountable bottlenecks such as difficulty in controlling crystal size, long preparation time, and difficulty in integrating single crystals with substrates. In contrast, perovskite polycrystalline films are easier to fabricate over large areas. In addition, a sufficiently thick perovskite absorption layer is required to ensure sufficient X-ray absorption, typically requiring a thickness of several hundred micrometers. Currently, slurry coating is commonly used to prepare thick perovskite films. However, slurry coating results in thick perovskite films with numerous pores, internal inhomogeneity, and poor mechanical strength, making them prone to cracking or detachment. These problems stem from the high viscosity and low fluidity of the perovskite slurry, making uniform slurry spreading impossible during the coating process. The aforementioned problems severely affect the sensitivity, resolution, and stability of X-ray flat panel detectors. Therefore, there is an urgent need to find a method for preparing uniform and stable perovskite thick films. Summary of the Invention

[0003] Therefore, embodiments of this application provide a method for preparing a perovskite thick film and an X-ray flat panel detector. The prepared perovskite thick film has higher density and uniformity, as well as better mechanical strength. When applied in X-ray detector devices, it can improve detection sensitivity and device performance.

[0004] In a first aspect, this application provides a method for preparing a perovskite thick film.

[0005] This application is achieved through the following technical solution:

[0006] A method for preparing a perovskite thick film, the method comprising:

[0007] A polymer masking film is applied to the area of ​​the array pixel electrode substrate other than the probe active area, exposing the probe active area.

[0008] An interface bonding layer is coated on the detection active area of ​​the array pixel electrode substrate;

[0009] A perovskite slurry containing polymer monomer additives is prepared, and the perovskite slurry is cast onto the interface bonding layer.

[0010] The array pixel electrode substrate and perovskite paste are transferred to a vibration table and vibration is turned on, so that the perovskite paste forms a thick perovskite film on the array pixel electrode substrate during the vibration process.

[0011] The vibrated array pixel electrode substrate and perovskite thick film are placed on a heating stage. The perovskite thick film is first heated to a first temperature to dry it, and then the temperature is adjusted to a second temperature to heat it to cause the polymer monomers in the perovskite thick film to polymerize and crosslink, forming the final perovskite thick film.

[0012] In a preferred embodiment of this application, the array pixel electrode substrate may be further configured to include any one of the following: hydrogenated amorphous silicon thin film transistor array substrate, metal oxide semiconductor transistor array substrate, indium gallium zinc oxide thin film transistor array substrate, area array electrode glass substrate, linear array electrode glass substrate, area array ITO electrode flexible PET substrate, or linear array ITO electrode flexible PET substrate.

[0013] In a preferred embodiment of this application, the polymer masking film may be further configured to include at least one of silicone rubber and polyimide film.

[0014] In a preferred embodiment of this application, the step of coating an interface connection layer on the detection active region of the array pixel electrode substrate may be further configured such that the thickness of the interface connection layer is 40 nm to 100 nm.

[0015] In a preferred embodiment of this application, the step of enabling vibration so that the perovskite paste forms a thick perovskite film on the array pixel electrode substrate during vibration can be further configured as follows:

[0016] The vibration frequency is set to 50Hz to 150Hz, and the vibration time is set to 1min to 10min.

[0017] In a preferred example of this application, the first temperature can be further set to 100°C and the second temperature to be 100°C to 150°C.

[0018] In a preferred embodiment of this application, the step of preparing the perovskite slurry containing polymer monomer additives may be further configured as follows:

[0019] Lead halide and amine halide, the precursor materials for perovskite, are dissolved in 2-methoxyethanol solvent in a stoichiometric ratio to form a precursor solution. The precursor solution is added dropwise to an antisolvent, causing perovskite microcrystals to precipitate. The precipitate is then filtered to obtain a precipitate. The precipitate is dried, ground, and sieved to obtain perovskite powder. The perovskite powder is then mixed with an organic solvent and a polymer monomer to obtain a perovskite slurry.

[0020] In a preferred embodiment of this application, the polymer monomer may be further configured to include one or more of 1,6-hexanediol diacrylate, octafluoro-1,6-hexanediol diacrylate, dimethylaminoethyl methacrylate, and ethoxylated trimethylolpropane triacrylate.

[0021] In a preferred embodiment of this application, the perovskite thick film may be further configured such that its chemical composition is MAPbI3 and FA. x MA 1-x PbI3, FA x Cs 1-x At least one of PbI3, MAPbBr3, and FAPbBr3, wherein 0 ≤ x ≤ 1.

[0022] Secondly, this application provides an X-ray flat panel detector.

[0023] This application is achieved through the following technical solution:

[0024] An X-ray flat panel detector, wherein the absorption layer of the X-ray flat panel detector is a perovskite thick film prepared by the preparation method described in the first aspect.

[0025] In summary, compared with the prior art, the beneficial effects of the technical solution provided in this application include at least the following: In the preparation process of the perovskite thick film, the vibration-assisted casting process enables the high-viscosity perovskite slurry to be uniformly distributed on the array pixel electrode substrate, forming a flat film layer. Simultaneously, it eliminates air bubbles and pores in the slurry, improving the density and uniformity of the perovskite thick film. Adding polymer monomers to the perovskite slurry allows for in-situ polymerization and cross-linking during the perovskite thick film annealing process, forming a three-dimensional network structure. This improves the mechanical strength of the perovskite thick film and simultaneously passivates grain boundary defects, reduces dark current, and enhances device stability. Furthermore, this preparation method is simple, adaptable to backplanes of different sizes, and easily scalable. When this perovskite thick film is applied to X-ray detectors, the high density and uniformity of the perovskite thick film effectively improves detection sensitivity and enhances device performance. Attached Figure Description

[0026] Figure 1 A schematic diagram of the structure of an X-ray flat panel detector provided in an exemplary embodiment of this application;

[0027] Figure 2 A scanning electron microscope image of the surface of a perovskite thick film provided as an exemplary embodiment of this application;

[0028] Figure 3 A cross-sectional scanning electron microscope image of a perovskite thick film provided for an exemplary embodiment of this application;

[0029] Figure 4 The X-ray response sensitivity of the X-ray flat panel detector provided as an exemplary embodiment of this application under different bias voltages.

[0030] Explanation of reference numerals in the attached figures:

[0031] Metal electrode layer-11, hole blocking layer-12, electron transport layer-13, perovskite thick film-14, hole transport layer-15, array pixel electrode-16, glass substrate-17. Detailed Implementation

[0032] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

[0033] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0034] Furthermore, the term "and / or" in this application is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. Additionally, the character " / " in this application, unless otherwise specified, generally indicates that the preceding and following related objects have an "or" relationship.

[0035] The embodiments of this application will now be described in further detail with reference to the accompanying drawings.

[0036] S1: A polymer masking film is applied to the area on the array pixel electrode substrate other than the probe active area, so that the probe active area is exposed.

[0037] The array pixel electrode substrate includes any one of the following: hydrogenated amorphous silicon thin-film transistor array (TFT) substrate, metal-oxide-semiconductor transistor array (CMOS) substrate, indium gallium zinc oxide thin-film transistor array (IGZO) substrate, area array electrode glass substrate, linear array electrode glass substrate, area array ITO electrode flexible PET substrate, or linear array ITO electrode flexible PET substrate. The size of the detection active area of ​​the array pixel electrode substrate is 15*15mm. 2 ~150*150mm 2A rectangular polymer masking film of a certain thickness is applied to the areas other than the active detection region. The center of the polymer masking film has a hollowed-out area, the area of ​​which is the same as the area of ​​the active detection region. The thickness of the polymer masking film is the same as the thickness of the perovskite thick film to be prepared. Covering the active detection region with a polymer masking film, while exposing the active region, helps ensure high-quality deposition of the subsequent perovskite thick film and improves the controllability and precision of the preparation process. Specifically, the polymer masking film includes at least one of polyimide film and silicone rubber.

[0038] S2: Apply an interface bonding layer to the detection active area of ​​the array pixel electrode substrate.

[0039] The interface bonding layer is made of a polymer that combines charge transport and adhesion properties, including at least one of poly[bis(4-phenyl)(4-butylphenyl)amine] (poly-TPD) and poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid (PEDOT:PSS). The polymer is prepared into a solution and then coated onto the active detection region using methods such as spin coating, drop coating, or spray coating. The thickness of the interface bonding layer is 40 nm to 100 nm. The thickness of the interface bonding layer can be 40 nm, 50 nm, 60 nm, 75 nm, 80 nm, 90 nm, or 100 nm, but is not limited to these values.

[0040] The interface bonding layer helps to strengthen the connection between the array pixel electrode substrate and the perovskite thick film. It ensures good contact between the two, reduces voids and defects at the interface, and thus improves the overall structural stability. Simultaneously, the interface bonding layer has charge transport capabilities, promoting efficient charge transfer at the interface junctions.

[0041] S3: Prepare a perovskite slurry containing polymer monomer additives, and cast the perovskite slurry onto the interface bonding layer.

[0042] After processing the array pixel electrode substrate, the perovskite paste is prepared. It should be noted that the preparation of the perovskite paste can be performed before or simultaneously with the processing of the array pixel electrode substrate.

[0043] Lead halide and amine halide, the precursor materials for perovskite, are dissolved in 2-methoxyethanol solvent at a dosage ratio to form a precursor solution. The precursor solution is added dropwise to an antisolvent, and perovskite microcrystals precipitate out. The precipitate is filtered to obtain the precipitate. The precipitate is dried, ground, and sieved to obtain perovskite powder. The perovskite powder is then mixed with organic solvent and polymer monomer to obtain a perovskite slurry.

[0044] Perovskite precursor materials (lead halide and amine halide salts) were dissolved in 2-methoxyethanol solvent in a stoichiometric ratio to form a precursor solution with a concentration greater than 2 mol / L. The precursor solution was then added dropwise to an antisolvent, precipitating perovskite microcrystals. Ethyl acetate could be used as the antisolvent, with a volume ratio of precursor solution to antisolvent of 1:40. The mixed solution was filtered to obtain the precipitate, which was then dried. The dried precipitate was ground and sieved (400 mesh) to obtain perovskite powder with a particle size of 10 μm–50 μm. The perovskite powder was further mixed with an organic solvent and polymer monomers to obtain a perovskite slurry. The perovskite slurry was then cast onto the interface bonding layer of the detection active region.

[0045] The perovskite precursor raw materials include any one of lead halide PbX2 (X = Cl, Br, I), MAX, or FAX. In MAX, MA represents methylammonium and X represents a halogen element; in FAX, FA represents formamidinium and X represents a halogen element. The polymer monomers include one or more of 1,6-hexanediol diacrylate, octafluoro-1,6-hexanediol diacrylate, dimethylaminoethyl methacrylate, and ethoxylated trimethylolpropane triacrylate. The organic solvents include one or more of butyrolactone, valerate, isopropanol, butanol, pentanol, hexanol, cyclohexanol, terpineol, and propylene glycol butyl ether.

[0046] S4: Transfer the array pixel electrode substrate and perovskite paste to the vibration table, turn on the vibration, so that the perovskite paste forms a thick perovskite film on the array pixel electrode substrate during the vibration process.

[0047] The array pixel electrode substrate and perovskite paste were transferred to a vibration table, and the vibration frequency and time were set. Vibration was then initiated. The vibration frequency was set to 50Hz–150Hz, and the vibration time to 1min–10min. During continuous vibration, the perovskite paste can level out, eliminating air bubbles and reducing voids in the final perovskite thick film, thus improving tap density and uniformity. Increased tap density represents increased perovskite material per unit volume, which helps enhance X-ray absorption and photoelectric conversion capabilities. Simultaneously, improved uniformity increases the detection efficiency of optoelectronic devices using this perovskite film.

[0048] S5: The vibrated array pixel electrode substrate and perovskite thick film are placed on a heating stage. The perovskite thick film is first heated to a first temperature to dry it, and then the temperature is adjusted to a second temperature to heat it to cause the polymer monomers in the perovskite thick film to polymerize and crosslink, forming the final perovskite thick film.

[0049] The first temperature is the drying temperature, set to 100℃, with a heating rate of 2℃ / min and a drying time of 1.0 h. The second temperature is the polymerization temperature of the polymer monomers in the perovskite slurry, set to 100℃ to 150℃. The second temperature is set according to the polymerization temperature of the polymer monomers. For example, the heating temperature for 1,6-hexanediol diacrylate, octafluoro-1,6-hexanediol diacrylate, and ethoxylated trimethylolpropane triacrylate is 150℃, and the heating time is 15 min; the heating temperature for dimethylaminoethyl methacrylate is 100℃, and the heating time is 1.0 h.

[0050] This application also provides an X-ray flat panel detector, wherein the absorption layer of the X-ray flat panel detector is a perovskite thick film prepared by the above-described preparation method. Further, an electron transport layer, a hole blocking layer, and a metal electrode layer are deposited on the perovskite thick film, while a glass substrate is disposed on the lower surface of the array pixel electrode substrate. Specifically, an electron transport layer C is deposited on the surface of the perovskite thick film. 60 Further in the electron transport layer C 60 A hole-blocking layer (BCP) is deposited on the surface of the electron transport layer, and a chromium electrode layer is then deposited on the surface of the BCP layer to obtain an X-ray flat panel detector. 60 The thickness of the layer is 30 nm, the hole blocking layer (BCP) is 10 nm, and the thickness of the chromium electrode layer is 60 nm.

[0051] Example 1:

[0052] A 200 μm thick polyimide film is adhered to the area outside the detection active region of the ITO glass substrate of the array pixel electrode. The area of ​​the detection active region is 15 mm². 2 ×15mm 2 A chlorobenzene solution of poly-TPD, an interface bonding layer material, was spin-coated onto the exposed active detection region at 2000 rpm for 40 seconds to form the interface bonding layer.

[0053] Preparation of perovskite slurry: Lead iodide (PbI₂), methylamine iodide (MAI), and formamidinium iodide (FAI) were dissolved in 2-methoxyethanol at a molar ratio of 2:1:1 to prepare a perovskite precursor solution with a concentration of 2.5 mol / L. Subsequently, a certain amount of the precursor solution was added dropwise to ethyl acetate under stirring to generate MA. 0.5 FA 0.5 PbI3 microcrystal precipitation, filtered to obtain MA 0.5 FA 0.5 PbI3 powder, after vacuum drying, is ground and sieved to obtain MA with uniform size. 0.5 FA 0.5 PbI3 powder; 10 mmol of MA 0.5 FA 0.5PbI3 powder was mixed with 1 mL of butyrolactone solvent and 50 μL of 1,6-hexanediol diacrylate and stirred until homogeneous to obtain MA. 0.5 FA 0.5 PbI3 slurry.

[0054] 0.1 g of MA was cast onto the detection active region coated with the interface bonding layer. 0.5 FA 0.5 The PbI3 paste was transferred to a vibration stage and vibrated for 5 minutes at a frequency of 50 Hz to spread the paste across the entire active detection area. The array pixel electrode substrate and perovskite paste were then transferred to a heating stage and dried at 100°C for 1 hour. The temperature was then increased to 150°C and held for 15 minutes. After heating, the temperature was reduced to room temperature at a rate of 10°C / min to form the MA. 0.5 FA 0.5 PbI3 perovskite thick film.

[0055] in MA 0.5 FA 0.5 A 30 nm thick electron transport layer C is sequentially deposited on the surface of the PbI3 perovskite thick film. 60 An X-ray flat panel detector is formed by a 10 nm thick BCP layer and a 60 nm thick chromium electrode layer. The structure of the X-ray flat panel detector is as follows: Figure 1 As shown, from top to bottom, the layers are: metal electrode layer 11, hole blocking layer 12, electron transport layer 13, perovskite thick film 14, hole transport layer 15, array pixel electrode 16, and glass substrate 17.

[0056] Example 2

[0057] A 200 μm thick polyimide film is adhered to the area outside the detection active region of the ITO glass substrate of the array pixel electrode. The area of ​​the detection active region is 15 mm². 2 ×15mm 2 A chlorobenzene solution of poly-TPD, the interface bonding layer material, was spin-coated onto the exposed active detection region at 2000 rpm for 40 seconds.

[0058] Preparation of perovskite slurry: Lead iodide (PbI₂), methylamine iodide (MAI), and formamidinium iodide (FAI) were dissolved in 2-methoxyethanol at a molar ratio of 2:1:1 to prepare a perovskite precursor solution with a concentration of 2.5 mol / L. Subsequently, a certain amount of the precursor solution was added dropwise to ethyl acetate under stirring to generate MA. 0.5 FA 0.5 PbI3 microcrystal precipitation, filtered to obtain MA 0.5 FA 0.5 PbI3 powder, after vacuum drying, is ground and sieved to obtain MA with uniform size. 0.5 FA0.5 PbI3 powder; 10 mmol of MA 0.5 FA 0.5 PbI3 powder was mixed with 1 mL of butyrolactone solvent and stirred until homogeneous to obtain MA. 0.5 FA 0.5 PbI3 slurry.

[0059] 0.1 g of MA was cast onto the detection active region coated with the interface bonding layer. 0.5 FA 0.5 The PbI3 paste was transferred to a vibration stage and vibrated for 5 minutes at a frequency of 50 Hz to spread the paste across the entire active detection area. The array pixel electrode substrate and perovskite paste were then transferred to a heating stage and dried at 100°C for 1 hour. The temperature was then increased to 150°C and held for 15 minutes. After heating, the temperature was reduced to room temperature at a rate of 10°C / min to form the MA. 0.5 FA 0.5 PbI3 perovskite thick film.

[0060] in MA 0.5 FA 0.5 A 30 nm thick electron transport layer C is sequentially deposited on the surface of the PbI3 perovskite thick film. 60 An X-ray flat panel detector is formed by a 10nm thick BCP layer and a 60nm thick chromium electrode layer.

[0061] The difference between Example 2 and Example 1 is that no polymer monomers were added in the preparation of the perovskite slurry in Example 2.

[0062] Example 3

[0063] A 200 μm thick polyimide film is adhered to the area outside the detection active region of the ITO glass substrate of the array pixel electrode. The area of ​​the detection active region is 15 mm². 2 ×15mm 2 A chlorobenzene solution of poly-TPD, the interface bonding layer material, was spin-coated onto the exposed active detection region at 2000 rpm for 40 seconds.

[0064] Preparation of perovskite slurry: Lead iodide (PbI₂), methylamine iodide (MAI), and formamidinium iodide (FAI) were dissolved in 2-methoxyethanol at a molar ratio of 2:1:1 to prepare a perovskite precursor solution with a concentration of 2.5 mol / L. Subsequently, a certain amount of the precursor solution was added dropwise to ethyl acetate under stirring to generate MA. 0.5 FA 0.5 PbI3 microcrystal precipitation, filtered to obtain MA 0.5 FA 0.5 PbI3 powder, after vacuum drying, is ground and sieved to obtain MA with uniform size.0.5 FA 0.5 PbI3 powder; 10 mmol of MA 0.5 FA 0.5 PbI3 powder was mixed with 1 mL of butyrolactone solvent and 50 μL of 1,6-hexanediol diacrylate and stirred until homogeneous to obtain MA. 0.5 FA 0.5 PbI3 slurry.

[0065] 0.1 g of MA was cast onto the detection active region coated with the interface bonding layer. 0.5 FA 0.5 The PbI3 paste was applied to the entire detection active area of ​​the array pixel electrode substrate using a glass rod and allowed to stand for 5 minutes. The array pixel electrode substrate and perovskite paste were then transferred to a heating stage and dried at 100°C for 1 hour. The temperature was then increased to 150°C and held for 15 minutes. After heating, the temperature was reduced to room temperature at a rate of 10°C / min to form the MA. 0.5 FA 0.5 PbI3 perovskite thick film.

[0066] in MA 0.5 FA 0.5 A 30 nm thick electron transport layer C is sequentially deposited on the surface of the PbI3 perovskite thick film. 60 An X-ray flat panel detector is formed by a 10nm thick BCP layer and a 60nm thick chromium electrode layer.

[0067] MA obtained in Example 1 0.5 FA 0.5 The PbI3 thick film did not crack, while the MA obtained in Example 2 0.5 FA 0.5 The PbI3 thick film developed surface cracks due to the absence of polymer monomers during perovskite slurry preparation, affecting film uniformity and stability; Example 3, without external vibration, yielded MA. 0.5 FA 0.5 The surface of the PbI3 thick film is relatively uneven and the uniformity is poor.

[0068] Figure 2 MA obtained in Example 1 0.5 FA 0.5 The surface scanning electron microscope image of the PbI3 thick film shows that the surface of the formed perovskite thick film is relatively smooth. Figure 3 MA obtained in Example 1 0.5 FA 0.5 A cross-sectional scanning electron microscope image of the PbI3 thick film shows that the thickness of the formed perovskite thick film is approximately 200 μm.

[0069] The X-ray response of the X-ray flat panel detector obtained in Example 1 was tested by varying the X-ray dose under different bias voltages. The results are as follows: Figure 4 As shown in Figure a, the detector's photocurrent increases significantly with increasing X-ray dose, exhibiting excellent X-ray response. Linear fitting of the device photocurrent under different doses yields the following results: Figure 4 As shown in b, the sensitivity of the X-ray flat panel detector is thus obtained as 11260 μC Gy. air -1 cm -2 .

[0070] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the above-described division of functional units and modules is used as an example. In practical applications, the above functions can be assigned to different functional units and modules as needed, that is, the internal structure of the system described in this application can be divided into different functional units or modules to complete all or part of the functions described above.

Claims

1. A method for preparing a perovskite thick film, characterized in that, The preparation method includes: A polymer masking film is applied to the area of ​​the array pixel electrode substrate other than the detection active area, so that the detection active area is exposed. The thickness of the polymer masking film is the same as the thickness of the perovskite thick film to be prepared. An interface connection layer is coated on the detection active region of the array pixel electrode substrate. The interface connection layer is a polymer that has both charge transport and bonding functions. A perovskite slurry containing polymer monomer additives is prepared, and the perovskite slurry is cast onto the interface bonding layer. The array pixel electrode substrate and perovskite paste are transferred to a vibration table and vibration is turned on, so that the perovskite paste forms a thick perovskite film on the array pixel electrode substrate during the vibration process. The vibrated array pixel electrode substrate and perovskite thick film are placed on a heating stage. The perovskite thick film is first heated to a first temperature to dry it, and then the temperature is adjusted to a second temperature to cause the polymer monomers in the perovskite thick film to polymerize and crosslink, forming the final perovskite thick film. The first temperature is 100°C and the second temperature is 100°C to 150°C.

2. The method for preparing perovskite thick films according to claim 1, characterized in that, The array pixel electrode substrate includes any one of the following: hydrogenated amorphous silicon thin film transistor array substrate, metal oxide semiconductor transistor array substrate, indium gallium zinc oxide thin film transistor array substrate, area array electrode glass substrate, linear array electrode glass substrate, area array ITO electrode flexible PET substrate, or linear array ITO electrode flexible PET substrate.

3. The method for preparing perovskite thick films according to claim 1, characterized in that, The polymer shielding film includes at least one of silicone rubber and polyimide film.

4. The method for preparing perovskite thick films according to claim 1, characterized in that, In the step of coating an interface connection layer on the detection active region of the array pixel electrode substrate: The thickness of the interface bonding layer is 40 nm to 100 nm.

5. The method for preparing perovskite thick films according to claim 1, characterized in that, In the step of activating vibration to form a thick perovskite film on the array pixel electrode substrate during vibration: The vibration frequency was set to 50 Hz to 150 Hz, and the vibration time was set to 1 min to 10 min.

6. The method for preparing perovskite thick films according to claim 1, characterized in that, The step of preparing the perovskite slurry containing polymer monomer additives is as follows: Lead halide and amine halide, perovskite precursor raw materials, are dissolved in 2-methoxyethanol solvent at a dosage ratio to form a precursor solution. The precursor solution is added dropwise to the antisolvent, and perovskite microcrystals are precipitated. The precipitate is filtered to obtain the precipitate. The precipitate is dried, ground, and sieved to obtain perovskite powder. The perovskite powder is then stirred and mixed with organic solvent and polymer monomer to obtain perovskite slurry.

7. The method for preparing perovskite thick films according to claim 6, characterized in that, The polymer monomers include one or more of 1,6-hexanediol diacrylate, octafluoro-1,6-hexanediol diacrylate, dimethylaminoethyl methacrylate, and ethoxylated trimethylolpropane triacrylate.

8. The method for preparing a perovskite thick film according to any one of claims 1 to 7, characterized in that, The chemical composition of the perovskite thick film is MAPbI3, FA x MA 1-x PbI3, FA x Cs 1-x At least one of PbI3, MAPbBr3, and FAPbBr3, wherein 0 ≤ x ≤ 1.

9. An X-ray flat panel detector, characterized in that, The absorption layer of the X-ray flat panel detector is a perovskite thick film prepared by the preparation method described in any one of claims 1 to 7.

Citation Information

Patent Citations

  • Preparation method of composite perovskite thick film X-ray detector

    CN117956812A