Method for preparing high-performance planar detector by adjusting solvent components and material synthesis method
By adjusting the solvent composition and preparation method, the growth of perovskite film was optimized, the thermal stability and environmental stability problems of perovskite materials were solved, and the service life and response capability of perovskite X-ray detectors were improved.
Patent Information
- Application Number
- CN202510829368.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-20
- Publication Date
- 2025-09-19
AI Technical Summary
The thermal stability and environmental stability of perovskite materials affect the service life of the device, restricting the development of perovskite X-ray detectors. It is necessary to improve the X-ray response of the detector while increasing the service life of the device.
High-performance planar detectors were prepared by adjusting the solvent components, and FAPb0.99Bi0.01I3 perovskite materials were prepared in large quantities by wet ball milling. Perovskite slurry was prepared by different solvent component ratios, and perovskite film was prepared by doctor blade coating. The growth of perovskite film during annealing was optimized, and the quality and X-ray response of perovskite film were improved.
The X-ray response of perovskite film devices has been improved, and a simple large-scale preparation method for perovskite materials has been provided. The solvent selection is environmentally friendly, which improves the radiation response of the material devices.
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Figure CN120676843A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of X-ray detectors, and in particular to a method for preparing a high-performance planar detector and a material synthesis method by adjusting solvent components. Background Art
[0002] X-rays are short-wavelength electromagnetic waves with strong penetrating power. They can penetrate metal, human bones, wood and other objects. The penetrating power is closely related to the intensity of the X-rays and the density of the penetrated object. X-ray detectors are divided into direct X-ray detectors and indirect X-ray detectors. When X-rays hit a direct X-ray detector, electron-hole pairs are generated. Subsequently, under the action of an external electric field, the electrons and holes move to both ends to form a current. The current of each pixel is then read on the TFT backplane. After the current is amplified and transmitted, it is finally imaged through analog-to-digital conversion.
[0003] Perovskite X-ray detectors, as an emerging photodetector device, have excellent properties such as high carrier mobility, high sensitivity, long carrier lifetime, low dark current, and low detection limit. They are a promising X-ray detection material.
[0004] Perovskite X-ray detectors are primarily categorized into three types: single crystal devices, wafer devices, and planar devices. The fabrication process for planar detectors offers significant potential for optimization, and process optimization allows for further control of film quality, thickness, and density. Perovskite planar detectors hold great promise for rapid and stable X-ray imaging.
[0005] At present, the thermal stability and environmental stability of perovskite materials affect the service life of the device and restrict the development of perovskite X-ray detectors. Therefore, while improving the X-ray response of the detector, it is also very necessary to improve the service life of the device. This is a real problem that needs to be solved urgently. Summary of the Invention
[0006] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid blurring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.
[0007] 1. Technical problems to be solved:
[0008] In order to solve the above-mentioned problem that the thermal stability and environmental stability of current perovskite materials affect the service life of the device and restrict the development of perovskite X-ray detectors, it is very necessary to increase the service life of the device while improving the X-ray response of the detector. The present invention is proposed.
[0009] Therefore, the purpose of the present invention is to provide a method for preparing a high-performance planar detector and a material synthesis method by adjusting the solvent components, and to prepare FAPb in large quantities by wet ball milling. 0.99 Bi 0.01 The invention discloses a method for preparing an I3 perovskite material, wherein the prepared powder can show an excellent black phase α-FAPbI3, and then a 4.5M perovskite slurry is prepared by adding the perovskite powder into the slurry using different solvent component ratios, and the perovskite film is prepared by doctor blade coating. The selection of the solvent optimizes the growth of the perovskite film during annealing, improves the quality of the perovskite film, and promotes the improvement of the X-ray response of the perovskite film device. The invention provides a method for preparing the perovskite material, which is simple and easy to prepare in large quantities, and the selection of the solvent is environmentally friendly. At the same time, the adjustment of the solvent component can improve the radiation response of the material device.
[0010] 2. Technical solution:
[0011] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:
[0012] A high-performance planar detector is prepared by adjusting the solvent composition, including adjusting the solvent composition to prepare a slurry, scraping the resulting thick film, and vapor-depositing a metal electrode on the upper end of the perovskite thick film. The slurry synthesized by adjusting the solvent composition is composed of 2-methoxyethanol, acetonitrile, γ-valerolactone and N,N-dimethylformamide in different proportions. The device configuration of the synthesized slurry is a flat-panel detector.
[0013] As a preferred solution of the present invention for preparing a high-performance planar detector by adjusting the solvent composition, the metal electrode is a gold electrode, and the metal electrode of the perovskite film is plated by vacuum evaporation. When evaporating the electrode Au, the vacuum pressure of the instrument is set to 2×10 -4 Pa, the thickness of the gold electrode is 85nm, and the perovskite material is prepared:
[0014] S1: Preparation of bulk FAPb using wet ball milling 0.99 Bi 0.01 I3 perovskite materials;
[0015] S2: Preparation of perovskite slurry using acetonitrile solvent and 2-ME mixed solvent;
[0016] S3: Perovskite slurry was prepared using a mixed solvent of γ-valerolactone and 2-ME.
[0017] As a preferred embodiment of the present invention, a method for preparing a high-performance planar detector by adjusting the solvent composition comprises the following steps:
[0018] S1: Preparation of FAPb 0.99 Bi 0.01 I3 perovskite materials;
[0019] S2: The materials are mixed with different solvent components to prepare slurry;
[0020] S3: The slurry is scraped onto an ITO glass substrate, annealed, and a metal electrode is evaporated on the surface.
[0021] As a preferred embodiment of the present invention, the method for preparing a high-performance planar detector by adjusting the solvent composition is as follows: 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0022] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0023] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0024] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol as a solvent, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0025] S4: Place the ITO glass after the perovskite film is scraped on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0026] As a preferred embodiment of the present invention, the method for preparing a high-performance planar detector by adjusting the solvent composition is as follows: 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The synthesis method of the I3 planar detector comprises the following steps:
[0027] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0028] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0029] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and γ-valerolactone as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0030] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0031] As a preferred embodiment of the present invention's method for preparing a high-performance planar detector by adjusting solvent components, the solvents used are 2-methoxyethanol and γ-valerolactone in a ratio of 7:3 to prepare the slurry.
[0032] As a preferred embodiment of the present invention, the method for preparing a high-performance planar detector by adjusting the solvent composition is as follows: 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0033] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0034] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0035] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and acetonitrile as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0036] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0037] As a preferred embodiment of the present invention's method for preparing a high-performance planar detector by adjusting solvent components, the solvents used are 2-methoxyethanol and acetonitrile in a ratio of 7:3 to prepare the slurry.
[0038] As a preferred embodiment of the present invention, the method for preparing a high-performance planar detector by adjusting the solvent composition is as follows: 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0039] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0040] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0041] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and N,N-dimethylformamide as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0042] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0043] As a preferred embodiment of the present invention's method for preparing a high-performance planar detector by adjusting solvent components, the solvents used are 2-methoxyethanol:N,N-dimethylformamide in a ratio of 7:3 to synthesize the slurry.
[0044] 3.Beneficial effects:
[0045] Compared with the prior art, the present invention has the following beneficial effects:
[0046] This method prepares high-performance planar detectors and material synthesis by adjusting solvent components, and uses wet ball milling to prepare FAPb in large quantities. 0.99 Bi 0.01 A method for preparing I3 perovskite material, and the prepared powder can show an excellent black phase α-FAPbI3. Then, by using different solvent component ratios, perovskite powder is added thereto to prepare a 4.5M perovskite slurry, and the perovskite film is prepared by doctor blade coating. The choice of solvent optimizes the growth of the perovskite film during annealing, improves the quality of the perovskite film, and promotes the improvement of the X-ray response of the perovskite film device.
[0047] This method of preparing high-performance planar detectors and material synthesis by adjusting solvent components provides a simple preparation method for perovskite materials, which is easy to prepare in large quantities. The choice of solvent is environmentally friendly. At the same time, the adjustment of solvent components can improve the radiation response of material devices. BRIEF DESCRIPTION OF THE DRAWINGS
[0048] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be derived from these drawings without inventive effort. Among them:
[0049] Figure 1 Schematic diagram of an embodiment of a method for preparing a high-performance planar detector and material synthesis by adjusting solvent components of the present invention;
[0050] Figure 2 The present invention is a method for preparing a high-performance planar detector and a material synthesis method by adjusting the solvent composition to prepare the FAPb 0.99 Bi 0.01 Schematic diagram of electron microscopy testing of I3 perovskite powder;
[0051] Figure 3 A comparison diagram of the perovskite film of the present invention for preparing a high-performance planar detector by adjusting the solvent composition and the material synthesis method;
[0052] Figure 4 Schematic diagram of electrical performance testing of a perovskite X-ray detector using a material synthesis method and a high-performance planar detector prepared by adjusting solvent components according to the present invention;
[0053] Figure 5 Schematic diagram of optical performance testing of a perovskite X-ray detector using a material synthesis method and a high-performance planar detector prepared by adjusting solvent components according to the present invention;
[0054] Figure 6 A schematic diagram of the sensitivity of an X-ray detector device under different bias voltages in a method for preparing a high-performance planar detector and a material synthesis method by adjusting solvent components of the present invention;
[0055] Figure 7 The present invention is a method for preparing a high-performance planar detector and a material synthesis method by adjusting the solvent composition at a bias voltage of 15V, 253μGy air s -1 Schematic diagram of the dose rate under X-ray irradiation. DETAILED DESCRIPTION
[0056] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below with reference to the accompanying drawings.
[0057] The present invention is described in detail with reference to schematic diagrams. For ease of illustration, cross-sectional views illustrating device structures may be partially enlarged and not to scale when describing embodiments of the present invention. Furthermore, the schematic diagrams are merely illustrative and should not limit the scope of the present invention. Furthermore, in actual production, three-dimensional dimensions, including length, width, and depth, should be included.
[0058] The orientation or positional relationship indicated in the terms is based on the orientation or positional relationship shown in the drawings and is only for the convenience of describing the present invention and simplifying the description. It does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation. Therefore, it should not be understood as a limitation on the present invention.
[0059] The term "connection" should be understood broadly. For example, "connection" can mean fixed, detachable, or integral; mechanical or electrical; direct or indirect through an intermediary; or internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention.
[0060] The embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
[0061] The present invention provides a schematic diagram of the overall structure of an embodiment of a method for preparing a high-performance planar detector and material synthesis by adjusting solvent components, including:
[0062] See also Figure 1-Figure 7 In this embodiment, a method for preparing a high-performance planar detector and material synthesis by adjusting the solvent composition includes adjusting the solvent composition to prepare a slurry by scraping to obtain a thick film and vapor-depositing a metal electrode on the top of the perovskite thick film. The slurry synthesized by adjusting the solvent composition is composed of 2-methoxyethanol, acetonitrile, γ-valerolactone and N,N-dimethylformamide in different proportions, and the device configuration of the synthesized slurry is a flat-panel detector.
[0063] It is worth noting that in order to ensure the normal use of the metal electrode, specifically, the metal electrode is a gold electrode, and the metal electrode of the perovskite film is plated by vacuum evaporation. When evaporating the electrode Au, the vacuum pressure of the instrument is set to 2×10 -4 Pa, the thickness of the gold electrode is 85nm, and the perovskite material is prepared:
[0064] S1: Preparation of bulk FAPb using wet ball milling 0.99 Bi 0.01 I3 perovskite materials;
[0065] S2: Preparation of perovskite slurry using acetonitrile solvent and 2-ME mixed solvent;
[0066] S3: Perovskite slurry was prepared using a mixed solvent of γ-valerolactone and 2-ME.
[0067] Next, in order to prepare, specifically, the following steps are included:
[0068] S1: Preparation of FAPb 0.99 Bi 0.01 I3 perovskite materials;
[0069] S2: The materials are mixed with different solvent components to prepare slurry;
[0070] S3: The slurry is scraped onto an ITO glass substrate, annealed, and a metal electrode is evaporated on the surface.
[0071] At the same time, in order to achieve the preparation, specifically, FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0072] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0073] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0074] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol as a solvent, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0075] S4: Place the ITO glass after the perovskite film is scraped on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0076] Further, in order to continue to realize the preparation, specifically, FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The synthesis method of the I3 planar detector comprises the following steps:
[0077] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0078] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0079] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and γ-valerolactone as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0080] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0081] It is worth noting that, in order to continue to realize the preparation, specifically, the solvent 2-methoxyethanol:γ-valerolactone is used to synthesize the slurry in a ratio of 7:3.
[0082] Subsequently, in order to continue to achieve the preparation, specifically, FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0083] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0084] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0085] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and acetonitrile as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0086] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0087] Next, in order to ensure the preparation coordination, specifically, the solvent 2-methoxyethanol: acetonitrile was used in a ratio of 7:3 to synthesize the slurry.
[0088] Meanwhile, in order to continue the preparation, specifically, FAPb 0.99 Bi 0.01The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps:
[0089] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0090] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0091] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and N,N-dimethylformamide as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate.
[0092] S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
[0093] Finally, in order to ensure the ratio, specifically, the solvent 2-methoxyethanol:N,N-dimethylformamide was used in a ratio of 7:3 to synthesize the slurry.
[0094] Example 1:
[0095] A high-performance planar detector fabricated by adjusting solvent composition includes a conductive substrate, a thick perovskite film, and metal electrodes. The thick perovskite film is formed by doctor blade coating a slurry synthesized from a mixture of solvents including 2-methoxyethanol, γ-valerolactone, acetonitrile, and N,N-dimethylformamide. The device configuration of the synthesized slurry is a flat-panel detector.
[0096] As one of the preferred embodiments of the present invention, the metal electrode is a gold electrode or a copper electrode.
[0097] As one of the preferred embodiments of the present invention, the ratio of 2-methoxyethanol to γ-valerolactone is 7:3.
[0098] As one of the preferred embodiments of the present invention, the ratio of 2-methoxyethanol to acetonitrile is 7:3.
[0099] As one of the preferred embodiments of the present invention, the ratio of 2-methoxyethanol to N,N-dimethylformamide is 7:3.
[0100] As one of the preferred methods of the present invention, the synthetic slurry is scraped to form a 500 μm thick perovskite film, and the thick film is annealed on a heating table at 120° C.
[0101] The present invention also provides the above-mentioned synthesis method for preparing a high-performance planar detector by adjusting the solvent components, which comprises the following steps.
[0102] S1: Preparation of FAPb0.99Bi0.01I3 perovskite material by wet ball milling;
[0103] S2: Adjust different solvent components to synthesize perovskite slurry and apply it to prepare perovskite film;
[0104] S3: Evaporating metal electrodes on the surface of the perovskite film;
[0105] The device configuration of the material is a planar detection device. The synthesis method for preparing a high-performance planar detector by adjusting the solvent composition includes the following steps:
[0106] S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours;
[0107] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0108] S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol as solvent, and apply a 500 μm thick perovskite film on an ITO glass substrate;
[0109] S4: Place the ITO glass after the perovskite film is scraped on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0110] Furthermore, a perovskite slurry was synthesized by modifying the 2-methoxyethanol solvent with other solvents and then coated onto an ITO glass substrate to obtain a complete perovskite film. The device configuration of the material is a flat-panel detector. The preparation method of the perovskite X-ray flat-panel detector device includes the following steps:
[0111] S1: Formamidine iodide, bismuth iodide and lead iodide were placed in a ball mill, ball mill beads and ethyl acetate solvent were added, and the ball mill was started and operated at 600 r / min for 4 hours;
[0112] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0113] S3: Prepare a 4.5M slurry with a solvent ratio of 2-methoxyethanol:γ-valerolactone (7:3) and 2-methoxyethanol:acetonitrile (7:3), and then apply a 500 μm thick perovskite film on an ITO glass substrate.
[0114] S4: Place the ITO glass after the perovskite film is scraped on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0115] Furthermore, the metal electrode of the perovskite film was plated by vacuum evaporation. When evaporating the electrode Au, the vacuum pressure of the instrument was set to 2×10-4Pa, and the thickness of the gold electrode was 85nm.
[0116] See also Figure 1 The present invention prepares FAPb by scraping the mixed solvent synthetic slurry 0.99 Bi 0.01 I3 perovskite X-ray detector, FAPb prepared by wet ball milling 0.99 Bi 0.01 I3 perovskite powder, the perovskite powder material shows excellent α-FAPbI3 XRD peak, without doping excess lead iodide peak and δ-FAPbI3 yellow phase XRD peak.
[0117] See also Figure 2 , the prepared FAPb 0.99 Bi 0.01 I3 perovskite powder was subjected to electron microscope scanning test, and the perovskite powder material showed good size uniformity.
[0118] In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the following examples are given for illustration. It should be noted that the following examples do not limit the scope of protection claimed in the present invention.
[0119] Unless otherwise specified, the raw materials, reagents, or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.
[0120] Example 2:
[0121] Preparation of FAPb by blade coating of mixed solvent synthetic slurry 0.99 Bi 0.01 I3 perovskite X-ray detector;
[0122] S1: 1.2038 g of formamidine iodide (FAI), 0.0413 g of bismuth iodide (BiI3) and 3.1948 g of lead iodide (PbI2) were placed in a ball mill, 12 ball mill beads and 5 ml of ethyl acetate solvent were added, and the ball mill was started at a speed of 600 r / min and taken out after running for 4 hours;
[0123] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0124] S3: Weigh 0.8545g FAPb 0.99 Bi0.01 A 4.5M slurry of I3 material was prepared using 210 μl of 2-methoxyethanol and 90 μl of acetonitrile as solvents and stirred for 10 min. The ITO glass substrate was fixed at the bottom, and a scraper was set at a distance of 500 μm from the glass. The slurry was placed on the glass and scraped to obtain a wet perovskite film.
[0125] S4: Place the ITO glass with the wet perovskite film after the scraping process on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0126] S5: Vacuum evaporation was performed on the annealed perovskite film at a vacuum chamber pressure of 2×10 -4 Under the conditions of , an 85nm thick metal electrode was evaporated on the surface of the perovskite film.
[0127] Example 3:
[0128] Preparation of FAPb by blade coating of mixed solvent synthetic slurry 0.99 Bi 0.01 I3 perovskite X-ray detector;
[0129] S1: 1.2038 g of formamidine iodide (FAI), 0.0413 g of bismuth iodide (BiI3) and 3.1948 g of lead iodide (PbI2) were placed in a ball mill, 12 ball mill beads and 5 ml of ethyl acetate solvent were added, and the ball mill was started at a speed of 600 r / min and taken out after running for 4 hours;
[0130] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0131] S3: Weigh 0.8545g FAPb 0.99 Bi 0.01 A 4.5M slurry of I3 material was prepared using 210 μl of 2-methoxyethanol and 90 μl of γ-valerolactone as solvents and stirred for 10 minutes. The ITO glass substrate was fixed at the bottom, and a scraper was set at a distance of 500 μm from the glass. The slurry was placed on the glass and scraped to obtain a wet perovskite film.
[0132] S4: Place the ITO glass with the wet perovskite film after the scraping process on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0133] s5: Vacuum evaporation was used on the annealed perovskite film at a vacuum chamber pressure of 2×10 -4 Under the conditions of , an 85nm thick metal electrode was evaporated on the surface of the perovskite film.
[0134] Example 4:
[0135] Preparation of FAPb by blade coating of mixed solvent synthetic slurry 0.99 Bi 0.01 I3 perovskite X-ray detector;
[0136] S1: 1.2038 g of formamidine iodide (FAI), 0.0413 g of bismuth iodide (BiI3) and 3.1948 g of lead iodide (PbI2) were placed in a ball mill, 12 ball mill beads and 5 ml of ethyl acetate solvent were added, and the ball mill was started at a speed of 600 r / min and taken out after running for 4 hours;
[0137] S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material;
[0138] S3: Weigh 0.8545g FAPb 0.99 Bi 0.01 A 4.5M slurry of I3 material was prepared using 210 μl of 2-methoxyethanol and 90 μl of N,N-dimethylformamide as solvents and stirred for 10 minutes. The ITO glass substrate was fixed at the bottom, and a scraper was set at a distance of 500 μm from the glass. The slurry was placed on the glass and scraped to obtain a wet perovskite film.
[0139] S4: Place the ITO glass with the wet perovskite film after the scraping process on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
[0140] s5: Vacuum evaporation was used on the annealed perovskite film at a vacuum chamber pressure of 2×10 -4 Under the conditions of , an 85nm thick metal electrode was evaporated on the surface of the perovskite film.
[0141] Comparative Example:
[0142] Comparison of optical photos of perovskite films, see the attached Figure 3 :
[0143] The perovskite films obtained above were compared and the results are shown in the attached Figure 3 It can be seen that the thick film of the comparative example shows obvious unevenness after blade coating annealing, and this situation is significantly improved in the embodiment. However, small holes appear on the surface of the film during the annealing process. It can be seen that the uniformity and neatness of the perovskite film in the embodiment are relatively good.
[0144] The electrical and optical properties of the perovskite X-ray detectors prepared in the above embodiments and comparative examples were tested, and the results are shown in the attached figure. Figure 4 and attached Figure 5 shown.
[0145] Attachment Figure 3The following are time-current X-ray response graphs for the three detector devices, one for the example and the other for the comparative example. Under the same bias voltage and X-ray energy, the comparative example's X-ray response reaches 1 nA, the one for the example reaches 3 nA, and the one for the example reaches 6 nA. This demonstrates that the present invention not only reduces the dark current of X-ray detectors but also improves their X-ray responsiveness.
[0146] Attachment Figure 5 The ray response of the embodiment under different bias voltages and different X-ray doses is shown. It can be seen that the ray response increases with the increase of dose rate and voltage, reaching a maximum of about 60nA, far exceeding the ray response of the device in the comparative example.
[0147] Attachment Figure 6 The sensitivity of the X-ray detector device under different bias voltages is shown in the embodiment. As the voltage increases, the sensitivity of the device increases and reaches a maximum value of 1218 uc gy-1 cm-2 at 30 V.
[0148] Attachment Figure 7 For example, at a bias voltage of 15V, 253μGy air s -1 Under X-ray irradiation with a dose rate of , the device can maintain response unchanged for 1400s under unpackaged conditions, indicating that the process can maintain excellent stability of the device.
[0149] In addition, the circuits, electronic components and modules involved in the present invention are all existing technologies and can be fully implemented by those skilled in the art. Needless to say, the content protected by the present invention does not involve improvements to internal structures and methods.
[0150] Combine Figure 1-Figure 7 In this embodiment, a method for preparing a high-performance planar detector and material synthesis by adjusting the solvent components is provided. For specific use, please refer to any of the above embodiments.
[0151] Although the present invention has been described above with reference to embodiments, various modifications may be made thereto and equivalent components may be substituted without departing from the scope of the present invention. In particular, as long as there are no structural conflicts, the various features of the embodiments disclosed herein may be combined with each other in any manner, and the omission of an exhaustive description of such combinations in this specification is solely for the sake of space and resource conservation. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.
Claims
1. A method for preparing a high-performance planar detector by adjusting solvent components, characterized in that: The invention includes adjusting the solvent composition to prepare a thick film obtained by scraping the slurry and vapor-depositing a metal electrode on the upper end of the perovskite thick film. The slurry synthesized by adjusting the solvent composition is composed of 2-methoxyethanol, acetonitrile, γ-valerolactone and N,N-dimethylformamide in different proportions. The device configuration of the synthesized slurry is a flat-panel detection.
2. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 1, wherein: The metal electrode is a gold electrode, and the metal electrode of the perovskite film is plated by vacuum evaporation. When the electrode Au is evaporated, the vacuum pressure of the instrument is set to 2×10 -4 Pa, the thickness of the gold electrode is 85nm, and the perovskite material is prepared: S1: Preparation of bulk FAPb using wet ball milling 0.99 Bi 0.01 I3 perovskite materials; S2: Preparation of perovskite slurry using acetonitrile solvent and 2-ME mixed solvent; S3: Perovskite slurry was prepared using a mixed solvent of γ-valerolactone and 2-ME.
3. The method for preparing a high-performance planar detector by adjusting the solvent composition according to any one of claims 1 to 2, characterized in that: The following steps are involved: S1: Preparation of FAPb 0.99 Bi 0.01 I3 perovskite materials; S2: The materials are mixed with different solvent components to prepare slurry; S3: The slurry is scraped onto an ITO glass substrate, annealed, and a metal electrode is evaporated on the surface.
4. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 3, characterized in that: The FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps: S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours; S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material; S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol as a solvent, and apply a 500 μm thick perovskite film on an ITO glass substrate. S4: Place the ITO glass after the perovskite film is scraped on a heating table preheated to 120°C for annealing. After heating for 2 hours, turn off the heating table and cool for 1 hour.
5. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 4, characterized in that: The FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The synthesis method of the I3 planar detector comprises the following steps: S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours; S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material; S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and γ-valerolactone as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate. S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
6. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 5, characterized in that: The solvents used were 2-methoxyethanol and γ-valerolactone in a ratio of 7:3 to synthesize the slurry.
7. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 6, characterized in that: The FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps: S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours; S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material; S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and acetonitrile as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate by scraping. S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
8. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 7, characterized in that: The solvent used was 2-methoxyethanol:acetonitrile in a ratio of 7:3 to synthesize the slurry.
9. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 8, characterized in that: The FAPb 0.99 Bi 0.01 The I3 perovskite material was prepared by wet ball milling using ethyl acetate as solvent. The device configuration of the material is a planar detector. 0.99 Bi 0.01 The preparation method of the I3 planar detector comprises the following steps: S1: Place formamidine iodide, bismuth iodide and lead iodide into a ball mill, add ball mill beads and ethyl acetate solvent, start the ball mill, and run it at 600 r / min for 4 hours; S2: placing the perovskite material obtained after ball milling in an oven for 12 hours to obtain a dried material; S3: Prepare a 4.5M slurry of the material using 2-methoxyethanol and N,N-dimethylformamide as solvents, and apply a 500 μm thick perovskite film on an ITO glass substrate. S4: Place the ITO glass coated with the perovskite film on a preheated heating platform at 120°C for annealing. After heating for 2 hours, turn off the heating platform and cool for 1 hour.
10. The method for preparing a high-performance planar detector by adjusting solvent components according to claim 9, characterized in that: The solvent used was 2-methoxyethanol:N,N-dimethylformamide in a ratio of 7:3 to synthesize the slurry.