A method for preparing a large-area characteristic element filter plate and its application

Abstract

This application relates to the field of X-ray detection equipment technology, and particularly to a method for preparing a large-area characteristic element filter plate and its application. The method includes: mixing oxide powder containing filter elements, polyvinyl butyral, and a composite organic reagent to obtain a mixed slurry; wherein the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2≤3:1; ball milling the mixed slurry to obtain a ball-milled slurry; casting the ball-milled slurry to obtain an oxide film containing filter elements; and heat-treating the oxide film containing filter elements to obtain a large-area characteristic element filter plate. This method, by introducing polyvinyl butyral and a composite organic reagent into the oxide powder and organically combining it with ball milling and casting techniques, successfully achieves precise control over the forming thickness of the oxide film.

Description

Technical Field

[0001] This application relates to the field of X-ray detection equipment technology, and in particular to a method for preparing a large-area characteristic element filter plate and its application. Background Technology

[0002] In X-ray detection technology, effectively detecting multi-energy X-rays is an important research direction. X-ray filters, especially those based on the absorption edge of characteristic elements (K-sides), offer a significant avenue for this research. Existing technologies, by introducing characteristic element filters, enable X-ray detectors to more effectively distinguish X-rays of different energies, thereby improving the energy resolution of the detector. Furthermore, by adjusting the elemental composition and thickness of the filter, the energy resolution of the X-ray detector for specific energies can be enhanced or weakened, thus improving the contrast and clarity of the X-ray image. Based on the ability of characteristic element filters to identify and analyze the X-ray characteristics of different elements, the application areas of X-ray detectors can be further expanded, for example, by applying X-ray detectors with characteristic element filters in fields such as medical imaging, geological exploration, and materials science.

[0003] Currently, apart from malleable elemental metal filter plates which are relatively easy to fabricate, other element-specific filter plates are quite difficult to process. Due to the characteristics of X-rays, element-specific filter plates need to contain only the filtering element or only impurity elements with atomic numbers lower than the filtering element; otherwise, the absorption of multi-energy X-rays will be affected, failing to achieve the intended purpose of characteristic X-ray filtering. To address this challenge, oxides containing the filtering element can be used as raw materials for fabricating element-specific filter plates. However, these methods cannot precisely control the thickness of large-area element-specific filter plates, making it difficult for existing element-specific filter plates to meet the requirements for precise X-ray spectrum modulation.

[0004] The current methods for preparing specific element filter plates include: (1) dispersing oxide powder in a polymer organic solution and then producing it by spraying; (2) mixing oxide powder with an organic polymer and then molding it by hot pressing. Summary of the Invention

[0005] This application provides a method for preparing a large-area characteristic element filter plate and its application, in order to solve the following technical problem: how to improve the accuracy of the thickness of a large-area specific element filter plate during the preparation stage.

[0006] In a first aspect, this application provides a method for preparing a large-area feature element filter plate, the method comprising: An oxide powder containing a filtering element, polyvinyl butyral, and a composite organic reagent are mixed to obtain a mixed slurry; wherein the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2≤3:1; The mixed slurry is ball-milled to obtain a ball-milled slurry; The ball milled slurry was subjected to casting to obtain an oxide film containing filtering elements; The oxide film containing the filtering element is heat-treated to obtain a large-area feature element filter plate.

[0007] Optionally, the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2 = (2.5~3.0):1.

[0008] Optionally, the oxide powder may include at least one of the following: vanadium oxide, chromium oxide, manganese oxide, gallium oxide, strontium oxide, germanium oxide, yttrium oxide, ruthenium oxide, antimony oxide, tellurium oxide, lanthanum oxide, cerium oxide, gadolinium oxide, neodymium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, hafnium oxide, and bismuth oxide.

[0009] Optionally, the oxide powder containing the filtering element, polyvinyl butyral, and composite organic reagent are mixed to obtain a mixed slurry, including the following steps: The oxide powder containing the filtering element is mixed with polyvinyl butyral to obtain a mixed powder. The mixed powder and the composite organic reagent are mixed to obtain a mixed slurry; The mixed slurry is subjected to ultrasonic treatment to remove air bubbles.

[0010] Optionally, the composite organic reagent includes ethanol, ethyl acetate and polyethylene glycol, wherein the volume V1 of ethanol, the volume V2 of ethyl acetate and the volume V3 of polyethylene glycol satisfy the relationship: V1:V2:V3=(2.5~3.5):1:2.

[0011] Optionally, the ball mill rotation speed is ≥300 r / min, and the ball milling time is 64 h to 80 h.

[0012] Optionally, the step of casting the ball-milled slurry to obtain an oxide film containing filtering elements includes the following steps: The ball-milled slurry was subjected to casting to obtain a coarse oxide film containing filtering elements; The rough oxide film containing the filtering element is scraped flat to obtain an oxide film containing the filtering element.

[0013] Optionally, the thickness of the oxide film is 50 μm to 400 μm.

[0014] Optionally, the temperature of the heat treatment is 45℃ to 55℃.

[0015] Secondly, this application provides an X-ray detector comprising a large-area feature element filter plate prepared by the method described in the first aspect.

[0016] The technical solutions provided in this application have the following advantages compared with the prior art: This application provides a method for preparing a large-area feature element filter plate. The method involves mixing oxide powder and polyvinyl butyral. Due to the large number of long branches in polyvinyl butyral, it possesses good flexibility, a low glass transition temperature, high tensile strength, and high impact resistance. Furthermore, the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2≤3:1, ensuring that the oxide powder contains a sufficient amount of polyvinyl butyral. The aforementioned properties of the sufficient oxide powder can effectively improve the film layer formed by the oxide powder. The method improves the mechanical properties of polyvinyl butyral (PVB) powder. Furthermore, the addition of the composite organic reagent not only enhances the dispersion uniformity of the oxide powder in PPB powder but also improves the film-forming properties of both the oxide powder and PPB powder. Subsequently, ball milling further improves the dispersion and particle size of the oxide powder in the mixed slurry, enabling the oxide powder to form a large-area film. Finally, casting allows for the reaction between PPB powder and the composite organic reagent in the ball-milled slurry to form a large-area oxide film, and also allows for precise control of the oxide film's thickness, thus achieving precise control over the thickness of large-area element-specific filter plates. Therefore, this method, by introducing PPB powder and composite organic reagent components into the oxide powder, combined with ball milling and casting techniques, can precisely control the thickness of the oxide film. Attached Figure Description

[0017] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this application and, together with the description, serve to explain the principles of this application.

[0018] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1This is a schematic flowchart of a method for preparing a large-area feature element filter plate provided in an embodiment of this application; Figure 2 This application provides a detailed flowchart illustrating a method for preparing a large-area feature element filter plate. Figure 3 A schematic diagram of a large-area feature element filter plate obtained by a method for preparing a large-area feature element filter plate according to an embodiment of this application; Figure 4 An X-ray imaging result of the oxide film of the large-area feature element filter plate provided in Comparative Example 1 of this application; Figure 5 An X-ray imaging result of the oxide film of the large-area feature element filter plate provided in Embodiment 1 of this application; Figure 6 An X-ray imaging result of the oxide film of the large-area feature element filter plate provided in Embodiment 2 of this application; Figure 7 An enlarged view of the X-ray imaging results of the oxide thin film of the large-area feature element filter plate provided in Embodiment 1 of this application; Figure 8 Scanning electron microscope (SEM) image of a large-area feature element filter plate of a multilayer oxide thin film provided in Embodiment 1 of this application. Detailed Implementation

[0020] 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.

[0021] Various embodiments of this application may exist in the form of a range; it should be understood that the description in the form of a range is merely for convenience and brevity and should not be construed as a hard limitation on the scope of this application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within that range; for example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single numbers within the range, such as 1, 2, 3, 4, 5, and 6, regardless of the range; in addition, whenever a numerical range is indicated herein, it means including any referenced number (fraction or integer) within the indicated range.

[0022] In this document, terms such as “comprising” mean “including but not limited to”. Relational terms such as “first” and “second” are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. “And / or” describes the relationship between related objects, indicating that there can be three relationships, for example, A and / or B can mean: A alone, A and B simultaneously, or B alone; where A and B can be singular or plural. “At least one” means one or more, “more” means two or more; “at least one,” “at least one of the following,” or similar expressions refer to any combination of these items, including any combination of single or plural items; for example, “at least one of a, b, or c,” or “at least one of a, b, and c,” can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple. "Parts representation" such as parts by weight or parts by mass indicates the proportional relationship between components. In the proportional relationships discussed in this article, the parameters that need to be described by proportion should be understood as the first term of the proportion in the order of description, and the proportion figures should be understood as the second term of the proportion. For example, if the mass ratio of substance A, substance B, and substance C is 1:2:3, then substances A, B, and C should correspond one-to-one with the proportion figures in the proportion in the order of description, that is, the mass of substance A: the mass of substance B: the mass of substance C = 1:2:3.

[0023] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this article can be purchased from the market or prepared by existing methods.

[0024] It should be noted that, regarding the prior art (1) described in the background art, the inventors have found that the disadvantages of this method are: dust pollution from the coating, high coating consumption, low utilization rate, harm to human health and the environment, and potential explosions and fires caused by the accumulation of organic solvent vapors to a certain extent under poor ventilation conditions. In addition, the success rate of this method is extremely low and the requirements for the spraying process are extremely high, requiring experienced engineers to spray a relatively smooth and uniform film, and the thickness of the film layer is uncontrollable. Regarding the prior art (2) described in the background art, the inventors have found that the particle size of the matrix material - metal oxide powder - obtained by this method is generally 300 mesh, which is relatively coarse. This makes the filter obtained by this method often uneven and the effective thickness cannot be guaranteed. In the actual use stage, the X-ray detector will cause distortion of the detection signal due to the scattering and diffraction characteristics of uneven and coarse particles. In addition, the hot pressing stage of this method requires a mold, so in the case of preparing large-area filters, a specific mold needs to be designed, and the mold opening cost is relatively large.

[0025] As the applications of X-ray detectors require precise modulation of the X-ray spectrum, this necessitates accurate control of the filter plate thickness. Therefore, there is an urgent need for more precise thickness control methods to meet this requirement.

[0026] Figure 1 An exemplary schematic diagram of a method for preparing a large-area feature element filter plate according to an embodiment of this application is shown; like Figure 1 As shown in the embodiment of this application, a method for preparing a large-area feature element filter plate is provided, the method comprising: S1. Mix oxide powder containing filtering elements, polyvinyl butyral, and composite organic reagent to obtain a mixed slurry; wherein the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2≤3:1; S2. The mixed slurry is ball-milled to obtain a ball-milled slurry; S3. The ball-milled slurry is subjected to casting treatment to obtain an oxide film containing filtering elements; S4. The oxide film containing the filtering element is subjected to heat treatment to obtain a large-area feature element filter plate.

[0027] It should be noted that polyvinyl butyral (PVB) is a product obtained by the condensation of polyvinyl alcohol and butyraldehyde under acid solvent catalysis. This results in the polyvinyl butyral molecule having a long branched chain, which gives it good flexibility, a low glass transition temperature, high tensile strength, and high impact strength.

[0028] It should be noted that the ball milling can be carried out inside a ball mill; the casting process can be carried out inside a casting machine tank.

[0029] It should be noted that this large-area feature element filter board can be cut according to actual needs to meet the requirements of large-area feature element filter board use.

[0030] It should be noted that the embodiments of this application provide a method for preparing a large-area characteristic element filter plate, which has unique innovation and significant advantages in the fields of materials science and fabrication processes. Specifically: In the initial stage of this method, the oxide powder and polyvinyl butyral are carefully mixed. Polyvinyl butyral, as a high-performance polymer, contains a large number of long branches in its molecular structure. It is the presence of these long branches that endows polyvinyl butyral with many excellent properties. For example, its good flexibility allows it to interact and blend better with other materials; its low glass transition temperature allows it to exhibit a relatively ideal processing state at relatively low temperatures; its high tensile strength ensures that the final product is not easily broken when subjected to external tensile forces; and its high impact strength enhances the product's resistance to external impacts.

[0031] During the mixing process, a strict ratio exists between the mass of the oxide powder (m1) and the mass of polyvinyl butyral (m2), i.e., m1:m2 ≤ 3:1. This ratio is crucial, ensuring that the oxide powder contains a sufficient amount of polyvinyl butyral. This sufficient amount of polyvinyl butyral, combined with the oxide powder, allows it to fully utilize its properties, effectively improving the mechanical properties of the film formed by the oxide powder. For example, when the film is subjected to external forces, the high tensile strength and impact resistance of polyvinyl butyral can work synergistically with the oxide powder to resist damage, thereby enhancing the overall stability and durability of the film.

[0032] Furthermore, the addition of composite organic reagents is another crucial step in this method. The role of these composite organic reagents is not only reflected in improving the uniformity of oxide powder dispersion in polyvinyl butyral. In the mixed system, the composite organic reagents effectively reduce the agglomeration of oxide powders, allowing them to be more uniformly dispersed within the polyvinyl butyral matrix, thus ensuring the consistency of the final film's performance. Simultaneously, the composite organic reagents also significantly improve the film-forming properties of both the oxide powder and polyvinyl butyral. They improve the interfacial compatibility between the oxide powder and polyvinyl butyral, enabling the oxide powder to better bond with polyvinyl butyral during film formation, resulting in a denser and more uniform film structure.

[0033] After mixing, the slurry is further processed using ball milling. During ball milling, the continuous impact and grinding action of the grinding balls further improves the dispersion of the oxide powder in the slurry. Through ball milling, potentially large agglomerates are broken down into smaller particles, resulting in a more uniform distribution of the oxide powder in the slurry. Simultaneously, ball milling effectively refines the particle size of the oxide powder. Smaller particle size helps the oxide powder to assemble more tightly in the subsequent film-forming process, thus facilitating the formation of large-area continuous films.

[0034] Finally, the casting process is a crucial step in the fabrication of large-area characteristic element filter plates. During casting, a series of physical and chemical reactions occur between the polyvinyl butyral and the composite organic reagents in the ball-milled slurry. These reactions result in a more stable bond between the two, enabling the formation of a large-area continuous oxide film. Furthermore, the casting process offers a significant advantage: precise control over the thickness of the oxide film. By accurately adjusting the parameters of the casting equipment, such as the casting speed and slurry concentration, precise control over the oxide film thickness can be achieved, thus meeting the stringent thickness accuracy requirements of large-area specific element filter plates.

[0035] In summary, the embodiments of this application provide a method for preparing a large-area feature element filter plate. This method successfully achieves precise control of the oxide film forming thickness by ingeniously introducing polyvinyl butyral and composite organic reagent components into the oxide powder and organically combining them with ball milling and casting technology. This provides an efficient and reliable technical solution for the preparation of large-area feature element filter plates.

[0036] In some alternative embodiments, the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2 = (2.5~3.0):1.

[0037] In these embodiments, the mass m1 of the oxide powder and the mass m2 of polyvinyl butyral can satisfy the relationship: m1:m2=(2.5~3.0):1, which further ensures that the oxide powder has a sufficient amount of polyvinyl butyral. The sufficient amount of oxide powder can effectively improve the mechanical properties of the film formed by the oxide powder, thereby improving the film-forming properties of the subsequent oxide powder and polyvinyl butyral.

[0038] The mass m1 of the oxide powder can be 2.5, 2.6, 2.7, 2.8, 2.9 or 3.0.

[0039] In some alternative embodiments, the oxide powder may be of at least one of the following types: vanadium oxide, chromium oxide, manganese oxide, gallium oxide, strontium oxide, germanium oxide, yttrium oxide, ruthenium oxide, antimony oxide, tellurium oxide, lanthanum oxide, cerium oxide, gadolinium oxide, neodymium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, hafnium oxide, and bismuth oxide.

[0040] In these embodiments, the oxide powder may include at least one of the following: vanadium oxide, chromium oxide, manganese oxide, gallium oxide, strontium oxide, germanium oxide, yttrium oxide, ruthenium oxide, antimony oxide, tellurium oxide, lanthanum oxide, cerium oxide, gadolinium oxide, neodymium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, hafnium oxide, and bismuth oxide, so that the oxide powder can include most types of oxide powders, making the selection of oxide powders broad, thereby improving the universality of the method.

[0041] Figure 2 A detailed flowchart illustrating a method for fabricating a large-area feature element filter plate according to an embodiment of this application is shown by way of example. In some alternative implementations, such as Figure 2 As shown, oxide powder containing filtering elements, polyvinyl butyral, and composite organic reagents are mixed to obtain a mixed slurry, including the following steps: S101. Mix oxide powder containing filtering elements with polyvinyl butyral to obtain a mixed powder; S102. The mixed powder and the composite organic reagent are mixed to obtain a mixed slurry; S103. The mixed slurry is subjected to ultrasonic treatment to remove air bubbles from the mixed slurry.

[0042] In these embodiments, the oxide powder and polyvinyl butyral are first mixed to ensure thorough mixing. Then, a composite organic reagent is added. Based on the functional characteristics of the composite organic reagent, the polyvinyl butyral and oxide powder can be thoroughly mixed. Finally, ultrasonic treatment is performed to remove air bubbles from the mixed slurry, thereby improving the uniformity of the oxide film obtained by subsequent casting processing, thus obtaining a large-area oxide film.

[0043] It should be noted that grinding balls can be added to the mixed slurry before the ultrasonic treatment stage, so that the air bubbles introduced by the grinding balls can be removed during the subsequent ultrasonic treatment process.

[0044] In some optional embodiments, the composite organic reagent includes ethanol, ethyl acetate and polyethylene glycol, wherein the volume V1 of ethanol, the volume V2 of ethyl acetate and the volume V3 of polyethylene glycol satisfy the relationship: V1:V2:V3 = (2.5~3.5):1:2.

[0045] In these embodiments, the composite organic reagent may include ethanol, ethyl acetate, and polyethylene glycol, and the volumes of ethanol V1, ethyl acetate V2, and polyethylene glycol V3 may satisfy the relationship: V1:V2:V3 = (2.5~3.5):1:2, so that the composite organic reagent contains sufficient amounts of ethanol, ethyl acetate, and polyethylene glycol. Sufficient amounts of ethanol and ethyl acetate can act as dispersants to fully disperse the oxide powder and polyvinyl butyral, and sufficient amounts of polyethylene glycol can act as binders to promote full bonding between the oxide powder and polyvinyl butyral, thereby improving the interaction effect between polyvinyl butyral and oxide powder, thus facilitating the subsequent casting process to obtain a large-area oxide film.

[0046] The volume V1 of the ethanol can be 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4 or 3.5.

[0047] It should be noted that polyacrylic acid can also be added to this composite organic reagent to enhance the film-forming properties between the oxide powder and polyvinyl butyral, thereby ultimately obtaining an oxide film that meets the requirements for thickness and mechanical properties.

[0048] In some optional embodiments, the ball mill rotates at a speed of ≥300 r / min, and the ball milling time is 64 h to 80 h.

[0049] In these embodiments, the ball milling speed can be 300 r / min, and the ball milling time can be 64 h to 80 h, so that the ball milling has sufficient speed and time. Ball milling with sufficient speed and time can break the oxide powder of the mixed slurry into fine particles, and at the same time, it can fully mix the other components of the mixed slurry evenly, so as to facilitate the subsequent casting process to obtain a large area oxide film.

[0050] It should be noted that the ball milling process can be as follows: after ball milling for a period of time, polyvinyl butyral or ethanol can be added to the mixed slurry to adjust the viscosity of the mixed slurry.

[0051] In some optional embodiments, the step of casting the ball-milled slurry to obtain an oxide film containing filtering elements includes the following steps: S301. The ball milling slurry is subjected to casting treatment to obtain a coarse oxide film containing filtering elements; S302. The rough oxide film containing the filtering element is scraped flat to obtain an oxide film containing the filtering element.

[0052] In these embodiments, the leveling process is performed simultaneously with the ball milling slurry casting process, and the leveling process can be performed according to the required oxide film thickness to obtain an oxide film that meets the thickness requirements.

[0053] In some alternative embodiments, the thickness of the oxide film is 50 μm to 400 μm.

[0054] In these embodiments, the thickness of the oxide film can be 50 μm to 400 μm, so that the oxide film has sufficient thickness to facilitate obtaining a large-area feature element filter plate with sufficient thickness after subsequent heat treatment.

[0055] The thickness of the oxide film can be 50 μm, 100 μm, 150 μm, 200 μm, 250 μm, 300 μm, 350 μm or 400 μm.

[0056] In some alternative embodiments, the heat treatment temperature is 45°C to 55°C.

[0057] In these embodiments, the heat treatment temperature can be 45°C to 55°C, so that the heat treatment has a sufficient temperature, and the heat treatment at a sufficient temperature can allow the oxide film to be fully heated to form a large-area feature element filter plate.

[0058] The heat treatment temperature can be 45℃, 46℃, 47℃, 48℃, 49℃, 50℃, 51℃, 52℃, 53℃, 54℃ or 55℃.

[0059] Based on a general inventive concept, embodiments of this application provide an X-ray detector, which includes a large-area feature element filter plate prepared by the method described above.

[0060] The X-ray detector is based on the above-described preparation method. The specific steps of the preparation method can be referred to the above embodiments. Since the X-ray detector adopts some or all of the technical solutions of the above embodiments, it has at least all the beneficial effects brought about by the technical solutions of the above embodiments, which will not be elaborated here.

[0061] The present application is further illustrated below with reference to specific embodiments. Experimental methods in the following embodiments that do not specify specific conditions are generally determined according to national / industry standards; if there is no corresponding national / industry standard, they are performed according to general international standards, conventional conditions, or conditions recommended by the manufacturer.

[0062] Example 1 like Figure 2 As shown, a method for preparing a large-area feature element filter plate includes: S101. Mix oxide powder containing filtering elements with polyvinyl butyral to obtain mixed powder; wherein the mass m1 of oxide powder and the mass m2 of polyvinyl butyral satisfy the relationship: m1:m2=3.0:1; S102. Mix the mixed powder and the composite organic reagent to obtain a mixed slurry; S103. The mixed slurry is subjected to ultrasonic treatment to remove air bubbles; S2. The mixed slurry is ball-milled to obtain a ball-milled slurry; S301. The ball-milled slurry is subjected to casting treatment to obtain a coarse oxide film containing filtering elements; S302. The rough oxide film containing the filtering element is scraped flat, and the height of the scraper from the worktable is set to 150μm to obtain the oxide film containing the filtering element. S4. The oxide film containing the filtering element is heat-treated to obtain the following: Figure 3 The large-area feature element filter plate shown.

[0063] The type of oxide powder is gadolinium oxide.

[0064] The composite organic reagent includes ethanol, ethyl acetate and polyethylene glycol. The volumes of ethanol (V1), ethyl acetate (V2) and polyethylene glycol (V3) satisfy the relationship: V1:V2:V3=3.0:1:2.

[0065] The ball mill rotated at 300 r / min for 72 h.

[0066] The oxide film has a thickness of 100 μm.

[0067] The heat treatment temperature is 50℃.

[0068] Example 2 Compared to Example 1, the differences in this example are as follows, while the rest are the same: The oxide powder is lanthanum oxide.

[0069] Example 3 Compared to Example 1, the differences in this example are as follows, while the rest are the same: The mass m1 of the oxide powder and the mass m2 of polyvinyl butyral satisfy the relationship: m1:m2=2.5:1.

[0070] The volumes of ethanol (V1), ethyl acetate (V2), and polyethylene glycol (V3) satisfy the relationship: V1:V2:V3 = 2.5:1:2.

[0071] The ball mill rotated at 300 r / min for 66 h.

[0072] The oxide film has a thickness of 150 μm.

[0073] The heat treatment temperature is 45℃.

[0074] Example 4 Compared to Example 1, the differences in this example are as follows, while the rest are the same: The mass m1 of the oxide powder and the mass m2 of polyvinyl butyral satisfy the relationship: m1:m2=2.8:1.

[0075] The volumes of ethanol (V1), ethyl acetate (V2), and polyethylene glycol (V3) satisfy the relationship: V1:V2:V3 = 3.5:1:2.

[0076] The ball milling time was 76 hours.

[0077] The oxide film has a thickness of 300 μm.

[0078] The heat treatment temperature is 55℃.

[0079] Comparative Example 1 Based on the content disclosed in Example 1, the following modifications are made: Oxides without filtering elements are used directly with traditional filter boards.

[0080] Comparative Example 2 Based on the content disclosed in Example 1, the following modifications are made: No polyvinyl butyral is added.

[0081] Relevant experimental and effect data: 1. Product Morphology: The morphology of the large-area feature element filter plate obtained in Example 1 is as follows. Figure 3 As shown.

[0082] 2. Performance testing: (1) The oxide films of Comparative Example 1, Example 1 and Example 2 were collected, and their imaging results under specific X-rays were measured, such as... Figure 4 , Figure 5 and Figure 6 As shown. By Figure 4 , Figure 5 and Figure 6 As can be seen, the method for preparing a large-area characteristic element filter plate provided in this application embodiment has a high accuracy in measuring X-rays.

[0083] (2) The imaging results of the oxide thin film in Example 1 are as follows: Figure 7As shown, this indicates that the detection accuracy of the oxide film meets the application requirements.

[0084] (3) The oxide film of Example 1 was multilayered to obtain a large-area characteristic element filter plate, and its scanning electron microscope results are as follows. Figure 8 As shown.

[0085] Depend on Figure 8 As can be seen, the method for preparing a large-area feature element filter plate provided in this application embodiment is to successfully achieve precise control of the oxide film forming thickness by ingeniously introducing polyvinyl butyral and composite organic reagent components into the oxide powder and organically combining them with ball milling and casting technology.

[0086] 3. Product Performance Distribution: Large-area feature element filter plates from Examples 1 to 4, and Comparative Example 2, were adjusted within a geometric dimension of 20cm × 100cm. The effective thickness of the large-area feature element filter plates in each example and comparative example was measured to be precisely controllable within the range of 100μm to 1000μm. Simultaneously, different sized areas were randomly selected on the surface of each large-area feature element filter plate, and their effective thickness was measured and compared. The error rate of the effective thickness on the surface of the same large-area feature element filter plate was statistically analyzed, and the results are shown in Table 1. Error rate = (Effective thickness in a certain area - Average thickness of the large-area feature element filter plate) / Average thickness of the large-area feature element filter plate Table 1. Error rate of effective surface thickness for each embodiment and comparative example.

[0087] As shown in Table 1, the method for preparing a large-area feature element filter plate provided in this application introduces polyvinyl butyral and composite organic reagent components into the oxide powder, and combines them with ball milling and casting technology to successfully achieve precise control of the oxide film forming thickness, so that the error rate in any area of ​​the large-area feature element filter plate is within ±5%, which meets the actual use requirements.

[0088] Compared to Example 1, Comparative Example 2 did not use polyvinyl butyral, which made it difficult for the oxide film to be evenly distributed, resulting in an error rate that significantly exceeded the actual application requirement of ±5%.

[0089] In summary, the present application provides a method for preparing a large-area feature element filter plate. This method successfully achieves precise control over the thickness of the oxide film by ingeniously introducing polyvinyl butyral and composite organic reagents into the oxide powder and organically combining it with ball milling and casting technology. This provides an efficient and reliable technical solution for the preparation of large-area feature element filter plates.

[0090] In addition, this application provides a method for preparing a large-area feature element filter plate. This method involves mixing oxide powder, polyvinyl butyral, and composite organic reagents, and then preparing a large-area feature element filter plate with good uniformity and controllable thickness through a process similar to ceramic casting.

[0091] Furthermore, this application provides a method for preparing a large-area feature element filter plate, which reduces the particle size of the oxide powder through ball milling. Additionally, when a large-area filter plate is required, a casting machine can be used to extend the length of the oxide film to obtain a feature element filter plate with a larger area. Subsequently, a variable pressure thickness gauge can be used to control the thickness of the feature element filter plate to the micrometer level.

[0092] Furthermore, the embodiments of this application provide a method for preparing a large-area feature element filter plate. The error rate of the effective thickness of the large-area feature element filter plate obtained by this method is controlled within ±5%, which can ensure the practical application of the large-area feature element filter plate. In order to ensure the correct application of these feature element filter plates, a series of imaging experiments are conducted, and the gray value distribution and changes of the imaging object are observed by superimposing filter plates, which meets the actual use requirements.

[0093] The above description is merely a specific embodiment of this application, enabling those skilled in the art to understand or implement this application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this application. Therefore, this application is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed in this application.

Claims

1. A method for preparing a large-area feature element filter plate, the method comprising: An oxide powder containing a filtering element, polyvinyl butyral, and a composite organic reagent are mixed to obtain a mixed slurry; wherein the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2≤3:1; The mixed slurry is ball-milled to obtain a ball-milled slurry; The ball milled slurry was subjected to casting to obtain an oxide film containing filtering elements; The oxide film containing the filtering element is heat-treated to obtain a large-area feature element filter plate.

2. According to the method of claim 1, the mass m1 of the oxide powder and the mass m2 of the polyvinyl butyral satisfy the relationship: m1:m2 = (2.5~3.0):

1.

3. The method according to claim 1 or 2, wherein the oxide powder comprises at least one of the following: vanadium oxide, chromium oxide, manganese oxide, gallium oxide, strontium oxide, germanium oxide, yttrium oxide, ruthenium oxide, antimony oxide, tellurium oxide, lanthanum oxide, cerium oxide, gadolinium oxide, neodymium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, hafnium oxide, and bismuth oxide.

4. The method according to claim 1, comprising mixing oxide powder containing filtering elements, polyvinyl butyral, and composite organic reagent to obtain a mixed slurry, including the following steps: The oxide powder containing the filtering element is mixed with polyvinyl butyral to obtain a mixed powder. The mixed powder and the composite organic reagent are mixed to obtain a mixed slurry; The mixed slurry is subjected to ultrasonic treatment to remove air bubbles.

5. The method according to claim 1 or 4, wherein the composite organic reagent comprises ethanol, ethyl acetate and polyethylene glycol, and the volume V1 of ethanol, the volume V2 of ethyl acetate and the volume V3 of polyethylene glycol satisfy the relationship: V1:V2:V3=(2.5~3.5):1:

2.

6. The method according to claim 1, wherein the rotational speed of the ball mill is ≥300 r / min, and the ball milling time is 64 h to 80 h.

7. The method according to claim 1, wherein the step of casting the ball-milled slurry to obtain an oxide film containing filtering elements comprises the following steps: The ball-milled slurry was subjected to casting to obtain a coarse oxide film containing filtering elements; The rough oxide film containing the filtering element is scraped flat to obtain an oxide film containing the filtering element.

8. The method according to claim 7, wherein the thickness of the oxide film is 50 μm to 400 μm.

9. The method according to claim 1, wherein the heat treatment temperature is 45°C to 55°C.

10. An X-ray detector comprising a large-area feature element filter plate prepared by the method according to any one of claims 1 to 9.

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