Multi-dimensional gradient material high-flux additive preparation and ultrafast X-ray in-situ high-flux characterization method

Abstract

The invention provides a multi-dimensional gradient material high-flux preparation and in-situ high-flux characterization method. The method comprises the steps that powder raw materials with different components are prepared, the materials are constructed layer by layer through multi-channel powder feeding additive manufacturing equipment, and meanwhile melting, solidification, phase change and defect generation behaviors of the materials are monitored in real time through a synchrotron radiation ultrafast X-ray technology. The multi-channel powder feeding system and the synchrotron radiation ultrafast X-ray imaging and diffraction combined measurement technology are adopted, and complex behaviors of materials with different components can be monitored in real time. The prepared material has a predetermined component gradient and a microstructure, and the component gradient is achieved by adjusting the powder feeding rate of powder raw materials with different components and has the characteristic of continuous change in at least one dimension. The method provides an efficient material preparation and characterization means for the fields of material science and engineering.

Description

Technical Field

[0001] The present invention belongs to the technical field of preparation and characterization of multidimensional gradient materials, and relates to a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, and in particular to a method for high-throughput additive preparation and ultrafast X-ray in-situ high-throughput characterization of multidimensional gradient materials. Background Art

[0002] The development of materials plays an irreplaceable role in driving technological progress and improving industrial standards. For a long time, new materials research has often relied on a trial-and-error approach, employing a sequential, iterative process of first formulating hypotheses and then validating them to continually approach the target material. This inefficiency and high cost have become bottlenecks in new materials R&D. This approach not only consumes significant time and resources, but also often struggles to predict and explain the complex behavior of materials, leading to extended R&D cycles and increased costs.

[0003] In order to overcome these limitations, the field of materials science has begun to adopt high-throughput preparation and characterization technology. This technology accumulates a large amount of data in a short period of time through efficient parallel experiments, screens materials, and thus develops new materials with excellent performance. High-throughput preparation technologies mainly include the following: a. Thin film deposition technology based on vapor deposition (PVD): This technology can precisely control the growth of thin films at the atomic scale. By changing the deposition parameters (such as temperature, pressure, power, etc.), thin film materials with different compositions and structures can be prepared. b. Diffusion multi-node technology: By precisely controlling the diffusion process of different materials, gradient changes in composition and structure can be achieved at the microscopic scale, thereby preparing multi-dimensional gradient materials with continuous gradient changes. c. Laser additive manufacturing technology: Use a laser beam to melt powder and build materials layer by layer. By adjusting the laser parameters and powder feeding rate, gradient changes in material composition and structure can be achieved.

[0004] High-throughput material characterization techniques primarily include: a. Micro-area composition and structure characterization: Using instruments such as scanning electron microscopes (SEMs) and transmission electron microscopes (TEMs) to precisely analyze the microstructure and composition of materials. b. Micro-area optical property characterization: Using instruments such as spectrometers and photometers to characterize the optical properties of materials (such as absorption, emission, and scattering). c. Micro-area mechanical property characterization: Using instruments such as nanoindenters and atomic force microscopes (AFMs) to characterize the mechanical properties of materials (such as hardness and elastic modulus).

[0005] However, the high-throughput preparation and characterization techniques for these materials are all performed independently, requiring high-throughput preparation followed by high-throughput characterization. This results in long data acquisition cycles and limited data volumes, as well as the inability to capture key information such as the microstructural evolution of the material during preparation. This severely limits the application of high-throughput techniques in materials research and development.

[0006] Therefore, how to find a more suitable method to solve the shortcomings of existing technologies has become one of the urgent problems to be solved by many front-line researchers in the industry. Summary of the Invention

[0007] In view of this, the technical problem to be solved by the present invention is to provide a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, in particular, a method for high-throughput additive preparation and ultrafast X-ray in-situ high-throughput characterization of multidimensional gradient materials. The present invention aims to prepare multidimensional gradient materials with composition gradients by additive manufacturing technology, and to perform real-time in-situ characterization using synchrotron radiation ultrafast X-ray technology. The method includes preparing powder raw materials of different compositions, building the material layer by layer through a multi-channel powder feeding additive manufacturing device, and using synchrotron radiation ultrafast X-ray technology to monitor the melting, solidification, phase change and defect generation behavior of the material in real time.

[0008] The present invention provides a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, comprising the following steps:

[0009] 1) Providing powdered raw materials with different ingredients;

[0010] The powder includes single element powder and / or alloy powder;

[0011] 2) placing the powder raw materials into at least two independently controlled powder barrels of a multi-channel powder feeding additive manufacturing device;

[0012] Among them, each powder barrel corresponds to a powder raw material;

[0013] 3) According to the composition variation range of the multi-dimensional gradient material to be prepared, the speed variation range of the powder barrel is set through the computer control system to achieve gradient variation of the composition;

[0014] 4) Setting the device's lateral movement speed, range, and path, as well as its longitudinal movement distance, to form a three-dimensional structure, and referring to the set parameters, laser melting the powder and building the material layer by layer to produce a multidimensional gradient material;

[0015] During the preparation process, a synchrotron radiation ultrafast X-ray device is used to simultaneously perform real-time in-situ characterization of the state of one or more of the melting, solidification, phase change and defects of the material.

[0016] Preferably, the number of powder raw materials with different components is greater than or equal to two;

[0017] Each powder material has a different particle size distribution.

[0018] Preferably, the multi-channel powder feeding additive manufacturing device includes at least two independently controlled powder cylinders;

[0019] Each of the powder cartridges is equipped with a powder delivery rate control system.

[0020] Preferably, the multi-channel powder feeding system of the multi-channel powder feeding additive manufacturing device is specifically configured such that each channel is independently controlled and independently controlled in multiple directions simultaneously, so as to prepare multi-dimensional gradient materials with a composition gradient.

[0021] Preferably, the synchrotron radiation ultrafast X-ray device is specifically a synchrotron radiation ultrafast X-ray device with imaging and diffraction measurement functions;

[0022] The synchrotron radiation ultrafast X-ray device includes an X-ray source and a detector.

[0023] Preferably, the X-ray source is specifically an X-ray source having adjustable intensity and wavelength, capable of generating an X-ray beam for imaging and diffraction;

[0024] The detector is specifically a detector that has time resolution and spatial resolution and can receive and record signals after the X-ray beam interacts with the material.

[0025] Preferably, the real-time in-situ characterization includes data acquisition and processing steps.

[0026] Preferably, the data collection and processing steps specifically include:

[0027] Collect in-situ data obtained by synchrotron radiation ultrafast X-ray technology, including one or more of the following: melt pool morphology, temperature distribution, phase transformation process, and defect information;

[0028] The collected data is analyzed in real time to evaluate the microstructure and properties of the material, using algorithms and software for data processing.

[0029] Preferably, the composition gradient of the multi-dimensional gradient material is obtained by adjusting the powder feeding rate of powder raw materials with different compositions;

[0030] The composition gradient is specifically a composition gradient having a continuously changing characteristic in at least one dimension.

[0031] Preferably, the method further comprises step 5), evaluating the microstructure and performance of the material based on the results of the real-time in-situ characterization, and screening the material composition that meets the design requirements;

[0032] The method further includes adjusting parameters of the additive manufacturing device and repeating step 4) until a material composition that meets the design requirements is obtained.

[0033] The present invention provides a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, comprising the following steps: first, providing powder feedstocks of different compositions; the powders may include single element powders and / or alloy powders; then, placing the powder feedstocks into at least two independently controlled powder hoppers of a multi-channel powder feeding additive manufacturing device; wherein each powder hopper corresponds to a type of powder feedstock; then, according to the composition variation range of the desired multidimensional gradient material, the rotation speed variation range of the powder hoppers is set by a computer control system to achieve a gradient variation in composition; finally, the lateral movement speed, movement range, movement path, and longitudinal movement distance of the device are set to form a three-dimensional structure; and, referring to the set parameters, the powders are laser-melted and the material is constructed layer by layer to prepare the multidimensional gradient material; during the preparation process, a synchrotron radiation ultrafast X-ray device is simultaneously used to perform real-time in-situ characterization of the state of one or more of the melting, solidification, phase change, and defects of the material. Compared with the prior art, the present invention innovatively designs a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials with specific steps, providing a method for high-throughput additive preparation and in-situ ultrafast X-ray characterization of multidimensional gradient materials. The present invention prepares multidimensional gradient materials with composition gradients through additive manufacturing technology, and uses synchrotron radiation ultrafast X-ray technology for real-time in-situ characterization. The method includes preparing powder raw materials of different compositions, building the material layer by layer through a multi-channel powder feeding additive manufacturing device, and using synchrotron radiation ultrafast X-ray technology to monitor the melting, solidification, phase change and defect generation behavior of the material in real time. The device includes a multi-channel powder feeding system and synchrotron radiation ultrafast X-ray imaging and diffraction measurement technology, which can monitor the complex behavior of materials with different components in real time. The prepared material has a predetermined composition gradient and microstructure, and the composition gradient is achieved by adjusting the powder feeding rate of powder raw materials with different compositions, and has the characteristic of continuous change in at least one dimension. The method and device provide an efficient material preparation and characterization means for the field of materials science and engineering.

[0034] The high-throughput preparation and synchronous real-time in-situ characterization method provided by the present invention can achieve high-efficiency material preparation: through multi-channel powder feeding additive manufacturing equipment, multi-dimensional gradient materials with composition gradients can be prepared in parallel, which greatly shortens the material preparation time and improves the efficiency of material research and development; at the same time, precise composition control: the independent control function of each powder barrel enables the powder feeding rate of different powder raw materials to be accurately adjusted, thereby achieving continuous gradient changes in material composition in at least one dimension, providing a more precise control means for studying the relationship between material composition and performance; and real-time in-situ characterization: using synchrotron radiation ultrafast X-ray technology, the melting, solidification, phase change and defect generation behavior of the material can be characterized in real time in situ during the material preparation process, providing an in-depth understanding of the microscopic dynamic process of the material. High temporal and spatial resolutions are achieved: the high temporal and spatial resolutions of the synchrotron X-ray source and detector enable the capture of high-speed dynamic processes of changes in the microstructure of materials, providing reliable data support for the prediction and optimization of material properties; data collection and analysis are also possible: by collecting in-situ data obtained by synchrotron ultrafast X-ray technology, including melt pool morphology, temperature distribution, phase change process and defect information, the microstructure and properties of materials can be analyzed and evaluated in real time, and specific algorithms and software can be used for data processing, thereby accelerating the research and development of new materials; in addition, it also has an integrated device design: the device of this method includes a multi-channel powder feeding system and synchrotron ultrafast X-ray imaging and diffraction measurement technology, which realizes the integration of preparation and characterization processes, further shortens the data acquisition cycle, increases the amount of data, and can obtain key information of the material in the preparation process; and predetermined properties of the material: the multidimensional gradient material prepared by the method of the present invention has a predetermined composition gradient and microstructure, providing a customized material solution for specific applications.

[0035] By combining high-throughput additive manufacturing technology and ultrafast X-ray in-situ characterization technology, the present invention not only improves the efficiency of material preparation and characterization, but also provides a powerful tool for the field of materials science, which helps to accelerate the discovery and performance optimization of new materials, promote technological progress and improve industrial level. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 A schematic diagram of the process of synchrotron radiation ultrafast X-ray imaging and diffraction characterization provided by the present invention;

[0037] Figure 2 is the diffraction signal of the synchrotron radiation ultrafast X-ray in Example 1 of the present invention;

[0038] Figure 3 It is the imaging signal of the synchrotron radiation ultrafast X-ray in Example 1 of the present invention. DETAILED DESCRIPTION

[0039] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples. However, it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention rather than limiting the patent claims of the present invention.

[0040] All noun expressions and abbreviations in the present invention are conventional noun expressions and abbreviations in this field. Each noun expression and abbreviation is clear and unambiguous in its relevant application field. Those skilled in the art can clearly, accurately and uniquely understand them based on the noun expressions and abbreviations.

[0041] All raw materials of the present invention are not particularly limited in their sources and can be purchased from the market or prepared according to conventional methods well known to those skilled in the art.

[0042] There is no particular limitation on the purity of all raw materials in the present invention. The present invention preferably uses analytically pure materials or materials of conventional purity in the field of high-throughput additive manufacturing of multidimensional gradient materials.

[0043] The present invention provides a method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, comprising the following steps:

[0044] 1) Providing powdered raw materials with different ingredients;

[0045] The powder includes single element powder and / or alloy powder;

[0046] 2) placing the powder raw materials into at least two independently controlled powder barrels of a multi-channel powder feeding additive manufacturing device;

[0047] Among them, each powder barrel corresponds to a powder raw material;

[0048] 3) According to the composition variation range of the multi-dimensional gradient material to be prepared, the speed variation range of the powder barrel is set through the computer control system to achieve gradient variation of the composition;

[0049] 4) Setting the device's lateral movement speed, range, and path, as well as its longitudinal movement distance, to form a three-dimensional structure, and referring to the set parameters, laser melting the powder and building the material layer by layer to produce a multidimensional gradient material;

[0050] During the preparation process, a synchrotron radiation ultrafast X-ray device is used to simultaneously perform real-time in-situ characterization of the state of one or more of the melting, solidification, phase change and defects of the material.

[0051] The present invention first provides powder raw materials with different components;

[0052] In the present invention, the powder includes single element powder and / or alloy powder, and can be single element powder or alloy powder.

[0053] In the present invention, the number of the powder raw materials with different components is preferably greater than or equal to two.

[0054] In the present invention, each powder raw material preferably has a different particle size distribution.

[0055] The present invention then places the powder raw materials into at least two independently controlled powder barrels of a multi-channel powder feeding additive manufacturing device;

[0056] Among them, each powder barrel corresponds to a powder raw material.

[0057] In the present invention, the multi-channel powder feeding additive manufacturing device preferably includes at least two independently controlled powder cylinders.

[0058] In the present invention, each of the powder cartridges is preferably equipped with a powder delivery rate control system.

[0059] In the present invention, the multi-channel powder feeding system of the multi-channel powder feeding additive manufacturing device is preferably independently controlled in each channel and independently controlled in multiple directions at the same time, so as to prepare multi-dimensional gradient materials with composition gradients.

[0060] The present invention then sets the rotation speed variation range of the powder barrel through a computer control system according to the composition variation range of the multi-dimensional gradient material to be prepared, thereby achieving gradient variation of the composition.

[0061] Finally, the present invention sets the lateral movement speed, movement range and movement path of the device, as well as the longitudinal movement distance, to form a three-dimensional structure. Referring to the set parameters, the laser melts the powder and builds the material layer by layer to prepare a multi-dimensional gradient material.

[0062] During the preparation process, a synchrotron radiation ultrafast X-ray device is used to simultaneously perform real-time in-situ characterization of the state of one or more of the melting, solidification, phase change and defects of the material.

[0063] In the present invention, the synchrotron radiation ultrafast X-ray device is preferably a synchrotron radiation ultrafast X-ray device with imaging and diffraction combined measurement functions.

[0064] In the present invention, the synchrotron radiation ultrafast X-ray device preferably includes an X-ray source and a detector.

[0065] In the present invention, the X-ray source is preferably an X-ray source having adjustable intensity and wavelength and capable of generating X-ray beams for imaging and diffraction.

[0066] In the present invention, the detector is preferably a detector having time resolution and spatial resolution, and capable of receiving and recording signals after the X-ray beam interacts with the material.

[0067] In the present invention, the real-time in-situ characterization preferably includes data acquisition and processing steps.

[0068] In the present invention, the data collection and processing steps specifically include:

[0069] The in-situ data obtained by synchrotron radiation ultrafast X-ray technology are collected, preferably including one or more of the molten pool morphology, temperature distribution, phase change process and defect information, more preferably the molten pool morphology, temperature distribution, phase change process or defect information.

[0070] The collected data is analyzed in real time to evaluate the microstructure and properties of the material, using algorithms and software for data processing.

[0071] In the present invention, the composition gradient of the multi-dimensional gradient material is preferably obtained by adjusting the powder feeding rate of powder raw materials with different components.

[0072] In the present invention, the composition gradient is preferably a composition gradient having a continuously changing characteristic in at least one dimension.

[0073] In the present invention, the method further comprises a preferred step 5), evaluating the microstructure and performance of the material based on the results of the real-time in-situ characterization, and screening the material composition that meets the design requirements;

[0074] In the present invention, the method preferably further comprises adjusting parameters of the additive manufacturing device and repeating step 4) until a material composition meeting the design requirements is obtained.

[0075] The present invention is to complete and refine the overall technical solution, better ensure the structure and properties of multidimensional gradient materials, and further improve the efficiency and accuracy of the efficient preparation and characterization of multidimensional gradient materials. The above-mentioned high-throughput additive preparation of multidimensional gradient materials and ultrafast X-ray in-situ high-throughput characterization method can specifically include the following contents:

[0076] A method for high-throughput additive manufacturing of multi-dimensional gradient materials and ultrafast X-ray in-situ high-throughput characterization, the method comprising the following steps:

[0077] a. Prepare powder raw materials of different compositions, including pure element powders or alloy powders, each powder having a different chemical composition and / or particle size distribution;

[0078] b. placing the powder feedstock in at least two independently controlled powder hoppers of a multi-channel powder feeding additive manufacturing device, each hopper corresponding to a type of powder feedstock; each hopper is equipped with a precise powder delivery rate control system;

[0079] c. According to the composition variation range of the multi-dimensional gradient material to be prepared, the speed variation range of the powder barrel is set through the computer control system to achieve gradient variation of the composition;

[0080] d. Setting the lateral movement speed, movement range and movement path of the workbench, as well as the longitudinal movement distance, to form a three-dimensional structure;

[0081] e. Preparation of multidimensional gradient materials according to the set parameters, in which the laser melts the powder and builds the material layer by layer;

[0082] f. During the preparation process, synchrotron radiation ultrafast X-ray technology is used to perform real-time in-situ characterization of the material's melting, solidification, phase change, and defect generation behaviors.

[0083] Specifically, the multi-channel powder feeding additive manufacturing device includes at least two independently controlled powder cylinders, each of which is equipped with a precise powder delivery rate control system.

[0084] Specifically, the synchrotron radiation ultrafast X-ray technology includes imaging and diffraction joint measurement technology, specifically: a. X-ray source, used to generate X-ray beams for imaging and diffraction, with adjustable intensity and wavelength; b. detector, used to receive and record signals after the X-ray beam interacts with the material, with high temporal resolution and spatial resolution.

[0085] Specifically, the data acquisition and processing steps include: a. collecting in-situ data obtained by synchrotron radiation ultrafast X-ray technology, including but not limited to melt pool morphology, temperature distribution, phase change process and defect information; b. performing real-time analysis of the collected data to evaluate the microstructure and properties of the material, and using specific algorithms and software for data processing.

[0086] Specifically, the device of the method includes: a. a multi-channel powder feeding system for simultaneously preparing multidimensional gradient materials with composition gradients in multiple directions, with each channel independently controlled to achieve complex composition gradients; b. synchrotron radiation ultrafast X-ray imaging and diffraction joint measurement technology for real-time monitoring of the melting, solidification, phase change and defect generation behavior of materials with different components, including an X-ray source and a high-resolution detector.

[0087] The present invention also provides a multi-dimensional gradient material for high-throughput additive manufacturing, which is prepared by the method described in the above technical solution and has a predetermined composition gradient and microstructure.

[0088] Specifically, the composition gradient of the material is achieved by adjusting the powder feeding rate of powder raw materials with different compositions, and the composition gradient has the characteristic of continuous change in at least one dimension.

[0089] See also Figure 1, Figure 1 This is a schematic diagram of the process of synchrotron radiation ultrafast X-ray imaging and diffraction characterization provided by the present invention.

[0090] The above content of the present invention provides a method for high-throughput additive preparation of multidimensional gradient materials and ultrafast X-ray in-situ high-throughput characterization. The present invention prepares multidimensional gradient materials with composition gradients through additive manufacturing technology, and uses synchrotron radiation ultrafast X-ray technology for real-time in-situ characterization. The method includes preparing powder raw materials of different compositions, building the material layer by layer through a multi-channel powder feeding additive manufacturing device, and using synchrotron radiation ultrafast X-ray technology to monitor the melting, solidification, phase change and defect generation behavior of the material in real time. The device includes a multi-channel powder feeding system and synchrotron radiation ultrafast X-ray imaging and diffraction measurement technology, which can monitor the complex behavior of materials with different components in real time. The prepared material has a predetermined composition gradient and microstructure, and the composition gradient is achieved by adjusting the powder feeding rate of powder raw materials with different compositions, and has the characteristic of continuous change in at least one dimension. The method and device provide an efficient material preparation and characterization means for the field of materials science and engineering.

[0091] The high-throughput preparation and synchronous real-time in-situ characterization method provided by the present invention can achieve high-efficiency material preparation: through multi-channel powder feeding additive manufacturing equipment, multi-dimensional gradient materials with composition gradients can be prepared in parallel, which greatly shortens the material preparation time and improves the efficiency of material research and development; at the same time, precise composition control: the independent control function of each powder barrel enables the powder feeding rate of different powder raw materials to be accurately adjusted, thereby achieving continuous gradient changes in material composition in at least one dimension, providing a more precise control means for studying the relationship between material composition and performance; and real-time in-situ characterization: using synchrotron radiation ultrafast X-ray technology, the melting, solidification, phase change and defect generation behavior of the material can be characterized in real time in situ during the material preparation process, providing an in-depth understanding of the microscopic dynamic process of the material. High temporal and spatial resolutions are achieved: the high temporal and spatial resolutions of the synchrotron X-ray source and detector enable the capture of high-speed dynamic processes of changes in the microstructure of materials, providing reliable data support for the prediction and optimization of material properties; data collection and analysis are also possible: by collecting in-situ data obtained by synchrotron ultrafast X-ray technology, including melt pool morphology, temperature distribution, phase change process and defect information, the microstructure and properties of materials can be analyzed and evaluated in real time, and specific algorithms and software can be used for data processing, thereby accelerating the research and development of new materials; in addition, it also has an integrated device design: the device of this method includes a multi-channel powder feeding system and synchrotron ultrafast X-ray imaging and diffraction measurement technology, which realizes the integration of preparation and characterization processes, further shortens the data acquisition cycle, increases the amount of data, and can obtain key information of the material in the preparation process; and predetermined properties of the material: the multidimensional gradient material prepared by the method of the present invention has a predetermined composition gradient and microstructure, providing a customized material solution for specific applications.

[0092] By combining high-throughput additive manufacturing technology and ultrafast X-ray in-situ characterization technology, the present invention not only improves the efficiency of material preparation and characterization, but also provides a powerful tool for the field of materials science, which helps to accelerate the discovery and performance optimization of new materials, promote technological progress and improve industrial level.

[0093] In order to further illustrate the present invention, the following is a detailed description of a method for high-throughput preparation and in-situ high-throughput characterization of a multidimensional gradient material provided by the present invention in combination with the examples. However, it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided only to further illustrate the features and advantages of the present invention, rather than to limit the claims of the present invention. The scope of protection of the present invention is not limited to the following examples.

[0094] Example

[0095] A high-throughput additive manufacturing and ultrafast X-ray in-situ high-throughput characterization method for multi-dimensional gradient Nb-Ti-Zr-Hf-Ta high-entropy alloys.

[0096] (1) Raw material preparation. Five powder raw materials with different compositions were prepared, namely pure Nb, pure Ti, pure Zr, pure Hf and pure Ta powders. The powders were spherical or nearly spherical in shape, and had a particle size distribution between 20 μm and 100 μm.

[0097] (2) Additive manufacturing equipment setup. A multi-channel powder feeding additive manufacturing device was used. The device contained five independently controlled powder barrels, each corresponding to a different type of powder feedstock. The rotational speed of each barrel was set to vary between 0 and 1000 mm / min through a computer control system, while the sum of the rotational speeds of the five barrels was maintained at 1000 mm / min.

[0098] (3) Printing parameter settings. Set the workbench's horizontal movement speed to 600 mm / min; movement range to 0 mm to 20 mm; movement path to horizontal reciprocating movement; vertical movement mode to move down 0.3 mm after each layer is printed; and laser power to 1200 W.

[0099] (4) Material preparation. According to the set parameters, a multi-dimensional gradient Nb-Ti-Zr-Hf-Ta high entropy alloy was prepared, in which the powder was laser melted and the material was built layer by layer.

[0100] (5) In-situ characterization. During the preparation process, synchrotron radiation ultrafast X-ray technology is used to perform real-time in-situ characterization of the material's melting, solidification, phase change, and defect generation behaviors. The detector receives and records the signal after the X-ray beam interacts with the material.

[0101] (6) Data acquisition and processing. Collect in-situ data obtained by synchrotron ultrafast X-ray technology, including but not limited to melt pool morphology, phase transformation process, and defect information. Analyze the collected data to evaluate the microstructure and properties of materials with different compositions, and use specific algorithms and software for data processing.

[0102] (7) Result evaluation. Based on the results of the real-time analysis, evaluate the material's microstructure and properties and select the material composition that meets the design requirements. If necessary, adjust the parameters of the additive manufacturing equipment and repeat steps 4 to 6 until satisfactory results are obtained.

[0103] (8) Material performance testing. Further performance tests, such as hardness test and tensile test, were conducted on the optimized Nb-Ti-Zr-Hf-Ta high entropy alloy to verify its performance.

[0104] See also Figure 2 , Figure 2It is the diffraction signal of the synchrotron radiation ultrafast X-ray in Example 1 of the present invention.

[0105] See also Figure 3 , Figure 3 It is the imaging signal of the synchrotron radiation ultrafast X-ray in Example 1 of the present invention.

[0106] Through the above steps, multidimensional gradient Nb-Ti-Zr-Hf-Ta high-entropy alloys with predetermined composition gradients and microstructures can be efficiently prepared, and the performance of the materials can be monitored and evaluated in real time through ultrafast X-ray in situ high-throughput characterization technology.

[0107] The above describes in detail a method for high-throughput additive preparation and ultrafast X-ray in-situ high-throughput characterization of multidimensional gradient materials provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above examples is intended only to facilitate understanding of the method and its core concepts, including the best mode, of the present invention, and to enable any person skilled in the art to practice the present invention, including the manufacture and use of any device or system, and the implementation of any combined method. It should be noted that, without departing from the principles of the present invention, a person skilled in the art may make several improvements and modifications to the present invention, and such improvements and modifications fall within the scope of protection of the claims of the present invention. The scope of patent protection for the present invention is defined by the claims and may include other embodiments that can be conceived by those skilled in the art. If these other embodiments have structural elements that are not different from the literal language of the claims, or if they include equivalent structural elements that are not substantially different from the literal language of the claims, then these other embodiments are also intended to be included within the scope of the claims.

Claims

1. A method for high-throughput preparation and in-situ high-throughput characterization of multidimensional gradient materials, characterized in that: The following steps are involved: 1) Providing powdered raw materials with different ingredients; The powder includes single element powder and / or alloy powder; 2) placing the powder raw materials into at least two independently controlled powder barrels of a multi-channel powder feeding additive manufacturing device; Among them, each powder barrel corresponds to a powder raw material; 3) According to the composition variation range of the multi-dimensional gradient material to be prepared, the speed variation range of the powder barrel is set through the computer control system to achieve gradient variation of the composition; 4) Setting the device's lateral movement speed, range, and path, as well as its longitudinal movement distance, to form a three-dimensional structure, and referring to the set parameters, laser melting the powder and building the material layer by layer to produce a multidimensional gradient material; During the preparation process, a synchrotron radiation ultrafast X-ray device is used to simultaneously perform real-time in-situ characterization of the state of one or more of the melting, solidification, phase change and defects of the material.

2. The method according to claim 1, characterized in that The number of the powder raw materials with different components is greater than or equal to two; Each powder material has a different particle size distribution.

3. The method according to claim 1, characterized in that The multi-channel powder feeding additive manufacturing device includes at least two independently controlled powder cylinders; Each of the powder cartridges is equipped with a powder delivery rate control system.

4. The method according to claim 1, wherein The multi-channel powder feeding system of the multi-channel powder feeding additive manufacturing device is specifically characterized in that each channel is independently controlled and independently controlled in multiple directions at the same time, so as to be used for preparing multi-dimensional gradient materials with composition gradients.

5. The method according to claim 1, wherein The synchrotron radiation ultrafast X-ray device is specifically a synchrotron radiation ultrafast X-ray device with imaging and diffraction measurement functions; The synchrotron radiation ultrafast X-ray device includes an X-ray source and a detector.

6. The method according to claim 5, characterized in that The X-ray source is specifically an X-ray source having adjustable intensity and wavelength, capable of generating an X-ray beam for imaging and diffraction; The detector is specifically a detector that has time resolution and spatial resolution and can receive and record signals after the X-ray beam interacts with the material.

7. The method according to claim 1, characterized in that The real-time in-situ characterization includes data acquisition and processing steps.

8. The method according to claim 7, characterized in that The data collection and processing steps specifically include: Collect in-situ data obtained by synchrotron radiation ultrafast X-ray technology, including one or more of the following: melt pool morphology, temperature distribution, phase transformation process, and defect information; The collected data is analyzed in real time to evaluate the microstructure and properties of the material, using algorithms and software for data processing.

9. The method according to claim 1, characterized in that The composition gradient of the multi-dimensional gradient material is specifically obtained by adjusting the powder feeding rate of powder raw materials with different compositions; The composition gradient is specifically a composition gradient having a continuously changing characteristic in at least one dimension.

10. The method according to claim 1, characterized in that The method further comprises step 5), evaluating the microstructure and performance of the material based on the results of the real-time in-situ characterization, and screening the material composition that meets the design requirements; The method further includes adjusting parameters of the additive manufacturing device and repeating step 4) until a material composition that meets the design requirements is obtained.

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