In-situ high-temperature X-ray coupling system

Abstract

The invention discloses an in-situ high-temperature X-ray coupling system which comprises an X-ray diffraction unit, an X-ray imaging unit and an in-situ high-temperature testing unit, the X-ray diffraction unit and the X-ray imaging unit are arranged in a crossed mode, and the in-situ high-temperature testing unit is located at the crossed point. The X-ray diffraction unit and the X-ray imaging unit are respectively provided with an emergent end and a receiving end. In the invention, the X-ray diffraction unit and the X-ray imaging unit are arranged to be in cross distribution, light rays emitted from the emitting ends of the X-ray diffraction unit and the X-ray imaging unit can penetrate through the in-situ high-temperature testing unit and enter the receiving end, so that the in-situ high-temperature testing unit can be implemented in a laboratory environment, and meanwhile, different in-situ high-temperature testing units are selected for joint characterization; and the equipment cost and the use threshold are greatly reduced, and the accessibility and the application range of the technology are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of integrated in-situ characterization of material synthesis performance, and more particularly to an in-situ high-temperature X-ray coupling system. Background Art

[0002] In current research in the fields of materials science and energy, the structural evolution and mechanical behavior of samples in a high-temperature environment are crucial for revealing their properties and failure mechanisms. However, such research faces technical challenges, especially in simultaneously achieving dynamic characterization of crystal structures and three-dimensional morphologies. Currently, the existing technologies closest to the technology of the present application are mainly characterization methods based on single X-ray diffraction (XRD) or computed tomography (CT), as well as indirect research means of testing the two technologies successively and then combining the results. The XRD technology can provide crystal phase information of crystalline materials under specific conditions, such as crystal structure, phase transformation behavior, and stress state. However, traditional XRD devices are usually designed to focus on single-point or two-dimensional detection and cannot simultaneously obtain the three-dimensional structure information of samples, which limits its application in the study of complex-structured materials. On the other hand, X-ray CT technology is good at providing three-dimensional morphology data of samples, and through reconstruction algorithms, the microscopic structure distribution and morphological changes of materials can be intuitively displayed. However, the CT technology is usually less sensitive to the crystallographic information of materials and is difficult to accurately reveal the crystal phase changes and stress field distribution. In recent years, some researchers have tried to combine XRD and CT to form XRD-CT technology to solve the deficiencies of the above single technologies. For example, some literature reports XRD-CT systems based on synchrotron radiation sources, which have achieved joint analysis of crystal phases and three-dimensional structures of materials under dynamic loading conditions through the high brightness and high collimation of synchrotron radiation. However, the application of such technologies highly depends on synchrotron radiation facilities, with high experimental costs and complex equipment, which limits their wide application under laboratory conditions. In addition, the complexity of technology integration is also the reason why it is difficult to simply superimpose the two technologies to achieve the functions of XRD and CT. For example, to combine XRD and CT, two different scanning systems need to be integrated, which will not only increase the complexity of the hardware but also require the development of new software and algorithms to process the data of both. For example, CT data are continuous spatial images, while XRD data are measurement data for specific crystal planes and diffraction angles, and effectively fusing the two requires a high technical threshold. In addition, XRD itself has high requirements for samples, such as the flatness and size of samples, while CT is often applied to scanning larger objects or the human body, which makes it necessary to customize the equipment when combining the two, thus increasing the R & D and manufacturing costs. More importantly, the different working principles of the two also cause difficulties in combining them: for example, XRD mainly focuses on the microscopic structure of materials, while CT focuses more on the imaging of macroscopic structures. Although both use X-rays, the information they obtain is completely different, and combining them requires overcoming problems in signal processing and data integration.

[0003] Meanwhile, the above single device is usually designed for medium and low temperature environments and is difficult to meet the characterization requirements under high temperature conditions. For high temperature experiments, existing research mostly uses separate high temperature XRD or high temperature CT devices. For example, a high temperature furnace combined with an XRD test system can be used to study the crystal structure changes of samples at high temperatures; while the high temperature CT system mainly focuses on macroscopic structure changes such as thermal expansion, pore formation, or crack propagation in materials. However, these two types of devices are often independent during the testing process and cannot synchronously obtain crystal phase information and three-dimensional morphology changes, resulting in a problem of multi-scale information disconnection when studying the complex behavior of materials. In addition, some literature has also proposed ideas for integrating multi-dimensional data through indirect methods, such as separately testing XRD and CT data under different experimental conditions for the same sample, and then performing post-analysis on the two types of data through algorithms. However, this indirect integration method is not only time-consuming, but also the change of testing conditions may lead to inconsistent data, thus affecting the reliability of research results.

[0004] In summary, although certain progress has been made in the prior art in realizing the combined characterization of XRD and CT, there are still important deficiencies: First, most existing solutions rely on synchrotron radiation facilities. Although their high brightness and high collimation can achieve refined XRD-CT tests, the experimental equipment is complex, the cost is high, and special facilities are required for support, which limits their popularity and practical application in ordinary laboratories. In addition, the integration of XRD and CT functions in existing commercial devices has limited progress. Most devices can only perform separate characterizations of the two technologies at room temperature and are difficult to meet the joint testing requirements under high temperature conditions. Even if there are high temperature XRD or high temperature CT devices, most of them belong to independent testing systems and cannot synchronously obtain crystal structure and three-dimensional morphology change information in a single experiment, resulting in information disconnection in multi-physical field characterization and making it difficult to accurately reveal the behavior of complex materials. Second, some research relies on indirect integration methods for XRD and CT data, that is, separately testing and integrating through post-algorithms under different experimental conditions. This method is not only complex in operation and low in data acquisition efficiency, but may also introduce errors due to small changes in experimental conditions, resulting in the reliability and repeatability of test results being affected. Summary of the Invention

[0005] The technical problem to be solved by the present invention is how to provide an X-ray combined characterization system that is feasible in an ordinary laboratory environment and can simultaneously and synchronously perform XRD and CT tests in a high temperature environment.

[0006] The present invention achieves the solution to the above technical problems through the following technical means: An in-situ high-temperature X-ray coupling system, characterized in that it includes an X-ray machine, a detector, a sample rotating table, and a horizontal adjuster. Two X-ray machines and two detectors are respectively connected to corresponding horizontal adjusters and can move relative to the center of the sample rotating table. The two X-ray machines and the two detectors are arranged in a cross shape with the sample rotating table as the center. The angular difference between the two X-ray machines is 90°. Both the X-ray machine and the detector can rotate around the center of the sample rotating table. A heating chamber is also connected to the central rotating end of the sample rotating table. The light rays emitted by the two X-ray machines can both pass through the heating chamber and be incident on the corresponding detector. The heating chamber is provided with a heating field arranged in a spherical shape, and the heating field can heat the test piece to a set temperature or a set temperature range.

[0007] As a preferred technical solution, the heating chamber includes an upper heating chamber body and a lower heating chamber body. The upper heating chamber body and the lower heating chamber body are symmetrically arranged up and down and are connected by a window film. The plane where the window film is located is coplanar with the plane where the output end of the X-ray machine is located to ensure that the X-rays in this plane can all pass through freely.

[0008] As a preferred technical solution, a plurality of heat sources are provided on the heating chamber. The plurality of heat sources are arranged in a spherical shape, and a sample holder is provided in the heating chamber.

[0009] As a preferred technical solution, the plurality of heat sources are respectively located on the upper heating chamber body and the lower heating chamber body and are evenly distributed in an envelope manner. The extension lines of the axes of the plurality of heat sources can intersect at the center point of the heating chamber.

[0010] As a preferred technical solution, the heat source includes a halogen lamp and a halogen lamp fixing seat. A halogen lamp installation hole adapted to the halogen lamp fixing seat is opened on the outer wall of the heating chamber, and a halogen lamp extending into the heating chamber is fixedly connected to the halogen lamp fixing seat.

[0011] As a preferred technical solution, a plurality of windows are provided on the heating chamber, and the windows are fixedly connected to the chamber body through window fixing pieces.

[0012] As a preferred technical solution, a serpentine cooling channel is also embedded in the heating chamber, and a water-cooling joint inlet and a water-cooling joint outlet connected to the serpentine cooling channel are provided on the heating chamber.

[0013] As a preferred technical solution, the output end of the sample rotating table is in transmission connection with the heating chamber and can drive the heating chamber to rotate around its axis.

[0014] As a preferred technical solution, the two X-ray machines include an X-ray imaging machine and an X-ray diffractometer, and the two detectors include a detector one and a detector two.

[0015] As a preferred technical solution, a thermocouple air hole fixing seat is further fixedly connected to the heating chamber, and a thermocouple extending into the heating chamber is fixedly connected to the thermocouple air hole fixing seat.

[0016] The beneficial effects of the present invention are as follows:

[0017] (1) In the present invention, two sets of X-ray machines and two sets of detectors are arranged in a cross shape with the sample rotating table as the center. The light emitted by the two sets of X-ray machines can both pass through the heating chamber and be incident on the corresponding detectors, enabling it to be implemented in a laboratory environment, greatly reducing the equipment cost and usage threshold, improving the accessibility and application range of the technology, overcoming the problem that the prior art cannot meet the combined characterization under high-temperature conditions. Through the heating device and the environmental control system, the sample can simultaneously perform XRD crystal phase detection and CT three-dimensional structure reconstruction under dynamic heating, cooling, and constant temperature conditions, thereby meeting the comprehensive research requirements for crystal phase changes, structural evolution, and mechanical behavior of materials under high-temperature conditions.

[0018] (2) In the present invention, through the setting of multiple heat sources and serpentine cooling channels, the sample on the sample holder can simultaneously perform XRD crystal phase detection and CT three-dimensional structure reconstruction under dynamic heating, cooling, and constant temperature conditions. By adopting synchronous acquisition and data fusion technology, real-time linkage of XRD and CT data is achieved, avoiding the error problems introduced by multiple experimental conditions in traditional indirect integration methods, significantly improving the reliability of test results and experimental efficiency. By optimizing the radiation source, detector, and algorithm, crystal phase information and morphological changes can be accurately captured at the microscale, providing important support for studying the performance and failure mechanism of materials in a high-temperature environment. Description of the Drawings

[0019] Figure 1 It is a schematic diagram of the overall structure provided by an embodiment of the present invention;

[0020] Figure 2 It is a front view structure schematic diagram provided by an embodiment of the present invention;

[0021] Figure 3 It is a side view structure schematic diagram provided by an embodiment of the present invention;

[0022] Figure 4 It is a top view structure schematic diagram provided by an embodiment of the present invention;

[0023] Reference numerals of the drawings: 1. Halogen lamp mounting hole; 2. Upper heating cavity; 3. Window film; 4. Lower heating cavity; 5. Base; 6. Window; 7. Inlet of upper water-cooling joint; 8. Inlet of lower water-cooling joint; 9. Window fixing piece; 10. Sample base; 11. Support frame; 12. Outlet of upper water-cooling; 13. Outlet of lower water-cooling; 14. Halogen lamp terminal; 15. Halogen lamp fixing seat; 16. Halogen lamp; 17. Air inlet hole; 18. Thermocouple; 19. Fixing seat of thermocouple air hole; 20. Exhaust hole; 21. X-ray diffractometer; 22. Detector 1; 23. X-ray imager; 24. Detector 2; 25. Sample rotating table. Detailed implementation manners

[0024] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0025] Refer to Figure 1 , an in-situ high-temperature X-ray coupling system, comprising two sets of X-ray machines, two sets of detectors, a sample rotating table, and a horizontal adjuster. The two sets of X-ray machines and the two sets of detectors are respectively connected with corresponding horizontal adjusters and can move relative to the center of the sample rotating table. The two sets of X-ray machines and the two sets of detectors are arranged in a cross shape with the sample rotating table 25 as the center. The angular difference between the two sets of X-ray machines is 90°. The two sets of X-ray machines and the two sets of detectors can all rotate around the center 25 of the sample rotating table. The central rotating end of the sample rotating table 25 is also connected with a heating cavity. The heating cavity is provided with a spherical heating field, and the heating field can heat the test piece to a set temperature or a set temperature range. The heating cavity is a closed cavity structure, and the cavity is provided with a plurality of heat sources. The two sets of X-ray machines respectively include an X-ray diffractometer 21 and an X-ray imager 23. The two sets of detectors include a detector 1 22 and a detector 2 24. The X-ray diffractometer 21 and the detector 1 22 are located on both sides of the center of the sample rotating table 25. The X-ray imager 23 and the detector 2 24 are located on both sides of the center of the sample rotating table 25, and the angular difference between the X-ray imager 23 and the X-ray diffractometer 22 is 90°.

[0026] Refer to Figure 2, the cavity includes a heating upper cavity 2 and a heating lower cavity 4. The heating upper cavity 2 and the heating lower cavity 4 are arranged opposite to each other vertically and are connected by a window film 3. The plane where the window film 3 is located is coplanar with the plane of the exit ends of the X-ray diffractometer 21 and the X-ray imager 23. The heat sources are evenly and envelopingly distributed on the heating upper cavity 2 and the heating lower cavity 4. In this embodiment, a total of six groups of heat sources are provided, among which three groups are provided on each of the heating upper cavity 2 and the heating lower cavity 4. The heating upper cavity 2 and the heating lower cavity 4 are both hemispherical; it should be noted that the window film 3 is an annular structure and can be made of materials with high X-ray transmission, such as polymer materials, carbon materials, beryllium metal, aluminum and other materials. The thickness at the center of the window film 3 ≤ 150 microns. The X-ray machine can penetrate the window film 3, then penetrate the measured high-temperature sample, and reach the two detectors, so as to simultaneously and synchronously characterize the crystal diffraction and imaging of the measured high-temperature sample, and form a high-resolution three-dimensional reconstructed topography of the measured high-temperature sample.

[0027] The heat sources include halogen lamps 16 and halogen lamp fixing seats 15. Halogen lamp mounting holes 1 adapted to the halogen lamp fixing seats 15 are provided on the outer walls of the heating upper cavity 2 and the heating lower cavity 4. The halogen lamp fixing seats 15 are fixedly connected with halogen lamps 16 extending into the cavity. In this embodiment, six halogen lamps 16, six halogen lamp fixing seats 15, and six halogen lamp mounting holes 1 are provided. The power of each halogen lamp 16 can reach up to 300W at most. Of course, other non-contact infrared lamps can also be used to provide heat;

[0028] Refer to Figure 2 , Figure 3 , a plurality of visibly observable windows 6 are provided on the cavity. The material of the windows 6 can be selected from materials with high visible light band transmittance, such as quartz or sapphire. In this embodiment, two windows 6 are respectively provided on the heating upper cavity 2 and the heating lower cavity 4. The windows 6 are fixedly connected to the heating upper cavity 2 or the heating lower cavity 4 through window fixing pieces 9. One end of the window fixing piece 9 facing the heating upper cavity 2 or the heating lower cavity 4 is provided with a sealing ring. A thermocouple air hole fixing seat 19 is also fixedly connected to the heating upper cavity 2. A thermocouple 18 extending into the cavity is fixedly connected to the thermocouple air hole fixing seat 19. The thermocouple 18, a sample base 10 is fixedly connected to the center of the bottom of the heating lower cavity 4. The top of the sample base 10 extends to the center of the cavity, and its top is used to place the sample. Both the heating upper cavity 2 and the heating lower cavity 4 are provided with serpentine cooling channels. Among them, the heating upper cavity 2 is provided with an upper water cooling joint inlet 7 and an upper water cooling outlet 12 communicating with the cooling channel on the heating upper cavity 2. The heating lower cavity 4 is provided with a lower water cooling joint inlet 8 and a lower water cooling outlet 13 communicating with the cooling channel on the heating lower cavity 4. The upper water cooling joint inlet 7, the upper water cooling outlet 12, the lower water cooling joint inlet 8, and the lower water cooling outlet 13 are connected to an external cold source, so as to perform cooling.

[0029] Refer toFigure 1 , two sets of X-ray machines and two sets of detectors can also move relative to the center of the sample turntable 25. The heating chamber is fixedly connected to the rotating output end of the sample turntable 25. The rotating end of the sample turntable 25 is in transmission connection with the in-situ high-temperature testing unit and can drive the in-situ high-temperature testing unit to rotate around its axis. A base 5 is also fixedly connected to the bottom of the heating chamber. The base 5 can also achieve height adjustment. One end of the base 5 extending into the cavity is fixed with a ceramic seat sample holder, which can support the sample and is heat-resistant and heat-insulating at the same time. The base 5 is fixedly connected to the lower heating cavity 4, so that 360° rotation can be achieved. In this embodiment, the X-ray diffractometer 21 and the X-ray imager 23 can select commercial high-power small focal spot X-ray machines to detect the signal of the sample point of the focused spot. The detector one 22 and the detector two 24 select commercial panel detectors, and the pixel size point is less than 60um. The X-ray diffractometer 21, the detector one 22, the X-ray imager 23, and the detector two 24 are all installed on the fixed end of the horizontal adjuster. The horizontal adjuster can be a horizontal displacement table or a linear module in the prior art. The purpose of this structure is to ensure that the X-ray diffractometer 21, the detector one 22, the X-ray imager 23, and the detector two 24 can all move back and forth. For XRD, different diffraction ranges and angle resolution function selections can be achieved by the detector one 22 at different distances from the sample; for CT, the distance between the detector two 23 and the sample can achieve the selection of the sample spatial resolution;

[0030] The sample turntable 25 is located at the center of the whole system and can select a general commercial rotary displacement table, which is mainly used to control the 360° rotation of the sample, facilitating the acquisition of CT imaging data, and at the same time can also reduce the interference of the polycrystalline structure of the crystal material on the diffraction signal. Therefore, various different samples and in-situ testing devices can be connected to the sample turntable 25 for the combined characterization of XRD and CT in the laboratory. Considering the internal space of the in-situ high-temperature testing device and the X-ray energy of the X-ray testing part, the cylindrical sample size needs to meet the size requirement: ≤φ6mm. The sample is heated at different temperatures (RT-800°C) by a heat source, and in-situ XRD-CT analysis is carried out continuously and at multiple angles in cooperation with X-rays to study the influence mechanism of the microcrystalline structure of the material on temperature.

[0031] Usage method: First, fix the sample on the sample holder at the top of the base 5, place the sample in the cavity by adjusting the sample base 5, place the window film 3 between the upper heating cavity and the lower heating cavity. After installing the built-in sealing ring, fasten the upper heating cavity 2 and the lower heating cavity 4 together with screws. Connect the external power supply and the cold source, i.e., the water chiller, fix the device on the sample rotating table 25, align it with the X-ray path, then achieve temperature control. At the same time, start equipment such as the X-ray source and the water chiller, and adjust the front and back positions of the detector according to the required detection angle range and resolution requirements. Collect XRD-CT spectral data under different conditions such as temperature and angle.

[0032] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An in-situ high temperature X-ray coupling system, characterized in that: It includes two sets of X-ray machines, two sets of detectors, a sample rotating table, and a horizontal adjuster. The two sets of X-ray machines and the two sets of detectors are respectively connected to corresponding horizontal adjusters and can move relative to the center of the sample rotating table. The two sets of X-ray machines and the two sets of detectors are arranged in a cross shape with the sample rotating table as the center. The angle difference between the two sets of X-ray machines is 90°. The optical machines and detectors can rotate around the center of the sample rotating table. The central rotating end of the sample rotating table is also connected to a heating cavity. The emitted light of the two sets of X-ray machines can pass through the heating cavity and be incident on the corresponding detector. The heating cavity is provided with a heating field arranged in a spherical shape, and the heating field can heat the test piece to a set temperature or a set temperature range.

2. An in-situ high temperature X-ray coupling system according to claim 1, characterized in that: The heating chamber comprises an upper heating chamber and a lower heating chamber, the upper heating chamber and the lower heating chamber are arranged opposite to each other and connected through a window film, and the plane where the window film is located is coplanar with the plane where the two sets of X-ray machine output ends are located.

3. An in-situ high temperature X-ray coupling system according to claim 2, characterized in that: The heating chamber is provided with a plurality of heat sources, which are arranged in a spherical shape, and a sample holder is provided in the heating chamber.

4. The in-situ high temperature X-ray coupling system according to claim 3, characterized in that: The multiple heat sources are respectively located on the upper heating cavity and the lower heating cavity, and are evenly distributed in an envelope manner. The extension lines of the axes of the multiple heat sources can intersect at the center point of the heating cavity.

5. The in-situ high temperature X-ray coupling system according to claim 2, characterized in that: The heat source comprises a halogen lamp and a halogen lamp fixing seat. A halogen lamp mounting hole matching the halogen lamp fixing seat is provided on the outer wall of the heating cavity. The halogen lamp fixing seat is fixedly connected with a halogen lamp extending into the heating cavity.

6. The in-situ high temperature X-ray coupling system according to claim 5, characterized in that: The heating chamber is provided with a plurality of windows, and the windows are connected and fastened to the heating chamber via window fixing sheets.

7. The in-situ high temperature X-ray coupling system according to claim 2, characterized in that: A serpentine cooling channel is also embedded in the heating chamber, and a water cooling joint inlet and a water cooling joint outlet which are connected with the serpentine cooling channel are provided on the heating chamber.

8. The in-situ high temperature X-ray coupling system according to claim 1, characterized in that: The output end of the sample rotating platform is transmission-connected to the heating chamber and can drive the heating chamber to rotate with its axis as the rotating shaft.

9. The in-situ high temperature X-ray coupling system according to claim 1, characterized in that: The two sets of X-ray machines include an X-ray imaging machine and an X-ray diffraction machine, and the two sets of detectors include detector one and detector two.

10. The in-situ high temperature X-ray coupling system according to claim 1, characterized in that: The heating chamber is also fixedly connected with a thermocouple air hole fixing seat, and the thermocouple air hole fixing seat is fixedly connected with a thermocouple extending into the heating chamber.

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