High-throughput, high-temperature in-situ X-ray absorption spectroscopy research device and its operation method

Abstract

This disclosure relates to a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device and its operation method. The device includes: a vacuum furnace module with an opening at the top, X-ray incident apertures and corresponding X-ray exit apertures with their optical axes aligned on two opposite sides, and a vacuum interface for connecting to an external vacuum pump on the other side; and a heating module that extends into and connects to the vacuum furnace module through the opening, including a sample holder, heating elements, and thermocouples. The heating elements and thermocouples are positioned adjacent to the sample holder and heat the sample holder and measure its temperature. The X-ray incident aperture and X-ray exit aperture have a combined shape of two upper and lower semicircles and a rectangle with a horizontal length equal to the diameter of the semicircles and a vertical length less than the diameter of the semicircles. The sample holder has multiple grooves for accommodating multiple sample chambers, and the grooves are surrounded by clearance slots.

Description

Technical Field

[0001] This invention relates to the field of in-situ research technology, and in particular to a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device and its operation method. Background Technology

[0002] X-ray absorption fine structure (XAFS) spectroscopy, due to its locality, elemental selectivity, sensitivity, orientation, and versatility, has become a powerful tool for studying the structure of matter, with wide applications in materials, energy, chemistry, environment, and life sciences. As research progresses, the interest in and demand for in-situ studies of samples under actual working conditions is growing, necessitating the development of corresponding experimental methods and techniques.

[0003] High-temperature in-situ XAFS, which enables online research on high-temperature molten salt structures, phase transitions, material growth, and service processes, has attracted widespread attention from researchers both domestically and internationally. However, most high-temperature in-situ XAFS research devices developed at home and abroad currently suffer from various problems, bringing additional difficulties to experiments. For example, although some devices have achieved both transmission and fluorescence measurement modes, practical use has revealed that the XAFS signal quality measured in fluorescence mode is poor. Testing special samples under high-temperature conditions, such as those that are air-sensitive, volatile, liquid at the experimental temperature, toxic, or / and radioactive, is difficult and limited in methods, posing a dual risk of sample deterioration and device contamination, making it difficult to guarantee the accuracy and authenticity of the experiments. Most current research devices are large in size, have limited heating rates, and can only perform single-sample testing. Heating, cooling, and sample replacement are time-consuming, resulting in low efficiency. Summary of the Invention

[0004] This invention aims to solve the problems of poor compatibility of existing high-temperature in-situ X-ray absorption spectroscopy research devices with fluorescence measurement modes, low experimental accuracy and authenticity, and low efficiency caused by processes such as heating, cooling and sample replacement.

[0005] According to one aspect of the present invention, a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device is provided, which may include: a vacuum furnace module, the top of which is provided with an opening, and two opposite sides of the vacuum furnace module are respectively provided with X-ray incident light-transmitting holes and corresponding X-ray exit light-transmitting holes with their optical axes aligned on the same straight line, and the other side of the vacuum furnace module is provided with a vacuum interface for connecting to an external vacuum pumping device; and a heating module, which extends into and is connected to the vacuum furnace module through the opening of the vacuum furnace module, and includes a sample holder, a heating element, and a thermocouple, the heating element and the thermocouple being positioned adjacent to the sample holder and used to heat the sample holder and measure its temperature; wherein the X-ray incident light-transmitting hole and the X-ray exit light-transmitting hole have a combined shape of two upper and lower semicircles and a rectangle with a horizontal length equal to the diameter of the semicircle and a vertical length less than the diameter of the semicircle, and the sample holder is provided with multiple grooves for accommodating multiple sample chambers, and the grooves are provided with clearance slots around their perimeter.

[0006] Furthermore, a window film, which is a polyimide film, can be covered on the X-ray entrance aperture and the X-ray exit aperture.

[0007] Furthermore, a carbon film can be provided on the inner side of the window film.

[0008] Furthermore, the outer side of the vacuum furnace module can be provided with X-ray entrance window flange and X-ray exit window flange, which correspond to the X-ray entrance light passage and X-ray exit light passage, respectively. The X-ray entrance window flange and X-ray exit window flange are connected to the vacuum furnace module by threaded connection.

[0009] Furthermore, the inner rings of the X-ray entrance window flange and the X-ray exit window flange can be chamfered at 50°.

[0010] Furthermore, the sample chamber can be sealed using high-temperature ceramic adhesive or graphite adhesive.

[0011] Furthermore, the heating module can be connected to the vacuum furnace module via a threaded connection.

[0012] Furthermore, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may further include a cooling medium circulation module, which is connected to the vacuum furnace module and the heating module through pipelines to form a loop, and the pipelines are equipped with cooling medium.

[0013] Furthermore, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may further include an external control module, which includes a PID temperature controller connected to a thermocouple, a fuse connected to a power input, and a thyristor module connecting the PID temperature controller, the heating element, and the fuse.

[0014] According to another aspect of the present invention, an operating method for a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device is provided, which may include:

[0015] In the transmission X-ray absorption spectrum measurement mode, the high-throughput high-temperature in-situ X-ray absorption spectrum research device is placed perpendicular to the X-ray incident direction, and its position is adjusted so that the optical axes of the X-ray incident aperture and the X-ray exit aperture coincide with the X-ray incident direction; or in the fluorescence X-ray absorption spectrum measurement mode, the high-throughput high-temperature in-situ X-ray absorption spectrum research device is placed at a 45° angle relative to the X-ray incident direction, and its position is adjusted so that the optical axes of the X-ray incident aperture and the X-ray exit aperture form a 45° angle with the X-ray incident direction.

[0016] According to an embodiment of the present invention, a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device and its operation method are provided, which have at least the following advantages: (1) Real-time measurement of samples under actual working conditions can be carried out, and the deterioration and leakage of samples during the testing process can be effectively prevented, thereby improving the accuracy and authenticity of the experiment; (2) While ensuring the quality of measurement data in transmission mode and fluorescence mode, the present invention can conveniently and quickly switch measurement modes, thereby achieving the goal of taking into account different measurement modes and improving the compatibility of fluorescence measurement mode; (3) High-temperature in-situ XAFS measurement of at least two samples can be achieved in one heating, which greatly saves experimental time and improves the utilization rate of time and experimental efficiency. Attached Figure Description

[0017] The description herein refers to the accompanying drawings, in which the same reference numerals denote the same parts throughout the drawings.

[0018] Figure 1 This is a schematic diagram of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0019] Figure 2 This is a schematic diagram of the heating module in a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0020] Figure 3 This is a schematic diagram of the irregular flange of the X-ray incident window in a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0021] Figure 4 This is a schematic diagram of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention in fluorescence measurement mode.

[0022] Figure 5 This is a flowchart of the operation method of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0023] Figure label:

[0024] 100 Vacuum furnace, 110 Base plate, 120 Support column

[0025] 130 Furnace body; 131 Cavity; 132 Opening

[0026] 133 Threaded hole; 134 X-ray entrance aperture; 136 Vacuum interface.

[0027] 137, 138 Cooling medium channel interface; 140 X-ray incident window irregular flange

[0028] 141 Countersunk hole 200 Heating device 210 Top plate

[0029] 211 Heating element; 212 Thermocouple; 213 Boss

[0030] 214, 215 Cooling medium channel interface; 220 Sample holder

[0031] 221 Groove 222 Baffle 223 Sample Chamber Detailed Implementation

[0032] Various embodiments of the present disclosure will now be described in detail with reference to the accompanying drawings. However, the elements and features of the present disclosure may be configured or arranged in different ways to form other embodiments, which may be variations of any disclosed embodiment.

[0033] In this disclosure, references to various features (e.g., elements, structures, modules, components, steps, operations, characteristics, etc.) included in “one embodiment,” “example embodiment,” “embodiment,” “another embodiment,” “some embodiments,” “multiple embodiments,” “other embodiments,” “alternative embodiments,” etc., are intended to indicate that any such feature is included in one or more embodiments of this disclosure, but may or may not be combined in the same embodiments.

[0034] In this disclosure, the terms “comprising,” “including,” “having,” and “containing” are open-ended. As used in the appended claims, these terms specify the presence of the said element but do not exclude the presence or addition of one or more other elements. The terms in the claims do not exclude the device from including additional components, such as interface units, circuitry, etc.

[0035] Embodiments will now be described with reference to the accompanying drawings, wherein the same reference numerals indicate the same elements.

[0036] Figure 1 This is a schematic diagram of the structure of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention. Figure 2This is a schematic diagram of the heating module in a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research apparatus according to an embodiment of the present invention. Figure 3 A schematic diagram of the irregular flange of the X-ray incident window in a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention is shown. Figure 4 This is a schematic diagram of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research apparatus according to an embodiment of the present invention in fluorescence measurement mode. (Refer to...) Figures 1 to 3 The high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may include a vacuum furnace (also known as a vacuum furnace module) 100 and a heating device (also known as a heating module) 200.

[0037] In this embodiment, the vacuum furnace 100 may be located on a scissor lift or an optical platform, and the heating device 200 may be positioned above the vacuum furnace 100.

[0038] In an embodiment, the vacuum furnace 100 may include a base plate 110, on which four support columns 120 may be provided, and a furnace body 130 may be provided on the four support columns 120. The furnace body 130 contains a cavity 131, and an opening 132 may be provided at its top. An O-ring may be provided around the opening 132, and threaded holes 133 may be provided at the four corners of the top of the furnace body 130.

[0039] In this embodiment, the support column 120 may be composed of a screw and a smooth rod. The screw corresponds to the threaded hole at the bottom of the furnace body 130, and the support column 120 is connected to the furnace body 130 through a threaded connection. The smooth rod has a clearance groove at the top for easy wrench installation and a threaded hole at the bottom.

[0040] In this embodiment, the inner side of the base plate 110 may be provided with four countersunk holes for connecting the furnace body 130. Each countersunk hole corresponds to the support column 120 installed at the bottom of the furnace body 130 and is connected by threads. The outer side of the base plate 110 is provided with eight through holes for fixing to the scissor lift platform or optical platform. The center of each hole is 100mm away from the center of the base plate 110 and the phase angle between adjacent through holes is 45°.

[0041] In this embodiment, X-ray incident light transmission holes 134 and corresponding X-ray exit light transmission holes (with the same structure and size as X-ray incident light transmission holes 134, not shown) can be provided through the two opposite sides of the furnace body 130, and the optical axes of X-ray incident light transmission holes 134 and X-ray exit light transmission holes can be located on the same straight line.

[0042] In an embodiment, an O-ring may be provided around the X-ray entrance aperture 134 and the X-ray exit aperture.

[0043] In one embodiment, a vacuum port 136 communicating with the vacuum furnace cavity 131 may be provided on the other side of the furnace body 130. The vacuum port 136 may be connected to an external vacuum device (not shown, for example, a vacuum pump).

[0044] In an embodiment, the heating device 200 may include a sample holder 220, a heating element 211, and a thermocouple 212. The heating element 211 and thermocouple 212 are positioned adjacent to the sample holder 220 and are used to heat the sample holder 220 and measure its temperature. In a specific example, such as Figure 1 As shown, the heating device 200 may include a top plate 210, a sample holder 220 may be provided below the top plate 210, and a heating element 211 that penetrates the top plate 210 and the sample holder 220 and a thermocouple 212 that passes through the top plate 210 and extends into the sample holder 220 may be provided above the top plate 210.

[0045] In one embodiment, the top plate 210 of the heating device 200 may have two deep holes symmetrically arranged on both sides of the axial direction for placing the heating element 211, and a small hole is provided near one of the deep holes for inserting the thermocouple 212.

[0046] In an embodiment, the front of the sample holder 220 of the heating device 200 may be provided with a plurality of grooves for placing the sample chamber 223, and a baffle 222 for fixing the sample chamber 223 is provided near the grooves. A small hole is provided on the back of the sample holder 220 at the position between the grooves for placing the temperature measuring end of the thermocouple 212.

[0047] In an embodiment, the sample chamber 223 can be a cuboid with a length of 16 mm, a width of 1-3 mm, and a depth of 15-35 mm for holding the sample, and the wall thickness around the chamber is 1 mm. The material is isostatic graphite, pyrolytic graphite, or boron nitride.

[0048] In an embodiment, the top plate 210 of the heating device 200 may be provided with through holes at the four corners corresponding to the threaded holes 133 of the furnace body 130 of the vacuum furnace 100, thereby realizing the connection between the heating device 200 and the vacuum furnace 100.

[0049] In this embodiment, the heating element 211 may be a resistance wire, a heating tube encapsulated with a resistance wire, a silicon carbide rod, etc. For safety, insulation should be ensured when placing it into the heating device 200.

[0050] As described above, the top of the vacuum furnace 100 is provided with an opening 132 and the four corners of the top of the furnace body 130 can be provided with threaded holes 133. Therefore, the heating device 200 can be inserted into the vacuum furnace 100 through the opening 132, and the connection between the heating device 200 and the vacuum furnace 100 can be achieved through the threaded connection between the through hole of the heating device 200 and the threaded hole 133 of the furnace body 130.

[0051] Although the heating device 200 and the vacuum furnace 100 are shown to be connected and fixed by a threaded connection, the present invention is not limited to this and other connection methods can also be used.

[0052] In this embodiment, the sample holder 220 may be provided with multiple grooves for accommodating multiple sample chambers 223 (at least two), and the grooves may be provided with clearance grooves around them. Therefore, multiple samples can be processed at one time and the sample chambers 223 can be easily put into and taken out, thereby improving work efficiency.

[0053] To accommodate both transmission and fluorescence measurement modes, the shape and size of the X-ray entrance aperture 134 and the X-ray exit aperture of the vacuum furnace 100 can be designed.

[0054] In an embodiment, the X-ray incident aperture 134 and the X-ray exit aperture can be configured as a combination of two upper and lower semicircles and a rectangle whose length in the horizontal direction (i.e., the direction perpendicular to the height direction of the vacuum furnace 100) is equal to the diameter of the semicircle and whose length in the vertical direction (i.e., the height direction of the vacuum furnace 100) is less than the diameter of the semicircle.

[0055] In this embodiment, the dimensions of the combined shape of the two semicircles and rectangles of the X-ray entrance aperture 134 and the X-ray exit aperture can be set. Taking the X-ray entrance aperture 134 as an example, the dimensions of the combined shape of the two semicircles and rectangles of the X-ray entrance aperture 134 can be set according to the distance between the sample chamber 223 and the X-ray entrance aperture 134 (which can be regarded as the distance between the sample in the sample chamber 223 and the outermost edge of the X-ray entrance window flange 140 described below).

[0056] In fluorescence measurement mode, when the sample chamber 223 is too close to the X-ray incident light-transmitting aperture 134, it will affect the heating and heat preservation of the sample chamber 223. When it is too far from the X-ray incident light-transmitting aperture 134, the X-ray incident light-transmitting aperture 134 needs to be designed to be very large, which will result in a large size of the entire device.

[0057] In one embodiment, the distance between the sample chamber 223 and the X-ray incident light aperture 134 can be set to 24 mm, but the present invention is not limited thereto.

[0058] Taking the aforementioned distance of 24 mm as an example, in fluorescence measurement mode, the entire device is at a 45° angle to the incident X-ray, meaning the sample is at a 45° angle to the incident X-ray. At this point, the incident X-ray hits the center of the sample, and the distance between the sample and the outermost edge of the X-ray incident window flange 140 described below is 24 mm. Therefore, to ensure that most of the fluorescence signal can be emitted, the minimum diameter of the window (circular, because the fluorescence signal can be considered as the solid angle of a sphere in three dimensions) calculated geometrically is 1.414 × 6 × 2 + 24 × 2 = 65 mm (see...). Figure 4 That is, the minimum diameter of the semicircle in the combined shape of the two semicircles and the rectangle of the X-ray entrance aperture 134 is 65 mm. Optionally, in Figure 4 In order to improve the effect of fluorescence measurement, the incident X-ray must not be blocked within 6 mm.

[0059] As described above, in the combined shape of the X-ray entrance aperture 134, the horizontal length of the rectangle is equal to the diameter of the semicircle, and the vertical length is less than the diameter of the semicircle. Taking the diameter of the semicircle as 65mm as an example, the vertical length of the rectangle can be set to 50mm, but the present invention is not limited to this.

[0060] Since the X-ray exit aperture can be designed in the same way as the X-ray entrance aperture 134 described above, its description is omitted here.

[0061] In this embodiment, the X-ray incident aperture 134 and the X-ray exit aperture may be covered with a window film, and the window film may be a polyimide film to achieve high X-ray transmittance. For example, an aluminum-plated polyimide film may be used, but the invention is not limited thereto.

[0062] In this embodiment, a high-temperature resistant carbon film may be provided on the inner side of the window film to absorb the infrared thermal radiation emitted by the heating device 200 during heating, so that the temperature of the window film will not exceed the upper limit of use, and at the same time eliminate the influence of infrared signals on the X-ray absorption spectrum.

[0063] Return to reference Figure 1 The X-ray entrance window flange 140 and the X-ray exit window flange (with the same structure and size as the X-ray entrance window flange 140, not shown) can be set on the outside of the furnace body 130, respectively corresponding to the X-ray entrance aperture 134 and the X-ray exit aperture, and their inner rings can be the same in shape and size as the X-ray entrance aperture 134 and the X-ray exit aperture, respectively.

[0064] In this embodiment, the X-ray entrance window flange 140 may be provided with multiple countersunk holes 141 (as shown in the figure, for example, eight), and the X-ray exit window flange may also be provided with multiple countersunk holes (the structure and size are the same as the countersunk holes 141, not shown), and the X-ray entrance window flange 140 and the X-ray exit window flange may be fixed to the furnace body 130 by threaded connection.

[0065] In this embodiment, the inner rings of the X-ray incident window flange 140 and the X-ray exit window flange can be chamfered at 50° to avoid obstruction of the X-ray fluorescence signal during fluorescence mode measurement.

[0066] In this embodiment, when testing the sample, the sample chamber 223 can be sealed with high-temperature ceramic adhesive or graphite adhesive to isolate the sample from the atmosphere and prevent sample leakage.

[0067] In this embodiment, two sample chambers 223 containing samples can be placed on the sample rack 220 at the same time. By adjusting the height, two samples can be measured under one heating, thereby improving efficiency.

[0068] Further integration Figures 1 to 3 The procedure for sealing the vacuum furnace 100 with the heating device 200 for testing samples is provided as follows:

[0069] First, fix the sample chamber 223 to the heating device: place the sample chamber 223 into the groove 221 of the sample holder 220. Since the four corners of the groove 221 are provided with clearance grooves, the sample chamber 223 can be easily put in and taken out. Then, install the baffle 222 to fix it. Next, assemble the vacuum furnace 100 and the heating device 200: extend the heating device 200 into the cavity 131 through the top opening 132 of the furnace body 130. The protrusion 213 extending below the top plate 210 cooperates with the top opening 132 of the furnace body 130. A sealing ring is sandwiched between the furnace body 130 and the top plate 210. The through holes symmetrically arranged at the four corners of the top plate 210 correspond to the threaded holes provided at the top of the furnace body 130. The vacuum furnace 100 and the heating device 200 are sealed by threaded connection.

[0070] In this embodiment, the vacuum interface 136 can be a KF flange interface, which can be connected to a vacuum gauge, vacuum valve, and vacuum pump, and can be quickly connected and disassembled using vacuum clamps. The KF flange interface can be positioned on the left side of the sample to accommodate the limited space of the synchrotron X-ray absorption spectroscopy experimental station and avoid interference with other equipment in the station.

[0071] In this embodiment, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may further include a cooling medium circulation device (also known as a cooling medium circulation module). The furnace body 130 of the vacuum furnace 100 is provided with a cooling medium channel, and there are interfaces 137 and 138 on its exterior. The top plate 210 of the heating device 200 is provided with a cooling medium channel, and there are interfaces 214 and 215 on its exterior. A pipeline is used to connect either interface of the furnace body 130 and the top plate 210 to connect their cooling medium channels. The remaining two interfaces are connected to the cooling medium circulation device to form a cooling medium circulation loop, which is used to ensure that the furnace body 130 of the vacuum furnace 100, the top plate 210 of the heating device 200, and the window film covering the X-ray incident light transmission hole 134 and the X-ray exit light transmission hole are at a safe operating temperature.

[0072] In this embodiment, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may further include an external control cabinet (also called an external control module). This external control cabinet may include a PID temperature controller connected to thermocouple 212, a fuse connected to the power input, and a SCR module connecting the PID temperature controller, heating element 211, and fuse. The PID controller is primarily used for temperature control, the fuse is used for circuit protection, and the SCR module is used to control the current input to the heating element 211. During heating, a certain current is applied to the heating element 211 to raise the sample temperature. Simultaneously, the thermocouple 212 feeds back the measured temperature to the PID temperature controller. The PID temperature controller controls the current input to the heating element by adjusting the conduction angle of the SCR element, thereby achieving temperature control.

[0073] Figure 5 This is a flowchart of the operation method of a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0074] like Figure 5 As shown, the operation method of the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention includes: in the measurement mode of transmission X-ray absorption spectroscopy, placing the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device perpendicular to the X-ray incident direction, and adjusting the position so that the optical axes of the X-ray incident aperture and the X-ray exit aperture coincide with the X-ray incident direction; or in the measurement mode of fluorescence X-ray absorption spectroscopy, placing the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device at a 45° angle relative to the X-ray incident direction, and adjusting the position so that the optical axes of the X-ray incident aperture and the X-ray exit aperture form a 45° angle with the X-ray incident direction.

[0075] Specifically, in the transmission X-ray absorption spectrum measurement mode, the high-throughput high-temperature in-situ X-ray absorption spectrum research device provided in this embodiment of the invention is placed perpendicular to the X-ray incident direction. The position is adjusted so that the optical axes of the X-ray incident aperture 134 and the X-ray exit aperture coincide with the X-ray incident direction, and then it is fixed to the scissor lift platform or optical platform with bolts. At this time, X-rays enter the cavity 131 through the X-ray incident aperture 134 and are incident on the sample chamber 223, while the transmitted X-rays exit through the X-ray exit aperture.

[0076] Specifically, in the fluorescence X-ray absorption spectroscopy measurement mode, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device provided in this embodiment of the invention is placed at a 45° angle relative to the X-ray incident direction. The position is adjusted so that the optical axes of the X-ray incident aperture 134 and the X-ray exit aperture are at a 45° angle to the X-ray incident direction, and then it is fixed to a scissor lift platform or optical platform with bolts. At this time, X-rays enter the cavity 131 through the X-ray incident aperture 134 and are incident on the sample chamber 223. The generated X-ray fluorescence is also emitted through the X-ray incident aperture 134.

[0077] The high-throughput high-temperature in-situ X-ray absorption spectroscopy research apparatus and its operation method provided by embodiments of the present invention were used to study air-sensitive liquid molten salt samples at 550 degrees Celsius. This included measuring the X-ray absorption spectra of LiCl-KCl-YCl3 and α-radioactive LiCl-KCl-UCl3 and LiCl-KCl-UCl4 molten salts in transmission mode, and measuring the X-ray absorption spectrum of LiCl-KCl-SmCl3 molten salt in fluorescence mode. The expected experimental objectives were achieved, and the testing efficiency was significantly improved. This demonstrates that the apparatus and its operation method are feasible for conducting high-temperature in-situ X-ray absorption spectroscopy experiments.

[0078] According to embodiments of the present invention, irregularly shaped X-ray incident and exit windows are designed by combining the characteristics of transmission spectroscopy and fluorescence spectroscopy, which can achieve both measurement modes while ensuring data quality. Furthermore, by designing multiple grooves on the sample holder to accommodate sample chambers, high-throughput measurement is achieved, effectively improving machine time utilization. It can be used for high-temperature in-situ XAFS studies of both conventional and special samples.

[0079] The methods, processes, and / or operations described herein can be executed by code or instructions that run on a computer, processor, controller, or other signal processing device. The computer, processor, controller, or other signal processing device can be the apparatus described herein, or an apparatus other than the elements described herein. Because the algorithms constituting the basis of the methods or the operation of the computer, processor, controller, or other signal processing device are described in detail, the code or instructions used to implement the operations of the method embodiments can convert a computer, processor, controller, or other signal processing device into a dedicated processor for executing the methods herein.

[0080] In addition, another embodiment may include a computer-readable medium, such as a non-transitory computer-readable medium, for storing the above-described code or instructions. The computer-readable medium may be volatile or non-volatile memory or other storage device removably or permanently coupled to a computer, processor, controller, or other signal processing device to execute code or instructions for performing the operations of the method or apparatus embodiments described herein.

[0081] The controllers, processors, control circuits, devices, modules, units, multiplexers, logic, interfaces, decoders, drivers, generators, and other signal generation and signal processing features disclosed herein can be implemented, for example, as non-transient logic, which may include hardware, software, or both. When at least partially implemented as hardware, the controllers, processors, control circuits, devices, modules, units, multiplexers, logic, interfaces, decoders, drivers, generators, and other signal generation and signal processing features can be any of various integrated circuits, including but not limited to application-specific integrated circuits, field-programmable gate arrays, combinations of logic gates, systems-on-a-chip, microprocessors, or other types of processing or control circuitry.

[0082] While this teaching has been described with reference to specific embodiments, it will be apparent to those skilled in the art that various changes and modifications may be made to this disclosure without departing from the spirit and scope of the disclosure as defined by the appended claims. Furthermore, embodiments may be combined to form other embodiments.

Claims

1. A high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device, characterized in that, include: The vacuum furnace module has an opening at the top, and X-ray entrance and exit holes with their optical axes aligned on two opposite sides. The other side of the vacuum furnace module has a vacuum interface for connecting to an external vacuum pumping device. as well as A heating module extends into and is connected to the vacuum furnace module through an opening in the vacuum furnace module. The heating module includes a sample holder, a heating element, and a thermocouple. The heating element and the thermocouple are positioned adjacent to the sample holder and are used to heat the sample holder and measure its temperature. The X-ray entrance aperture and the X-ray exit aperture have a combined shape of two upper and lower semicircles and a rectangle whose horizontal length is equal to the diameter of the semicircles and whose vertical length is less than the diameter of the semicircles. The sample holder is provided with multiple grooves for accommodating multiple sample chambers, and the grooves are provided with anti-cavity slots around their perimeter.

2. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, The X-ray incident aperture and the X-ray exit aperture are covered with a window film, which is a polyimide film.

3. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 2, characterized in that, A carbon film is provided on the inner side of the window film.

4. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, The outer side of the vacuum furnace module is provided with an X-ray entrance window flange and an X-ray exit window flange, which correspond to the X-ray entrance light-transmitting hole and the X-ray exit light-transmitting hole, respectively. The X-ray entrance window flange and the X-ray exit window flange are connected to the vacuum furnace module by threaded connection.

5. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 4, characterized in that, The inner rings of the X-ray incident window flange and the X-ray exit window flange are provided with a 50° chamfer.

6. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, The sample chamber is sealed using high-temperature ceramic adhesive or graphite adhesive.

7. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, The heating module is connected to the vacuum furnace module via a threaded connection.

8. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, It further includes a cooling medium circulation module, which is connected to the vacuum furnace module and the heating module through pipelines to form a loop, and the pipelines are provided with cooling medium.

9. The high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that, The device further includes an external control module, which includes a PID temperature controller connected to the thermocouple, a fuse connected to the power input, and a thyristor module connecting the PID temperature controller, the heating element, and the fuse.

10. A method for operating a high-throughput, high-temperature in-situ X-ray absorption spectroscopy research apparatus according to any one of claims 1-9, characterized in that, include: In the transmission X-ray absorption spectrum measurement mode, the high-throughput high-temperature in-situ X-ray absorption spectrum research device is placed perpendicular to the X-ray incident direction, and its position is adjusted so that the optical axes of the X-ray incident aperture and the X-ray exit aperture coincide with the X-ray incident direction; or In the measurement mode of fluorescence X-ray absorption spectroscopy, the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device is placed at a 45° angle relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident aperture and the X-ray exit aperture are at a 45° angle to the X-ray incident direction.

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