High-flux high-temperature in-situ X-ray absorption spectrum research device and operation method thereof

Abstract

The invention relates to a high-flux high-temperature in-situ X-ray absorption spectrum research device and an operation method thereof, and the device comprises a vacuum furnace module, the top of which is provided with an opening, and two opposite side surfaces of which are respectively provided with an X-ray incident light through hole and a corresponding X-ray emergent light through hole, the optical axes of which are located on the same straight line, a vacuum interface connected with an external vacuum-pumping device is arranged on the other side surface; the heating module extends into the vacuum furnace module through the opening of the vacuum furnace module and is connected with the vacuum furnace module, the heating module comprises a sample rack, a heating element and a thermocouple, and the heating element and the thermocouple are positioned to be adjacent to the sample rack and are used for heating the sample rack and measuring the temperature; the X-ray incident light-transmitting hole and the X-ray emergent light-transmitting hole have a combined shape of an upper semicircle, a lower semicircle and a rectangle, the length of the rectangle in the horizontal direction is equal to the diameter of the semicircles, and the length of the rectangle in the vertical direction is smaller than the diameter of the semicircles, a plurality of grooves for accommodating a plurality of sample chambers are formed in the sample rack, and clearance grooves are formed in the peripheries of the grooves.

Description

Technical Field

[0001] The present invention relates to the technical field of in-situ research, and in particular to a high-throughput high-temperature in-situ X-ray absorption spectrum research device and an operating method thereof. Background Art

[0002] X-ray Absorption Fine Structure (XAFS) spectroscopy has become a powerful means to study the structure of matter due to its locality, element selectivity, sensitivity, orientation and extensiveness, and has been widely used in the fields of materials, energy, chemistry, environment and life sciences. As research gradually deepens, the interest in in-situ research of samples under actual working conditions is growing, and the demand is increasing, and the corresponding experimental methods and techniques are urgently needed.

[0003] Among them, high-temperature in-situ XAFS can realize online research on high-temperature molten salt structure, material phase change, material growth and service process, etc., and has attracted widespread attention from scientific researchers at home and abroad. However, most of the high-temperature in-situ XAFS research devices currently developed at home and abroad have various problems, which bring additional difficulties to the experiment. For example, although some devices have achieved both transmission and fluorescence measurement modes, it is found in actual use that the quality of XAFS signals measured in fluorescence mode is poor; the testing of special samples such as air-sensitive, volatile, liquid at experimental temperature, toxic or / and radioactive under high temperature conditions is difficult and the means are limited. There are dual risks of sample deterioration and contamination of the device, making it difficult to ensure the accuracy and authenticity of the experiment; most of the current research devices are large in size and have limited heating rates. They can only realize single-sample testing. Heating, cooling and sample replacement take a long time, resulting in low efficiency. Summary of the invention

[0004] The present invention aims to solve the problems of poor compatibility of existing high-temperature in-situ X-ray absorption spectrum 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 spectrum research device is provided, which may include: a vacuum furnace module, wherein an opening is provided at the top of the vacuum furnace module, and X-ray incident light holes and corresponding X-ray exit light holes whose optical axes are located on the same straight line are respectively provided on two opposite sides of the vacuum furnace module, and a vacuum interface for connecting to an external vacuum pumping device is provided on the other side of the vacuum furnace module; and a heating module, which extends into the vacuum furnace module through the opening of the vacuum furnace module and is connected to the vacuum furnace module, and the heating module comprises a sample rack, a heating element and a thermocouple, wherein the heating element and the thermocouple are positioned adjacent to the sample rack and are used to heat the sample rack and measure the temperature; wherein the X-ray incident light hole and the X-ray exit light hole have a combined shape of two upper and lower semicircles and a rectangle whose horizontal length is equal to the diameter of the semicircle and whose vertical length is less than the diameter of the semicircle, and the sample rack is provided with a plurality of grooves for accommodating a plurality of sample chambers, and air avoidance grooves are provided around the grooves.

[0006] Furthermore, the X-ray incident light hole and the X-ray exit light hole may be covered with a window film, and the window film is a polyimide film.

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

[0008] Furthermore, an X-ray incident window shaped flange and an X-ray exit window shaped flange corresponding to the X-ray incident light hole and the X-ray exit light hole respectively may be provided on the outside of the vacuum furnace module, and the X-ray incident window shaped flange and the X-ray exit window shaped flange are connected to the vacuum furnace module by threaded connection.

[0009] Furthermore, the inner circles of the X-ray incident window shaped flange and the X-ray exit window shaped flange may be provided with a chamfer of 50°.

[0010] Furthermore, the sample chamber may be sealed using high temperature ceramic glue or graphite glue.

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

[0012] Furthermore, the high-throughput high-temperature in-situ X-ray absorption spectrum 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 a cooling medium is arranged in the pipelines.

[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 the thermocouple, a fuse connected to the 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, a method for operating a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device is provided, which may include: In the measurement mode of transmission X-ray absorption spectrum, the high-flux high-temperature in-situ X-ray absorption spectrum research device is placed vertically relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole coincide with the X-ray incident direction; or in the measurement mode of fluorescence X-ray absorption spectrum, the high-flux high-temperature in-situ X-ray absorption spectrum research device is placed at an angle of 45° relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole are at a 45° angle to the X-ray incident direction.

[0015] According to an embodiment of the present invention, a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device and an operating method thereof are provided, which have at least the following advantages: (1) real-time measurement of samples under actual working conditions can be carried out, and deterioration and leakage of samples during the test process can be effectively prevented, thereby improving the accuracy and authenticity of the experiment; (2) while ensuring the quality of measurement data in the transmission mode and the fluorescence mode, the present invention can conveniently and quickly switch the measurement mode, take into account different measurement modes, and improve the compatibility of the fluorescence measurement mode; (3) high-temperature in-situ XAFS measurement of at least two samples can be achieved under one heating, which greatly saves experimental machine time and improves machine time utilization and experimental efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The description herein refers to the drawings, wherein like reference numerals refer to like parts throughout.

[0017] Figure 1 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.

[0018] Figure 2 Schematic diagram of the structure of a heating module in a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0019] Figure 3 Schematic diagram of the structure of the special-shaped flange of the X-ray incident window in the high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0020] Figure 4 Schematic diagram of a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device in a fluorescence measurement mode according to an embodiment of the present invention.

[0021] Figure 5 The present invention is a flowchart of an operating method of a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0022] Reference numerals: 100 Vacuum furnace 110 Bottom plate 120 Support column

[0023] 130 furnace body 131 cavity 132 opening

[0024] 133 Threaded hole 134 X-ray incident light hole 136 Vacuum interface

[0025] 137, 138 Cooling medium channel interface 140 X-ray incident window special-shaped flange

[0026] 141 countersunk hole 200 heating device 210 top plate

[0027] 211 heating element 212 thermocouple 213 boss

[0028] 214, 215 cooling medium channel interface 220 sample holder

[0029] 221 groove 222 baffle 223 sample chamber DETAILED DESCRIPTION

[0030] Various embodiments of the present disclosure will be described in detail below in conjunction with 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.

[0031] In the present 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 features are included in one or more embodiments of the present disclosure, but may or may not be combined in the same embodiment.

[0032] In this disclosure, the terms "comprises", "includes", "has", and "contains" are open ended. As used in the appended claims, these terms specify the presence of the elements described but do not preclude the presence or addition of one or more other elements. The terms of the claims do not preclude the device from including additional components, such as interface units, circuits, etc.

[0033] The embodiments will now be described with reference to the drawings, wherein like reference numerals refer to like elements.

[0034] Figure 1 is a schematic structural diagram of a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention, Figure 2is a schematic diagram of the structure of a heating module in a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention, Figure 3 A schematic structural diagram of a special-shaped flange of an X-ray incident window in a high-throughput, high-temperature in-situ X-ray absorption spectrum research device according to an embodiment of the present invention is shown. Figure 4 Schematic diagram of a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device in a fluorescence measurement mode according to an embodiment of the present invention. Figures 1 to 3 The high-throughput high-temperature in-situ X-ray absorption spectroscopy research device may include a vacuum furnace (also referred to as a vacuum furnace module) 100 and a heating device (also referred to as a heating module) 200 .

[0035] In an embodiment, the vacuum furnace 100 may be located on a scissor lift table or an optical table, and the heating device 200 may be disposed above the vacuum furnace 100 .

[0036] In an embodiment, the vacuum furnace 100 may include a base plate 110, four support columns 120 may be provided on the base plate 110, a furnace body 130 may be provided on the four support columns 120, the furnace body 130 has a cavity 131 inside, an opening 132 may be provided on the top, an "O"-shaped sealing 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.

[0037] In an embodiment, the support column 120 can be composed of a screw rod and a smooth rod. The screw rod corresponds to the threaded hole at the bottom of the furnace body 130. The support column 120 is connected to the furnace body 130 through a threaded connection. A clearance groove is provided on the top of the smooth rod for convenient installation of a wrench, and a threaded hole is provided at the bottom.

[0038] In an embodiment, four countersunk holes for connecting to the furnace body 130 may be provided on the inner side of the base plate 110, each of which corresponds to the support column 120 installed at the bottom of the furnace body 130, and is connected by a threaded connection; eight through holes are provided on the outer side of the base plate 110 for fixing it on a scissor lift or an optical platform, and the center of each hole is 100 mm away from the center of the base plate 110 and the phase angle between adjacent through holes is 45°.

[0039] In an embodiment, an X-ray incident light hole 134 and a corresponding X-ray exit light hole (having the same structure and size as the X-ray incident light hole 134, not shown) may be provided on two opposite sides of the furnace body 130, and the optical axes of the X-ray incident light hole 134 and the X-ray exit light hole may be located on the same straight line.

[0040] In an embodiment, an “O” type sealing ring may be provided around the X-ray incident light hole 134 and the X-ray exit light hole.

[0041] In an embodiment, a vacuum port 136 communicating with the vacuum furnace chamber 131 may be provided on the other side of the furnace body 130 , and the vacuum port 136 may be connected to an external vacuum device (not shown, for example, a vacuum pump).

[0042] In an embodiment, the heating device 200 may include a sample holder 220, a heating element 211 and a thermocouple 212, wherein the heating element 211 and the thermocouple 212 are positioned adjacent to the sample holder 220 and are used to heat the sample holder 220 and measure the temperature. Figure 1 As shown, the heating device 200 may include a top plate 210 , a sample holder 220 may be disposed below the top plate 210 , a heating element 211 penetrating the top plate 210 and the sample holder 220 , and a thermocouple 212 penetrating the top plate 210 and extending into the sample holder 220 may be disposed above the top plate 210 .

[0043] In an embodiment, two deep holes may be symmetrically provided on both axial sides of the top plate 210 of the heating device 200 for placing the heating element 211 , and a small hole may be provided near one of the deep holes for inserting the thermocouple 212 .

[0044] In an embodiment, the front side of the sample holder 220 of the heating device 200 may be provided with a plurality of grooves for placing the sample chamber 223, a baffle 222 for fixing the sample chamber 223 is provided near the grooves, and a small hole is provided on the back side of the sample holder 220 at a position between the grooves for placing the temperature measuring end of the thermocouple 212.

[0045] In an embodiment, the sample chamber 223 may be a cuboid having a cavity of 16 mm in length, 1-3 mm in width, 15-35 mm in depth for holding the sample and a wall thickness of 1 mm around the cavity, and the material thereof is isostatic graphite, pyrolytic graphite, or boron nitride.

[0046] In an embodiment, through holes corresponding to the threaded holes 133 of the furnace body 130 of the vacuum furnace 100 may be provided at four corners of the top plate 210 of the heating device 200 , so as to achieve connection between the heating device 200 and the vacuum furnace 100 .

[0047] In an embodiment, the heating element 211 may be a resistance wire, a heating tube encapsulated with a resistance wire, a silicon carbon rod, etc. To ensure safety, attention should be paid to insulation when placing the heating device 200.

[0048] As described above, an opening 132 is provided at the top of the vacuum furnace 100 and threaded holes 133 may be provided at the four corners of the top of the furnace body 130. Therefore, the heating device 200 may extend into the vacuum furnace 100 through the opening 132 of the vacuum furnace 100, and the connection between the heating device 200 and the vacuum furnace 100 may 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.

[0049] Although it is shown above that the heating device 200 and the vacuum furnace 100 are connected and fixed by means of threaded connection, the present invention is not limited thereto, and other connection methods may also be used.

[0050] In an embodiment, a plurality of grooves for accommodating a plurality of sample chambers 223 (at least two) may be provided on the sample rack 220, and air-avoiding grooves may be provided around the grooves. Therefore, a plurality of samples may be processed at one time and the sample chambers 223 may be conveniently placed in and taken out, thereby improving work efficiency.

[0051] In order to take both transmission and fluorescence measurement modes into consideration, the shapes and sizes of the X-ray incident light hole 134 and the X-ray exit light hole of the vacuum furnace 100 may be designed.

[0052] In an embodiment, the X-ray incident light hole 134 and the X-ray exit light hole can be set to a combination shape 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.

[0053] In an embodiment, the size of the combined shape of the two semicircles and the rectangle of the X-ray incident light hole 134 and the X-ray exit light hole can be set. Taking the X-ray incident light hole 134 as an example, the size of the combined shape of the two semicircles and the rectangle of the X-ray incident light hole 134 can be set according to the distance between the sample chamber 223 and the X-ray incident light hole 134 (which can be regarded as the distance between the sample in the sample chamber 223 and the outermost side of the X-ray incident window shaped flange 140 described below).

[0054] In the fluorescence measurement mode, when the sample chamber 223 is too close to the X-ray incident light hole 134, it will affect the heating and insulation of the sample chamber 223. When it is too far away from the X-ray incident light hole 134, the X-ray incident light hole 134 needs to be designed to be very large, which results in a large volume of the entire device.

[0055] In an embodiment, the distance between the sample chamber 223 and the X-ray incident light hole 134 may be set to 24 mm, but the present invention is not limited thereto.

[0056] Taking the above distance of 24 mm as an example, in the fluorescence measurement mode, the entire device is at an angle of 45° to the incident X-ray, that is, the sample is at an angle of 45° to the incident X-ray. At this time, the incident X-ray hits the center of the sample, and the distance between the sample and the outermost side of the X-ray incident window shaped flange 140 described below is 24 mm. Therefore, in order to ensure that most of the fluorescence signal can be emitted, the minimum diameter of the window (circular, because the fluorescence signal can be regarded as the solid angle of a sphere in three dimensions) calculated according to geometry is 1.414 × 6 × 2 + 24 × 2 = 65 mm (see Figure 4 ). That is, the minimum diameter of the semicircle in the combination of the two semicircles and the rectangle of the X-ray incident light hole 134 is 65 mm. Figure 4 In order to improve the effect of fluorescence measurement, the 6 mm around the incident X-ray cannot block the light.

[0057] As described above, the horizontal length of the rectangle in the combined shape of the X-ray incident light hole 134 is equal to the semicircle diameter, and the vertical length is less than the semicircle diameter. Taking the semicircle diameter of 65 mm as an example, the vertical length of the rectangle can be set to 50 mm, but the present invention is not limited thereto.

[0058] Since the X-ray exit aperture can be designed in the same manner as the X-ray incident aperture 134 described above, the present invention omits its description here.

[0059] In an embodiment, the X-ray incident light hole 134 and the X-ray exit light hole 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 present invention is not limited thereto.

[0060] In an embodiment, a high temperature resistant carbon film may be provided inside the window film to absorb infrared heat radiation emitted by the heating device 200 during heating, so that the temperature of the window film does not exceed the upper limit of use, while eliminating the influence of infrared signals on the X-ray absorption spectrum.

[0061] Return to reference Figure 1 The X-ray incident window special-shaped flange 140 and the X-ray exit window special-shaped flange (the structure and size are the same as the X-ray incident window special-shaped flange 140, not shown) can be arranged on the outside of the furnace body 130, and can correspond to the X-ray incident light hole 134 and the X-ray exit light hole respectively, and the inner circles of the two can be the same as the shape and size of the X-ray incident light hole 134 and the X-ray exit light hole respectively.

[0062] In an embodiment, a plurality of countersunk holes 141 (as shown in the figure, for example, eight) may be provided on the X-ray incident window shaped flange 140, and a plurality of countersunk holes (with the same structure and size as the countersunk holes 141, not shown) may be provided on the X-ray exit window shaped flange, and the X-ray incident window shaped flange 140 and the X-ray exit window shaped flange may be fixed to the furnace body 130 by threaded connection.

[0063] In an embodiment, the inner circles of the X-ray incident window shaped flange 140 and the X-ray exit window shaped flange may be provided with a 50° chamfer to prevent the X-ray fluorescence signal from being blocked during fluorescence mode measurement.

[0064] In an embodiment, when testing a sample, high temperature ceramic glue or graphite glue may be used to seal the sample chamber 223 to isolate the sample from the atmosphere and prevent the sample from leaking.

[0065] In an embodiment, two sample chambers 223 containing samples may be placed on the sample holder 220 at the same time, and the height may be adjusted to achieve measurement of two samples during one heating, thereby improving efficiency.

[0066] Further integration Figures 1 to 3 , a process of connecting and sealing the vacuum furnace 100 and the heating device 200 for testing a sample is provided, as follows: First, fix the sample chamber 223 to the heating device: put the sample chamber 223 into the groove 221 of the sample holder 220. Since the four corners of the groove 221 are provided with air avoidance grooves, the sample chamber 223 can be easily put in and taken out, and then the baffle 222 is installed to fix it; then, 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, and the boss 213 extending from the bottom of 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 arranged on the top of the furnace body 130. The sealing of the vacuum furnace 100 and the heating device 200 is achieved through threaded connection.

[0067] In an embodiment, the vacuum interface 136 may be a KF flange interface, which may be connected to a vacuum gauge, a vacuum valve, and a vacuum pump, and may be quickly connected and disassembled through a vacuum clamp. The KF flange interface may be placed on the left side of the sample to adapt to the narrow space of the synchrotron radiation X-ray absorption spectrum experimental station and avoid interference with other equipment in the experimental station.

[0068] In an embodiment, the high-throughput, high-temperature in-situ X-ray absorption spectrum research device may further include a cooling medium circulation device (also referred to as a cooling medium circulation module). A cooling medium channel is provided in the furnace body 130 of the vacuum furnace 100, and interfaces 137 and 138 are provided on the outside thereof. A cooling medium channel is provided in the top plate 210 of the heating device 200, and interfaces 214 and 215 are provided on the outside thereof. A pipeline is used to connect any interface of the furnace body 130 and the top plate 210 so that the cooling medium channels of the two are connected, and 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 hole 134 and the X-ray exit light hole are at a safe working temperature.

[0069] In an embodiment, the high-throughput high-temperature in-situ X-ray absorption spectrum research device may also include an external control cabinet (also referred to as an external control module), which may include a PID temperature controller connected to the thermocouple 212, a fuse connected to the power input, and a thyristor module connecting the PID temperature controller, the heating element 211 and the fuse. The PID controller is mainly used to achieve temperature control, the fuse is used to protect the circuit, and the thyristor module is used to control the current input of the heating element 211. During the heating process, the sample is heated by applying a certain current to the heating element 211, and 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 thyristor element, thereby achieving temperature control.

[0070] Figure 5 The present invention is a flowchart of an operating method of a high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to an embodiment of the present invention.

[0071] like Figure 5 As shown, the operating method of the high-flux high-temperature in-situ X-ray absorption spectrum research device of an embodiment of the present invention includes: in the measurement mode of the transmission X-ray absorption spectrum, the high-flux high-temperature in-situ X-ray absorption spectrum research device is placed vertically relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole coincide with the X-ray incident direction; or in the measurement mode of the fluorescence X-ray absorption spectrum, the high-flux high-temperature in-situ X-ray absorption spectrum research device is placed at an angle of 45° relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole are at a 45° angle to the X-ray incident direction.

[0072] Specifically, in the measurement mode of the transmission X-ray absorption spectrum, the high-throughput high-temperature in-situ X-ray absorption spectrum research device provided by the embodiment of the present invention is placed vertically relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole 134 and the X-ray exit light hole coincide with the X-ray incident direction, and then bolted to the scissor lift or optical platform. At this time, the X-ray enters the cavity 131 from the X-ray incident light hole 134, is incident on the sample chamber 223, and the transmitted X-ray is emitted from the X-ray exit light hole.

[0073] Specifically, in the measurement mode of the fluorescence X-ray absorption spectrum, the high-throughput high-temperature in-situ X-ray absorption spectrum research device provided by the embodiment of the present invention is placed at an angle of 45° relative to the incident direction of the X-rays, and the position is adjusted so that the optical axes of the X-ray incident light hole 134 and the X-ray exit light hole are at an angle of 45° to the incident direction of the X-rays, and then bolted to the scissor lift or optical platform. At this time, the X-rays enter the cavity 131 from the X-ray incident light hole 134, and are incident on the sample chamber 223, and the generated X-ray fluorescence is also emitted from the X-ray incident light hole 134.

[0074] According to the high-throughput, high-temperature in-situ X-ray absorption spectroscopy research device and the operating method thereof provided in the embodiments of the present invention, an air-sensitive liquid molten salt sample was studied at 550 degrees Celsius, including measuring the X-ray absorption spectra of LiCl-KCl-YCl3 and α-radioactive LiCl-KCl-UCl3 and LiCl-KCl-UCl4 molten salts in the transmission mode, and measuring the X-ray absorption spectrum of LiCl-KCl-SmCl3 molten salt in the fluorescence mode. The expected experimental goals were achieved and the test efficiency was greatly improved, which proves that the device and the operating method thereof are feasible for conducting high-temperature in-situ X-ray absorption spectroscopy experiments.

[0075] According to an embodiment of the present invention, by combining the characteristics of the transmission spectrum and the fluorescence spectrum to design special-shaped X-ray incident and exit windows, both measurement modes are taken into account while ensuring data quality, and by designing multiple grooves for accommodating sample chambers on the sample holder, high-throughput measurement is achieved, effectively improving machine time utilization, and can be used for high-temperature in-situ XAFS research on conventional samples and special samples.

[0076] The methods, processes and / or operations described herein can be performed by codes or instructions run by computers, processors, controllers or other signal processing devices. Computers, processors, controllers or other signal processing devices can be devices described herein, or devices outside the elements described herein. Since the algorithms constituting the operation of the method basis or computers, processors, controllers or other signal processing devices are described in detail, the codes or instructions for implementing the operation of the method embodiments can convert computers, processors, controllers or other signal processing devices into special processors for performing the methods herein.

[0077] In addition, another embodiment may include a computer-readable medium, such as a non-transitory computer-readable medium, for storing the above code or instructions. The computer-readable medium may be a volatile or non-volatile memory or other storage device that is removably or fixedly connected to a computer, processor, controller or other signal processing device to run code or instructions for performing the operations of the method embodiments or apparatus embodiments herein.

[0078] The controllers, processors, control circuits, devices, modules, units, multiplexers, logic, interfaces, decoders, drivers, generators, and other signal generation and signal processing features of the embodiments disclosed herein may be implemented, for example, as non-transient logic, which may include hardware, software, or both. When implemented at least in part as hardware, the controllers, processors, control circuits, devices, modules, units, multiplexers, logic, interfaces, decoders, drivers, generators, and other signal generation and signal processing features may be, for example, any of a variety of 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 circuits.

[0079] Although the present teaching has been described with respect to specific embodiments, it is obvious to those skilled in the art that, according to the present disclosure, various changes and modifications may be made without departing from the spirit and scope of the present disclosure as defined in the appended claims. In addition, the 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: A vacuum furnace module, wherein the top of the vacuum furnace module is provided with an opening, two opposite sides of the vacuum furnace module are respectively provided with an X-ray incident light hole and a corresponding X-ray exit light hole whose optical axes are located 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; as well as A heating module, the heating module extends into the vacuum furnace module through the opening of the vacuum furnace module and is connected to the vacuum furnace module, the heating module comprises 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 the temperature; The X-ray incident light hole and the X-ray exit light hole have a shape of a combination of two upper and lower semicircles and a rectangle whose horizontal length is equal to the diameter of the semicircle and whose vertical length is less than the diameter of the semicircle. The sample rack is provided with a plurality of grooves for accommodating a plurality of sample chambers, and air-avoiding grooves are arranged around the grooves.

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 light hole and the X-ray exit light hole are covered with a window film, and the window film 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 arranged 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 outside of the vacuum furnace module is provided with an X-ray incident window shaped flange and an X-ray exit window shaped flange corresponding to the X-ray incident light hole and the X-ray exit light hole respectively, and the X-ray incident window shaped flange and the X-ray exit window shaped 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 circles of the X-ray incident window special-shaped flange and the X-ray exit window special-shaped flange are provided with a chamfer of 50°.

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 with high temperature ceramic glue or graphite glue.

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 by 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 comprises a cooling medium circulation module, wherein the cooling medium circulation module is connected with the vacuum furnace module and the heating module through a pipeline to form a loop, and a cooling medium is arranged in the pipeline.

9. The high-throughput high-temperature in-situ X-ray absorption spectroscopy research device according to claim 1, characterized in that: It 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 device according to any one of claims 1 to 9, characterized in that: include: In the transmission X-ray absorption spectrum measurement mode, the high-flux high-temperature in-situ X-ray absorption spectrum research device is placed vertically relative to the X-ray incident direction, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole coincide with the X-ray incident direction; or In the measurement mode of fluorescence X-ray absorption spectrum, the high-throughput high-temperature in-situ X-ray absorption spectrum research device is placed at an angle of 45° relative to the incident direction of the X-rays, and the position is adjusted so that the optical axes of the X-ray incident light hole and the X-ray exit light hole are at an angle of 45° to the incident direction of the X-rays.

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