A wide temperature range in-situ cell suitable for XAFS transmission mode

Abstract

The present invention provides a wide-temperature-range in-situ cell body suitable for XAFS transmission mode, comprising a bottom plate, the top surface of which is symmetrically fixedly connected to vertical plates, an auxiliary detection assembly installed between two sets of vertical plates, an opening and closing assembly installed on one side of the two sets of vertical plates, one end of the opening and closing assembly connected to the auxiliary detection assembly; the auxiliary detection assembly comprises a protective box, the two sets of vertical plates are fixedly connected to the protective box, the two sides of the protective box are respectively provided with circular holes, the bottom surface of the protective box is fixedly connected to an air intake connector, one side of the protective box is fixedly connected to an exhaust connector, the inner cavities of the air intake connector and the exhaust connector are respectively connected to the inner cavity of the protective box, and the two ends of the top surface of the protective box are respectively fixedly connected to a water inlet connector and a drain connector. The present invention realizes automatic loading and unloading of materials and detection of loaded materials through the mutual cooperation of the auxiliary detection assembly, the opening and closing assembly, and the loading and unloading assemblies.

Description

Technical Field

[0001] The present invention relates to the technical field of XAFS transmission mode, and in particular to a wide temperature range in-situ cell body suitable for XAFS transmission mode. Background Art

[0002] An in-situ X-ray absorption fine structure (XAFS) cell is an experimental device used to monitor local structural changes in materials under reaction conditions in real time. It is widely used in research in catalysis, energy materials (such as batteries and fuel cells), and chemical engineering. The technique can operate at high temperatures, high pressures, or in electrochemical environments, providing critical structural information about the dynamic behavior of materials under extreme conditions.

[0003] Currently, existing technologies, such as US20180052114A1 and EP3252501B1, have optimized the design of in-situ XAFS cells, focusing on improving their stability and reliability under harsh reaction conditions such as high temperature, high pressure, and corrosion resistance. These technologies meet the experimental needs of fields such as catalytic reactions and energy storage and conversion, allowing researchers to study the dynamic structural evolution of materials under conditions close to actual working conditions.

[0004] However, the application of existing technologies in low-temperature environments (such as liquid nitrogen and liquid helium temperature zones) still has significant limitations:

[0005] 1. For example, the lowest operating temperature of the high-temperature reaction pool in patent EP3252501B1 is only -50°C, which cannot cover the liquid helium temperature range;

[0006] 2. Electrochemical cell patents (e.g., US20180052114A1) focus on electrolyte management and ignore the problem of enhanced X-ray scattering caused by ice crystal formation in samples at low temperatures;

[0007] 3. XAFS experiments require the use of low-absorption X-ray transmission windows (such as polyimide, silicon nitride, etc.), but the mechanical properties and thermal stability of these materials in ultra-low temperature environments need to be optimized. Summary of the Invention

[0008] In view of the deficiencies in the prior art, the present invention provides an in-situ cell body with a wide temperature range suitable for XAFS transmission mode, which solves the problems mentioned in the background art.

[0009] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0010] A wide temperature range in-situ cell body suitable for XAFS transmission mode comprises a bottom plate, the top surface of the bottom plate is symmetrically fixedly connected to a vertical plate, an auxiliary detection component is installed between two groups of the vertical plates, an opening and closing component is installed on one side of the two groups of the vertical plates, one end of the opening and closing component is connected to the auxiliary detection component, a loading and unloading component is installed on the top surface of the bottom plate and on one side of the auxiliary detection component, one end of the auxiliary loading and unloading component is connected to the auxiliary detection component; the auxiliary detection component comprises a protection box, the protection box is fixedly connected between the two groups of the vertical plates, and circular holes are respectively provided on both sides of the protection box. An air inlet joint is fixedly connected to the bottom surface of the protection box, and an exhaust joint is fixedly connected to one side of the protection box. The inner cavities of the air inlet joint and the exhaust joint are respectively communicated with the inner cavity of the protection box. The two ends of the top surface of the protection box are respectively fixedly connected with the water inlet joint and the drainage joint. A U-shaped channel is provided inside the protection box, and the two ends of the U-shaped channel are respectively communicated with the water inlet joint and the drainage joint. A material storage component is installed in the middle of the inner cavity of the protection box, and a first sealing component and a second sealing component are respectively installed on both sides of the protection box. The first sealing component is respectively connected to the opening and closing component and the loading and unloading components.

[0011] Furthermore, the material storage component includes an H-shaped block, a nitrogen inlet joint and a nitrogen exhaust joint. The middle part of the inner cavity of the protection box is fixedly connected to the H-shaped block, the middle part of the H-shaped block is provided with a stepped placement hole, and a nitrogen channel is provided inside the H-shaped block. The top surface of the protection box is fixedly connected to the nitrogen inlet joint, and the bottom surface of the protection box is fixedly connected to the nitrogen exhaust joint. The nitrogen inlet joint and the nitrogen exhaust joint are respectively connected to the nitrogen channel.

[0012] Furthermore, the nitrogen channel includes a vertical channel and an L-shaped channel, one end of the vertical channel is connected to the nitrogen inlet joint, the middle of the vertical channel is connected to the L-shaped channel, and one end of the L-shaped channel is connected to the nitrogen exhaust joint.

[0013] Furthermore, the material storage component also includes a first thermocouple, a second thermocouple and a heating rod, one end of the first thermocouple penetrates the top surface of the protection box and extends to one side of the step placement hole, one end of the second thermocouple penetrates the bottom surface of the protection box and extends to one side of the step placement hole, the first thermocouple and the second thermocouple are staggered in front and back, and there are two groups of heating rods, one end of the two groups of heating rods respectively penetrates the top surface of the protection box and extends to both sides of the step placement hole.

[0014] Furthermore, the first sealing component includes a sealing plate, one side of the protective box is fixedly connected to the sealing plate, the two ends of one side of the sealing plate are respectively fixedly connected to the first water-cooling joint and the second water-cooling joint, a U-shaped water-cooling channel is provided inside the sealing plate, the two ends of the U-shaped water-cooling channel are respectively connected to the first water-cooling joint and the second water-cooling joint, a ray hole is provided in the middle of the sealing plate, and a beryllium plate is fixedly connected to the ray hole; the second sealing component adopts the same structure as the first sealing component.

[0015] Furthermore, the opening and closing assembly includes a sliding rail and an L-shaped rod, one side of the two groups of vertical plates is fixedly connected to the sliding rail, an I-shaped block is slidably connected in the sliding rail, the top surface of the I-shaped block is fixedly connected to a sealing plate, one side of one of the vertical plates is fixedly connected to the L-shaped rod, one side of the L-shaped rod is fixedly connected to an opening and closing hydraulic rod, and the output end of the opening and closing hydraulic rod is fixedly connected to one side of the sealing plate.

[0016] Furthermore, the loading and unloading assembly includes a workbench, the top surface of the base plate is fixedly connected to the workbench, the top surface of the workbench is respectively fixedly connected to a U-shaped frame and a flip pneumatic rod, a flip shaft is rotatably connected inside the U-shaped frame, the surface of the flip shaft is symmetrically fixedly connected to a limit bar, one end of the flip shaft surface is fixedly connected to a flip gear, the output end of the flip pneumatic rod is fixedly connected to a flip rack, and the flip rack is meshed with the flip gear.

[0017] Furthermore, the upper and lower material components also include a feeding component and a square block, an axial hole is provided in the middle of the square block, the middle of the square block slides on the surface of the flip shaft through the axial hole, a limiting hole is provided on the inner wall of the axial hole, the limiting hole slides on the surface of the limiting bar, one side of the square block is fixedly connected to a T-shaped sleeve, the surface of the T-shaped sleeve is rotatably connected to a connecting rod, one end of the connecting rod is fixedly connected to one side of the sealing plate, and a feeding component is installed on one side of the square block.

[0018] Furthermore, the feeding component includes a lifting hydraulic rod, one side of the square block is fixedly connected to the lifting hydraulic rod, the output of the lifting hydraulic rod is fixedly connected to the motor box, a switching motor is fixedly connected inside the motor box, the output end of the switching motor is rotatably connected to the switching shaft through a gear set, and one end of the switching shaft is fixedly connected to a fixed block.

[0019] Furthermore, the feeding component also includes a fixed rod and a forming cylinder, the fixed block is fixedly connected to the forming cylinder, the bottom of the inner wall of the forming cylinder is fixedly connected to a forming hydraulic rod, the output end of the forming hydraulic rod is fixedly connected to a pressure plate, one end of the forming cylinder is provided with a placement hole, a powder sheet clip is placed in the placement hole, the inner wall of the placement hole is provided with an adsorption hole, an adsorption cavity is provided inside the forming cylinder, the bottom surface of the forming cylinder is fixedly connected to the adsorption plate, the inner cavity of the adsorption plate is connected to the adsorption cavity through a three-way pipe, the top surface of the workbench is fixedly connected to the fixed rod, and one end of the fixed rod is fixedly connected to the forming cover.

[0020] The present invention provides a wide-temperature-range in-situ cell suitable for XAFS transmission mode. Compared with the prior art, it has the following advantages:

[0021] 1. The auxiliary detection component enables the testing of powder samples. During testing, the sample can be heated to a maximum of 600 degrees Celsius and cooled to a minimum of -180 degrees Celsius. Real-time monitoring is performed during heating and cooling to ensure the required temperature. The device also uses multiple U-shaped channels to protect the device during heating and cooling, ensuring that it can conduct experiments for up to 10 hours and meet the requirements of XAFS experiments under extreme temperature conditions.

[0022] 2. The sealing plate in the first sealing component can be opened and closed by the opening and closing assembly. When the sealing plate is opened, the feeding component will be driven to move so that the feeding component is located on one side of the stepped placement hole, which is convenient for later loading. When the sealing plate is closed, it will be convenient for later testing of the loaded materials. At the same time, the sealing plate will keep the feeding component away from the protective box, making it convenient for the staff to add the next powder material to be tested into the loading and unloading assembly, which is convenient for later pressing and molding for testing.

[0023] 3. Through the mutual cooperation of the flip pneumatic rod and the flip axis in the loading and unloading components, when the feeding component is in a vertical state, it is convenient for the staff to add the material to be tested, and the powdered material is pressed into granules, which is convenient for later testing. When the feeding component is in a horizontal state, the previously tested powder sheet clip is removed. After removal, the new powder sheet clip is placed in the stepped placement hole. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0025] Figure 1 Shows an overall schematic diagram of the present invention;

[0026] Figure 2 Shows another perspective schematic diagram of the present invention as a whole;

[0027] Figure 3 Shows a schematic diagram of the opening and closing assembly of the present invention;

[0028] Figure 4 A schematic diagram of the auxiliary detection component of the present invention is shown;

[0029] Figure 5 shows a schematic diagram of the first sealing component of the present invention;

[0030] Figure 6 A schematic diagram showing another perspective of the first sealing component of the present invention is shown;

[0031] Figure 7 A partial cross-sectional diagram of the first sealing component of the present invention is shown;

[0032] Figure 8 Shows a schematic diagram of the protection box of the present invention;

[0033] Figure 9 A schematic diagram of the protective box of the present invention from another perspective is shown;

[0034] Figure 10 A partial cross-sectional diagram of the protection box of the present invention is shown;

[0035] Figure 11 A partial cross-sectional schematic diagram of the protection box of the present invention from another perspective is shown;

[0036] Figure 12 Shows a schematic diagram of the loading and unloading assembly of the present invention;

[0037] Figure 13 Shows a schematic diagram of the disassembly of the loading and unloading components of the present invention;

[0038] Figure 14 A partial enlarged schematic diagram of the loading and unloading assembly of the present invention is shown;

[0039] Figure 15 A partial cross-sectional diagram of the loading and unloading assembly of the present invention is shown;

[0040] Figure 16 Another schematic diagram of the structure of the overall dynamic diagram of the present invention is shown;

[0041] As shown in the figure:

[0042] 100, bottom plate;

[0043] 200, vertical board;

[0044] 300, auxiliary detection assembly; 301, protective box; 302, circular hole; 303, air inlet connector; 304, exhaust connector; 305, water inlet connector; 306, drain connector; 307, U-shaped channel; 308, H-shaped block; 309, nitrogen inlet connector; 310, nitrogen exhaust connector; 311, stepped placement hole; 312, vertical channel; 313, L-shaped channel; 314, first thermocouple; 315, second thermocouple; 316, heating rod; 317, sealing plate; 318, first water-cooling connector; 319, second water-cooling connector; 320, U-shaped water-cooling channel; 321, ray hole; 322, beryllium sheet;

[0045] 400, opening and closing assembly; 401, slide rail; 402, L-shaped rod; 403, I-shaped block; 404, opening and closing hydraulic rod;

[0046] 500, loading and unloading assembly; 501, workbench; 502, U-shaped frame; 503, flip pneumatic rod; 504, flip shaft; 505, limit bar; 506, flip gear; 507, flip rack; 508, square block; 509, shaft hole; 510, limit hole; 511, T-shaped sleeve; 512, connecting rod; 513, lifting hydraulic rod; 514, motor box; 515, switching motor; 516, switching shaft; 517, fixing block; 518, fixing rod; 519, forming cylinder; 520, forming hydraulic rod; 521, pressure plate; 522, placement hole; 523, powder sheet clamp; 524, adsorption hole; 525, adsorption chamber; 526, adsorption plate; 527, three-way pipe; 528, forming cover. DETAILED DESCRIPTION

[0047] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0048] Example

[0049] To solve the technical problems in the background technology, the following wide temperature range in-situ cell suitable for XAFS transmission mode is provided:

[0050] Combine Figures 1-16As shown, the present invention provides a wide temperature range in-situ cell body suitable for XAFS transmission mode, including a bottom plate 100, the top surface of the bottom plate 100 is symmetrically fixedly connected with a vertical plate 200, an auxiliary detection component 300 is installed between the two groups of vertical plates 200, an opening and closing component 400 is installed on one side of the two groups of vertical plates 200, one end of the opening and closing component 400 is connected to the auxiliary detection component 300, a loading and unloading component 500 is installed on the top surface of the bottom plate 100 and located on one side of the auxiliary detection component 300, one end of the auxiliary loading and unloading component 500 is connected to the auxiliary detection component 300; the auxiliary detection component 300 includes a protective box 301, the protective box 301 is fixedly connected between the two groups of vertical plates 200, and circular holes are respectively provided on both sides of the protective box 301. 302. An air inlet connector 303 is fixedly connected to the bottom surface of the protection box 301, and an exhaust connector 304 is fixedly connected to one side of the protection box 301. The inner cavities of the air inlet connector 303 and the exhaust connector 304 are respectively connected to the inner cavity of the protection box 301. The two ends of the top surface of the protection box 301 are respectively fixedly connected to the water inlet connector 305 and the drainage connector 306. A U-shaped channel 307 is provided inside the protection box 301. The two ends of the U-shaped channel 307 are respectively connected to the water inlet connector 305 and the drainage connector 306. A material storage component is installed in the middle of the inner cavity of the protection box 301. A first sealing component and a second sealing component are respectively installed on both sides of the protection box 301. The first sealing component is respectively connected to the opening and closing component 400 and the loading and unloading component 500.

[0051] The detection of powder samples is achieved through the auxiliary detection component. During the test, the sample can be heated to a maximum of 600 degrees and dropped to a minimum of -180 degrees Celsius. It is also monitored in real time during heating and cooling to ensure the required temperature for detection. During heating and cooling, the device also protects the device through multiple U-shaped channels to prevent it from being affected, ensuring that the device can conduct experiments for up to 10 hours and will also meet the requirements of XAFS experiments under extreme temperature conditions.

[0052] By cooperating with the air inlet connector 303 and the air outlet connector 304, the protective box 301 can be evacuated to reduce the absorption and scattering of X-rays by the internal gas.

[0053] Through the cooperation among the water inlet joint 305 , the drainage joint 306 and the U-shaped channel 307 , the protection box 301 is cooled, thereby preventing the protection box 301 from being damaged due to high temperature.

[0054] In this embodiment, the material storage component includes an H-shaped block 308, a nitrogen inlet connector 309 and a nitrogen exhaust connector 310. The H-shaped block 308 is fixedly connected to the middle of the inner cavity of the protection box 301. A stepped placement hole 311 is provided in the middle of the H-shaped block 308. A nitrogen channel is provided inside the H-shaped block 308. The top surface of the protection box 301 is fixedly connected to the nitrogen inlet connector 309, and the bottom surface of the protection box 301 is fixedly connected to the nitrogen exhaust connector 310. The nitrogen inlet connector 309 and the nitrogen exhaust connector 310 are respectively connected to the nitrogen channel.

[0055] The step placement hole 311 can be used to limit the installation of the powder sheet clip 523, which is convenient for later detection and prevents the powder sheet clip 523 from escaping from the step placement hole 311 during detection.

[0056] In this embodiment, the nitrogen channel includes a vertical channel 312 and an L-shaped channel 313. One end of the vertical channel 312 is connected to the nitrogen inlet connector 309, the middle of the vertical channel 312 is connected to the L-shaped channel 313, and one end of the L-shaped channel 313 is connected to the nitrogen exhaust connector 310.

[0057] Through the cooperation of the nitrogen inlet connector 309, the nitrogen exhaust connector 310, the vertical channel 312 and the L-shaped channel 313, the sample can be quickly cooled down to -180 degrees Celsius after the nitrogen is injected.

[0058] In this embodiment, the material storage component also includes a first thermocouple 314, a second thermocouple 315 and a heating rod 316. One end of the first thermocouple 314 penetrates the top surface of the protective box 301 and extends to one side of the step placement hole 311. One end of the second thermocouple 315 penetrates the bottom surface of the protective box 301 and extends to one side of the step placement hole 311. The first thermocouple 314 and the second thermocouple 315 are staggered in front and back. There are two groups of heating rods 316. One end of the two groups of heating rods 316 respectively penetrates the top surface of the protective box 301 and extends to both sides of the step placement hole 311.

[0059] Through the cooperation of the first thermocouple 314 and the second thermocouple 315, the maximum and minimum temperatures of the sample in the H-block 308 can be detected in real time, and the feedback control system adjusts the liquid nitrogen flow and heating power according to the set temperature to ensure the accuracy of temperature control.

[0060] Through two sets of heating rods 316, the objects can be heated up to 600 degrees, which is suitable for most material testing;

[0061] In this embodiment, the first sealing component includes a sealing plate 317, and the sealing plate 317 is fixedly connected to one side of the protective box 301. The two ends of one side of the sealing plate 317 are respectively fixedly connected to the first water-cooling joint 318 and the second water-cooling joint 319. A U-shaped water-cooling channel 320 is provided inside the sealing plate 317, and the two ends of the U-shaped water-cooling channel 320 are respectively connected to the first water-cooling joint 318 and the second water-cooling joint 319. A ray hole 321 is provided in the middle of the sealing plate 317, and a beryllium plate 322 is fixedly connected to the ray hole 321; the second sealing component adopts the same structure as the first sealing component.

[0062] The first water-cooling joint 318, the second water-cooling joint 319 and the U-shaped water-cooling channel 320 cooperate with each other to cool the sealing plate 317, thereby preventing the sealing plate 317 from being damaged or poorly sealed due to high temperature.

[0063] The beryllium sheet 322 can ensure the penetration and filtration of X-rays, and can also prevent damage in high and low temperature conditions.

[0064] In this embodiment, the opening and closing assembly 400 includes a sliding rail 401 and an L-shaped rod 402. The sliding rail 401 is fixedly connected to one side of the two groups of vertical plates 200. An I-shaped block 403 is slidably connected inside the sliding rail 401. The top surface of the I-shaped block 403 is fixedly connected to a sealing plate 317. One side of one of the vertical plates 200 is fixedly connected to the L-shaped rod 402. One side of the L-shaped rod 402 is fixedly connected to an opening and closing hydraulic rod 404. The output end of the opening and closing hydraulic rod 404 is fixedly connected to one side of the sealing plate 317.

[0065] The sealing plate in the first sealing component can be opened and closed through the opening and closing component 400. When the sealing plate is opened, it will drive the movement of the feeding component so that the feeding component is located on one side of the stepped placement hole, which is convenient for later loading. The closing of the sealing plate will facilitate the later inspection of the loaded material. At the same time, the sealing plate will keep the feeding component away from the protective box 301, making it convenient for the staff to add the next powder material that needs to be tested into the loading and unloading component 500, which is convenient for the later pressing and molding for inspection.

[0066] In this embodiment, the loading and unloading assembly 500 includes a workbench 501, the top surface of the base plate 100 is fixedly connected to the workbench 501, the top surfaces of the workbench 501 are respectively fixedly connected to a U-shaped frame 502 and a flipping pneumatic rod 503, a flipping shaft 504 is rotatably connected inside the U-shaped frame 502, the surface of the flipping shaft 504 is symmetrically fixedly connected to a limit bar 505, one end of the surface of the flipping shaft 504 is fixedly connected to a flipping gear 506, the output end of the flipping pneumatic rod 503 is fixedly connected to a flipping rack 507, and the flipping rack 507 is meshed with the flipping gear 506.

[0067] By flipping the pneumatic rod 503, the flip shaft 504 is driven to rotate, thereby driving the rotation of the square block 508 and the feeding component. When the feeding component is in a vertical state, it is convenient for the staff to add materials that need to be tested, and the powdered materials are pressed into granules to facilitate subsequent testing. When the feeding component is in a horizontal state, the previously tested powder sheet clip 523 is removed. After removal, the new powder sheet clip 523 is placed in the stepped placement hole 311.

[0068] In this embodiment, the loading and unloading assembly 500 also includes a feeding component and a square block 508. An axial hole 509 is provided in the middle of the square block 508. The middle of the square block 508 slides on the surface of the flip shaft 504 through the axial hole 509. A limiting hole 510 is provided on the inner wall of the axial hole 509. The limiting hole 510 slides on the surface of the limiting bar 505. A T-shaped sleeve 511 is fixedly connected to one side of the square block 508. The surface of the T-shaped sleeve 511 is rotatably connected to a connecting rod 512. One end of the connecting rod 512 is fixedly connected to one side of the sealing plate 317. A feeding component is installed on one side of the square block 508.

[0069] Through the connecting rod 512, the sealing plate 317 can drive the feeding component to slide along the flip axis 504 during the movement, so as to facilitate the feeding component to one side of the protection box 301 for later loading, or to transport it to the side away from the protection box 301 for later manual feeding.

[0070] In this embodiment, the feeding component includes a lifting hydraulic rod 513, and the lifting hydraulic rod 513 is fixedly connected to one side of the square block 508. The output of the lifting hydraulic rod 513 is fixedly connected to the motor box 514, and the switching motor 515 is fixedly connected inside the motor box 514. The output end of the switching motor 515 is connected to the switching shaft 516 through a gear set, and one end of the switching shaft 516 is fixedly connected to the fixed block 517.

[0071] By cooperating with each other by lifting the hydraulic rod 513 and switching the motor 515, the subsequent loading and unloading of materials can be facilitated.

[0072] In this embodiment, the feeding component also includes a fixed rod 518 and a forming cylinder 519. The forming cylinder 519 is fixedly connected to the fixed block 517, and the forming hydraulic rod 520 is fixedly connected to the bottom of the inner wall of the forming cylinder 519. The output end of the forming hydraulic rod 520 is fixedly connected to the pressure plate 521. A placement hole 522 is provided at one end of the forming cylinder 519, and a powder sheet clip 523 is placed in the placement hole 522. An adsorption hole 524 is provided on the inner wall of the placement hole 522. An adsorption chamber 525 is provided inside the forming cylinder 519. The bottom surface of the forming cylinder 519 is fixedly connected to the adsorption plate 526. The inner cavity of the adsorption plate 526 is connected to the adsorption chamber 525 through a three-way pipe 527. The top surface of the workbench 501 is fixedly connected to the fixed rod 518, and one end of the fixed rod 518 is fixedly connected to the forming cover 528.

[0073] Through the cooperation of the forming cylinder 519, the forming hydraulic rod 520, the pressure plate 521, the placement hole 522 and the forming cover 528, the powder material can be pressed into granules, which is convenient for subsequent loading and testing.

[0074] Through the cooperation between the adsorption hole 524 and the adsorption cavity 525, the pressed powder sheet clip 523 can be adsorbed and fixed in the forming cylinder 519, which is convenient for subsequent transportation and loading.

[0075] The adsorption plate 526 facilitates the removal of the powder sheet clip 523 from the stepped placement hole 311 later.

[0076] The working principle and use process of the present invention:

[0077] In use:

[0078] Preparation before loading;

[0079] First, the staff puts the powder to be tested into the forming cylinder 519, and the powder will fall onto the top of the pressing plate 521. After a certain amount of powder is put in, the addition will stop and the powder clip 523 will be installed. When placing the powder clip 523, first align the large diameter of the powder clip 523 with the placement hole 522 and put it in. After it is placed, the material preparation is completed.

[0080] Pressing powder into shape:

[0081] First, the lifting hydraulic rod 513 is started, and the lifting hydraulic rod 513 will drive the forming cylinder 519 to move upward. As the forming cylinder 519 moves, the top surface of the forming cylinder 519 will contact the bottom surface of the forming cover 528. After the contact, the forming cylinder 519 can be sealed, and the sealed forming cylinder 519 will fix the powder sheet clamp 523 in the placement hole 522. At this time, the molding hydraulic rod 520 is started, and the molding hydraulic rod 520 will drive the pressure plate 521 and the powder on the top surface of the pressure plate 521 to move upward, so that the powder enters the powder sheet clamp 523 and presses the powder into sheets, so that the sheet-shaped powder is located in the powder sheet clamp 523. After the pressing and molding, the molding hydraulic rod 520 will stop pressing, and at the same time, the lifting hydraulic rod 513 will be started again, so that the lifting hydraulic rod 513 drives the forming cylinder 519 to move downward, and separates the forming cylinder 519 from the forming cover 528.

[0082] Adjust the angle of the forming cylinder 519;

[0083] Due to the reset of the forming cylinder 519, at this time, the external vacuum pump is started, and the vacuum pump will use the vacuum tube to start adsorption vacuum to the adsorption chamber 525. When the adsorption chamber 525 is evacuated, at this time, under the action of the adsorption hole 524, the powder sheet clip 523 is adsorbed and fixed in the placement hole 522, thereby preventing the powder sheet clip 523 from escaping from the placement hole 522 when the angle is adjusted; after adsorption, at this time, the flip pneumatic rod 503 is started, and when the flip pneumatic rod 503 works, it will drive the flip rack 507 to move When the flip rack 507 moves, the flip gear 506 is driven to rotate, thereby driving the flip shaft 504 and the limit bar 505 to rotate. When the flip shaft 504 rotates, the square block 508 is driven to rotate, thereby driving the lifting hydraulic rod 513, the motor box 514, the forming cylinder 519, the powder sheet clamp 523, etc. to rotate. When the forming cylinder 519 rotates, it will turn the forming cylinder 519 from a vertical state to a horizontal state, and the flip pneumatic rod 503 will stop working.

[0084] Prepare for loading:

[0085] First, the staff will remove all the bolts on one side of the sealing plate 317 on the first sealing component. After removal, the sealing plate 317 will no longer be fixed to the protection box 301. At this time, the opening and closing hydraulic rod 404 is started. The opening and closing hydraulic rod 404 will push the I-shaped block 403 and the sealing plate 317 to move. When the sealing plate 317 moves, the connecting rod 512 will be driven to move. When the connecting rod 512 moves, the square block 508 will be driven to slide along the surface of the flip shaft 504. When the square block 508 moves, the forming cylinder 519 will be driven to move. When the sealing plate 317 moves, the connecting rod 512 will be driven to move. When the forming cylinder 519 is completely moved away from one side of the protection box 301, the forming cylinder 519 will also move to the center of the circular hole 302. At this time, the opening and closing hydraulic rod 404 stops working, and at the same time, the lifting hydraulic rod 513 is started. When the lifting hydraulic rod 513 works, it will drive the forming cylinder 519 to move toward one side of the H-shaped block 308, and after one side of the forming cylinder 519 contacts one side of the H-shaped block 308, the lifting hydraulic rod 513 will stop working, and at the same time, the forming hydraulic rod 520 will be started. When the forming hydraulic rod 520 works, the powder sheet clip 523 containing powder can be pushed into the stepped placement hole 311. The loading is completed. After loading, the lifting hydraulic rod 513 will drive the forming cylinder 519 to reset. After resetting, the opening and closing hydraulic rod 404 will drive the forming cylinder 519 and the sealing plate 317 to reset. After the sealing plate 317 is reset, the staff will fix the sealing plate 317 to the protection box 301 through bolts; (Before loading, it may be necessary to remove the powder sheet clip 523 in the step placement hole 311. When removing it, first, start the switching motor 515. The switching motor 515 drives the switching shaft 516 to rotate. When the switching shaft 516 rotates, it will drive the fixing block 517 rotates, so that the positions of the forming cylinder 519 and the adsorption disk 526 are swapped. After the swap, the hydraulic rod 513 is lifted to make one side of the adsorption disk 526 contact with the powder sheet clamp 523 after detection. After contact, the powder sheet clamp 523 is adsorbed on the side of the adsorption disk 526 by using an external vacuum pump. After adsorption, the hydraulic rod 513 is lifted to drive the forming cylinder 519 and the adsorption disk 526 to reset. After reset, the positions of the adsorption disk 526 and the forming cylinder 519 are switched again by the switching motor 515. After the switch, it is convenient to load the new powder sheet clamp 523 later.

[0086] Prepare for testing:

[0087] During testing, first, the staff heats or cools the material according to the test requirements:

[0088] During heating, by starting the two sets of heating rods 316, the heating rods 316 begin to heat the H-shaped block 308. During heating, the first thermocouple 314 and the second thermocouple 315 are used to detect the H-shaped block 308 in real time, and the information during the detection is transmitted to the external display screen for the convenience of the staff to watch it later. The maximum temperature of the heating rod 316 can be heated to 600 degrees Celsius. When the powder in the powder sheet holder 523 is heated, the external water pump is started. The water pump injects external cooling water into the water inlet joint 305 and the first water cooling joint 318 respectively. At this time, the cooling water will be respectively from the U-shaped channel 307 and the U-shaped water cooling channel 320. The powder flows through the protective box 301 and is finally discharged from the drainage joint 306 and the second water-cooling joint 319 respectively to prevent the protective box 301, the first sealing component and the second sealing component from overheating due to high temperature. When the powder is heated to the specified temperature, the heating is stopped and the external vacuum pump is started. When the vacuum pump is working, it will evacuate the inside of the protective box 301 under the action of the exhaust joint 304 to prevent the X-rays from being absorbed or scattered by the air inside. After evacuation, the X-rays will enter from one side of the first sealing component and exit from the other side of the second sealing component. Since beryllium sheets are used, they can withstand high temperatures and ensure the transmission rate.

[0089] During the temperature drop test, it is only necessary to discharge the liquid nitrogen from the outside through the nitrogen inlet connector 309. The discharged liquid nitrogen will enter the vertical channel 312, and then flow into the L-shaped channel 313 from the vertical channel 312. Finally, it will be discharged from the nitrogen exhaust connector 310. The discharged nitrogen will begin to cool the powder on the powder sheet holder 523. When the temperature drops to the specified temperature, it will be vacuumed. After vacuuming, X-ray detection will be performed.

[0090] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply the existence of any such actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or elements inherent to such process, method, article, or device. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or device comprising the element.

[0091] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A wide temperature range in-situ cell suitable for XAFS transmission mode, characterized by: The invention comprises a bottom plate, the top surface of which is symmetrically fixedly connected to a vertical plate, an auxiliary detection component is installed between two groups of the vertical plates, an opening and closing component is installed on one side of the two groups of the vertical plates, one end of the opening and closing component is connected to the auxiliary detection component, and a loading and unloading component is installed on the top surface of the bottom plate and on one side of the auxiliary detection component, one end of the loading and unloading component is connected to the auxiliary detection component; The auxiliary detection assembly includes a protection box, a protection box is fixedly connected between the two groups of vertical plates, circular holes are respectively provided on both sides of the protection box, an air inlet joint is fixedly connected to the bottom surface of the protection box, an exhaust joint is fixedly connected to one side of the protection box, the inner cavities of the air inlet joint and the exhaust joint are respectively communicated with the inner cavity of the protection box, the two ends of the top surface of the protection box are respectively fixedly connected with the water inlet joint and the drainage joint, a U-shaped channel is provided inside the protection box, the two ends of the U-shaped channel are respectively communicated with the water inlet joint and the drainage joint, a material storage component is installed in the middle of the inner cavity of the protection box, a first sealing component and a second sealing component are respectively installed on both sides of the protection box, and the first sealing component is respectively connected to the opening and closing component and the loading and unloading component; The loading and unloading assembly includes a workbench, the top surface of the base plate is fixedly connected to the workbench, the top surface of the workbench is respectively fixedly connected to a U-shaped frame and a flip pneumatic rod, a flip shaft is rotatably connected inside the U-shaped frame, the surface of the flip shaft is symmetrically fixedly connected to a limit bar, one end of the flip shaft surface is fixedly connected to a flip gear, the output end of the flip pneumatic rod is fixedly connected to a flip rack, and the flip rack is meshed with the flip gear; The upper and lower material components also include a feeding component and a square block, an axial hole is provided in the middle of the square block, the middle of the square block slides on the surface of the flip shaft through the axial hole, a limiting hole is provided on the inner wall of the axial hole, the limiting hole slides on the surface of the limiting bar, one side of the square block is fixedly connected to a T-shaped sleeve, the surface of the T-shaped sleeve is rotatably connected to a connecting rod, one end of the connecting rod is fixedly connected to one side of the sealing plate, and a feeding component is installed on one side of the square block; The feeding component includes a lifting hydraulic rod, one side of the square block is fixedly connected to the lifting hydraulic rod, the output of the lifting hydraulic rod is fixedly connected to the motor box, the motor box is fixedly connected to the switching motor, the output end of the switching motor is rotatably connected to the switching shaft through a gear set, and one end of the switching shaft is fixedly connected to a fixed block; The feeding component also includes a fixed rod and a forming cylinder, the fixed block is fixedly connected to the forming cylinder, the bottom of the inner wall of the forming cylinder is fixedly connected to a forming hydraulic rod, the output end of the forming hydraulic rod is fixedly connected to a pressure plate, one end of the forming cylinder is provided with a placement hole, a powder sheet clip is placed in the placement hole, the inner wall of the placement hole is provided with an adsorption hole, an adsorption cavity is provided inside the forming cylinder, the bottom surface of the forming cylinder is fixedly connected to the adsorption plate, the inner cavity of the adsorption plate is connected to the adsorption cavity through a three-way pipe, the top surface of the workbench is fixedly connected to the fixed rod, and one end of the fixed rod is fixedly connected to the forming cover.

2. The wide temperature range in-situ cell suitable for XAFS transmission mode according to claim 1, characterized in that: The material storage component includes an H-shaped block, a nitrogen inlet joint and a nitrogen exhaust joint. The H-shaped block is fixedly connected to the middle of the inner cavity of the protection box. A stepped placement hole is provided in the middle of the H-shaped block. A nitrogen channel is provided inside the H-shaped block. The top surface of the protection box is fixedly connected to the nitrogen inlet joint, and the bottom surface of the protection box is fixedly connected to the nitrogen exhaust joint. The nitrogen inlet joint and the nitrogen exhaust joint are respectively connected to the nitrogen channel.

3. The wide temperature range in-situ cell suitable for XAFS transmission mode according to claim 2, characterized in that: The nitrogen channel includes a vertical channel and an L-shaped channel. One end of the vertical channel is connected to the nitrogen inlet joint, the middle of the vertical channel is connected to the L-shaped channel, and one end of the L-shaped channel is connected to the nitrogen exhaust joint.

4. The wide temperature range in-situ cell suitable for XAFS transmission mode according to claim 3, characterized in that: The material storage component also includes a first thermocouple, a second thermocouple and a heating rod. One end of the first thermocouple passes through the top surface of the protection box and extends to one side of the step placement hole. One end of the second thermocouple passes through the bottom surface of the protection box and extends to one side of the step placement hole. The first thermocouple and the second thermocouple are staggered in front and back. There are two groups of heating rods in total. One end of the two groups of heating rods respectively passes through the top surface of the protection box and extends to both sides of the step placement hole.

5. The wide temperature range in-situ cell suitable for XAFS transmission mode according to claim 4, characterized in that: The first sealing component includes a sealing plate, one side of the protective box is fixedly connected to the sealing plate, the two ends of one side of the sealing plate are respectively fixedly connected to the first water-cooling joint and the second water-cooling joint, a U-shaped water-cooling channel is provided inside the sealing plate, the two ends of the U-shaped water-cooling channel are respectively connected to the first water-cooling joint and the second water-cooling joint, a ray hole is provided in the middle of the sealing plate, and a beryllium plate is fixedly connected to the ray hole; the second sealing component adopts the same structure as the first sealing component.

6. The wide temperature range in-situ cell suitable for XAFS transmission mode according to claim 5, characterized in that: The opening and closing assembly includes a sliding rail and an L-shaped rod. One side of the two groups of vertical plates is fixedly connected to the sliding rail. An I-shaped block is slidably connected in the sliding rail. The top surface of the I-shaped block is fixedly connected to a sealing plate. One side of one of the vertical plates is fixedly connected to the L-shaped rod. One side of the L-shaped rod is fixedly connected to an opening and closing hydraulic rod. The output end of the opening and closing hydraulic rod is fixedly connected to one side of the sealing plate.

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