Wide-temperature-zone in-situ pool body suitable for XAFS transmission mode

By designing a wide temperature zone in situ pool suitable for XAFS transmission mode, the limitations of application in the existing technology in low temperature environments are solved, and the stable detection of samples in the extreme temperature range is achieved, ensuring the reliability and accuracy of XAFS experiments.

CN120352456AActive Publication Date: 2025-07-22HEFEI IN-SITU TECH CO LTD

Patent Information

Application Number
CN202510840346.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-23
Publication Date
2025-07-22
Estimated Expiration
2045-06-23

AI Technical Summary

Technical Problem

The existing XAFS in situ pools have limitations in the application of low temperature environments, especially the insufficient coverage of liquid nitrogen and liquid helium temperature zones, and the formation of sample ice crystals at low temperatures leads to enhanced X-ray scattering, and the mechanical properties and thermal stability of the transmission window materials in extremely low temperature environments are insufficient.

Method used

A wide temperature zone in-situ pool suitable for XAFS transmission mode is designed, including auxiliary detection components, opening and closing components and loading and unloading components. The high and low temperature control and sealing of samples are achieved through a variety of channels and sealing structures, and the temperature regulation and protection of nitrogen channels and water-cooling systems are combined to ensure the stability of the device under extreme temperature conditions.

Benefits of technology

Real-time temperature monitoring and control of the sample in the range of minus 180 degrees to 600 degrees is achieved, ensuring that the device operates stably in experiments up to 10 hours, meeting the XAFS experimental needs under extreme temperature conditions, and avoiding the influence of X-ray absorption and scattering.

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Abstract

The invention provides a wide-temperature-zone in-situ pool body suitable for an XAFS transmission mode. The wide-temperature-zone in-situ pool body comprises a bottom plate, vertical plates are symmetrically and fixedly connected to the top face of the bottom plate, an auxiliary detection assembly is installed between the two vertical plates, an opening and closing assembly is installed on one sides of the two vertical plates, and one end of the opening and closing assembly is connected with the auxiliary detection assembly; the auxiliary detection assembly comprises a protection box, the protection box is fixedly connected between the two sets of vertical plates, round holes are formed in the two sides of the protection box respectively, an air inlet connector is fixedly connected to the bottom face of the protection box, and an exhaust connector is fixedly connected to one side of the protection box; inner cavities of the air inlet connector and the air outlet connector are communicated with an inner cavity of the protection box, and the two ends of the top face of the protection box are fixedly connected with a water inlet connector and a water drainage connector respectively. Through mutual cooperation of the auxiliary detection assembly, the opening and closing assembly and the feeding and discharging assembly, automatic feeding and discharging can be achieved, and fed materials can be detected.
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Description

Technical Field

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

[0002] The X-ray absorption fine structure (XAFS) in-situ cell is an experimental device for real-time monitoring of local structural changes of materials under reaction conditions, and is widely used in the research of fields such as catalysis, energy materials (such as batteries, fuel cells), and chemical engineering. This technology can work in high-temperature, high-pressure or electrochemical environments, providing key structural information for the dynamic behavior of materials under extreme conditions; Currently, in the prior art such as US20180052114A1 and EP3252501B1, the design of the XAFS in-situ cell has been optimized, mainly focusing on improving its stability and reliability under harsh reaction conditions such as high temperature, high pressure, and corrosion resistance. These technologies meet the experimental requirements in fields such as catalytic reactions, energy storage and conversion, enabling researchers to study the dynamic structural evolution of materials under conditions close to actual working conditions; However, the application of the prior art in low-temperature environments (such as liquid nitrogen, liquid helium temperature ranges) still has significant limitations: 1. The minimum operating temperature of the high-temperature reaction cell in the patent EP3252501B1 is only -50°C, and it cannot cover the liquid helium temperature range; 2. Electrochemical cell patents (such as US20180052114A1) focus on electrolyte management and ignore the problem of enhanced X-ray scattering caused by the formation of ice crystals in the sample at low temperatures; 3. XAFS experiments require the use of X-ray transmission windows with low absorption rates (such as polyimide, silicon nitride, etc.), but the mechanical properties and thermal stability of these materials in extremely low-temperature environments still need to be optimized. Summary of the Invention

[0003] Aiming at the deficiencies of the prior art, the present invention provides a wide-temperature in-situ cell suitable for XAFS transmission mode, which solves the problems mentioned in the background art.

[0004] To achieve the above objectives, the present invention is realized through the following technical solutions: An in-situ cell body with a wide temperature range suitable for the XAFS transmission mode, including a bottom plate. On the top surface of the bottom plate, vertical plates are symmetrically and fixedly connected. An auxiliary detection component is installed between the two groups of vertical plates. An opening and closing component is installed on one side of the two groups of vertical plates. One end of the opening and closing component is connected to the auxiliary detection component. On the top surface of the bottom plate and on one side of the auxiliary detection component, a loading and unloading component is installed. One end of the auxiliary loading and unloading component is connected to the auxiliary detection component; the auxiliary detection component includes a protection box. A protection box is fixedly connected between the two groups of vertical plates. Round holes are respectively arranged 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. At both ends of the top surface of the protection box, a water inlet joint and a drain joint are respectively fixedly connected. A U-shaped channel is arranged inside the protection box. The two ends of the U-shaped channel are respectively communicated with the water inlet joint and the drain 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. The first sealing component is respectively connected to the opening and closing component and the loading and unloading component.

[0005] Further, the material storage component includes an H-shaped block, a nitrogen inlet joint and a nitrogen outlet joint. An H-shaped block is fixedly connected to the middle of the inner cavity of the protection box. A stepped placement hole is arranged in the middle of the H-shaped block. A nitrogen channel is arranged inside the H-shaped block. A nitrogen inlet joint is fixedly connected to the top surface of the protection box. A nitrogen outlet joint is fixedly connected to the bottom surface of the protection box. The nitrogen inlet joint and the nitrogen outlet joint are respectively communicated with the nitrogen channel.

[0006] Further, the nitrogen channel includes a vertical channel and an L-shaped channel. One end of the vertical channel is communicated with the nitrogen inlet joint. The middle of the vertical channel is communicated with the L-shaped channel. One end of the L-shaped channel is communicated with the nitrogen outlet joint.

[0007] Further, the material storage component also includes a first thermocouple, a second thermocouple and a heating rod. One end of the first thermocouple penetrates through the top surface of the protection box and extends to one side of the stepped placement hole. One end of the second thermocouple penetrates through the bottom surface of the protection box and extends to one side of the stepped placement hole. The first thermocouple and the second thermocouple are arranged in a front-back staggered manner. There are two groups of heating rods in total. One ends of the two groups of heating rods respectively penetrate through the top surface of the protection box and extend to both sides of the stepped placement hole.

[0008] Further, the first sealing component includes a sealing plate. One side of the protection box is fixedly connected with the sealing plate. At both ends of one side of the sealing plate, a first water-cooling joint and a second water-cooling joint are respectively fixedly connected. Inside the sealing plate, a U-shaped water-cooling channel is arranged. Both ends of the U-shaped water-cooling channel are internally communicated with the first water-cooling joint and the second water-cooling joint respectively. A ray hole is arranged in the middle of the sealing plate, and a beryllium sheet is fixedly connected in the ray hole; the second sealing component has the same structure as the first sealing component.

[0009] Further, the opening and closing component includes a slide rail and an L-shaped rod. One side of the two vertical plates is fixedly connected with the slide rail. An I-shaped block is slidably connected in the slide rail. The top surface of the I-shaped block is fixedly connected with the sealing plate. One side of one of the vertical plates is fixedly connected with the L-shaped rod. One side of the L-shaped rod is fixedly connected with an opening and closing hydraulic rod, and the output end of the opening and closing hydraulic rod is fixedly connected with one side of the sealing plate.

[0010] Further, the loading and unloading component includes a workbench. The top surface of the bottom plate is fixedly connected with the workbench. A U-shaped frame and a flipping pneumatic rod are respectively fixedly connected to the top surface of the workbench. A flipping shaft is rotatably connected inside the U-shaped frame. Limiting strips are symmetrically fixedly connected to the surface of the flipping shaft. One end of the surface of the flipping shaft is fixedly connected with a flipping gear. The output end of the flipping pneumatic rod is fixedly connected with a flipping rack, and the flipping rack is meshed with the flipping gear.

[0011] Further, the loading and unloading component further includes a feeding component and a square block. A shaft hole is arranged in the middle of the square block. The middle of the square block is slidably located on the surface of the flipping shaft through the shaft hole. A limiting hole is arranged on the inner wall of the shaft hole, and the limiting hole is slidably located on the surface of the limiting strip. One side of the square block is fixedly connected with a T-shaped sleeve. A connecting rod is rotatably connected to the surface of the T-shaped sleeve. One end of the connecting rod is fixedly connected with one side of the sealing plate. A feeding component is installed on one side of the square block.

[0012] Further, the feeding component includes a lifting hydraulic rod. One side of the square block is fixedly connected with the lifting hydraulic rod. The output of the lifting hydraulic rod is fixedly connected with a motor box. A switching motor is fixedly connected inside the motor box. The output end of the switching motor is rotationally connected with a switching shaft through a gear set. One end of the switching shaft is fixedly connected with a fixing block.

[0013] Further, the feeding component further includes a fixing rod and a forming cylinder. The forming cylinder is fixedly connected inside the fixing block. At the bottom of the inner wall of the forming cylinder, there is a fixedly connected forming hydraulic rod. The output end of the forming hydraulic rod is fixedly connected with a pressing plate. One end of the forming cylinder is provided with a placing hole. A powder sheet clip is placed in the placing hole. The inner wall of the placing hole is provided with adsorption holes. An adsorption cavity is arranged inside the forming cylinder. The bottom surface of the forming cylinder is fixedly connected with an adsorption disc. The inner cavity of the adsorption disc is communicated with the adsorption cavity through a three-way pipe. The top surface of the workbench is fixedly connected with a fixing rod, and one end of the fixing rod is fixedly connected with a forming cover.

[0014] The present invention provides an in-situ cell body with a wide temperature range suitable for the XAFS transmission mode. Compared with the prior art, it has the following beneficial effects: 1. The detection of powder samples is realized through the auxiliary detection component. During the detection, the sample can be heated up to 600 degrees at most and cooled down to minus 180 degrees at least. And during heating and cooling, it is monitored in real time to ensure the required temperature for detection. During heating and cooling, the device is also protected by multiple U-shaped channels, so that the device is not affected, ensuring that the device can conduct experiments for up to 10 hours and also meeting the XAFS experiment requirements under extreme temperature conditions; 2. The opening and closing of the sealing plate in the first sealing component can be realized through the opening and closing component. When the sealing plate is opened, it will drive the movement of the feeding component, making the feeding component located on one side of the stepped placing hole, facilitating later feeding. And when the sealing plate is closed, it will facilitate the later detection of the fed materials. At the same time, the sealing plate will make the feeding component away from the protection box, facilitating the staff to add the next powder material to be detected into the loading and unloading component, and facilitating later pressing and forming for detection; 3. Through the mutual cooperation of the flipping pneumatic rod and the flipping shaft in the loading and unloading component, when the feeding component is in a vertical state, it is convenient for the staff to add the materials to be detected and press the powdery materials into granular form, facilitating later detection. When the feeding component is in a horizontal state, the previously detected powder sheet clip is removed. After removal, a new powder sheet clip is placed into the stepped placing hole. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0016] Figure 1 Shows the overall schematic diagram of the present invention; Figure 2 Shows another perspective schematic diagram of the whole of the present invention; Figure 3 Shows a schematic diagram of the opening and closing assembly of the present invention; Figure 4 Shows a schematic diagram of the auxiliary detection assembly of the present invention; Figure 5 Shows a schematic diagram of the first sealing member of the present invention; Figure 6 Shows another perspective schematic diagram of the first sealing member of the present invention; Figure 7 Shows a partial sectional schematic diagram of the first sealing member of the present invention; Figure 8 Shows a schematic diagram of the protection box of the present invention; Figure 9 Shows another perspective schematic diagram of the protection box of the present invention; Figure 10 Shows a partial sectional schematic diagram of the protection box of the present invention; Figure 11 Shows a partial sectional schematic diagram of another perspective of the protection box of the present invention; Figure 12 Shows a schematic diagram of the loading and unloading assembly of the present invention; Figure 13 Shows a disassembled schematic diagram of the loading and unloading assembly of the present invention; Figure 14 Shows a partially enlarged schematic diagram of the loading and unloading assembly of the present invention; Figure 15 Shows a partial sectional schematic diagram of the loading and unloading assembly of the present invention; Figure 16 Shows another dynamic structure schematic diagram of the whole of the present invention; As shown in the figure: 100, bottom plate; 200, vertical plate; 300, auxiliary detection assembly; 301, protection box; 302, round hole; 303, air inlet joint; 304, exhaust joint; 305, water inlet joint; 306, drain joint; 307, U-shaped channel; 308, H-shaped block; 309, nitrogen inlet joint; 310, nitrogen discharge joint; 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 joint; 319, second water cooling joint; 320, U-shaped water cooling channel; 321, ray hole; 322, beryllium sheet; 400, opening and closing assembly; 401, slide rail; 402, L-shaped rod; 403, I-shaped block; 404, opening and closing hydraulic rod; 500. Loading and unloading assembly; 501. Workbench; 502. U-shaped frame; 503. Tipping pneumatic rod; 504. Tipping shaft; 505. Limit strip; 506. Tipping gear; 507. Tipping 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. Fixed block; 518. Fixed rod; 519. Forming cylinder; 520. Forming hydraulic rod; 521. Pressure plate; 522. Placing hole; 523. Powder sheet clip; 524. Adsorption hole; 525. Adsorption cavity; 526. Adsorption disc; 527. Three-way pipe; 528. Forming cover. Detailed implementation manners

[0017] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below. Apparently, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.

[0018] Embodiment To solve the technical problems in the background art, the following in-situ cell body with a wide temperature range applicable to the XAFS transmission mode is provided: Combined with Figures 1 - 16As shown in the figure, an in-situ cell body with a wide temperature range suitable for the XAFS transmission mode provided by the present invention includes a bottom plate 100. On the top surface of the bottom plate 100, vertical plates 200 are symmetrically and fixedly connected. An auxiliary detection component 300 is installed between the two groups of vertical plates 200. One side of the two groups of vertical plates 200 is provided with an opening and closing component 400. One end of the opening and closing component 400 is connected to the auxiliary detection component 300. On the top surface of the bottom plate 100 and on one side of the auxiliary detection component 300, a loading and unloading component 500 is installed. 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 protection box 301. A protection box 301 is fixedly connected between the two groups of vertical plates 200. Circular holes 302 are respectively arranged on both sides of the protection box 301. An air inlet joint 303 is fixedly connected to the bottom surface of the protection box 301. An exhaust joint 304 is fixedly connected to one side of the protection box 301. The inner cavities of the air inlet joint 303 and the exhaust joint 304 are respectively communicated with the inner cavity of the protection box 301. Water inlet joints 305 and drain joints 306 are respectively fixedly connected to both ends of the top surface of the protection box 301. A U-shaped channel 307 is arranged inside the protection box 301. Both ends of the U-shaped channel 307 are internally communicated with the water inlet joint 305 and the drain joint 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.

[0019] The detection of powder samples is realized through the auxiliary detection component. During the detection, the sample can be heated up to 600 degrees at most and cooled down to minus 180 degrees at least. And it is monitored in real time during heating and cooling to ensure the required temperature for detection. During heating and cooling, the device is also protected by multiple U-shaped channels, so that the device is not affected, ensuring that the device can conduct experiments for up to 10 hours and also meeting the XAFS experiment requirements under extreme temperature conditions.

[0020] Through the mutual cooperation of the air inlet joint 303 and the exhaust joint 304, the protection box 301 can be evacuated, reducing the absorption and scattering of X-rays by the internal gas; Through the mutual cooperation of the water inlet joint 305, the drain joint 306 and the U-shaped channel 307, the protection box 301 is cooled down to avoid damage to the protection box 301 due to high temperature.

[0021] In this embodiment, the material storage component includes an H-shaped block 308, a nitrogen inlet joint 309, and a nitrogen outlet joint 310. The middle part of the inner cavity of the protection box 301 is fixedly connected with the H-shaped block 308. A stepped placement hole 311 is arranged in the middle of the H-shaped block 308. A nitrogen channel is arranged inside the H-shaped block 308. The top surface of the protection box 301 is fixedly connected with the nitrogen inlet joint 309, and the bottom surface of the protection box 301 is fixedly connected with the nitrogen outlet joint 310. The nitrogen inlet joint 309 and the nitrogen outlet joint 310 are respectively communicated with the nitrogen channel.

[0022] Through the stepped placement hole 311, the installation and limitation of the powder sheet clamp 523 can be realized, which is convenient for later detection and also avoids the powder sheet clamp 523 from detaching from the stepped placement hole 311 during detection.

[0023] 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 communicated with the nitrogen inlet joint 309, the middle part of the vertical channel 312 is communicated with the L-shaped channel 313, and one end of the L-shaped channel 313 is communicated with the nitrogen outlet joint 310.

[0024] Through the mutual cooperation of the nitrogen inlet joint 309, the nitrogen outlet joint 310, the vertical channel 312, and the L-shaped channel 313, after injecting nitrogen, the sample can be quickly cooled, and the lowest temperature can be reduced to minus 180 degrees.

[0025] In this embodiment, the material storage component further includes a first thermocouple 314, a second thermocouple 315, and a heating rod 316. One end of the first thermocouple 314 penetrates through the top surface of the protection box 301 and extends to one side of the stepped placement hole 311. One end of the second thermocouple 315 penetrates through the bottom surface of the protection box 301 and extends to one side of the stepped placement hole 311. The first thermocouple 314 and the second thermocouple 315 are arranged in a front-back staggered manner. There are two groups of heating rods 316. One ends of the two groups of heating rods 316 respectively penetrate through the top surface of the protection box 301 and extend to both sides of the stepped placement hole 311.

[0026] Through the mutual cooperation of the first thermocouple 314 and the second thermocouple 315, the highest and lowest temperatures of the sample in the H-shaped block 308 can be detected in real time, and the control system can adjust the liquid nitrogen flow rate and heating power according to the set temperature to ensure the accuracy of temperature control.

[0027] Through the two groups of heating rods 316, the item can be heated to a maximum of 600 degrees to adapt to the detection of most materials; In this embodiment, the first sealing component includes a sealing plate 317. One side of the protection box 301 is fixedly connected to the sealing plate 317. At both ends on one side of the sealing plate 317, a first water-cooling joint 318 and a second water-cooling joint 319 are respectively fixedly connected. An "U"-shaped water-cooling channel 320 is arranged inside the sealing plate 317. Both ends of the "U"-shaped water-cooling channel 320 are internally communicated with the first water-cooling joint 318 and the second water-cooling joint 319 respectively. A ray hole 321 is arranged in the middle of the sealing plate 317, and a beryllium sheet 322 is fixedly connected inside the ray hole 321; the second sealing component adopts the same structure as the first sealing component.

[0028] Through the mutual cooperation of the first water-cooling joint 318, the second water-cooling joint 319 and the "U"-shaped water-cooling channel 320, the temperature reduction of the sealing plate 317 can be realized, and the situation that the sealing plate 317 is damaged or the sealing is not tight due to high temperature can be avoided; Through the beryllium sheet 322, the penetration of the X-ray can be ensured, and the problem of being not easily damaged under high temperature and low temperature conditions can also occur.

[0029] In this embodiment, the opening and closing assembly 400 includes a slide rail 401 and an "L"-shaped rod 402. One side of the two sets of vertical plates 200 is fixedly connected to the slide rail 401. An I-shaped block 403 is slidably connected inside the slide rail 401. The top surface of the I-shaped block 403 is fixedly connected to the 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, and the output end of the opening and closing hydraulic rod 404 is fixedly connected to one side of the sealing plate 317.

[0030] Through the opening and closing assembly 400, the opening and closing of the sealing plate in the first sealing component can be realized. 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 detecting the loaded materials. At the same time, the sealing plate will keep the feeding component away from the protection box 301, which is convenient for the staff to add the next powder material to be detected into the loading and unloading component 500, and is convenient for later pressing and forming for detection.

[0031] In this embodiment, the loading and unloading component 500 includes a workbench 501. The top surface of the bottom plate 100 is fixedly connected to the workbench 501. The top surface of the workbench 501 is 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. Symmetrically fixed strips 505 are fixedly connected to the surface of the flipping shaft 504. 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.

[0032] By flipping the pneumatic rod 503, the rotation 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 the vertical state, it is convenient for the staff to add the materials to be detected, and the powdery materials are pressed into granular form for convenient later detection. When the feeding component is in the horizontal state, the previously detected powder sheet clamp 523 is removed. After removal, a new powder sheet clamp 523 is placed into the stepped placement hole 311.

[0033] In this embodiment, the loading and unloading assembly 500 further includes a feeding component and a square block 508. A shaft hole 509 is provided in the middle of the square block 508. The middle of the square block 508 is located on the surface of the rotation shaft 504 and slides through the shaft hole 509. A limiting hole 510 is provided on the inner wall of the shaft hole 509 and slides on the surface of the limiting strip 505. A T-shaped sleeve 511 is fixedly connected to one side of the square block 508. A connecting rod 512 is rotatably connected to the surface of the T-shaped sleeve 511. 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.

[0034] Through the connecting rod 512, it is convenient for the sealing plate 317 to drive the feeding component to slide along the rotation shaft 504 during the movement process, which is convenient to convey the feeding component to one side of the protection box 301 for convenient later feeding, or to convey it to the side far from the protection box 301 for convenient later manual feeding.

[0035] In this embodiment, the feeding component includes a lifting hydraulic rod 513. A 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 with a motor box 514. A switching motor 515 is fixedly connected inside the motor box 514. The output end of the switching motor 515 is rotationally connected to a switching shaft 516 through a gear set. One end of the switching shaft 516 is fixedly connected with a fixed block 517.

[0036] Through the mutual cooperation of the lifting hydraulic rod 513 and the switching motor 515, it is convenient for later feeding and unloading.

[0037] In this embodiment, the feeding component further includes a fixing rod 518 and a forming cylinder 519. The forming cylinder 519 is fixedly connected inside the fixing block 517. The bottom of the inner wall of the forming cylinder 519 is fixedly connected with a forming hydraulic rod 520. The output end of the forming hydraulic rod 520 is fixedly connected with a pressure plate 521. One end of the forming cylinder 519 is provided with a placing hole 522. A powder sheet clip 523 is placed in the placing hole 522. The inner wall of the placing hole 522 is provided with adsorption holes 524. An adsorption cavity 525 is arranged inside the forming cylinder 519. The bottom surface of the forming cylinder 519 is fixedly connected with an adsorption disc 526. The inner cavity of the adsorption disc 526 is communicated with the adsorption cavity 525 through a three-way pipe 527. The top surface of the workbench 501 is fixedly connected with a fixing rod 518. One end of the fixing rod 518 is fixedly connected with a forming cover 528.

[0038] Through the mutual cooperation of structures such as the forming cylinder 519, the forming hydraulic rod 520, the pressure plate 521, the placing hole 522 and the forming cover 528, the powder material can be pressed into granular shape, which is convenient for later feeding and detection. Through the mutual cooperation of the adsorption holes 524 and the adsorption cavity 525, the pressed and formed powder sheet clip 523 can be adsorbed and fixed in the forming cylinder 519, which is convenient for later conveying and feeding.

[0039] Through the adsorption disc 526, it is convenient to remove the powder sheet clip 523 in the stepped placing hole 311 later.

[0040] The working principle and usage process of the present invention: In the use state: Preparation before feeding; First, the staff puts the powder to be detected into the forming cylinder 519, and the put powder will fall onto the top of the pressure plate 521. After a certain amount of powder is put, the feeding will stop, and the powder sheet clip 523 will be installed. When placing the powder sheet clip 523, first align the large mouth diameter of the powder sheet clip 523 with the placing hole 522 and put it in. After putting it in, the preparation of the material is completed. Pressing the powder material into shape: First, start the lifting hydraulic rod 513. 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 contact, the sealing of the forming cylinder 519 can be achieved. The sealed forming cylinder 519 will fix the powder sheet clamp 523 in the placement hole 522. At this time, start the forming hydraulic rod 520. The forming 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 is pressed into a sheet, and the sheet-shaped powder is located in the powder sheet clamp 523. After pressing and forming, the forming hydraulic rod 520 will stop pressing. 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; Adjust the angle of the forming cylinder 519; Due to the reset of the forming cylinder 519, at this time, start the external vacuum pump. The vacuum pump will use the vacuum tube to start adsorbing and evacuating the adsorption cavity 525. When the adsorption cavity 525 is evacuated, at this time, under the action of the adsorption hole 524, the powder sheet clamp 523 is adsorbed and fixed in the placement hole 522, preventing the powder sheet clamp 523 from detaching from the placement hole 522 during the angle adjustment; after adsorption, at this time, start the flipping pneumatic rod 503. When the flipping pneumatic rod 503 works, it will drive the flipping rack 507 to move. As the flipping rack 507 moves, it will drive the flipping gear 506 to rotate, thereby driving the rotating shaft 504 and the limiting strip 505 to rotate. As the rotating shaft 504 rotates, it will drive the square block 508 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, the forming cylinder 519 will change from a vertical state to a horizontal state, and the flipping pneumatic rod 503 will stop working; Prepare for feeding: First, the staff removes all the bolts on one side of the sealing plate 317 on the first sealing component. After the 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 moving along with the sealing plate 317, it will drive the connecting rod 512 to move. When moving along with the connecting rod 512, it will drive the square block 508 to slide along the surface of the turning shaft 504. When moving along with the square block 508, it will drive the forming cylinder 519 to move. When the sealing plate 317 completely moves away from one side of the protection box 301, at this time, the forming cylinder 519 will also move to the center position of the circular hole 302. At this time, the work of the opening and closing hydraulic rod 404 is stopped. 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 towards 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 work of the lifting hydraulic rod 513 will be stopped. At the same time, the forming hydraulic rod 520 is started. When the forming hydraulic rod 520 works, the powder sheet clamp 523 containing powder can be pushed into the stepped placement hole 311, and the feeding is completed. After the feeding, at this time, the lifting hydraulic rod 513 will drive the forming cylinder 519 to reset. After the reset, at this time, 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 fixes the sealing plate 317 to the protection box 301 together through bolts; (Before feeding, it may be necessary to remove the powder sheet clamp 523 in the stepped placement hole 311. When removing, first, the switching motor 515 is started. The switching motor 515 drives the switching shaft 516 to rotate. When the switching shaft 516 rotates, it will drive the fixed block 517 to rotate, so that the positions of the forming cylinder 519 and the suction disc 526 are swapped. After the swap, through the lifting hydraulic rod 513, one side of the suction disc 526 is made to contact the powder sheet clamp 523 after detection. After the contact, using an external vacuum pump, the powder sheet clamp 523 is adsorbed on one side of the suction disc 526. After the adsorption, at this time, the lifting hydraulic rod 513 drives the forming cylinder 519 and the suction disc 526 to reset. After the reset, the positions of the suction disc 526 and the forming cylinder 519 are switched again through the switching motor 515. After the switching, it is convenient for feeding the new powder sheet clamp 523 in the later stage) Preparation for detection: During detection, first, the staff heats or cools the material according to the detection requirements: When heating, by starting two groups of heating rods 316, the heating rods 316 start to heat the H-shaped block 308. During heating, it is detected in real time by the first thermocouple 314 and the second thermocouple 315, and the information during detection is transmitted to the external display screen for the convenience of later staff to view. The maximum temperature of the heating rods 316 can reach 600 degrees Celsius. When heating the powder in the powder sheet clamp 523, at this time, start the external water pump. The water pump injects the external cooling water into the water inlet joint 305 and the first water cooling joint 318 respectively. At this time, the cooling water will flow through the U-shaped channel 307 and the U-shaped water cooling channel 320 respectively, and finally, it will be discharged from the drain joint 306 and the second water cooling joint 319 respectively, to avoid overheating of the protection box 301, the first sealing component and the second sealing component due to high temperature. When the powder is heated to the specified temperature, stop heating. At this time, start the external vacuum pump. When the vacuum pump works, under the action of the exhaust joint 304, the protection box 301 is evacuated to avoid the situation that X-rays are absorbed or scattered by the internal air. After evacuation, at this time, 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 not only withstand high temperatures but also ensure the transmittance; During cooling detection, only need to drain the external liquid nitrogen from the nitrogen inlet joint 309. The liquid nitrogen after drainage will enter the vertical channel 312, flow into the L-shaped channel 313 from the vertical channel 312, and finally, be discharged from the nitrogen drain joint 310. The nitrogen gas discharged starts to cool the powder on the powder sheet clamp 523. When it is cooled to the specified temperature, evacuate it, and after evacuation, perform X-ray detection.

[0041] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprising", "including" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "comprising an..." does not exclude the existence of additional identical elements in the process, method, article or device comprising the element.

[0042] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An in-situ cell body with a wide temperature range applicable to the XAFS transmission mode, characterized in that: It includes a bottom plate, on the top surface of which vertical plates are symmetrically and fixedly connected. An auxiliary detection component is installed between the two groups of vertical plates. An opening and closing component is installed on one side of the two groups of vertical plates. One end of the opening and closing component is connected to the auxiliary detection component. On the top surface of the bottom plate and on one side of the auxiliary detection component, a loading and unloading component is installed. One end of the auxiliary loading and unloading component is connected to the auxiliary detection component; The auxiliary detection component includes a protection box. The protection box is fixedly connected between the two groups of vertical plates. Circular holes are respectively arranged 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. Water inlet joints and drain joints are respectively fixedly connected to both ends of the top surface of the protection box. A U-shaped channel is arranged inside the protection box. The two ends of the U-shaped channel are respectively communicated with the water inlet joint and the drain 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. The first sealing component is respectively connected to the opening and closing component and the loading and unloading component.

2. The in-situ cell body with a wide temperature range applicable to the 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 outlet joint. The H-shaped block is fixedly connected to the middle of the inner cavity of the protection box. A stepped placement hole is arranged in the middle of the H-shaped block. A nitrogen channel is arranged inside the H-shaped block. The nitrogen inlet joint is fixedly connected to the top surface of the protection box. The nitrogen outlet joint is fixedly connected to the bottom surface of the protection box. The nitrogen inlet joint and the nitrogen outlet joint are respectively communicated with the nitrogen channel.

3. An in-situ cell body with a wide temperature range applicable to the 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 communicated with the nitrogen inlet joint. The middle of the vertical channel is communicated with the L-shaped channel. One end of the L-shaped channel is communicated with the nitrogen outlet joint.

4. An in-situ cell body with a wide temperature range applicable to the XAFS transmission mode according to claim 3, characterized in that: The material storage component further includes a first thermocouple, a second thermocouple and a heating rod. One end of the first thermocouple penetrates through the top surface of the protection box and extends to one side of the stepped placement hole. One end of the second thermocouple penetrates through the bottom surface of the protection box and extends to one side of the stepped placement hole. The first thermocouple and the second thermocouple are arranged in a front-back staggered manner. There are two groups of heating rods in total. One ends of the two groups of heating rods respectively penetrate through the top surface of the protection box and extend to both sides of the stepped placement hole.

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

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

7. An in-situ cell body with a wide temperature range applicable to the XAFS transmission mode according to claim 6, characterized in that: The loading and unloading assembly includes a workbench. The top surface of the bottom plate is fixedly connected with the workbench. The top surface of the workbench is fixedly connected with a U-shaped frame and a flipping pneumatic rod respectively. A flipping shaft is rotatably connected in the U-shaped frame. The surface of the flipping shaft is symmetrically fixedly connected with limiting strips. One end of the surface of the flipping shaft is fixedly connected with a flipping gear. The output end of the flipping pneumatic rod is fixedly connected with a flipping rack. The flipping rack is meshed with the flipping gear.

8. A wide-temperature in-situ cell body applicable to the XAFS transmission mode according to claim 7, characterized in that: The loading and unloading assembly further includes a feeding component and a square block. A shaft hole is provided in the middle of the square block. The middle of the square block is slidably located on the surface of the flipping shaft through the shaft hole. A limiting hole is provided in the inner wall of the shaft hole. The limiting hole is slidably located on the surface of the limiting strip. One side of the square block is fixedly connected with a T-shaped sleeve. A connecting rod is rotatably connected to the surface of the T-shaped sleeve. One end of the connecting rod is fixedly connected with one side of the sealing plate. A feeding component is installed on one side of the square block.

9. The in-situ cell body with a wide temperature range applicable to the XAFS transmission mode according to claim 8, characterized in that: The feeding component includes a lifting hydraulic rod. One side of the square block is fixedly connected with the lifting hydraulic rod. The output of the lifting hydraulic rod is fixedly connected with a motor box. A switching motor is fixedly connected in the motor box. The output end of the switching motor is rotationally connected with a switching shaft through a gear set. One end of the switching shaft is fixedly connected with a fixed block.

10. An in-situ cell body with a wide temperature range applicable to the XAFS transmission mode according to claim 9, characterized in that: The feeding component further includes a fixed rod and a forming cylinder. The forming cylinder is fixedly connected in the fixed block. A forming hydraulic rod is fixedly connected to the bottom of the inner wall of the forming cylinder. The output end of the forming hydraulic rod is fixedly connected with a pressing disc. A placing hole is provided at one end of the forming cylinder. A powder sheet clip is placed in the placing hole. An adsorption hole is provided in the inner wall of the placing hole. An adsorption cavity is provided inside the forming cylinder. The bottom surface of the forming cylinder is fixedly connected with an adsorption disc. The inner cavity of the adsorption disc is communicated with the adsorption cavity through a three-way pipe. The top surface of the workbench is fixedly connected with a fixed rod. One end of the fixed rod is fixedly connected with a forming cover.

Citation Information

Patent Citations

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