In-situ synchrotron radiation analysis device for tensile sample stress state and oxidation film component structure in high-temperature and high-pressure water
By designing an in-situ synchrotron radiation analysis device for the stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water, the problem of real-time monitoring of the dynamic changes in material stress state and oxide film composition under high-temperature and high-pressure water environment was solved, enabling in-situ analysis of key components of nuclear power plants and improving the safety and economy of nuclear power plants.
Patent Information
- Application Number
- CN202520049431.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-09
- Publication Date
- 2026-01-23
- Estimated Expiration
- 2035-01-09
AI Technical Summary
Existing technologies struggle to monitor the dynamic changes in surface stress and oxide film composition of materials in real time under high temperature and high pressure water conditions, especially under the service conditions of critical components in nuclear power plants, where in-situ analysis capabilities are lacking.
An in-situ synchrotron radiation analysis device for stress state and oxide film composition of tensile specimens in high temperature and high pressure water was designed. The device utilizes a high-pressure autoclave, pipelines, X-ray emitting/receiving devices, and an angle-adjusting base, combined with multiaxial diffraction, X-ray absorption spectroscopy, and fluorescence spectroscopy, to achieve real-time monitoring of material stress state and oxide film composition.
It enables real-time, in-situ monitoring of material stress state and oxide film composition under high temperature and high pressure water environment, filling the gap in existing technology and improving the understanding and prediction of stress corrosion cracking behavior.
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Figure CN223827490U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to material high temperature high pressure stress corrosion test technical field, concretely is a kind of high temperature high pressure water in tensile sample stress state and oxidation film component structure in situ synchrotron radiation analysis device, applicable to high temperature high pressure water environment by synchrotron radiation X ray real-time analysis material stress state and oxidation film component structure. BACKGROUND
[0002] With the continuous growth of global energy demand and the restriction of traditional fossil energy use, nuclear energy gradually becomes one of the important choices of energy transformation due to its cleanliness, efficiency and sustainability. However, in the actual operation process of nuclear power plants, material failure is always a key factor threatening the safe operation of equipment, among which stress corrosion cracking (SCC) is particularly significant. Studies have shown that the occurrence of SCC is usually influenced by multiple factors, including complex service environment conditions (such as high temperature, high pressure, strong corrosion, etc.), microstructure characteristics of materials and stress state. This failure mode not only has suddenness and concealment, but also is difficult to predict early through conventional detection means. Since some key components of nuclear power plants (such as reactor pressure vessels, steam generator pipes, etc.) are usually irreplaceable, the SCC problem directly affects the reliability of nuclear power equipment and becomes a key factor determining the service life of nuclear power plants. Therefore, it is of great significance to study the SCC behavior of nuclear materials under actual working conditions, to explore its influencing mechanism and control strategy, for improving the safety and economy of nuclear power plants.
[0003] In the mechanism of SCC, the interaction between the oxidation behavior of the material surface and the stress plays a crucial role. The oxidation film, as the key interface between the corrosion environment and the substrate material, its composition and structure evolution directly affect the film rupture behavior. At the same time, the stress state of the material directly affects the sensitivity of SCC, not only affecting crack initiation, but also affecting crack propagation rate and path. Therefore, accurate measurement of the complex stress state of the material under simulated service conditions (including processing residual stress, service stress, etc.) and dynamic measurement of the composition and structure of the surface oxidation film are important means to further understand the SCC behavior.
[0004] In existing technologies, research methods for stress corrosion cracking (SCC) mainly focus on characterization and analysis in the later stages of the experiment, typically by measuring the composition and structure of the oxide film after the stress corrosion test. However, this method struggles to capture the dynamic changes during the stress corrosion process, especially in achieving real-time characterization of the internal stress state of the material. Furthermore, existing devices lack the capability for real-time, in-situ analysis of the composition and structure of the oxide film on the material surface during SCC. To address these issues, there is an urgent need to develop a novel device capable of real-time detection of the surface stress state, oxide film composition, and structural changes of materials under high-temperature, high-pressure water (200–360℃, 4–20 MPa) stress corrosion conditions, to meet the characterization requirements of critical materials in nuclear power plants under extreme service conditions. Utility Model Content
[0005] The purpose of this invention is to provide an in-situ synchrotron radiation analysis device for the stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water, specifically designed to solve the problem of real-time analysis of material stress state and oxide film composition structure using synchrotron radiation X-rays in a high-temperature and high-pressure water environment.
[0006] The technical solution of this utility model is as follows:
[0007] An in-situ synchrotron radiation analysis device for stress state and oxide film composition of tensile specimens in high-temperature and high-pressure water comprises an autoclave, pipelines, a test end, an angle adjustment base, a back pressure valve, and an X-ray emitting / receiving device. The specific structure is as follows: An autoclave is located at the front of the device; the test end, X-ray emitting / receiving device, and angle adjustment base are located in the middle of the device. The test end is situated on the angle adjustment base, and the X-ray emitting / receiving device is located outside the reactor at the test end, corresponding to the tensile clamps and specimen inside the test end. The X-ray emitting / receiving device VI performs real-time in-situ monitoring of the sample during the experiment; a back pressure valve is installed at the end of the device. The autoclave and the test end are connected via pipelines, and the test end and the back pressure valve are also connected via pipelines. A high-temperature and high-pressure solution meeting the experimental conditions enters the test end of the experimental device through pipeline II and then exits through the back pressure valve to ensure solution flow within the reactor of the test end III.
[0008] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water includes an autoclave made of Inconel 625 nickel-based alloy, with insulation cotton installed on the outside of the autoclave body, and equipped with an inlet, an outlet, and a reactor connection port; the pipeline is made of Inconel 625 nickel-based alloy and is used to connect the autoclave cavity and the test end, and is equipped with start and stop valves.
[0009] The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high temperature and high pressure water consists of a motor, bushing, tensile shaft, water-cooled sealing bushing, reactor, cooling base, tensile fixture and specimen, and high-precision XYZ axis test platform. The specific structure is as follows: the tensile mechanism composed of motor, bushing, tensile shaft and water-cooled sealing bushing is connected to the tensile fixture and specimen inside the reactor. The reactor is fixed at the top center of the cooling base, and the cooling base is set on the high-precision XYZ axis test platform.
[0010] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high temperature and high pressure water has a reactor with a reactor inlet and a reactor outlet. The reactor inlet is connected to a high pressure vessel through a pipeline, and the reactor outlet is connected to a back pressure valve through a pipeline. By adjusting the back pressure valve, the high temperature and high pressure solution is sequentially passed through the high pressure vessel, the reactor inlet, the reactor, the reactor outlet, and the back pressure valve.
[0011] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water has symmetrically arranged sealing flanges at both ends of the reactor. An upper end cover and a lower end cover are respectively installed at both ends of the reactor via the sealing flanges. The entire reactor is sealed and securely connected to the upper and lower end covers via the sealing flanges and matching fastening bolts. Symmetrically arranged sealing flanges are provided on the sides of the reactor. Sapphire observation windows are installed on the sides of the reactor via the sealing flanges. The entire reactor is sealed and securely connected to the sapphire observation windows via the sealing flanges and matching fastening bolts.
[0012] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water has an X-ray emission / receiver device with an emitter and a receiver on both sides of the sapphire observation window of the reactor. By adjusting the high-precision XYZ axis test stage and angle adjustment base, X-rays pass through the emitter, irradiate the sample gauge length through the sapphire observation window, and then pass through the other side of the sapphire observation window to the receiver. The receiver of the X-ray emission / receiver device VI is connected to a computer.
[0013] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high temperature and high pressure water includes a tensile clamp and a specimen inside the reactor. The specimen is mounted on the upper clamp and lower clamp at both ends by pins. The upper clamp is connected to a tensile shaft, a bushing, and a motor in sequence. A water-cooled sealing bushing is provided at the junction between the upper end cover of one end of the reactor and the tensile shaft.
[0014] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water includes a cooling base at the bottom of the reactor, with an arc-shaped groove and slide rail corresponding to the bottom of the reactor; a cooling water inlet and outlet connected to the internal circulation channel of the cooling base are installed on the side of the cooling base; a high-precision XYZ axis test platform is installed at the bottom of the cooling base, and the position of the reactor is finely adjusted by bolts on the high-precision XYZ axis test platform.
[0015] The aforementioned in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water features a high-precision XYZ-axis test bench connected to an angle adjustment base. The angle adjustment base comprises an angle adjustment platform, a scissor-type height adjuster, pins, an angle indicator, and a main frame. The angle adjustment platform overlaps the top of the main frame, with a protrusion at the bottom center of the platform extending into a groove at the top center of the main frame. Pins are vertically inserted into one end of the protrusion and the corresponding groove, allowing the angle adjustment platform to swing around the groove via the pins. The bottom surface of the other end of the protrusion corresponds to the scissor-type height adjuster located within the groove. The scissor-type height adjuster consists of two sets of hinged connecting rods connected by a screw drive, allowing height adjustment by rotating the screw, further adjusting the swing angle of the angle adjustment platform. Simultaneously, an angle indicator is installed on the angle adjustment platform of the angle adjustment base to display the angle between the platform and the horizontal plane.
[0016] The design concept of this utility model is:
[0017] This utility model addresses the technical difficulties and research gaps in the study of stress cracking (SCC) of key materials in nuclear power plants under high temperature and high pressure water environment. Through innovative device design, it aims to achieve real-time, in-situ analysis of the stress state, oxide film composition, and structure of tensile specimens during the SCC process. Specifically, it includes the following design: (1) Using a high-pressure reactor and pipeline system, the solution flow is controlled by a back pressure valve to accurately simulate the actual working conditions of the high temperature and high pressure water environment in nuclear power plants. The solution is introduced into the reactor and kept in dynamic flow, providing a basic experimental environment guarantee for the study of SCC behavior. (2) The device combines a synchrotron X-ray emitting / receiving device with a sapphire observation window to achieve real-time dynamic monitoring of the stress state and surface oxide film composition and structure of the specimen during the SCC process, overcoming the limitation of traditional technology which can only perform post-analysis. (3) Through the combination design of a high-precision XYZ axis test bench and an angle adjustment base, the position and angle of the specimen during tensile loading and monitoring are adjustable to meet the test requirements of different incident angles of synchrotron radiation. (4) The device integrates real-time monitoring and precise control of multiple key parameters such as temperature, pressure, and tensile force.
[0018] The advantages and beneficial effects of this utility model are:
[0019] 1. This utility model device is equipped with a sapphire window that can withstand high pressure. Combined with a synchrotron radiation light source, it can acquire X-ray signals of high-temperature and high-pressure water tensile specimens in real time. It can also use multiaxial diffraction (multi-angle sin2ψ method), X-ray absorption spectroscopy (XAS), and X-ray fluorescence spectroscopy (XRF) to obtain real-time in-situ monitoring of the stress state and oxide film composition and structure of the tensile specimens, filling the technical gap that existing technologies cannot dynamically characterize in extreme environments.
[0020] 2. This utility model device is small and lightweight, which can meet the testing requirements of synchrotron radiation sources. The device is equipped with a high-precision XYZ axis test platform and angle adjustment base to ensure that the position and angle of the sample can be finely adjusted during the experiment to meet the needs of various complex experimental schemes. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the experimental apparatus of this utility model. In the diagram, Ⅰ is a high-pressure reactor; Ⅱ is a pipeline; Ⅲ is the test end; Ⅳ is an angle adjustment base; Ⅴ is a back pressure valve; Ⅵ is an X-ray emitting / receiving device; SR is a synchrotron radiation beam.
[0022] Figures 2-5 This is a schematic diagram of the structure of test terminal III. Figure 2 Main view, Figure 3 Left view, Figure 4 This is a top view. Figure 5 This is a 3D view. In the diagram, 1 is the motor; 2 is the bushing; 3 is the tension shaft; 4 is the water-cooled sealing bushing; 5 is the reactor; 6 is the cooling base; 7 is the tension fixture and specimen; 8 is the high-precision XYZ axis test bench; 501 is the upper end cover; 502 is the sealing flange; 503 is the reactor inlet; 504 is the reactor outlet; 505 is the sapphire observation window; 506 is the lower end cover; 601 is the cooling water inlet; and 602 is the cooling water outlet.
[0023] Figure 6 This is a schematic diagram of the tensile fixture and specimen. In the diagram, 701 is the upper fixture; 702 is the lower fixture; 703 is the pin; and 704 is the specimen.
[0024] Figure 7 This is a schematic diagram of the angle adjustment base. In the diagram, Ⅳ-1 is the angle adjustment platform (Ⅳ-11 boss); Ⅳ-2 is the scissor-type height adjuster; Ⅳ-3 is the pin; Ⅳ-4 is the angle indicator; and Ⅳ-5 is the main frame (Ⅳ-51 groove).
[0025] Figure 8 This is a schematic diagram of a scissor-type height adjuster. In the diagram, Ⅳ-21 is the connecting rod; Ⅳ-22 is the screw. Detailed Implementation
[0026] In its specific implementation, this utility model proposes an in-situ synchrotron radiation analysis device for the stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water. It mainly consists of a high-pressure reactor I, a pipeline II, a test end III, an angle adjustment base IV, a back pressure valve V, and an X-ray emitting / receiving device VI. The specific structure is as follows: The device is equipped with a high-pressure reactor I at the front; the test end III, X-ray emitting / receiving device VI, and angle adjustment base IV are located in the middle of the device. The test end III is situated on the angle adjustment base IV, and the X-ray emitting / receiving device VI is located outside the reactor 5 of the test end III, corresponding to the tensile clamp and specimen 7 within the test end III; a back pressure valve V is installed at the end of the device. The high-pressure reactor I is connected to the test end III via pipeline II, and the test end III and back pressure valve V are connected via pipeline. A high-temperature and high-pressure solution meeting the experimental conditions enters the test end III of the experimental device through pipeline II and is then discharged from the back pressure valve V, ensuring the flow of solution within the reactor 5 of the test end III. X-ray emitting / receiving device VI performs real-time in-situ monitoring of the sample during the experiment, with synchrotron radiation beam SR provided by the synchrotron radiation device.
[0027] The autoclave I is made of Inconel 625 nickel-based alloy and can simulate a high-temperature, high-pressure water environment to meet experimental requirements. The exterior of the autoclave is lined with insulation cotton to reduce the influence of external temperature on the internal environment, and it is equipped with an inlet, outlet, and reactor connection port. To meet the testing requirements of synchrotron radiation sources, this autoclave is compact in size, with a volume of approximately 2L.
[0028] Pipeline II is made of Inconel 625 nickel-based alloy and is used to conduct the high-temperature and high-pressure solution between the high-pressure reactor I cavity and the test end III. It is equipped with start and stop valves.
[0029] The test end III consists of a motor 1, a bushing 2, a tension shaft 3, a water-cooled sealing bushing 4, a reactor 5, a cooling base 6, a tension fixture and a specimen 7, and a high-precision XYZ axis test bench 8. The specific structure is as follows: The tension mechanism composed of the motor 1, bushing 2, tension shaft 3 and water-cooled sealing bushing 4 is connected to the tension fixture and specimen 7 inside the reactor 5. The reactor 5 is fixed at the top center of the cooling base 6, and the cooling base 6 is set on the high-precision XYZ axis test bench 8.
[0030] The reactor 5 of the test end III is equipped with a reactor inlet 503 and a reactor outlet 504. The reactor inlet 503 is connected to the high pressure vessel I through pipeline II, and the reactor outlet 504 is connected to the back pressure valve V through pipeline. By adjusting the back pressure valve V, the high temperature and high pressure solution passes sequentially through the high pressure vessel I, the reactor connection port, the reactor inlet 503, the reactor 5, the reactor outlet 504, and the back pressure valve V.
[0031] The reactor 5 at the test end III is symmetrically equipped with sealing flanges 502 at both ends. The upper end cover 501 and the lower end cover 506 are respectively installed at the two ends of the reactor 5 through the sealing flanges 502. The reactor 5 as a whole is sealed and fastened to the upper end cover 501 and the lower end cover 506 through the sealing flanges 502 and matching fastening bolts. The reactor 5 is symmetrically equipped with sealing flanges on the side. Sapphire observation windows 505 are respectively installed on the side of the reactor 5 through the sealing flanges. The reactor 5 as a whole is sealed and fastened to the sapphire observation windows 505 through the sealing flanges and matching fastening bolts. The sapphire observation windows 505 can withstand the high temperature and high pressure environment inside the reactor 5.
[0032] The reactor 5 in test end III is equipped with a tensile clamp and a specimen 7. The specimen 704 is mounted on the upper clamp 701 and the lower clamp 702 at both ends by pins 703. The upper clamp 701 is connected to the tensile shaft 3, the bushing 2, and the motor 1 in sequence to load the specimen 704 during the experiment. A water-cooled sealing bushing 4 is provided at the junction between the upper end cover 501 and the tensile shaft 3 at one end of the reactor 5 to ensure the internal environment of the reactor 5 and prevent leakage of the motor 1.
[0033] The reactor 5 in test terminal III is equipped with thermocouples and pressure gauges to monitor the internal temperature and pressure of reactor 5 in real time. Reactor 5 is wrapped with insulation cotton to reduce the influence of the external environment on the internal temperature of reactor 5.
[0034] The reactor 5 at the test end III is equipped with a cooling base 6 at its bottom. The cooling base 6 has an arc-shaped groove corresponding to the bottom of the reactor 5 to ensure the stability of the reactor 5 on the cooling base 6, and is equipped with a slide rail for easy sample installation. The side of the cooling base 6 is equipped with a cooling water inlet 601 and a cooling water outlet 602 connected to the internal circulation channel of the cooling base 6. Cooling is achieved through circulating cooling water to prevent the high temperature from affecting the temperature of the high-precision XYZ axis test bench 8 below. The high-precision XYZ axis test bench 8 is mounted at the bottom of the cooling base 6, and the position of the reactor 5 is fine-tuned using bolts on the high-precision XYZ axis test bench 8. In this invention, the precision requirement of the high-precision XYZ axis test bench 8 is less than 0.5 μm.
[0035] The bottom of the high-precision XYZ axis test bench 8 is connected to the angle adjustment base IV. The angle adjustment base IV consists of an angle adjustment platform IV-1, a scissor height adjuster IV-2, a pin IV-3, an angle indicator IV-4, and a main frame IV-5. The angle adjustment platform IV-1 is attached to the top of the main frame IV-5. The boss IV-11 at the bottom center of the angle adjustment platform IV-1 extends into the groove IV-51 at the top center of the main frame IV-5. The pin IV-3 is vertically inserted into one end of the boss IV-11 and the corresponding groove IV-51, allowing the angle adjustment platform IV-1 to swing around the groove IV-51 via the pin IV-3. The bottom surface of the other end of the boss IV-11 corresponds to the scissor height adjuster IV-2 provided in the groove IV-51. The scissor height adjuster IV-2 is composed of two sets of hinged connecting rods IV-21 connected by a screw IV-22. The height is adjusted by rotating the screw IV-22, which further adjusts the swing angle of the angle adjustment platform IV-1. Meanwhile, the angle adjustment platform IV-1 of the angle adjustment base IV is equipped with an angle indicator IV-4, which can display the angle between the angle adjustment platform IV-1 and the horizontal plane.
[0036] The emitter and receiver of the X-ray emitting / receiving device VI are located slightly away from each other on both sides of the sapphire observation window 505 of the reactor 5. By adjusting the high-precision XYZ axis test stage 8 and the angle adjustment base IV, X-rays can pass through the emitter, irradiate the sample gauge length through the sapphire observation window 505, and then pass through the other sapphire observation window 505 to the receiver. The receiver of the X-ray emitting / receiving device VI is connected to a computer to observe the stress state, oxide film composition and structure of the sample in real time.
[0037] Back pressure valve V is installed at the end of the entire system. During the test, the pressure of back pressure valve V is slightly lower than the pressure inside the high pressure vessel I chamber to ensure that the solution in reactor 5 at the test end III flows slowly.
[0038] X-ray emission / reception device VI, powered by a synchrotron radiation source, is used for signal acquisition and analysis to assess the stress state and oxide film structure of the samples. Multiaxial diffraction (multi-angle sin²ψ method) is employed, with synchrotron X-rays incident on the sample surface from multiple directions, and changes in diffraction peaks are recorded to measure the stress state. X-ray absorption spectroscopy (XAS) and X-ray fluorescence spectroscopy (XRF) are used to obtain compositional and structural information of the oxide film.
[0039] like Figures 1-8 As shown, this utility model proposes a method for using an in-situ synchrotron radiation analysis device for the stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water. The specific steps are as follows:
[0040] (1) Install the stress corrosion test tensile specimen, adjust the tensile shaft 3 so that the upper clamp 701 and the lower clamp 702 are fully extended out of the reactor 5, fix the tensile specimen 704 between the upper clamp 701 and the lower clamp 702 with the pin 703, and adjust the tensile shaft 3 until the tensile specimen 704, the upper clamp 701 and the lower clamp 702 are fully inserted into the reactor 5.
[0041] (2) Close the upper end cover 501 and the lower end cover 506, tighten the fixing bolts of the upper end cover 501 flange, the lower end cover 506 flange and the sealing flange 502 until the reactor 5 is completely sealed, and push the reactor 5 into the test position through the slide rail of the cooling base 6.
[0042] (3) Inject the solution into the high pressure vessel I, close the high pressure vessel I, adjust the water chemical parameters, and then raise the temperature; continuously purge the reactor 5 with high-purity nitrogen (volume purity 99.999%) for about 2 hours to fully purge the oxygen in the reactor 5, and then close the reactor inlet 503 and reactor outlet 504 of the reactor 5.
[0043] (4) Turn on the cooling water circulation of the cooling base 6 to avoid the high temperature of the experiment from affecting the high-precision XYZ axis test bench 8;
[0044] (5) Start motor 1 to load the tensile specimen 704 to reach the set load condition;
[0045] (6) Turn on the X-ray emitting / receiving device VI, adjust the X-ray incident angle and sample position, and perform real-time in-situ monitoring of the test area;
[0046] (7) Open the reactor connection port and adjust the back pressure valve V to be slightly lower than the pressure of the autoclave I to ensure that the experimental solution can be slowly discharged through the back pressure valve V after flowing into the reactor 5;
[0047] (8) Use a computer to monitor and record the relationship parameters of the system pressure, temperature and sample X-ray signal with time during the test, and analyze them in real time to obtain stress state and oxide film composition and structure information.
[0048] (9) After the test, shut off the operation of the heating device of the high pressure vessel I, turn off the motor 1, and close the water inlet valve; after draining the solution in the reactor 5, open the reactor 5, take out the tensile specimen 704, and the test is over.
[0049] The results show that this device simulates a high-temperature, high-pressure water environment using an autoclave and piping system, and controls solution flow using a back-pressure valve. The test end integrates tensile loading, cooling, and precise positioning functions, and the high-precision XYZ-axis test stage and angle adjustment base allow for flexible adjustment of the sample position and angle. A sapphire observation window, combined with a synchrotron X-ray emission / receiving device, enables real-time measurement of the sample's stress state and oxide film composition and structure. Techniques such as multiaxial diffraction (sin²ψ method), X-ray absorption spectroscopy (XAS), and fluorescence spectroscopy (XRF) are employed to achieve dynamic monitoring of the tensile sample's stress state and oxide film composition and structure.
Claims
1. An in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water, characterized in that, The apparatus consists of an autoclave, pipelines, a test end, an angle adjustment base, a back pressure valve, and an X-ray emitting / receiving device. The specific structure is as follows: The autoclave is located at the front; the test end, X-ray emitting / receiving device, and angle adjustment base are located in the middle. The test end is situated on the angle adjustment base, and the X-ray emitting / receiving device is located outside the reactor at the test end, corresponding to the tensile clamp and sample inside the test end. The X-ray emitting / receiving device VI monitors the sample in situ in real time during the experiment. A back pressure valve is installed at the end of the apparatus. The autoclave and the test end are connected via pipelines, and the test end and the back pressure valve are also connected via pipelines. A high-temperature, high-pressure solution meeting the experimental conditions enters the test end of the apparatus through pipeline II and then exits through the back pressure valve, ensuring the flow of solution within the reactor at test end III.
2. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 1, characterized in that, The test end consists of a motor, bushing, tension shaft, water-cooled sealing bushing, reactor, cooling base, tension fixture and specimen, and high-precision XYZ axis test platform. The specific structure is as follows: The tension mechanism composed of the motor, bushing, tension shaft and water-cooled sealing bushing is connected to the tension fixture and specimen inside the reactor. The reactor is fixed at the top center of the cooling base, which is set on the high-precision XYZ axis test platform.
3. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 2, characterized in that, The reactor is equipped with a reactor inlet and a reactor outlet. The reactor inlet is connected to the autoclave via a pipeline, and the reactor outlet is connected to the back pressure valve via a pipeline. By adjusting the back pressure valve, the high-temperature and high-pressure solution passes sequentially through the autoclave, the reactor inlet, the reactor, the reactor outlet, and the back pressure valve.
4. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 2, characterized in that, The reactor has symmetrical sealing flanges at both ends, and the upper end cover and lower end cover are respectively installed at both ends of the reactor through the sealing flanges. The entire reactor is sealed and fastened to the upper end cover and lower end cover through the sealing flanges and matching fastening bolts. The reactor has symmetrical sealing flanges on the side, and sapphire observation windows are respectively installed on the side of the reactor through the sealing flanges. The entire reactor is sealed and fastened to the sapphire observation windows through the sealing flanges and matching fastening bolts.
5. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 4, characterized in that, The reactor has an X-ray emission / receiving device with an emitter and a receiver on each side of the sapphire observation window. By adjusting the high-precision XYZ axis test stage and the angle adjustment base, the X-rays pass through the emitter, through the sapphire observation window to irradiate the sample gauge length, and then through the other side of the sapphire observation window to the receiver. The receiver of the X-ray emission / receiving device VI is connected to the computer.
6. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 2, characterized in that, The reactor is equipped with a tensile clamp and a specimen. The specimen is mounted on the upper clamp and the lower clamp respectively by pins at both ends. The upper clamp is connected to the tensile shaft, the bushing and the motor in sequence. A water-cooled sealing bushing is provided at the junction between the upper end cover of one end of the reactor and the tensile shaft.
7. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 2, characterized in that, The bottom of the reactor is equipped with a cooling base, which has an arc-shaped groove and slide rail corresponding to the bottom of the reactor. The side of the cooling base is equipped with a cooling water inlet and a cooling water outlet connected to the circulation channel inside the cooling base. The bottom of the cooling base is equipped with a high-precision XYZ axis test bench, and the position of the reactor is finely adjusted by bolts on the high-precision XYZ axis test bench.
8. The in-situ synchrotron radiation analysis device for stress state and oxide film composition structure of tensile specimens in high-temperature and high-pressure water according to claim 2, characterized in that, The bottom of the high-precision XYZ axis test bench is connected to an angle adjustment base. The angle adjustment base consists of an angle adjustment platform, a scissor height adjuster, a pin, an angle indicator, and a main frame. The angle adjustment platform is attached to the top of the main frame, and the boss in the middle of the bottom of the angle adjustment platform extends into the groove in the middle of the top of the main frame. The pin is vertically inserted into one end of the boss and the corresponding groove, allowing the angle adjustment platform to swing around the groove via the pin. The bottom surface of the other end of the boss corresponds to the scissor height adjuster located in the groove. The scissor height adjuster is composed of two sets of hinged connecting rods connected by a screw drive. The height is adjusted by rotating the screw, further adjusting the swing angle of the angle adjustment platform. At the same time, an angle indicator is provided on the angle adjustment platform of the angle adjustment base to display the angle between the angle adjustment platform and the horizontal plane.