In-situ environmental cell for material surface and interface damage characterization of multi-factor coupled corrosion

Abstract

The application provides a kind of for the material surface interface damage in-situ characterization environment bin of multi-factor coupling corrosion, it is related to in-situ detection equipment technical field, to solve the technical problem that cannot simulate marine atmospheric corrosion environment and provide in-situ test condition for sample in prior art;A kind of for the material surface interface damage in-situ characterization environment bin of multi-factor coupling corrosion, simulates the marine atmospheric corrosion environment of high humidity, high salt, temperature and other multi-factor coupling, wherein, salt fog generating device simulates the salt fog condition in marine atmosphere, laser heating module provides controllable thermal field, corrosion resistant loading platform provides controllable force field, so as to realize the simulation of thermal, salt, force multi-field coupling corrosion;At the same time, high temperature electrochemistry module can carry out in-situ monitoring of corrosion electrochemistry, X-ray entrance window and X-ray exit window allow X-ray diffractometer to carry out diffraction test, observation module directly carries out in-situ observation of corrosion, realizes the composite in-situ characterization technology under multi-factor simulation working condition.

Description

Technical Field

[0001] This invention relates to the field of in-situ testing equipment technology, specifically to an environmental chamber for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion. Background Technology

[0002] Key components of major marine equipment operate under complex conditions involving high humidity, high salinity, temperature, and stress for extended periods, subjecting their materials to corrosion damage caused by the coupling of multiple thermal, mechanical, and electrochemical fields. Particularly in the marine atmospheric environment, the coupling effect of the thermal field on the mechanical-salt corrosion process is particularly significant, leading to an order-of-magnitude increase in the corrosion rate and exhibiting nonlinear, unsteady, and accelerated failure characteristics.

[0003] Currently, electrochemical corrosion, mechano-electrochemical corrosion damage theories and thermodynamic models are relatively mature. However, a unified understanding of coupled corrosion damage under three or more physical fields has not yet been formed, especially the theory of multi-field corrosion damage caused by the thermal coupling of characteristic factors in marine environments. Therefore, it is urgent to conduct research on the corrosion damage behavior of materials under the coupled thermal, mechanical, and electrochemical fields in simulated marine atmospheric service environments, and to develop theories and evaluation models for multi-field coupled thermal, mechanical, and electrochemical corrosion damage, leading the development of marine materials corrosion science. Therefore, it is essential to develop an instrument that combines environmental simulation with in-situ / quasi-in-situ characterization in real-time environments, thereby establishing theories and evaluation models for multi-field coupled thermal, mechanical, and electrochemical corrosion damage, providing a theoretical basis for the surface and interface control of high-performance marine environmental materials. Simulation analysis of multi-field coupled thermal and electrochemical corrosion first requires simulating the marine atmospheric corrosion environment for the samples and providing in-situ testing conditions. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide an in-situ characterization environment chamber for material surface and interface damage in the context of multi-factor coupled corrosion, thereby solving the technical problem that existing technologies cannot simulate marine atmospheric corrosion environments and provide in-situ testing conditions for samples.

[0005] To address the aforementioned technical problems, this invention provides an in-situ characterization chamber for material surface and interface damage in the context of multi-factor coupled corrosion, comprising:

[0006] Warehouse body;

[0007] A corrosion-resistant loading stage is connected to the chamber and used to hold the sample laterally. The corrosion-resistant loading stage is equipped with leads for connecting to the sample.

[0008] A salt spray generator is connected to the chamber and sprays salt spray into the chamber.

[0009] Both the X-ray entrance window and the X-ray exit window are located on the upper part of the chamber and are arranged around the circumference of the chamber.

[0010] The high-temperature electrochemical module includes a driving component and a high-temperature electrode. The driving component drives the high-temperature electrode to swing horizontally and move vertically within the chamber, so that the high-temperature electrode comes into contact with the sample. The high-temperature electrode and the X-ray entrance window and X-ray exit window are distributed along the axial direction of the chamber.

[0011] A non-contact optical heating module is connected to the chamber and used to heat the sample;

[0012] The observation module connects to the chamber and is used to observe the samples.

[0013] With the above structure, the environmental chamber for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion of the present invention has the following advantages: By setting up a chamber body, a corrosion-resistant loading stage, a salt spray generator, an X-ray entrance window and an X-ray exit window, a high-temperature electrochemical module, a non-contact optical heating module, and an observation module, an integrated environmental chamber system is constructed, which can simulate a marine corrosion environment coupled with multiple factors such as high humidity, high salinity, stress, and temperature. Among them, the salt spray generator simulates the salt spray conditions in the marine atmosphere, the non-contact optical heating module provides a controllable thermal field, and the corrosion-resistant loading stage provides a stress field, thereby realizing the simulation of multi-field coupled corrosion of heat, salt, and force. Meanwhile, the X-ray entrance window and X-ray exit window allow the X-ray diffractometer to perform in-situ diffraction tests, and the observation module can directly perform in-situ corrosion observation, realizing in-situ characterization under simulated working conditions. Furthermore, the structure in which the high-temperature electrode and the X-ray entrance window and X-ray exit window are distributed along the axial direction of the chamber can be used for X-ray diffraction tests and electrochemical in-situ tests on the same sample. This solves the problem that existing technologies cannot simulate marine corrosion environments and provide in-situ testing conditions, and provides a foundation for the study of material corrosion damage behavior, mechanism revelation, and the establishment of evaluation models.

[0014] As an improvement, both the X-ray entrance window and the X-ray exit window are connected with polymer films. With this structure, the polymer films seal the X-ray entrance window and the X-ray exit window to prevent salt spray leakage, while not affecting the X-ray diffraction test. This ensures the accurate transmission of light signals during in-situ characterization, improves the reliability and data accuracy of long-term testing, and the chamber system sealed with polymer films can be vacuumed to achieve controllable adjustment for different environmental requirements.

[0015] As an improvement, the chamber is equipped with water channels surrounding the X-ray entrance window and the X-ray exit window, and the water channels are connected to a water supply device. This structure enables active cooling of the chamber, especially cooling of the polymer film inside the X-ray entrance window and the X-ray exit window, preventing the polymer film from being damaged by high temperature.

[0016] As an improvement, the high-temperature electrode includes a quartz tube, a counter electrode, and a reference electrode. The bottom of the quartz tube has an annular hole and a central hole, which are coaxially arranged. The counter electrode has an annular cross-section and is connected inside the annular hole. The reference electrode is columnar and is connected inside the central hole. Both the reference electrode and the counter electrode are made of platinum. The bottom ends of the counter electrode, the reference electrode, and the quartz tube are flush. An ion-conducting layer is connected to the bottom of the high-temperature electrode. The ion-conducting layer consists of a composite coating containing YSZ, with a total thickness of 50-200 μm. With this structure, since solid salt has low conductivity, the high-temperature electrode is designed as a columnar electrode. To ensure the collection of discrete corrosion signals on the working electrode (i.e., the sample), platinum is used for both the reference electrode and the counter electrode. The ion-conducting layer at the bottom of the high-temperature electrode forms a three-electrode circuit with the working electrode.

[0017] As an improvement, the drive assembly includes a frame, a first motor, a second motor, a connecting column, and a connecting block. The frame is connected to the upper end of the chamber. The connecting column is vertically rotatable and slidably connected to the frame. The lower end of the connecting column is located inside the chamber and connected to a horizontally positioned connecting block. A high-temperature electrode is connected to the bottom end of the connecting block and eccentrically positioned relative to the connecting column. A spring connects the high-temperature electrode to the connecting block, and a pressure sensor is connected to the high-temperature electrode. Both the first and second motors are connected to the frame and drive the connecting column to rotate and move vertically, respectively. This structure, by eccentrically positioning the high-temperature electrode and the connecting column, and utilizing the first and second motors to drive the rotation and vertical movement of the connecting column, solves the problem of space constraints in the upper part of the chamber. To address the limitations, the spatial layout was optimized. This driving method achieves a combined action of rotation for alignment and descent for sample contact, enabling the high-temperature electrode to smoothly and accurately contact the sample surface in a controllable manner. This ensures the reliability and consistency of the contact between the high-temperature electrode and the sample during electrochemical testing, providing a crucial guarantee for obtaining stable and repeatable in-situ electrochemical test data in complex simulation environments. The spring ensures a tight fit between the high-temperature electrode and the sample, and the pressure sensor can monitor and adjust the contact pressure between the high-temperature electrode and the sample in real time, ensuring the stability and consistency of the contact force during electrochemical testing. This avoids the impact of pressure changes on the electrochemical test results, improving the repeatability and accuracy of the test.

[0018] As an improvement, the drive assembly also includes a worm gear, a worm, a drive gear, and a gear set. The frame includes a fixed seat and a movable seat. The fixed seat is fixedly connected to the upper end of the chamber, and the movable seat is slidably connected to the upper end of the fixed seat vertically. The middle part of the connecting column is rotatably and slidably connected to the fixed seat, and the upper end of the connecting column is rotatably connected to the movable seat. The first motor is connected to the movable seat and drives the connecting column to rotate through the gear set. The second motor is connected to the fixed seat and the worm. The worm gear is rotatably connected to the fixed seat and has a drive gear coaxially mounted on it. The worm meshes with the worm gear. A rack portion is provided on the connecting column along the circumference, and the drive gear meshes with the rack portion. With this structure, the worm gear and rack structure enable the second motor to drive the vertical movement of the connecting column within a limited space. At the same time, the first motor can also independently drive the rotation of the connecting column through the gear set, achieving accurate positioning of the high-temperature electrode. This split-action design makes the two actions of the high-temperature electrode both independent and coordinated and precise, fundamentally solving the technical problem of achieving stable and reliable in-situ electrochemical contact in a compact space, and providing a key guarantee for obtaining high-precision multi-field coupled corrosion data.

[0019] As an improvement, a camera is connected to the high-temperature electrode; with this structure, the camera is used to observe the process of the high-temperature electrode contacting the sample via video.

[0020] As an improvement, the chamber is equipped with a salt spray outlet; this structure allows excess salt spray to be discharged, preventing excessively high air pressure inside the chamber.

[0021] As an improvement, the bottom of the corrosion-resistant loading stage is provided with a hollow section, and the non-contact optical heating module is a laser heating module. The laser heating module includes a two-dimensional galvanometer, a laser, and an infrared temperature measurement system located below the corrosion-resistant loading stage, and a light window is provided at the bottom of the chamber. With this structure, by setting a hollow section at the bottom of the corrosion-resistant loading stage, the laser can directly heat the sample from below, optimizing the spatial layout of the chamber. By controlling the laser and the two-dimensional galvanometer, the sample's back area of ​​any size and position can be continuously and uniformly heated. The infrared temperature measurement system irradiates the sample with infrared light from the hollow section to detect the sample temperature in real time, thereby realizing the adjustment of the heating temperature.

[0022] As an improvement, the observation module includes a long-focal-length microscope that is obliquely set and slidably connected to the upper part of the chamber in the horizontal direction. The long-focal-length microscope is at an angle of 40-60° with the sample plane. With this structure, the obliquely set long-focal-length microscope makes full use of the limited space inside the chamber. By moving the long-focal-length microscope, confocal imaging of the sample surface can be achieved, or the long-focal-length microscope can be fixed to scan and stitch images along the length of the sample, thus realizing the in-situ observation function.

[0023] As an improvement, the chamber is connected to a positioning laser device, and the upper part of the chamber is provided with a laser positioning hole through which the positioning laser of the positioning laser device passes. With this structure, in conjunction with a long-focal microscope, a positioning system is formed to ensure that the laser positioning point and the X-ray analysis point coincide when the X-ray diffractometer is in microfocal spot analysis mode.

[0024] As an improvement, the chamber is equipped with a track, and the corrosion-resistant loading platform is slidably connected to the track. The track is equipped with a water channel, which is connected to a water-cooling device. This structure enables the corrosion-resistant loading platform to be transferred between the environmental chamber and other modules, and the water-cooling device circulates water in the water channel to conduct excess heat. Attached Figure Description

[0025] Figure 1 This is a three-dimensional structural diagram of the present invention;

[0026] Figure 2 This is a three-dimensional structural diagram of the present invention with the compartment body removed;

[0027] Figure 3 This is a schematic diagram of the high-temperature electrode in this invention;

[0028] Figure 4 This is a three-dimensional structural diagram of the high-temperature electrochemical module in this invention;

[0029] Figure 5 This is a top view of the high-temperature electrochemical module in this invention;

[0030] Figure 6 for Figure 5 Sectional view of section AA;

[0031] Figure 7 for Figure 5 Cross-sectional view of the middle BB section.

[0032] Reference numerals: 1. Chamber body; 2. Corrosion-resistant loading stage; 3. Salt spray generator; 4. X-ray entrance window; 5. X-ray exit window; 6. Drive assembly; 61. Frame; 611. Fixed base; 612. Movable base; 62. First motor; 63. Second motor; 64. Connecting column; 65. Connecting block; 66. Worm gear; 67. Worm; 68. Drive gear; 69. Gear set; 7. High-temperature electrode; 71. Quartz tube; 72. Counter electrode; 73. Reference electrode; 8. Observation module; 9. Ion conduction layer; 10. Two-dimensional galvanometer; 11. Rack section; 12. Laser; 13. Laser positioning hole. Detailed Implementation

[0033] The following is a detailed description of the environmental chamber for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion according to the present invention, with reference to the accompanying drawings.

[0034] like Figures 1 to 7 As shown, an environmental chamber for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion is used to simulate multi-field corrosion conditions in marine environments. During use, it is set in the X-ray diffractometer (XRD) chamber and includes a chamber body 1, a corrosion-resistant loading stage 2, a salt spray generator 3, an X-ray entrance window 4, an X-ray exit window 5, a high-temperature electrochemical module, a non-contact optical heating module, and an observation module 8. The corrosion-resistant loading stage 2 is connected inside the chamber body 1 and is used to laterally clamp the sample. The corrosion-resistant loading stage 2 is equipped with a drive shaft with two sections of oppositely helical threads. Two movable seats are threaded onto the drive shaft, which is driven by a motor to rotate, allowing the two movable seats to clamp the sample and apply stress to it. Furthermore, the corrosion-resistant loading stage 2 is equipped with a lead wire for connecting to the sample. Specifically, the lead wire is located on one of the movable seats, allowing the sample to be connected to the lead wire after being placed on that seat.

[0035] like Figure 1 and Figure 2 As shown, the salt spray generator 3 is connected to the chamber 1 and sprays salt spray into the chamber 1. The salt spray generator 3 includes a water tank, a rotor flow meter, an ultrasonic atomizing device, and a heating device. The temperature adjustment range of the salt spray generator 3 is from room temperature to 60°C. The salt spray generator 3 can form a uniform dissolved salt spray environment on the sample surface. The corrosive environment of solid salt and molten salt on the sample surface is formed by heating the dissolved salt on the sample surface.

[0036] In salt spray generating device 3, a NaCl solution of a certain concentration is passed through an ultrasonic atomizing device. The ultrasonic atomizing device uses the high-frequency resonant ultrasonic energy of a ceramic atomizing plate to break down the liquid molecular structure of the NaCl solution, converting it into particles ranging from a few micrometers to one hundred micrometers in size, forming a naturally drifting mist. This mist is mixed with compressed air, and a temperature control and display system is used to achieve a constant pressure and temperature for the experimental salt spray airflow. An air generator connected to a pressure regulating valve controls and provides a stable airflow, which is then connected to a rotor flow meter to obtain a specific flow rate of airflow and introduce it into chamber 1. The water reservoir is made of glass, with a movable lid at the top for easy replenishment of the solution. An opening at the lower side connects to a valve that can adjust the liquid flow rate, and a rubber hose connects it to the salt spray nozzle of the ultrasonic atomizing device to provide NaCl salt spray for the salt spray experiment.

[0037] In addition, the chamber 1 is equipped with a salt spray outlet to discharge excess salt spray and prevent excessive air pressure inside the chamber 1.

[0038] like Figure 1As shown, X-ray entrance window 4 and X-ray exit window 5 are both located on the upper part of the chamber 1 and arranged circumferentially along the chamber 1. It should be noted that the arrangement of X-ray entrance window 4 and X-ray exit window 5 along the circumferential direction of the chamber 1 does not mean that the chamber 1 is a circular structure. In this invention, the circumferential and axial directions of the chamber 1 represent two directions of the chamber 1. The axial direction of the chamber 1 is its length direction, which is the length direction of the sample. The arrangement of X-ray entrance window 4 and X-ray exit window 5 along the circumferential direction of the chamber 1 means that X-ray entrance window 4 and X-ray exit window 5 are located in the same length direction of the chamber 1. In this embodiment, the chamber 1 includes a cuboid part and a cylindrical part. X-ray entrance window 4 and X-ray exit window 5 are located in the cylindrical part and distributed along its circumferential direction.

[0039] In addition, both the X-ray entrance window 4 and the X-ray exit window 5 are connected with polymer films to prevent salt spray leakage. This is used for X-ray diffraction testing under multiple corrosion conditions. Moreover, the chamber 1 system sealed with polymer films can be vacuumed to achieve controllable adjustment for different environmental requirements. In this embodiment, the polymer film is a polyimide film.

[0040] The chamber 1 is equipped with water channels surrounding the X-ray entrance window 4 and the X-ray exit window 5. These water channels are connected to a water supply device to maintain the inner wall temperature of the chamber 1 at or below 50°C, preventing high-temperature damage to the XRD process. Furthermore, the device cools the polymer films within the X-ray entrance window 4 and the X-ray exit window 5, preventing damage due to high temperatures. In this embodiment, the chamber 1 is made of a highly corrosion-resistant titanium alloy.

[0041] like Figure 1 and Figure 2 As shown, the high-temperature electrochemical module includes a driving component 6 and a high-temperature electrode 7. The driving component 6 drives the high-temperature electrode 7 to swing horizontally and move vertically within the chamber 1, causing the high-temperature electrode 7 to contact the sample. The high-temperature electrode 7, along with the X-ray entrance window 4 and the X-ray exit window 5, are distributed along the axial direction of the chamber 1. To address the need for simultaneous in-situ measurement of electrochemistry and diffraction under thermosalt conditions, and to meet the requirement of non-intermittent electrochemical testing, the sample is lengthened, dividing the parallel section of the sample into two parts: one for diffraction and the other for electrochemical testing. The sample material and size can be replaced according to actual conditions. The positions of the X-ray entrance window 4, the X-ray exit window 5, and the high-temperature electrode 7 correspond to the diffraction and electrochemical portions of the sample, respectively. The high-temperature electrochemical module has a potential fluctuation ≤ ±20mV and a current testing limit ≤ 0.05nA.

[0042] like Figure 3As shown, the high-temperature electrode 7 includes a quartz tube 71, a counter electrode 72, and a reference electrode 73. The bottom end of the quartz tube 71 has an annular hole and a central hole, all coaxially arranged. The counter electrode 72 has an annular cross-section and is connected within the annular hole. The reference electrode 73 is columnar and is connected within the central hole. Both the reference electrode 73 and the counter electrode 72 are made of platinum. The bottom ends of the counter electrode 72, the reference electrode 73, and the quartz tube 71 are flush. An ion-conducting layer 9 is connected to the bottom end of the high-temperature electrode 7. The ion-conducting layer 9 consists of a composite coating containing YSZ, with a total thickness of 50-200 μm. Due to the low conductivity of solid salt, the high-temperature electrode 7 is designed as a columnar electrode. To ensure the collection of discrete corrosion signals on the working electrode, the reference electrode 73 and the counter electrode 72 are made of platinum. The ion-conducting layer 9 at the bottom of the high-temperature electrode 7 forms a three-electrode circuit with the working electrode, where the sample is the working electrode.

[0043] The high-temperature electrode 7 is connected to a pressure sensor, which can monitor and adjust the contact pressure between the high-temperature electrode 7 and the sample in real time, ensuring the stability and consistency of the contact force during the electrochemical test, avoiding the impact of pressure changes on the electrochemical test results, and improving the repeatability and accuracy of the test.

[0044] like Figure 4 As shown, the drive assembly 6 includes a frame 61, a first motor 62, a second motor 63, a connecting column 64, and a connecting block 65. The frame 61 is connected to the upper end of the chamber 1. The connecting column 64 is vertically rotatable and slidably connected to the frame 61, that is, the rotation axis and sliding direction of the connecting column 64 are both vertical. The lower end of the connecting column 64 is located inside the chamber 1 and is connected to a horizontally arranged connecting block 65. The high-temperature electrode 7 is connected to the bottom end of the connecting block 65 and is eccentrically arranged with the connecting column 64. A spring is connected between the high-temperature electrode 7 and the connecting block 65. The first motor 62 and the second motor 63 are both connected to the frame 61 and drive the connecting column 64 to rotate and move vertically, respectively.

[0045] The high-temperature electrode 7 is also connected to a camera, which is used to observe the process of the high-temperature electrode 7 contacting the sample via video.

[0046] Furthermore, such as Figures 5 to 7As shown, the drive assembly 6 also includes a worm gear 66, a worm 67, a drive gear 68, and a gear set 69. The frame 61 includes a fixed seat 611 and a movable seat 612. The fixed seat 611 is fixedly connected to the upper end of the chamber 1, and the movable seat 612 is slidably connected to the upper end of the fixed seat 611 along the vertical direction. The movable seat 612 is provided with several guide rods that are slidably connected to the fixed seat 611. The middle part of the connecting column 64 is rotatably and slidably connected to the fixed seat 611, and the upper end of the connecting column 64 is rotatably connected to the movable seat 612. The first motor 62 is connected to the movable seat 612, and the first motor 62 drives the connecting column 64 to rotate through the gear set 69. Specifically, the output shaft of the first motor 62 is vertically arranged and connected to a gear. The connecting column 64 is also connected to a gear. These two gears transmit power through an intermediate gear, thereby driving the connecting column 64 to rotate by the first motor 62. The second motor 63 is connected to the fixed base 611. The output shaft of the second motor 63 is vertically arranged and connected to the worm 67. The worm wheel 66 is horizontally arranged and rotatably connected to the fixed base 611 and has a drive gear 68 coaxially arranged. The worm 67 meshes with the worm wheel 66. The connecting column 64 has a rack portion 11 along the circumferential direction. The drive gear 68 meshes with the rack portion 11. The second motor 63 drives the drive gear 68 to rotate through the worm 67 and the worm wheel 66. When the drive gear 68 rotates, it drives the connecting column 64 to move vertically.

[0047] A non-contact optical heating module is connected to the chamber 1 and used for heating the sample. Specifically, the bottom of the corrosion-resistant loading stage 2 has a hollow section. The non-contact optical heating module is a laser heating module, which includes a two-dimensional galvanometer 10, a laser 12, and an infrared temperature measurement system located below the corrosion-resistant loading stage 2. A light window is provided at the bottom of the chamber 1. The two-dimensional galvanometer 10, laser 12, and infrared temperature measurement system are all located outside the chamber 1. The laser is directed into the two-dimensional galvanometer 10, and the two-dimensional galvanometer 10 is controlled to continuously heat any area of ​​arbitrary size and position on the back of the sample. This method has higher temperature uniformity, with heating temperatures ranging from 20 to 850 degrees Celsius and heating areas ranging from 0 to 4 square centimeters. The infrared temperature measurement system irradiates the sample with infrared light from the hollow section to detect the sample temperature in real time. The laser power is adjusted through negative feedback to ensure the consistency of the sample temperature. The laser 12 is a fiber laser. In some other embodiments, the laser heating module can adopt a heating method with a homogenized light spot.

[0048] like Figure 1 and Figure 2As shown, the observation module 8 is connected to the chamber 1 and used for observing the sample. The observation module 8 includes a long-focal-length microscope that is obliquely set and slidably connected to the upper part of the chamber 1 in the horizontal direction. The long-focal-length microscope forms an angle of 40-60° with the sample plane. The observation module 8 is used to visualize the corrosion area under multi-field coupled corrosion. Due to space constraints, the long-focal-length microscope is used at a specific angle with the sample. In this embodiment, the long-focal-length microscope is incident at 55°. Confocal imaging of the sample surface is achieved by moving the long-focal-length microscope, or by fixing the long-focal-length microscope and scanning and stitching images along the length of the sample to ensure clear imaging in the tilted state, thus realizing the in-situ observation function. Specifically, the direction of movement of the long-focal-length microscope is along the axial direction of the cylindrical part, that is, the length direction of the sample. In some other embodiments, the long-focal-length microscope can be rotatably connected to the chamber 1, thereby achieving adjustment within the angle range of 40-90°.

[0049] Furthermore, such as Figure 1 and Figure 2 As shown, the chamber 1 is connected to a positioning laser device. The upper part of the chamber 1 is provided with a laser positioning hole 13 for the positioning laser of the positioning laser device to pass through. It works in conjunction with the long focal length microscope to form a positioning system, ensuring that the laser positioning point and the X-ray analysis point coincide when the X-ray diffractometer adopts the micro-focal spot analysis mode. In this embodiment, the laser positioning hole 13 is located between the X-ray entrance window 4 and the X-ray exit window 5.

[0050] In addition, a cover is provided at the top of the chamber 1, and the corrosion-resistant loading platform 2 can be placed in the chamber by opening the cover.

[0051] The chamber 1 is equipped with a track, and the corrosion-resistant loading platform 2 is slidably connected to the track. The track is equipped with a water channel, which is connected to a water cooling device to realize the transfer of the corrosion-resistant loading platform 2 between the environmental chamber and other modules. The water cooling device circulates water in the water channel to conduct excess heat.

[0052] This invention constructs an integrated environmental chamber system by setting up a chamber body 1, a corrosion-resistant loading platform 2, a salt spray generator 3, an X-ray entrance window 4 and an X-ray exit window 5, a high-temperature electrochemical module, a laser heating module, and an observation module 8. This system can simulate a marine corrosion environment with multiple coupled factors such as high humidity, high salinity, stress, and temperature. Specifically, the salt spray generator 3 simulates salt spray conditions in the marine atmosphere, the laser heating module provides a controllable thermal field, and the corrosion-resistant loading platform 2 provides a stress field, thereby achieving the simulation of corrosion coupled by multiple fields of heat, salt, and force. Meanwhile, the X-ray entrance window 4 and X-ray exit window 5 allow the X-ray diffractometer to perform in-situ diffraction tests, and the observation module 8 can directly perform in-situ corrosion observation, realizing in-situ characterization under simulated working conditions. Furthermore, the high-temperature electrode 7 and the structure of the X-ray entrance window 4 and X-ray exit window 5 distributed along the axial direction of the chamber 1 can be subjected to X-ray diffraction tests and electrochemical in-situ tests on the same sample, solving the problem that existing technologies cannot simulate marine corrosion environments and provide in-situ testing conditions. This provides a foundation for the study of material corrosion damage behavior, mechanism revelation, and the establishment of evaluation models.

[0053] The following example uses a titanium alloy sample: At room temperature, the salt spray generator 3 is turned on, controlling the salt spray temperature at 50℃, the flow rate at 0.7m / s, and the salt spray size at 1µm. After 10 minutes, the salt spray generator 3 is turned off, and the laser heating module is turned on. The laser power is adjusted using the negative feedback of the infrared thermometer to stabilize the titanium alloy sample at 850℃. The observation module 8 is turned on, magnified to 1000X, and the focus is adjusted until the image is clear. After the salt spray on the surface of the titanium alloy sample turns into a molten state, the high-temperature electrode 7 is lowered to perform in-situ electrochemical testing. Simultaneously, XRD experimental parameters are set to begin in-situ XRD testing. During the process of corrosion products appearing on the surface of the titanium alloy sample, continuous electrochemical and multiple XRD tests are performed. When the corrosion products no longer change, the electrochemical and XRD tests are stopped, and the high-temperature electrode 7 is raised. Stress is applied to the corrosion-resistant loading stage 2, and the stress-strain curve of the titanium alloy sample is tested, and the in-situ tensile fracture process of the titanium alloy sample is observed.

[0054] The embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited to the above-described embodiment. All other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

Claims

1. A chamber for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion, characterized in that, include: Warehouse body (1); A corrosion-resistant loading stage (2) is connected inside the chamber (1) and used to hold the sample laterally. The corrosion-resistant loading stage (2) is provided with a lead wire for connecting to the sample. A salt spray generator (3) is connected to the chamber (1) and sprays salt spray into the chamber (1); The X-ray entrance window (4) and the X-ray exit window (5) are both located on the upper part of the chamber (1) and are arranged around the circumference of the chamber (1); The high-temperature electrochemical module includes a driving component (6) and a high-temperature electrode (7). The driving component (6) drives the high-temperature electrode (7) to swing horizontally and move vertically within the chamber (1) so that the high-temperature electrode (7) comes into contact with the sample. The high-temperature electrode (7), the X-ray entrance window (4), and the X-ray exit window (5) are distributed along the axial direction of the chamber (1). A non-contact optical heating module is connected to the chamber (1) and used to heat the sample; The observation module (8) is connected to the chamber (1) and used to observe the sample; The drive assembly (6) includes a frame (61), a first motor (62), a second motor (63), a connecting column (64), and a connecting block (65). The frame (61) is connected to the upper end of the chamber (1). The connecting column (64) is vertically rotatable and slidably connected to the frame (61). The lower end of the connecting column (64) is located inside the chamber (1) and connected to the connecting block (65) arranged horizontally. The high-temperature electrode (7) is connected to the bottom end of the connecting block (65) and is eccentrically arranged with the connecting column (64). A spring is connected between the high-temperature electrode (7) and the connecting block (65). A pressure sensor is connected to the high-temperature electrode (7). The first motor (62) and the second motor (63) are both connected to the frame (61) and drive the connecting column (64) to rotate and move vertically, respectively. The high-temperature electrode (7) includes a quartz tube (71), a counter electrode (72), and a reference electrode (73). The bottom end of the quartz tube (71) is provided with an annular hole and a central hole. The annular hole, the central hole, and the quartz tube (71) are all coaxially arranged. The counter electrode (72) has an annular cross-section and is connected in the annular hole. The reference electrode (73) is columnar and is connected in the central hole. The reference electrode (73) and the counter electrode (72) are both made of platinum. The bottom ends of the counter electrode (72), the reference electrode (73), and the quartz tube (71) are all flush. The bottom end of the high-temperature electrode (7) is connected to an ion-conducting layer (9). The drive assembly (6) further includes a worm gear (66), a worm (67), a drive gear (68), and a gear set (69). The frame (61) includes a fixed seat (611) and a movable seat (612). The fixed seat (611) is fixedly connected to the upper end of the chamber (1). The movable seat (612) is slidably connected vertically to the upper end of the fixed seat (611). The middle part of the connecting column (64) is rotatably and slidably connected to the fixed seat (611). The upper end of the connecting column (64) is rotatably connected to the movable seat (612). The first motor (62) is connected to... The movable seat (612) is connected to the fixed seat (611) by the first motor (62) through the gear set (69), the second motor (63) is connected to the worm (67), the worm wheel (66) is rotatably connected to the fixed seat (611) and coaxially provided with the drive gear (68), the worm (67) meshes with the worm wheel (66), the connecting column (64) is provided with a rack (11) along the circumferential direction, and the drive gear (68) meshes with the rack (11).

2. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, Both the X-ray entrance window (4) and the X-ray exit window (5) are connected to a polymer film.

3. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 2, characterized in that, The chamber (1) is provided with a water channel surrounding the X-ray entrance window (4) and the X-ray exit window (5), and the water channel is connected to a water supply device.

4. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The ion-conducting layer (9) is composed of a composite coating containing YSZ, and the total thickness of the composite coating is 50-200 μm.

5. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The high-temperature electrode (7) is connected to a camera.

6. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The chamber (1) is equipped with a salt spray outlet.

7. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The bottom of the corrosion-resistant loading platform (2) is provided with a hollow part. The non-contact optical heating module is a laser heating module. The laser heating module includes a two-dimensional galvanometer (10), a laser (12) and an infrared temperature measurement system located below the corrosion-resistant loading platform (2). The bottom of the chamber (1) is provided with a light window.

8. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The observation module (8) includes a long-focus microscope that is obliquely set and slidably connected to the upper part of the chamber (1) in the horizontal direction. The long-focus microscope is at an angle of 40-60° with the sample plane.

9. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 8, characterized in that, The chamber (1) is connected to a positioning laser device, and the upper part of the chamber (1) is provided with a laser positioning hole (13) through which the positioning laser of the positioning laser device passes.

10. The environmental chamber for in-situ characterization of material surface and interface damage for multi-factor coupled corrosion as described in claim 1, characterized in that, The silo body (1) is provided with a track, and the corrosion-resistant loading platform (2) is slidably connected to the track. The track is provided with a water channel, and the water channel is connected to a water cooling device.

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