In-situ characterization system for material surface and interface damage in multi-factor coupled corrosion
By integrating X-ray diffractometer, electron microscope and other equipment into a multi-factor coupled in-situ corrosion characterization system, the problem of in-situ observation and dynamic evolution tracking of material surface interfaces under multi-field coupling environment has been solved, and the development of high safety performance of marine materials has been realized.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI
- Filing Date
- 2025-12-03
- Publication Date
- 2026-05-22
Smart Images

Figure CN121253422B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of in-situ testing equipment technology, specifically to an in-situ characterization system for material surface and interface damage in the context of multi-factor coupled corrosion. Background Technology
[0002] Key components of major marine equipment operate for extended periods in complex environments characterized by high humidity, high salinity, temperature, and stress, facing corrosion damage under the coupled effects of heat, force, and salt. Particularly in marine atmospheric environments, the coupling effect of heat, force, and salt is significant, greatly increasing the corrosion rate compared to single environmental factors, leading to nonlinear, unsteady, and accelerated failure of the materials.
[0003] However, the study of the microscopic mechanisms of damage behavior in materials under such multi-field coupling environments still faces significant challenges. On the one hand, there is a lack of effective means to conduct in-situ microscopic observations of material interfaces under simulated service conditions. On the other hand, because different analytical instruments (such as X-ray diffractometers and electron microscopes) are independent of each other, the transfer of samples between different instruments inevitably destroys the original state of the corrosion products, making it impossible to accurately track the dynamic evolution of the interface in the same region during corrosion. This lack of in-situ characterization analysis severely restricts a deep understanding of the multi-field coupling corrosion mechanism, thus affecting the development of marine materials with high safety performance. Therefore, there is an urgent need for an in-situ characterization system that can integrate environmental simulation and multi-field coupling to achieve accurate tracking of the damage process at the material corrosion interface. Summary of the Invention
[0004] To address the shortcomings of existing technologies, the present invention aims to provide an in-situ characterization system for material surface and interface damage in the context of multi-factor coupled corrosion. This system solves the technical problem that existing technologies cannot perform in-situ microscopic observation of material surfaces and interfaces under simulated service environments and accurately track the dynamic evolution of corrosion behavior at the same interface during corrosion.
[0005] To address the aforementioned technical problems, this invention provides an in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion, comprising:
[0006] X-ray diffractometer;
[0007] Electron microscopy;
[0008] The environmental chamber is located inside the X-ray diffractometer;
[0009] Salt spray generator connected to environmental chamber;
[0010] Both the X-ray entrance window and the X-ray exit window are located on the environmental chamber;
[0011] The transfer chamber and the pre-extraction chamber are connected at one end to the environmental chamber via a first gate valve, and at the other end of the transfer chamber through the side wall of the X-ray diffractometer and connected to one end of the pre-extraction chamber via a second gate valve. The other end of the pre-extraction chamber is connected to the electron microscope via a third gate valve.
[0012] Vacuum pump unit, connected to the pre-evacuation chamber and used to evacuate the pre-evacuation chamber alone or to simultaneously evacuate the transfer chamber and the pre-evacuation chamber;
[0013] The track assembly is located inside the environmental chamber, transfer chamber, pre-extraction chamber, and electron microscope;
[0014] A corrosion-resistant loading stage with a sliding connection track assembly for laterally clamping samples;
[0015] The first drive assembly is used to drive the corrosion-resistant loading stage to move along the track assembly between the environmental chamber, transfer chamber, pre-extraction chamber and electron microscope;
[0016] The multi-point heating module is used to heat samples in the environmental chamber, pre-extraction chamber, and electron microscope.
[0017] With the above structure, the in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion of the present invention has the following advantages: the corrosion-resistant loading stage holds the sample in an environmental chamber, and the salt spray generator simulates the salt spray conditions in the marine atmosphere. The multi-point 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. At the same time, the X-ray entrance window and X-ray exit window allow the X-ray diffractometer to perform in-situ diffraction tests, realizing in-situ phase analysis of corrosion products under simulated working conditions. After the X-ray diffraction test is completed, the system is driven by the first driving component. The corrosion-resistant loading stage enters the pre-evacuation chamber through the transfer chamber. The pre-evacuation chamber is pre-evacuated by the vacuum pump group, so that the corrosion-resistant loading stage can be smoothly introduced into the electron microscope for micro-area structure and micro-area composition analysis. During the pre-evacuation process and electron microscope testing, the sample is continuously heated by the multi-point heating module, which can maintain the consistency of the sample state in the X-ray diffractometer and electron microscope. At different heating sites, thermal, salt and force environmental experiments can be carried out, so as to conduct in-situ microscopic observation of the material surface and interface under simulated service environment, and accurately track the dynamic evolution of the surface and interface in the same area during corrosion.
[0018] As an improvement, the track assembly includes a first track, a second track, a third track, a fourth track, a fifth track, and a sixth track. The first and second tracks are located inside the environment chamber, the third track is located inside the transfer chamber, the fourth and fifth tracks are located inside the pre-extraction chamber, and the sixth track is located inside the electron microscope. The first, fifth, and sixth tracks are all arranged in the front-to-back direction, with the fifth and sixth tracks coaxially arranged. The second, third, and fourth tracks are all arranged in the left-to-right direction and are all coaxially arranged. The second, third, and fourth tracks are located between the first and fifth tracks. This structure optimizes the space utilization efficiency within the system and avoids the problems of system redundancy and large footprint caused by using a single long-distance track between the environment chamber, transfer chamber, pre-extraction chamber, and electron microscope.
[0019] As an improvement, the present invention also includes a sliding seat. The upper ends of the first, fifth, and sixth tracks are each provided with a first dovetail-shaped protrusion arranged in the front-back direction. The bottom end of the corrosion-resistant loading platform is provided with a first dovetail groove that slides through the first dovetail-shaped protrusion in the front-back direction. The upper ends of the second, third, and fourth tracks are each provided with a second dovetail groove that slides through the second dovetail groove in the left-right direction and extends to the first and fifth tracks in the left-right direction, respectively. The bottom end of the sliding seat is provided with a second dovetail-shaped protrusion that slides through the second dovetail groove. The upper end of the sliding seat is provided with a third dovetail-shaped protrusion that slides through the first dovetail groove in the front-back direction. With this structure, the corrosion-resistant loading platform can slide independently along the first track. After the corrosion-resistant loading platform is connected to the sliding seat, the sliding seat drives the corrosion-resistant loading platform to move along the second, third, and fourth tracks. After the sliding seat carries the corrosion-resistant loading platform into the fifth track, the corrosion-resistant loading platform still moves independently along the fifth and sixth tracks. The introduction of the sliding seat realizes the turning of the corrosion-resistant loading platform between tracks.
[0020] As an improvement, the first drive assembly includes a first push rod, a second push rod, a first drive motor, a gear, and a rack. The first push rod is slidably connected to the rear side wall of the environmental chamber in the front-to-back direction, and the second push rod is slidably connected to the rear side wall of the pre-extraction chamber in the front-to-back direction. The first and second push rods are rotatably connected to the environmental chamber and the pre-extraction chamber, respectively. The bottom end of the corrosion-resistant loading platform is provided with a slot. The side walls of the first and second push rods are provided with limiting protrusions. By rotating the first or second push rod, the limiting protrusions are engaged or disengaged from the slot. The rack is slidably connected to the right side wall of the environmental chamber in the left-to-right direction and is connected to a sliding seat. The first drive motor is connected to the outer wall of the environmental chamber and drives the gear to rotate. The gear meshes with the rack. With this structure, the limiting protrusions on the first and second push rods and the slot design at the bottom end of the corrosion-resistant loading platform allow the first and second push rods to be separated from the corrosion-resistant loading platform, facilitating the transfer of the corrosion-resistant loading platform between different chambers. The sliding seat always moves in the same direction. The first drive motor, gear, and rack achieve precise and automated control of the sliding seat.
[0021] As an improvement, both the first push rod and the second push rod have positioning protrusions on their side walls, and the bottom of the corrosion-resistant loading platform has a positioning groove. When the positioning protrusion is engaged in the positioning groove, the first push rod or the second push rod is rotated to make the limiting protrusion engage in the groove. With this structure, the positional relationship between the limiting protrusion and the groove is determined by the positioning protrusion and the positioning groove, so that the limiting protrusion can be accurately engaged in the groove.
[0022] As an improvement, water channels are provided in the first, fifth, and sixth tracks, and the water channels in the first, fifth, and sixth tracks are all connected to water supply devices. With this structure, water is circulated into the water channels by the water supply devices, and the first, fifth, and sixth tracks act as cold ends to conduct heat, thus avoiding deformation due to prolonged heating and ensuring the stability of the entire system during long-term operation in high-temperature environments.
[0023] As an improvement, the environmental chamber is connected to a second drive assembly. The corrosion-resistant loading stage includes a base, a first movable seat, a second movable seat, a transmission rod, a first worm gear, a first worm, a second worm gear, and a second worm. Both the first and second movable seats are slidably connected to the base in the front-to-back direction. The upper surfaces of the first and second movable seats are respectively provided with a first limiting groove and a second limiting groove for placing samples. The first and second limiting grooves are connected in the front-to-back direction. The transmission rod is rotatably connected to the base in the front-to-back direction. The transmission rod has a first threaded section and a second threaded section with opposite rotational directions along its axial direction. The first and second threaded sections are threadedly connected to the first and second movable seats, respectively. The transmission rod has a first worm gear. The first worm is rotatably connected to the base in the left-to-right direction and meshes with the first worm gear. The first worm has a second worm gear. The second worm is rotatably connected to one end of the base in the front-to-back direction and meshes with the second worm gear. A portion of the second worm gear is located away from the first movable seat. The end is provided with an interface for detachable connection with the second drive assembly, which drives the second worm gear to rotate. With this structure, the second drive assembly drives the second worm gear to rotate, which in turn drives the transmission rod to rotate via the second worm wheel, the first worm gear, and the first worm wheel. The first and second threaded sections on the transmission rod allow the first and second movable seats to move closer or further apart. The closer-approaching first and second movable seats clamp the sample within the first and second limiting grooves and apply a load to the sample. The interface enables detachable connection with the second drive assembly, allowing the corrosion-resistant loading stage to be separated from the second drive assembly, preventing the second drive assembly from being corroded by salt spray. It also allows the corrosion-resistant loading stage to be transferred between chambers. Furthermore, after the second drive assembly is separated from the corrosion-resistant loading stage, the worm wheel and worm gear self-lock the first and second movable seats, maintaining the load on the sample and ensuring that the stress state of the sample remains consistent in the X-ray diffractometer and electron microscope.
[0024] As an improvement, the second drive assembly includes a connecting plate, a second drive motor, and a drive rod. The connecting plate is slidably connected to the outside of the environmental chamber in the front-to-back direction. The drive rod is rotatably connected to the connecting plate and the environmental chamber and is slidably connected to the environmental chamber. The second drive motor is connected to the connecting plate and is used to drive the drive rod to rotate. One end of the drive rod is detachably connected to the interface. With this structure, the interface between the drive rod and the second worm gear is detachably connected, so that when the corrosion-resistant loading stage needs to move within the system, the second drive assembly can be disengaged from it to avoid interference. When a load needs to be applied, it can be precisely connected and torque can be transmitted through the sliding connecting plate.
[0025] As an improvement, the bottom of the corrosion-resistant loading stage is provided with a perforated section for laser transmission. The multi-point heating module includes a first non-contact optical heating device connected to the environmental chamber, a second non-contact optical heating device connected to the pre-extraction chamber, and a third non-contact optical heating device connected to the electron microscope. The first, second, and third non-contact optical heating devices all include temperature measuring components. With this structure, non-contact optical heating combined with temperature measurement and a perforated section at the bottom of the corrosion-resistant loading stage are used to achieve non-contact, localized, precise heating and real-time temperature monitoring. The temperature measurement enables closed-loop temperature control, ensuring that the temperature of the sample remains consistent in the X-ray diffractometer and electron microscope.
[0026] As an improvement, the other end of the pre-evacuation chamber can be disconnected from the third slide valve via a connecting assembly. With this structure, when the sample is tested in the electron microscope, the electron microscope is separated from the pre-evacuation chamber via the connecting assembly to prevent external vibrations from affecting the accuracy of the electron microscope test.
[0027] As an improvement, the connecting assembly includes a fixing bolt and a nut, with the nut located on the third slide valve. The fixing bolt passes through the pre-extraction chamber and is threadedly connected to the nut. This structure provides a simple, reliable, and cost-effective detachable connection solution. This mechanical fastening method ensures a stable connection and guarantees the clamping force required for vacuum sealing. At the same time, the assembly and disassembly process is simple and quick, requiring no special tools. Attached Figure Description
[0028] Figure 1 This is a three-dimensional structural diagram of the present invention;
[0029] Figure 2 This is a three-dimensional structural diagram of the environmental chamber in this invention;
[0030] Figure 3 This is a top view of the corrosion-resistant loading platform in this invention;
[0031] Figure 4 This is a cross-sectional schematic diagram of the first push rod and the corrosion-resistant loading platform in this invention;
[0032] Figure 5 for Figure 4 Enlarged view of part A in the middle;
[0033] Figure 6 This is a cross-sectional schematic diagram of the sliding seat and rack in this invention;
[0034] Figure 7 This is a three-dimensional structural diagram of the base in this invention;
[0035] Figure 8 This is a top view of the track assembly in this invention.
[0036] Reference numerals: 1. X-ray diffractometer; 2. Electron microscope; 3. Environmental chamber; 4. Salt spray generator; 5. X-ray entrance window; 6. X-ray exit window; 7. Transfer chamber; 8. Pre-extraction chamber; 9. First slide gate valve; 10. Second slide gate valve; 11. Third slide gate valve; 12. Vacuum pump assembly; 13. Corrosion-resistant loading stage; 131. Base; 132. First movable seat; 133. Second movable seat; 134. Transmission rod; 135. First worm gear; 136. First worm; 137. Second worm gear; 138. Second worm; 14. First track; 15. Second track; 16. Third... Track; 17. Fourth track; 18. Fifth track; 19. Sixth track; 20. First dovetail protrusion; 21. First dovetail groove; 22. Second dovetail groove; 23. Sliding seat; 24. Second dovetail protrusion; 25. Third dovetail protrusion; 26. First push rod; 27. Second push rod; 28. First drive motor; 29. Gear; 30. Rack; 31. Slot; 32. Limiting protrusion; 33. Positioning protrusion; 34. Positioning groove; 35. First limiting groove; 36. Second limiting groove; 37. Interface; 38. Connecting plate; 39. Second drive motor; 40. Drive rod. Detailed Implementation
[0037] The following is a detailed description of the in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to the present invention, with reference to the accompanying drawings.
[0038] like Figures 1 to 8As shown, an in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion includes an X-ray diffractometer 1, an electron microscope 2, an environmental chamber 3, a salt spray generator 4, an X-ray entrance window 5, an X-ray exit window 6, a transfer chamber 7, a pre-evacuation chamber 8, a vacuum pump group 12, a track assembly, a corrosion-resistant loading stage 13, a first drive assembly, and a multi-point heating module. The environmental chamber 3 is located inside the X-ray diffractometer 1. The salt spray generator 4 is connected to the environmental chamber 3 and is used to spray salt spray into the environmental chamber 3. The salt spray generator 4 includes a water reservoir, a rotor flow meter, an ultrasonic atomizing device, and a heating device. The temperature adjustment range of the salt spray generator 4 is from room temperature to 60°C. The salt spray generator 4 can form a uniform dissolved salt spray environment on the sample surface. The corrosion environment of solid salt and molten salt on the sample surface is formed by heating the dissolved salt on the sample surface. The specific structure and working principle of the salt spray generator 4 are existing technologies and will not be described in detail here.
[0039] like Figure 2 As shown, the X-ray entrance window 5 and the X-ray exit window 6 are both located on the environmental chamber 3. Specifically, the environmental chamber 3 includes a cuboid part and a cylindrical part. The X-ray entrance window 5 and the X-ray exit window 6 are located on the upper part of the cylindrical part and distributed along its circumference. Both the X-ray entrance window 5 and the X-ray exit window 6 are connected to a polymer film to prevent salt spray leakage. This is used for X-ray diffraction testing under multiple corrosion conditions. Moreover, the environmental chamber 3, which is sealed with a polymer film, can be evacuated, allowing it to be used in both atmospheric and low vacuum environments, thus achieving controllable adjustment for different environmental requirements. In this embodiment, the polymer film is a polyimide film.
[0040] like Figure 1 As shown, one end of the transfer chamber 7 is connected to the environmental chamber 3 via the first gate valve 9, and the other end of the transfer chamber 7 passes through the side wall of the X-ray diffractometer 1 and is connected to one end of the pre-evacuation chamber 8 via the second gate valve 10. Specifically, the left side wall of the X-ray diffractometer 1 is provided with an opening for the transfer chamber 7 to pass through. The first gate valve 9 is connected to the cuboid part of the environmental chamber 3. The other end of the pre-evacuation chamber 8 is connected to the electron microscope 2 via the third gate valve 11. The second gate valve 10 and the third gate valve 11 are located on two adjacent end faces of the pre-evacuation chamber 8. The vacuum pump group 12 is connected to the pre-evacuation chamber 8 and is used to evacuate the pre-evacuation chamber 8 alone or to evacuate the transfer chamber 7 and the pre-evacuation chamber 8 simultaneously.
[0041] The track assembly is located in the environmental chamber 3, transfer chamber 7, pre-extraction chamber 8 and electron microscope 2. The corrosion-resistant loading stage 13 is slidably connected to the track assembly and is used to hold the sample laterally. The first drive assembly is used to drive the corrosion-resistant loading stage 13 to move along the track assembly between the environmental chamber 3, transfer chamber 7, pre-extraction chamber 8 and electron microscope 2.
[0042] like Figure 8As shown, the track assembly includes a first track 14, a second track 15, a third track 16, a fourth track 17, a fifth track 18, and a sixth track 19. The first track 14 and the second track 15 are both located within the environmental chamber 3, the third track 16 is located within the transfer chamber 7, the fourth track 17 and the fifth track 18 are located within the pre-extraction chamber 8, and the sixth track 19 is located within the electron microscope 2. The first track 14, the fifth track 18, and the sixth track 19 are all arranged along the front-to-back direction, with the fifth track 18 and the sixth track 19 coaxial. The second track 15, the third track 16, and the fourth track 17 are all arranged along the left-to-right direction and are all coaxial. The second track 15, the third track 16, and the fourth track 17 are located between the first track 14 and the fifth track 18. Figure 8 The image also shows different track positions of the corrosion-resistant loading stage 13. This track layout optimizes the space utilization efficiency inside the system and avoids the problems of a long system and large footprint caused by using a single long track between the environmental chamber 3, transfer chamber 7, pre-extraction chamber 8 and electron microscope 2.
[0043] Furthermore, the present invention also includes a sliding seat 23, the upper ends of the first track 14, the fifth track 18 and the sixth track 19 are each provided with a first dovetail-shaped protrusion 20 arranged in the front-back direction, the bottom end of the corrosion-resistant loading platform 13 is provided with a first dovetail groove 21 that slides through the first dovetail-shaped protrusion 20 in the front-back direction, the upper ends of the second track 15, the third track 16 and the fourth track 17 are each provided with a second dovetail groove 22 that slides through the second track in the left-right direction and the second dovetail groove 22 extends to the first track 14 and the fifth track 18 in the left-right direction respectively, the bottom end of the sliding seat 23 is provided with a second dovetail-shaped protrusion 24 that slides through the second dovetail groove 22, and the upper end of the sliding seat 23 is provided with a third dovetail-shaped protrusion 25 that slides through the first dovetail groove 21 in the front-back direction.
[0044] In the initial state, the sliding seat 23 is located in the second dovetail groove 22 of the first track 14, and its third dovetail protrusion 25 is coaxial with the first dovetail protrusion 20 of the first track 14. At this time, the corrosion-resistant loading stage 13 can slide independently along the direction of the first track 14. The corrosion-resistant loading stage 13 moves forward to the X-ray diffraction position. When the corrosion-resistant loading stage 13 moves backward to connect with the sliding seat 23, the sliding seat 23 drives the corrosion-resistant loading stage 13 to move along the second track 15, the third track 16 and the fourth track 17. After the sliding seat 23 carries the corrosion-resistant loading stage 13 into the fifth track 18, the third dovetail protrusion 25 is coaxial with the first dovetail protrusion 20 of the fifth track 18. The corrosion-resistant loading stage 13 still moves independently along the fifth track 18 and the sixth track 19. The introduction of the sliding seat 23 realizes the turning of the corrosion-resistant loading stage 13 between the tracks. It should be noted that in this invention, the dovetail protrusions or dovetail grooves between the coaxial tracks are all coaxially arranged. The so-called coaxial arrangement means that the corresponding end faces between the tracks, between the dovetail protrusions, and between the dovetail grooves are flush.
[0045] like Figure 1 , Figure 4 and Figure 6 As shown, the first drive assembly includes a first push rod 26, a second push rod 27, a first drive motor 28, a gear 29, and a rack 30. The first push rod 26 is slidably connected to the rear side wall of the environmental chamber 3 in the front-to-back direction, and the second push rod 27 is slidably connected to the rear side wall of the pre-extraction chamber 8 in the front-to-back direction. The first push rod 26 and the second push rod 27 are rotatably connected to the environmental chamber 3 and the pre-extraction chamber 8, respectively. Figure 5 As shown, the bottom end of the corrosion-resistant loading platform 13 is provided with a slot 31, and the side walls of the first push rod 26 and the second push rod 27 are provided with limiting protrusions 32. By rotating the first push rod 26 or the second push rod 27, the limiting protrusions 32 are engaged or disengaged from the slot 31. After the limiting protrusions 32 are engaged in the slot 31, the corrosion-resistant loading platform 13 moves with the first push rod 26 or the second push rod 27. Furthermore, the side walls of the first push rod 26 and the second push rod 27 are provided with positioning protrusions 33, and the bottom end of the corrosion-resistant loading platform 13 is provided with a positioning groove 34. When the first push rod 26 or the second push rod 27 needs to be connected to the corrosion-resistant loading platform 13 after separation, when the positioning protrusions 33 are engaged in the positioning groove 34 during the sliding of the first push rod 26 or the second push rod 27, it indicates that the limiting protrusions 32 and the slot 31 are in the front-back direction. At this time, by rotating the first push rod 26 or the second push rod 27, the limiting protrusions 32 are engaged in the slot 31. Furthermore, by adding positioning protrusions 33 to the first push rod 26 and the second push rod 27, and providing corresponding positioning grooves 34 on the first track 14, the fifth track 18, and the sixth track 19, the positioning effect is further improved. The first track 14, the fifth track 18, and the sixth track 19 can be provided with clearance grooves to allow the first push rod 26 or the second push rod 27 to slide. The limiting protrusions 32 on the first push rod 26 and the second push rod 27, as well as the slot 31 at the bottom of the corrosion-resistant loading platform 13, allow the first push rod 26 and the second push rod 27 to be separated from the corrosion-resistant loading platform 13, facilitating the transfer of the corrosion-resistant loading platform 13 between different compartments.
[0046] like Figure 6 As shown, the rack 30 is slidably connected to the right side wall of the environmental chamber 3 in the left-right direction and connected to the sliding seat 23. The first drive motor 28 is connected to the outer wall of the environmental chamber 3 and drives the gear 29 to rotate. The gear 29 meshes with the rack 30.
[0047] like Figure 3As shown, the environmental chamber 3 is connected to a second drive assembly. The corrosion-resistant loading stage 13 includes a base 131, a first movable seat 132, a second movable seat 133, a transmission rod 134, a first worm gear 135, a first worm 136, a second worm gear 137, and a second worm 138. The first movable seat 132 and the second movable seat 133 are both slidably connected to the base 131 in the front-back direction. The upper end surfaces of the first movable seat 132 and the second movable seat 133 are respectively provided with a first limiting groove 35 and a second limiting groove 36 for placing samples. The first limiting groove 35 and the second limiting groove 36 are connected in the front-back direction. The transmission rod 134 is rotatably connected to the base 131 in the front-back direction. A first threaded segment and a second threaded segment with opposite rotation directions are provided along the axial direction. The first threaded segment and the second threaded segment are respectively threadedly connected to the first movable seat 132 and the second movable seat 133. A first worm wheel 135 is provided on the transmission rod 134. A first worm 136 is rotatably connected to the base 131 in the left-right direction and meshes with the first worm wheel 135. A second worm wheel 137 is provided on the first worm 136. A second worm 138 is rotatably connected to one end of the base 131 in the front-back direction and meshes with the second worm wheel 137. An interface 37 for detachable connection with the second drive assembly is provided on the end of the second worm 138 away from the first movable seat 132. The second drive assembly is used to drive the second worm 138 to rotate.
[0048] In this embodiment, there are two transmission rods 134 spaced apart from each other on the left and right. Each transmission rod 134 is provided with a first worm wheel 135. The first worm 136 is provided with two worm sections spaced apart from each other on the left and right sides. The two worm sections mesh with the two first worm wheels 135 respectively. The second worm wheel 137 is located between the two worm sections. In this embodiment, the first worm wheel 135 is located at the rear end of the transmission rod 134, the first worm 136 is located at the rear side of the first moving seat 132, the second worm 138 is located at the rear end of the base 131, and the interface 37 is located at the rear end of the second worm 138.
[0049] like Figure 2 As shown, the second drive assembly includes a connecting plate 38, a second drive motor 39, and a drive rod 40. The connecting plate 38 is slidably connected to the outside of the environmental chamber 3 in the front-back direction and is located on the rear side of the environmental chamber 3. The drive rod 40 is rotatably connected to the connecting plate 38 and the environmental chamber 3 and is slidably connected to the environmental chamber 3. The second drive motor 39 is connected to the connecting plate 38 and is used to drive the drive rod 40 to rotate. One end of the drive rod 40 is detachably connected to the interface 37.
[0050] The other end of the pre-extraction chamber 8 can be disconnected from the third slide valve 11 via a connecting assembly. In this embodiment, the connecting assembly includes a fixing bolt and a nut. The nut is located on the third slide valve 11. The fixing bolt passes through the pre-extraction chamber 8 and is threadedly connected to the nut. When the sample is tested in the electron microscope 2, the electron microscope 2 is separated from the pre-extraction chamber 8 via the connecting assembly to prevent external vibration from affecting the testing accuracy of the electron microscope 2.
[0051] The bottom of the corrosion-resistant loading stage 13 has a perforated section for laser transmission. The multi-point heating module is used to heat the samples in the environmental chamber 3, the pre-extraction chamber 8, and the electron microscope 2. The multi-point heating module includes a first non-contact optical heating device connected to the environmental chamber 3, a second non-contact optical heating device connected to the pre-extraction chamber 8, and a third non-contact optical heating device connected to the electron microscope 2. Each of the first, second, and third non-contact optical heating devices includes a temperature measuring component. In this embodiment, the first, second, and third non-contact optical heating devices are respectively a first laser heating device, a second laser heating device, and a third laser heating device. All components are infrared temperature measurement components. The first laser heating device and the second laser heating device have the same structure, both including a two-dimensional galvanometer, a laser and an infrared temperature measurement component. Light windows are provided at the bottom of the environmental chamber 3 and the bottom of the pre-extraction chamber 8. The laser is shone into the two-dimensional galvanometer and then directed onto the sample through the light window and the hollow part. By controlling the two-dimensional galvanometer, the sample back area of any size and position can be continuously heated. This method has higher temperature uniformity. The infrared temperature measurement component irradiates the sample with infrared light from the light window and the hollow part to detect the sample temperature in real time. The laser power is adjusted through negative feedback to ensure the consistency of the sample temperature.
[0052] A support frame is installed on the motor stage inside electron microscope 2. The support frame is located on the extension line of the sixth track 19. The corrosion-resistant loading stage 13 moves to the support frame via the sixth track 19, and the corrosion-resistant loading stage 13 performs electron microscope 2 tests on the support frame. The third laser heating device includes a focusing lens assembly, a total reflection mirror, and an infrared temperature measurement component. The focusing lens assembly is connected to one end of the support frame, and the total reflection mirror is connected to the support frame. The laser enters from the focusing lens assembly and is reflected twice by the fixed-band reflector and the total reflection mirror inside the focusing lens assembly before hitting the back of the sample through the hollow part. The infrared light also enters from the focusing lens assembly, passes through the fixed-band reflector, is reflected by the total reflection mirror, and hits the back of the sample through the hollow part. Similarly, the laser power is adjusted by negative feedback to ensure the consistency of the sample temperature, so that the temperature state of the sample in X-ray diffractometer 1 and electron microscope 2 can be kept consistent.
[0053] In addition, water channels are provided in the first track 14, the fifth track 18, the sixth track 19 and the support frame. The water channels in the first track 14, the fifth track 18, the sixth track 19 and the support frame are all connected to water supply devices, which circulate water into the water channels. The first track 14, the fifth track 18, the sixth track 19, the support frame and the motor platform serve as cold ends to conduct heat and prevent deformation and damage from prolonged heating, thus ensuring the stability of the entire system during long-term operation in high-temperature environments.
[0054] In this invention, the corrosion-resistant loading stage 13 holds the sample and is initially positioned in the environmental chamber 3. A salt spray generator 4 simulates the salt spray conditions in the marine atmosphere. A multi-point heating module provides a controllable thermal field, and the corrosion-resistant loading stage 13 provides a stress field, thus simulating multi-field coupled corrosion involving heat, salt, and force. Simultaneously, the X-ray entrance window 5 and X-ray exit window 6 allow the X-ray diffractometer 1 to perform in-situ diffraction tests, enabling in-situ phase analysis of corrosion products under simulated conditions. After completing the X-ray diffraction test, the first driving component drives the corrosion-resistant loading stage 13 through the transfer chamber 7 into the pre-extraction chamber 8. The vacuum pump unit 12 pre-evacuates the pre-evacuation chamber 8, allowing the corrosion-resistant loading stage 13 to smoothly enter the electron microscope 2 for micro-area structure and composition analysis. During the pre-evacuation process and the electron microscope 2 tests, the multi-point heating module continuously heats the sample, maintaining the consistency of the sample state in the X-ray diffractometer 1 and the electron microscope 2. Different heating sites can be used for thermal, saline, and force environmental experiments, enabling in-situ microscopic observation of the material surface and interface under simulated service conditions and accurately tracking the dynamic evolution of the surface and interface in the same area during corrosion. Furthermore, in some other embodiments, a high-temperature electrochemical module can be installed in the environmental chamber 3 to achieve in-situ electrochemical testing. Additionally, a gas needle is installed inside the electron microscope 2 to deliver trace amounts of oxygen to the sample, further mimicking the actual sample environment.
[0055] 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 system for in-situ characterization of material surface and interface damage in multi-factor coupled corrosion, characterized in that, include: X-ray diffractometer (1); Electron microscopy (2); An environmental chamber (3) is located inside the X-ray diffractometer (1); Salt spray generator (4) is connected to the environmental chamber (3); The X-ray entrance window (5) and the X-ray exit window (6) are both located on the environmental chamber (3); The transfer chamber (7) and the pre-extraction chamber (8) are connected at one end to the environmental chamber (3) via a first gate valve (9). The other end of the transfer chamber (7) passes through the side wall of the X-ray diffractometer (1) and is connected to one end of the pre-extraction chamber (8) via a second gate valve (10). The other end of the pre-extraction chamber (8) is connected to the electron microscope (2) via a third gate valve (11). The other end of the pre-extraction chamber (8) can be detached from the third gate valve (11) via a connecting assembly. The second gate valve (10) and the third gate valve (11) are located on two adjacent end faces of the pre-extraction chamber (8). A vacuum pump assembly (12) is connected to the pre-evacuation chamber (8) and is used to evacuate the pre-evacuation chamber (8) alone or simultaneously to the transfer chamber (7) and the pre-evacuation chamber (8); The track assembly is located in the environmental chamber (3), the transfer chamber (7), the pre-extraction chamber (8), and the electron microscope (2); A corrosion-resistant loading stage (13) is slidably connected to the track assembly and used for laterally clamping the sample; A first drive assembly is used to drive the corrosion-resistant loading stage (13) to move along the track assembly between the environmental chamber (3), the transfer chamber (7), the pre-extraction chamber (8), and the electron microscope (2); A multi-point heating module is used to heat the samples in the environmental chamber (3), the pre-extraction chamber (8), and the electron microscope (2); After the X-ray diffraction test is completed, the corrosion-resistant loading stage (13) is driven by the first driving component to enter the pre-evacuation chamber (8) through the transfer chamber (7). The vacuum pump group (12) pre-evacuates the pre-evacuation chamber (8) so that the corrosion-resistant loading stage (13) can smoothly enter the electron microscope (2).
2. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 1, characterized in that, The track assembly includes a first track (14), a second track (15), a third track (16), a fourth track (17), a fifth track (18), and a sixth track (19). The first track (14) and the second track (15) are both located in the environmental chamber (3), the third track (16) is located in the transfer chamber (7), the fourth track (17) and the fifth track (18) are located in the pre-extraction chamber (8), and the sixth track (19) is located in the electron microscope (2). The first track (14), the fifth track (18), and the sixth track (19) are all arranged in the front-back direction, and the fifth track (18) and the sixth track (19) are coaxial. The second track (15), the third track (16), and the fourth track (17) are all arranged in the left-right direction and are coaxial. The second track (15), the third track (16), and the fourth track (17) are located between the first track (14) and the fifth track (18).
3. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 2, characterized in that, It also includes a sliding seat (23). The upper ends of the first track (14), the fifth track (18) and the sixth track (19) are provided with a first dovetail protrusion (20) arranged in the front-back direction. The bottom end of the corrosion-resistant loading platform (13) is provided with a first dovetail groove (21) that slides and engages with the first dovetail protrusion (20) in the front-back direction. The upper ends of the second track (15), the third track (16) and the fourth track (17) are provided with a second dovetail groove (22) that slides and engages with the second dovetail groove (22) in the left-right direction. The second dovetail groove (22) extends to the first track (14) and the fifth track (18) in the left-right direction, respectively. The bottom end of the sliding seat (23) is provided with a second dovetail protrusion (24) that slides and engages with the second dovetail groove (22). The upper end of the sliding seat (23) is provided with a third dovetail protrusion (25) that slides and engages with the first dovetail groove (21) in the front-back direction.
4. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 3, characterized in that, The first drive assembly includes a first push rod (26), a second push rod (27), a first drive motor (28), a gear (29), and a rack (30). The first push rod (26) is slidably connected to the rear side wall of the environmental chamber (3) in the front-back direction, and the second push rod (27) is slidably connected to the rear side wall of the pre-extraction chamber (8) in the front-back direction. The first push rod (26) and the second push rod (27) are rotatably connected to the environmental chamber (3) and the pre-extraction chamber (8), respectively. The bottom end of the corrosion-resistant loading platform (13) is provided with a slot (31). Both the first push rod (26) and the second push rod (27) have limiting protrusions (32) on their side walls. By rotating the first push rod (26) or the second push rod (27), the limiting protrusions (32) are engaged or disengaged from the slots (31). The rack (30) is slidably connected to the right side wall of the environmental chamber (3) and connected to the sliding seat (23) in the left-right direction. The first drive motor (28) is connected to the outer wall of the environmental chamber (3) and drives the gear (29) to rotate. The gear (29) meshes with the rack (30).
5. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 4, characterized in that, The first push rod (26) and the second push rod (27) are provided with positioning protrusions (33) on their side walls. The bottom end of the corrosion-resistant loading platform (13) is provided with a positioning groove (34). When the positioning protrusion (33) is inserted into the positioning groove (34), the limiting protrusion (32) is inserted into the slot (31) by rotating the first push rod (26) or the second push rod (27).
6. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 2, characterized in that, Waterways are provided in the first track (14), the fifth track (18) and the sixth track (19), and water supply devices are connected to the waterways of the first track (14), the fifth track (18) and the sixth track (19).
7. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 1, characterized in that, The environmental chamber (3) is connected to a second drive assembly. The corrosion-resistant loading stage (13) includes a base (131), a first movable seat (132), a second movable seat (133), a transmission rod (134), a first worm gear (135), a first worm (136), a second worm gear (137), and a second worm (138). The first movable seat (132) and the second movable seat (133) are slidably connected to the base (131) in the front-back direction. The upper end face of the first movable seat (132) and the upper end face of the second movable seat (133) are respectively provided with a first limiting groove (35) and a second limiting groove (36) for placing samples. The first limiting groove (35) and the second limiting groove (36) are connected in the front-back direction. The transmission rod (134) is rotatably connected to the base (131) in the front-back direction. The transmission rod (134) is axially connected to the base (131). The transmission rod (134) is provided with a first threaded section and a second threaded section with opposite directions of rotation. The first threaded section and the second threaded section are respectively threadedly connected to the first moving seat (132) and the second moving seat (133). The transmission rod (134) is provided with a first worm wheel (135). The first worm (136) is rotatably connected to the base (131) in the left-right direction and meshes with the first worm wheel (135). The first worm (136) is provided with a second worm wheel (137). The second worm (138) is rotatably connected to one end of the base (131) in the front-back direction and meshes with the second worm wheel (137). The second worm (138) is provided with an interface (37) for detachably connecting with the second drive assembly at one end away from the first moving seat (132). The second drive assembly is used to drive the second worm (138) to rotate.
8. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 7, characterized in that, The second drive assembly includes a connecting plate (38), a second drive motor (39), and a drive rod (40). The connecting plate (38) is slidably connected to the outside of the environmental chamber (3) in the front-back direction. The drive rod (40) is rotatably connected to the connecting plate (38) and the environmental chamber (3) and is slidably connected to the environmental chamber (3). The second drive motor (39) is connected to the connecting plate (38) and is used to drive the drive rod (40) to rotate. One end of the drive rod (40) is detachably connected to the interface (37).
9. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 1, characterized in that, The bottom of the corrosion-resistant loading stage (13) is provided with a hollowed-out part for laser to pass through. The multi-point heating module includes a first non-contact optical heating device connected to the environmental chamber (3), a second non-contact optical heating device connected to the pre-extraction chamber (8), and a third non-contact optical heating device connected to the electron microscope (2). The first non-contact optical heating device, the second non-contact optical heating device, and the third non-contact optical heating device all include a temperature measuring component.
10. The in-situ characterization system for material surface and interface damage in multi-factor coupled corrosion according to claim 1, characterized in that, The connecting assembly includes a fixing bolt and a nut, the nut being disposed on the third slide valve (11), the fixing bolt passing through the pre-extraction chamber (8) and being threadedly connected to the nut.