In-situ atmosphere heating test device for scanning electron microscope

Abstract

The utility model belongs to the technical field of sample testing, and particularly relates to an in-situ atmosphere heating testing device for a scanning electron microscope, which comprises a heat insulation sealing box, the inside of the heat insulation sealing box is divided into a detection chamber and a temperature control equipment chamber through a heat insulation plate, atmosphere guide pipes are connected to two sides of the detection chamber, and a cold and hot medium container is arranged in the temperature control equipment chamber. A thermal manager connected with the cold and hot medium container is mounted at the bottom of the detection chamber, a sample is arranged on the top table surface of the thermal manager, stress detection mechanisms are mounted on the inner walls of the two sides of the detection chamber, and a camera driving mechanism is mounted in the detection chamber through a mounting plate. According to the utility model, microstructure morphology observation and component analysis under different temperatures, chemical atmospheres and stresses of a sample in a detection chamber are realized based on a cold and hot medium container, a stress detection mechanism, atmosphere input, conversion adjustment of gas types, cold and hot medium temperatures and setting of different stress fields; and the driving mechanism drives the camera to perform in-situ online test on the high-temperature reaction behavior of the material.

Description

Technical Field

[0001] This utility model belongs to the field of sample testing technology, specifically relating to an in-situ atmosphere heating testing device for scanning electron microscopes. Background Technology

[0002] Scanning electron microscopy (SEM), as an important tool for microscopic structure morphology and composition analysis, has been widely used in materials science, chemistry, biology, microelectronics, and many other fields. It features simple sample preparation, a wide range of adjustable magnification, high image resolution, large depth of field, and rich stereoscopic imaging. With the development of modern technology, other combined analytical functions of SEM have emerged, such as hot and cold stage systems, used to observe and analyze material phase transitions, recrystallization transformations, grain growth, oxidation reactions, gas reactions, element migration, and electronic device failure analysis during heating and freezing.

[0003] Some materials are frequently subjected to rapid temperature changes, scouring and compression by different reaction media, and are therefore inevitably subjected to thermal stress, compressive stress, and complex thermo-compressive coupled stresses. This leads to changes in the material's microstructure, resulting in microcracks and voids, and even cracking and spalling. The resulting material failures often become significant hidden dangers for industrial accidents. Therefore, studying the high-temperature reaction behavior and mechanisms of such materials under stress loading conditions is an important foundation for guiding the widespread and safe application of these materials. To accurately obtain the high-temperature interfacial reaction behavior of materials under complex stress, it is often necessary to coordinately control the temperature field, atmosphere field, and stress field during the sample reaction process, so as to make the material's service environment closer to reality and better reflect the nature of material failure.

[0004] However, most existing testing devices do not consider the effect of stress on materials and cannot simultaneously acquire online information on the evolution of the microstructure of the sample during the reaction process; therefore, they cannot accurately characterize the in-situ atmospheric heating test behavior and mechanism of materials under high-temperature stress fields. Summary of the Invention

[0005] To address the problems mentioned in the background section, this invention provides an in-situ atmosphere heating testing device for scanning electron microscopes.

[0006] To achieve the above objectives, this utility model provides the following technical solution: an in-situ atmosphere heating testing device for scanning electron microscopes, comprising a heat-insulated sealed box, the inside of which is divided into a detection chamber and a temperature control equipment chamber by a heat insulation plate, atmosphere conduits connected to both sides of the detection chamber, a cold / heat medium container disposed inside the temperature control equipment chamber, a heat management device connected to the cold / heat medium container mounted on the bottom of the detection chamber, a sample disposed on the top platform of the heat management device, stress detection mechanisms for clamping the sample mounted on both inner walls of the detection chamber, and a camera drive mechanism for real-time in-situ detection of the sample's reaction behavior mounted inside the detection chamber via a mounting plate.

[0007] As a preferred embodiment, the stress detection mechanism includes a stress loading device, a pressure sensor, and a pressure rod; the stress loading device is connected to the pressure rod, the pressure sensor is connected to the stress loading device, and the top of the pressure rod is clamped to both sides of the sample by a clamping block.

[0008] As a preferred embodiment, the camera driving mechanism includes a motor, a drive gear, a gear ring turntable, and a camera. The motor is mounted on one corner of the mounting plate, and a drive gear is mounted on the drive shaft at the top of the motor. The bottom of the gear ring turntable rotates on the slide groove of the mounting plate via a slider. The outer ring of the gear ring turntable is provided with a gear ring that meshes with the drive gear, and the camera is mounted on the inner side of the gear ring turntable.

[0009] As a preferred embodiment, an atmosphere input conduit is connected to the lower left side of the detection chamber, and an atmosphere output conduit is connected to the upper right side of the detection chamber.

[0010] As a preferred embodiment, the two sides of the cold and hot medium container are connected to the external cold and hot medium via cold medium pipelines and hot medium pipelines respectively through liquid column valves.

[0011] As a preferred embodiment, the top operating port of the heat-insulated sealing box is sealed with an openable and closable operating door.

[0012] As a preferred embodiment, a sample observation window is provided on the front end face of the heat-insulated sealing box at the detection position corresponding to the detection chamber. On both sides of the sample observation window, there are switch control panels for controlling the motor and stress loading device and a display observation screen that is wirelessly connected to the camera. The sample observation window is made of a high-transmittance silicon nitride film.

[0013] As a preferred embodiment, a temperature measuring instrument is also provided on the inner wall of the detection chamber.

[0014] Compared with the prior art, the beneficial effects of this utility model are:

[0015] This invention, based on a hot and cold medium container, a stress detection mechanism, and an atmosphere input in the detection chamber, enables the observation and compositional analysis of the microstructure morphology of a sample at different temperatures and chemical atmospheres within a single detection chamber by changing the gas type in the detection chamber and adjusting the temperature of the hot and cold medium. By controlling and setting different temperature fields, atmosphere fields, and stress fields, it is possible to coordinately regulate the temperature field, atmosphere field, and stress field during the reaction process of material samples at preset temperatures and in rapid cooling processes. Furthermore, by using a camera drive mechanism to drive a camera, in-situ online testing of the high-temperature reaction behavior of materials can be performed under conditions that more closely resemble actual service environments. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0017] Figure 2 This is a front view structural diagram of the present utility model;

[0018] Figure 3 This is a cross-sectional view of the longitudinal section of this utility model;

[0019] Figure 4 This is a schematic diagram of the internal structure of the present invention;

[0020] Figure 5 for Figure 4 A schematic diagram of the isometric cross-sectional structure of the AA plane.

[0021] Figure 6 This is a schematic diagram of the camera drive mechanism in this utility model;

[0022] Figure 7 This is a schematic diagram of the stress detection mechanism in this utility model.

[0023] Explanation of icon numbers:

[0024] 1. Insulated and sealed box; 11. Sample observation window; 12. Switch control panel; 13. Display observation screen; 14. Mounting plate;

[0025] 2. Operate the cabinet door;

[0026] 3. Stress detection mechanism; 31. Stress loading device; 32. Pressure sensor; 33. Pressure rod; 34. Clamping block;

[0027] 4. Camera drive mechanism; 41. Motor; 42. Drive gear; 43. Gear ring turntable; 44. Slider;

[0028] 5. Camera; 6. Thermal manager; 7. Sample;

[0029] 8. Cold and hot medium containers; 81. Cold medium pipelines; 82. Hot medium pipelines;

[0030] 9. Detection chamber; 91. Atmosphere output conduit; 92. Atmosphere input conduit. Detailed Implementation

[0031] The embodiments of this utility model are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this utility model, and should not be construed as limiting this utility model.

[0032] Example 1

[0033] Please see Figures 1-7 This utility model provides the following technical solution: an in-situ atmosphere heating test device for scanning electron microscope, comprising a heat-insulated sealed box 1, the inside of which is divided into a detection chamber 9 and a temperature control equipment chamber by a heat insulation plate; atmosphere conduits are connected to both sides of the detection chamber 9 to provide a vacuum or different atmosphere morphology testing environment for the sample 7 when testing its reaction behavior; a cold / heat medium container 8 is provided inside the temperature control equipment chamber; a heat management device 6 connected to the cold / heat medium container 8 is installed on the bottom of the detection chamber 9; the sample 7 is placed on the top platform of the heat management device 6; stress detection mechanisms 3 for clamping the sample 7 are installed on the inner walls of both sides of the detection chamber 9; and a reaction device for the sample 7 is installed inside the detection chamber 9 by a mounting plate 14. The camera drive mechanism 4 performs real-time in-situ detection of the behavior; in this embodiment, the hot and cold medium container 8 is injected into the hot medium container 8 through the hot medium pipeline 82, and the hot medium is heated to the preset temperature by the heat manager 6. Nitrogen, air and other inert test gases can be filled into the detection chamber 9 through the atmosphere input conduit 92 to the preset atmosphere partial pressure, so as to provide a preset atmosphere test environment for the sample 7; thereby realizing real-time monitoring of the temperature and atmosphere of the sample 7; and the drive gear 42 driven by the motor 41 drives the gear ring turntable 43 to rotate on the slide groove of the mounting plate 14 through the slider. The camera, including miniature microscope, camera, video camera, etc., performs in-situ detection of the test sample and feeds back to the display observation screen 13 for observation, which is simple and convenient.

[0034] In this embodiment, the stress detection mechanism 3 includes a stress loading device 31, a pressure sensor 32, and a pressure rod 33. The stress loading device 31 is connected to the pressure rod 33, and the pressure sensor 32 is connected to the stress loading device 31. The top of the pressure rod 33 is clamped on both sides of the sample 7 by a clamping block 34. The sample 7 is heated by the hot and cold medium container 8 through the heat manager 6, and the temperature of the sample in the detection chamber 9 is measured in real time by a temperature measuring instrument. The stress loading device 31 controls the pressure rod 33 to move horizontally to adjust the compressive stress loading on the sample 7, and the pressure sensor 32 senses the applied pressure value.

[0035] In this embodiment, the camera driving mechanism 4 includes a motor 41, a drive gear 42, a gear ring turntable 43, and a camera 5. The motor 41 is mounted on one corner of the mounting plate 14, and the drive gear 42 is mounted on the top drive shaft of the motor 41. The bottom of the gear ring turntable 43 rotates on the slide groove of the mounting plate 14 via a slider 44. The outer ring of the gear ring turntable 43 is provided with a gear ring that meshes with the drive gear 42, and the camera 5 is mounted on the inner side of the gear ring turntable 43. The motor 41 drives the drive gear 42 to drive the gear ring turntable 43 to rotate on the slide groove of the mounting plate 14 via the slider.

[0036] In this embodiment, an atmosphere input conduit 92 is connected to the lower left side of the detection chamber 9, and an atmosphere output conduit 91 is connected to the upper right side of the detection chamber 9; the atmosphere input conduit 92 can fill the detection chamber 9 with nitrogen, air and other inert test gases.

[0037] In this embodiment, the cold and hot medium container 8 is connected to the external cold and hot medium on both sides through cold medium pipeline 81 and hot medium pipeline 82 via liquid column valves; the heating range of the sample is 10 to 1000℃ through the cold and hot medium container 8 and the heat manager 6; the surface temperature of the test sample can be controlled by the heat manager 6.

[0038] In this embodiment, the top operating port of the heat-insulated sealing box 1 is sealed with an operating box door 2 that can be opened and closed.

[0039] In this embodiment, a sample observation window 11 is provided on the front end face of the heat-insulating sealing box 1 at the detection position corresponding to the detection chamber 9. On both sides of the sample observation window 11, there are switch control panel 12 for controlling the motor 41 and the stress loading device 31 and a display observation screen 13 wirelessly connected to the camera 5. The sample observation window 11 is made of a high-transmittance silicon nitride thin film.

[0040] In this embodiment, a temperature measuring instrument is also provided on the inner wall of the detection chamber 9.

[0041] The working principle and usage process of this utility model are as follows: When using this utility model, the staff places the sample 7 on the heat management unit 6 inside the detection chamber 9, starts the stress detection mechanism 3 to stably clamp the sample 7 on both sides, and closes the operation box door 2.

[0042] The hot and cold medium is injected into the hot and cold medium container 8 through the hot medium pipeline 82. The hot medium is then heated to the preset temperature by the heat manager 6. Nitrogen, air and other inert test gases can be filled into the detection chamber 9 through the atmosphere input conduit 9 to the preset atmosphere partial pressure, so as to provide a preset atmosphere test environment for the sample 7. This enables real-time monitoring of the temperature and atmosphere of the sample 7. The motor 41 drives the drive gear 42 to drive the gear ring turntable 43 to rotate on the slide groove of the mounting plate 14 via the slider. Cameras, including miniature microscopes, cameras and video cameras, perform in-situ detection of the test sample and feed the feedback to the display observation screen 13 for observation. It is simple and convenient.

[0043] Simultaneously, the sample 7 is heated by the heat management unit 6 via the hot and cold medium container 8, and the temperature of the sample in the detection chamber 9 is measured in real time by a temperature measuring instrument. The stress loading device 31 controls the pressure rod 33 to move horizontally to adjust the compressive stress loading on the sample 7, and the pressure sensor 32 senses the applied pressure value. Based on the atmosphere input on the hot and cold medium container 8, the stress detection mechanism 3, and the detection chamber 9, this device can coordinately regulate the temperature field, atmosphere field, and stress field of the material sample reaction process during the preset temperature and rapid cooling process by controlling and setting different temperature fields, atmosphere fields, and stress fields. Furthermore, the camera 5 is driven by the camera drive mechanism 4 to conduct in-situ online testing of the high-temperature reaction behavior of the material under conditions that are closer to the actual service environment.

[0044] Finally, it should be noted that the above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. An in-situ atmosphere heating test device for a scanning electron microscope, comprising a heat-insulated sealed box (1), the inside of the heat-insulated sealed box (1) is separated into a detection chamber (9) and a temperature control equipment cavity by a heat insulation plate, characterized in that: The detection chamber (9) is connected with atmosphere guide pipes on both sides, the temperature control equipment cavity is provided with cold and hot medium containers (8), the bottom of the detection chamber (9) is provided with a thermal manager (6) connected with the cold and hot medium containers (8), the top surface of the thermal manager (6) is provided with a sample (7), the inner walls of both sides of the detection chamber (9) are provided with stress detection mechanisms (3) for clamping the sample (7), and the inside of the detection chamber (9) is provided with a camera driving mechanism (4) for real-time in-situ detection of the reaction behavior of the sample (7) through the mounting plate (14).

2. The in-situ atmosphere heating test device for a scanning electron microscope according to claim 1, characterized by: The stress detection mechanism (3) comprises a stress loading device (31), a pressure sensor (32) and a pressure rod (33); the stress loading device (31) is connected with the pressure rod (33), the pressure sensor (32) is connected with the stress loading device (31), and the top end of the pressure rod (33) is clamped on both sides of the sample (7) through a clamping block (34).

3. The in-situ atmosphere heating test apparatus for a scanning electron microscope according to claim 1, characterized by: The camera driving mechanism (4) comprises a motor (41), a driving gear (42), a gear ring turntable (43) and a camera (5); the motor (41) is mounted on a corner of the mounting plate (14), the driving gear (42) is mounted on the driving shaft at the top of the motor (41), the gear ring turntable (43) rotates on the sliding groove of the mounting plate (14) through a sliding block (44) at the bottom, the outer ring of the gear ring turntable (43) is provided with a gear ring in gear connection with the driving gear (42), and the camera (5) is mounted on the inner side of the gear ring turntable (43).

4. The in-situ atmosphere heating test device for a scanning electron microscope according to claim 1, characterized by: The left lower side of the detection chamber (9) is connected with an atmosphere input guide pipe (92), and the right upper side of the detection chamber (9) is connected with an atmosphere output guide pipe (91).

5. The in-situ atmosphere heating test apparatus for a scanning electron microscope according to claim 1, characterized by: The cold and hot medium containers (8) are connected with the outside cold and hot medium through liquid column valves respectively through cold medium pipelines (81) and hot medium pipelines (82) on both sides.

6. The in-situ atmosphere heating test apparatus for a scanning electron microscope according to claim 1, characterized by: The operating box door (2) is sealingly and openably connected to the top operating opening of the heat insulation sealing box (1).

7. The in-situ atmosphere heating test device for a scanning electron microscope according to claim 1, characterized by: The sample observation window (11) is provided on the front end face of the heat insulation sealing box (1) corresponding to the detection position of the detection chamber (9), the left and right sides of the sample observation window (11) are respectively provided with a switch control panel (12) for controlling the motor (41) and the stress loading device (31) and a display observation screen (13) wirelessly connected with the camera (5), and the sample observation window (11) is made of a high-transmittance silicon nitride film.

8. The in-situ atmosphere heating test device for a scanning electron microscope according to claim 1, characterized by: The inner wall of the detection chamber (9) is also provided with a temperature measuring meter.

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