In-situ mechanical performance measurement device and analysis method using multiple techniques of scanning electron microscope

Abstract

To provide more novel technical means for scientifically establishing the relationship between the evolution of a material organization structure under a complex load and the dynamic response of a macro performance.SOLUTION: The invention discloses a scanning electron microscope multi-technology combined mechanical property in-situ testing device and an analysis method, and belongs to the technical field of precise scientific instruments and material micro-mechanical property tests. A tension and compression loading unit conducts tension and compression loading on a sample 652, a displacement platform moves the sample to an SE mode position and a Raman mode position of a scanning electron microscope. A rotation loading unit drives the sample to rotate synchronously, and in-situ testing is carried out at different angles. The obtained multi-scale data in different time spaces are aligned into a load-displacement curve by using the least common multiple of time coordinates, space registration on multiple attitudes of the sample into a reference coordinate system from coordinate system rotation and translation is carried out, and a multi-source data fusion analysis function is constructed.SELECTED DRAWING: Figure 13

Description

[Technical Field]

[0001] The present disclosure relates to the technical field of precision scientific instruments and microscopic mechanical performance testing of materials, and in particular to an in-situ mechanical performance measurement device and analysis method using a scanning electron microscope in combination with multiple detection technologies, which is referred to as an in-situ material measurement device using a scanning electron microscope in combination with five types of detection technologies and its sample preparation, testing and data processing methods, or an in-situ material measurement device and its sample preparation, testing and data processing methods, or a measuring device for a scanning electron microscope and its sample manufacturing, testing and data processing methods. [Background technology]

[0002] Scanning electron microscopes (SEMs) are widely used to characterize the microstructure of materials due to their advantages, including excellent imaging stereoscopic effect, large imaging depth of field, wide field of view, and continuously adjustable gain. By integrating various types of detectors into a SEM and utilizing the imaging characteristics of different detectors, micromorphological observation and analysis of materials can be performed across scales from macroscopic to mesoscopic to microscopic. The development of an in-situ test platform capable of performing mechanical and high-temperature synchronous loading inside a SEM is of great significance for studying the deformation, damage, and failure mechanisms of materials due to the combined effects of complex forces and thermal loading in practical application situations.

[0003] Based on the above characteristics, various in-situ mechanical performance testing equipment under scanning electron microscopes has been developed both at home and abroad. However, these equipments are only compatible with a single detector in the scanning electron microscope, and a single test cannot obtain one type of data among SEM / EBSD / SEM-DIC / Raman, or multiple tests can be conducted to obtain all four types of information for one batch of material, and it is not possible to simultaneously obtain four types of in-situ testing information for important areas of the material.

[0004] For example, five types of information, namely, microscopic morphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman), of materials under mechanical-thermal coupling can be collected simultaneously and analyzed through fusion analysis. This plays an important role in revealing the deformation and damage failure mechanism of materials under multi-layer mechanical-thermal coupling. Therefore, it is of great significance to research a method for characterizing the mechanical behavior of materials under mechanical-thermal coupling through in-situ testing using the five detection techniques in a scanning electron microscope. Summary of the Invention [Problem to be solved by the invention]

[0005] The purpose of this disclosure is to solve the problems in the prior art by providing an in-situ measurement device and analysis method for mechanical performance that combines multiple technologies in a scanning electron microscope. The mechanical loading of the sample is controlled by a tension-compression loading unit, the sample angle is controlled by rotating the loading unit, and the SE mode position and Raman mode position are converted by a displacement platform. The in-situ measurement of the sample in a scanning electron microscope using SEM, EDS, EBSD, SEM-DIC, and Raman can reveal the failure mechanism of material deformation damage in a multifaceted and profound way, providing a more novel technical means for scientifically establishing the relationship between the evolution of material microstructure under complex loading and the dynamic response of macroscopic performance. [Means for solving the problem]

[0006] In order to achieve the above object, the present disclosure provides the following aspects.

[0007] The present disclosure provides an in-situ mechanical performance measurement device using multiple techniques in a scanning electron microscope, comprising: a displacement platform; and an in-situ testing machine attached to the displacement platform, the in-situ testing machine comprising a fixture unit, a rotational loading unit, and a tension / compression loading unit, the fixture unit comprising a driving fixture group and a driven fixture group, the driving fixture group and the driven fixture group being clamped at both ends of a sample, the tension / compression loading unit being used to drive the driving fixture group and the driven fixture group to move in opposite or rearward directions, the displacement platform being used to move the sample to an SE mode position and a Raman mode position of a scanning electron microscope, and the rotational loading unit driving the driving fixture group and the driven fixture group to rotate synchronously, and performing SEM, EDS, EBSD, SEM-DIC, and Raman in-situ in-situ measurements on the sample at different angles while tension / compression loading the sample. Preferably, the rotary loading unit includes a precision moment motor and a rotary ball spline, the rotary ball spline is provided with a drive gear and a driven gear, the drive gear and the driven gear move along the axial direction of the rotary ball spline and rotate with the rotation of the rotary ball spline, the drive jig group includes a drive gear shaft meshing with the drive gear, the driven jig group includes a driven gear shaft meshing with the driven gear, and the drive gear shaft is connected to the precision moment motor. Preferably, the tension and pressure loading unit includes a bidirectional ball screw and a pair of offset loading nut seats attached to the bidirectional ball screw, one of the offset loading nut seats being connected to the driving jig group and the other offset loading nut seat being connected to the driven jig group, a pair of the bidirectional ball screws being provided, and their ends being geared to achieve synchronous rotation, with the axial direction of the sample and the axis of the bidirectional ball screw being located on the same plane. Preferably, the high-temperature loading unit includes a semicircular winding core and a rotating heat-conducting core, the rotating heat-conducting core is wrapped around the outside of the sample and rotates with the rotation of the sample, and the outer diameter side of the rotating heat-conducting core is attached to the inner diameter side of the semicircular winding core, so that heat from the semicircular winding core can be transferred to the sample by the rotating heat-conducting core at different angles of the sample. Preferably, a multi-layer heat insulating layer is provided on the outside of the semicircular winding core, the heat insulating layer is connected to a water-cooled plate with an open flow path, the water-cooled plate is connected to a first water-cooled piping path, the water-cooled plate is attached to the bottom plate of the in-situ testing machine via the heat insulating plate, and the offset loading nut seat is connected to a second water-cooled piping.

[0008] The present disclosure provides: a first sample preparation step of processing a measurement target material blank into a dumbbell-shaped sample of uniform thickness; a second sample preparation step, which includes polishing both the top and bottom surfaces of the sample, coating a paraffin film on the top surface of the sample after there is no obvious scratch on the top surface of the sample, and polishing the bottom surface of the sample to a mirror effect, and then immersing the sample in an electrolytic polishing solution to remove the bottom surface oxide layer, so that a clear pattern can be collected under EBSD; a third sample preparation step of ultrasonically cleaning the sample, removing the paraffin film on the upper surface of the sample, and thoroughly cleaning and drying the sample; a fourth sample preparation step in which 10 μm wide scale lines are etched at 5 mm intervals on the edges of the reference distance segments on the top and bottom surfaces of the sample, and five marking points are etched on each surface, denoted as o, a, b, c, d and o′, a′, b′, c′, d′, with the positions corresponding to each other two times to form characteristic marking points for spatial alignment; and a fifth sample preparation step of creating a speckle pattern image for SEM-DIC analysis on the underside of the sample. Preferably, in the first sample preparation step, both side surfaces of the sample are polished to have good adhesion with the inner groove surface of the rotating heat conduction core, thereby reducing the contact thermal resistance between the sample and the rotating heat conduction core in a vacuum; In the fifth sample preparation step, Al2O3 powder with a particle size of 500 μm is dissolved in anhydrous ethanol by ultrasonic vibration for 5 minutes, the cloudy solution is allowed to stand for 3 minutes, the upper layer of the clear liquid is placed in the upper pot of the airbrush, and the airflow size and spray distance are adjusted to spray the Al2O3 solution evenly onto the underside of the sample. The sample is then placed in an oven to dry, and the uniformly distributed Al2O3 particles form a speckle pattern.

[0009] The present disclosure provides: a first measurement step of mounting the sample on a fixture unit, evacuating the scanning electron microscope, adjusting the tungsten filament current to obtain clear imaging, adjusting the observation mode switching software, rotating the fixture unit to four states of 0°, 70°, 180°, and 360° of the sample, initializing the angle adjustment, moving the sample from the pole piece to under the Raman objective lens, returning it to its original position, initializing the position adjustment, and recording the corresponding spatial coordinate parameter A0 of the in-situ tester; S2: A second measurement step in which the tension / compression rate and loading displacement parameters are set in the mechanical loading interface, applied, and after reaching the target value, the loading is stopped and the current time is recorded while maintaining the set mechanical loading until the end. a third measurement step of operating the observation mode switching software to move the sample under the pole piece and rotate it to 0°, recording the spatial state information of the in-situ testing machine as A1, selecting the SE mode, and using the scanning electron microscope imaging software to control and operate various detectors sequentially to obtain in-situ tension / compression SEM and EDS images around point o on the top surface of the sample, and recording the corresponding collection times; a fourth measurement step of maintaining the position of the in-situ testing machine unchanged, rotating the sample by 70°, recording the spatial state information of the in-situ testing machine as A2, obtaining in-situ tensile / compression EBSD crystal structure information around point o on the upper surface of the sample, and then rotating the sample by 180°, obtaining a speckle distribution SEM image around point o' on the lower surface of the sample, recording the spatial state information of the in-situ testing machine as A3, and recording the corresponding image collection time; a fifth measurement step of moving a displacement platform, moving the sample under a Raman objective lens and rotating it to 0°, selecting a Raman mode, controlling Raman system imaging, acquiring a Raman image of the sample near point o on the upper surface, recording the spatial state information of the in-situ tester as A4, and recording the acquisition time; a sixth measurement step of applying the spatial state information A1 to the observation mode switching software, adjusting the in-situ testing machine to the observation initial state, setting the loading parameters again, and repeating steps S3, S4, and S5 after the loading is completed to obtain the second group of five types of in-situ observation data; The present invention provides a measurement method using the in-situ mechanical performance measurement device using the multi-technologies of the scanning electron microscope described above, which includes a seventh measurement step of repeating steps S3, S4, S5, and S6 above until the sample breaks, outputting the force and displacement curve of the sample recorded in the in-situ loading control software, inputting the acquired speckle distribution SEM image into Vic-2D processing software, and calculating to obtain the strain distribution on the underside of the sample. Preferably, in the second measurement step, the test target temperature is first input into the temperature loading interface of the in-situ loading control software, and after the monitored temperature of the sample reaches the set value, the subsequent contents of the tension / compression speed and loading displacement parameters are set to realize the force-thermal coupling effect on the sample.

[0010] The present disclosure includes a first data processing step of arranging the various types of micro-images and collection times acquired during the matching test, determining that the sample collection area is located on the reference distance segment of the sample, and mapping the acquired images to the force-time curve one by one; a second data processing step in which the collection times of the asynchronously acquired force-displacement curves, SEM images, EDS images, EBSD images, SEM-DIC images and Raman images are time-aligned, and the data acquired by the five detectors with low collection frequencies are converted into time nodes of the force-displacement curves with high sampling frequencies using a linear interpolation method; A third data processing step involves extracting initial images of the unstretched sample in four different orientations: sample 0° in SEM / EDS mode, sample 70° in EBSD mode, sample 180° in SEM-DIC mode, and sample 360° in Raman mode. A common Cartesian coordinate system is constructed with the o point of the sample 0° image in SEM / EDS mode as the common reference coordinate origin and the sample short side direction as the x-axis. For the other three orientations, each of the o points is used as the coordinate origin and the sample short side direction as the x-axis, respectively, to construct independent Cartesian coordinate systems. Using angle and translation transformation formulas, the data measured in each spatial coordinate system for each of these three orientations is transformed and merged without error into the common Cartesian coordinate system at the sample's 0°, thereby achieving spatial alignment. In the second and third data processing steps, the data from six different sources that have undergone spatiotemporal alignment are merged into one data source. Using the etched graticule lines in the sample preparation, a coordinate system is constructed with point o as the coordinate origin, and each point on the reference distance segment on the sample is assigned a clear coordinate (x i ,y i ), and convert the data obtained by SEM, EDS, EBSD, SEM-DIC, and Raman into a function φ(t) = (z1, z2, z3, z4, z5, t) with respect to time t, and convert the multi-source data into W = (x i , y i , φ(t)), and by inputting the coordinate parameters (x, y) of any point in the sample relative to the origin o and the corresponding time t during the loading process, the micro-morphology, element distribution, crystal structure, strain distribution, corresponding molecular information, and average stress of the sample at that point can be obtained, and the data processing method is characterized by including a fourth data processing step of independently and unifiedly analyzing the deformation damage and failure mechanism of the material under the force-thermal coupling action from five aspects. [Effects of the Invention]

[0011] The present disclosure provides the following technical advantages over the prior art. The present disclosure addresses the problem that conventional in-situ mechanical performance measurements under a scanning electron microscope can only obtain local area information using a single detector, or material damage information at different locations and different times using multiple detectors, making it difficult to obtain synchronous, isochronous, and multidimensional information on the micro-behavior of key areas related to material deformation, damage, and loss. In response, the present disclosure provides an in-situ mechanical performance measurement device that utilizes multiple technologies in a scanning electron microscope, and when applying tensile and compressive forces to a sample, the position of the in-situ testing machine relative to the pole piece (SE mode position) and the Raman objective lens (Raman mode position) can be adjusted to switch between the SE mode and Raman mode. The rotating loading unit controls the sample angle, and the relative angle between the sample and the pole piece can be adjusted to meet the imaging requirements of three different observation modes: SEM / EDS, SEM-DIC and EBSD. This allows for the acquisition of specific area micromorphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD) and molecular information (Raman) under mechanical load of the sample, providing a comprehensive and in-depth insight into the deformation damage and failure mechanism of materials, and providing a more novel technological means for scientifically establishing the relationship between the evolution of material microstructure and the dynamic response of macroscopic performance under complex loading. The present disclosure further provides a high-temperature loading unit that can apply high temperatures to the specimen while simultaneously applying tensile and compressive forces, enabling multifaceted and in-depth research into the deformation, damage, and failure mechanisms of materials under the action of force-thermal coupling. This disclosure designs a specific data processing method to integrate and analyze data such as micromorphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) through spatiotemporal alignment, which plays an important role in revealing the deformation and damage loss mechanisms of materials under the influence of thermal and mechanical coupling in a multifaceted and profound manner. [Brief explanation of the drawings]

[0012] [Figure 1]FIG. 1 is a technical roadmap of the present disclosure. [Figure 2] 1 is a schematic structural diagram of an in-situ mechanical performance measurement device using a scanning electron microscope with multiple combined technologies according to the present disclosure. [Figure 3] FIG. 3 is a partially enlarged schematic view of region 4A in FIG. 2. [Figure 4] FIG. 3 is a partially enlarged schematic view of region 5A in FIG. 2. [Figure 5] 1 is an overall configuration diagram of an in-situ testing machine according to the present disclosure. FIG. [Figure 6] FIG. 6 is a local enlarged schematic view of region 64A in FIG. 5. [Figure 7] FIG. 1 is a schematic diagram of a high temperature loading unit of the present disclosure. [Figure 8] FIG. 1 is a schematic diagram of the polishing, buffing, and laser marking steps in the sample preparation process of the present disclosure. [Figure 9] 1 is a schematic diagram of speckle production and spray application in the sample production process of the present disclosure. [Figure 10] 1 is a test flowchart of the measurement method of the present disclosure. [Figure 11] FIG. 1 is a schematic diagram illustrating how the present disclosure performs time alignment on five disparate data sources. [Figure 12] FIG. 1 is a schematic diagram of spatial alignment after sample rotation according to the present disclosure. [Figure 13] FIG. 1 is a principle diagram of the five detector parallel test timing of the present disclosure.

[0013] In order to more clearly describe the embodiments of the present disclosure or the technical solutions in the prior art, the drawings that need to be used in the embodiments will be briefly described. Obviously, the drawings in the following description are only some embodiments of the present disclosure, and those skilled in the art can obtain other drawings based on these drawings without paying creative labor. Here, 1, EBSD detector, 2, EDS detector, 3, SE detector, 4, pole piece, 5, Raman objective lens, 6, in-situ testing machine, 61, tensile loading unit, 611, bidirectional ball screw, 62, linear displacement precision measurement unit, 63, offset loading nut seat, 631, second water cooling pipe, 64, driven jig group, 641, driven jig body, 642, driven gear shaft, 643, needle bearing, 644, rotating connecting shaft, 645, precision tensile / compression force sensor, 64 6, second thrust ball bearing, 647, driven gear, 648, first thrust ball bearing, 649, rotating ball spline, 65, high-temperature loading unit, 651, first water-cooled pipe, 652, sample, 653, semicircular winding core, 654, driving jig body, 655, spring, 656, heat insulating layer, 657, water-cooled plate, 658, heat insulating plate, 659, rotating heat conduction core, 66, driving jig group, 67, precision moment motor, 71, X-direction displacement platform, 72, Y-direction displacement platform, 8, scanning electron microscope. DETAILED DESCRIPTION OF THE INVENTION

[0014] Hereinafter, the technical aspects of the embodiments of the present disclosure will be clearly and completely described with reference to the drawings in the embodiments of the present disclosure. Obviously, the described embodiments are only some embodiments of the present disclosure, but not all embodiments. Based on the embodiments in the present disclosure, all other embodiments obtained by those skilled in the art without paying creative labor belong to the scope of protection of the present disclosure.

[0015] The purpose of this disclosure is to solve the problems of the past by providing an in-situ mechanical performance measurement device and analysis method using a multi-technique combination of a scanning electron microscope. The scanning electron microscope is a scanning electron microscope, and the multi-technique combination refers to the combination of five detection techniques, including in-situ measurements such as SEM, EDS, EBSD, SEM-DIC, and Raman. The analysis method includes a sample preparation method, a measurement method, and a data processing method. This disclosure uses a tension-compression loading unit to control the mechanical loading of the sample, a rotation loading unit to control the sample angle, and a displacement platform to convert the SE mode position and Raman mode position, so that various in-situ measurements of SEM, EDS, EBSD, SEM-DIC, and Raman can be performed on the sample in the scanning electron microscope, which can reveal the deformation damage failure mechanism of the material in a multifaceted and profound way, and provide a more novel technical means for scientifically establishing the relationship between the evolution of material microstructure under complex loading and the dynamic response of macroscopic performance.

[0016] In order to make the above objects, features and advantages of the present disclosure more clearly comprehensible, the present disclosure will be described in more detail below in combination with the accompanying drawings and specific embodiments.

[0017] As shown in FIGS. 1 and 2 to 7, the present disclosure provides an in-situ mechanical performance measurement device using a multi-technique combination of a scanning electron microscope, which includes a displacement platform and an in-situ testing machine 6 attached to the displacement platform. The displacement platform includes an X-direction displacement platform 71 and a Y-direction displacement platform 72. The displacement platform can move the position of the in-situ testing machine 6 and convert it into different mode positions. The in-situ testing machine 6 includes a fixture unit, a rotation loading unit, and a tension / compression loading unit 61. The fixture unit includes a driving fixture group 66 and a driven fixture group 64. The driving fixture group 66 and the driven fixture group 64 are clamped at both ends of a sample 652. The tension / compression loading unit 61 is used to drive the driving fixture group 66 and the driven fixture group 64 to move in the opposite or rearward direction and to load a compressive force and a tensile force on the sample 652. The displacement platform is a pole piece of a scanning electron microscope 8. It can be moved to the SE mode position or the Raman mode position, which is the position of the Raman objective lens 5. The movement of the displacement platform can be controlled by the observation mode switching software. In the SE mode position, the rotary loading unit drives the driving fixture group 66 and the driven fixture group 64 to rotate synchronously, adjusting the imaging angle between the sample 652 and the five types of detectors. Furthermore, while loading the sample in tension and compression, SEM, EDS, EBSD, SEM-DIC, and Raman in-situ tests can be performed on samples at different angles.

[0018] The scanning electron microscope 8 uses a tungsten filament and includes five detectors: EBSD detector 1 (receiver), EDS detector 2 (receiver), SE detector 3 (receiver), pole piece 4 (transmitter), and Raman objective lens 5 (transmitter and receiver). By moving the in-situ tester 6 in the Y direction on the X-direction displacement platform 71 and the Y-direction displacement platform 72, the sample 652 can be positioned under the pole piece 4 or the Raman objective lens 5, allowing switching between SE mode and Raman mode. The imaging principle is as follows: an electron beam is emitted from the pole piece 4 and impinges on the surface of the sample 652, exciting the surface and generating secondary electrons. The secondary electrons are received by SE detector 3 and processed to obtain an SEM image; the secondary electrons are received by EBSD detector 1 and processed to obtain an EBSD image; and the secondary electrons are received by EDS detector 2 and processed to obtain an EDS image. On the other hand, SEM-DIC images are post-processed based on the SEM images, i.e., by identifying pixel changes in multiple images before and after the SEM images, and then processed using VIC-2D software, a series of mechanical, mathematical, and finite element calculations are performed to obtain the strain distribution of sample 652, known as the SEM-DIC image. However, for metal materials, the test is often buffed. In SEM-DIC software processing, the lack of feature points makes it difficult to accurately identify corresponding changes, so artificial speckle spraying is required. To simultaneously observe the micromorphology and strain distribution (SEM-DIC image information) of a single region on a single sample 652, one surface of the sample 652 is observed for micromorphology, and the other surface is sprayed with speckle spray, and an SEM image of that surface is acquired and processed before the SEM-DIC image can be obtained. Therefore, the sample 652 must be rotated completely. That is, in SEM mode, the sample 652 is at 0°, and in SEM-DIC mode, the sample 652 is at 180°.

[0019] In the conventional in-situ mechanical performance measurement under a scanning electron microscope 8, only local area information can be obtained using a single detector, or material damage information at different locations and different times can be obtained using multiple detectors, making it difficult to obtain the defects of the micro-behavior of key areas related to material deformation, damage, and loss in a synchronized, isochronous, and multidimensional manner. In response to this, the present disclosure provides an in-situ mechanical performance measurement device that uses multiple techniques of a scanning electron microscope, and uses a pole piece 4 (SE mode position) of an in-situ testing machine 6 to switch between SE mode and Raman mode when applying a tensile and compressive force to a sample 652. The position between the sample 652 (position) and the Raman objective lens 5 (Raman mode position) can be adjusted. The angle of the sample 652 can be controlled by a rotary loading unit, and the relative angle between the sample 652 and the pole piece 4 can be adjusted to meet the imaging requirements of three different observation modes: SEM / EDS, SEM-DIC, and EBSD. This allows the micro-morphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) of a specific area of ​​the sample 652 under mechanical action to be obtained, and the deformation damage and failure mechanism of the material can be revealed in a multifaceted and profound manner.

[0020] As shown in FIGS. 3 to 6 , the rotary loading unit includes a precision moment motor 67 and a rotary ball spline 649, the axial direction of which is parallel to the axial direction of the sample 652. The rotary ball spline 649 is provided with a drive gear (not shown, but structurally identical to the driven gear 647) and a driven gear 647. Taking the driven gear 647 as an example, the driven gear 647 is fitted into the spline groove of the rotary ball spline 649 to prevent relative rotation, but can move axially relative to the rotary ball spline 649. The rotary ball spline 649 is supported via a first thrust ball bearing 648, i.e., the rotary ball spline 649 and the driven gear 647 can rotate synchronously around the first thrust ball bearing 648. The installation mode of the drive gear refers to the installation mode of the driven gear 647. Therefore, the drive gear and the driven gear 647 can move axially along the rotary ball spline 649 and rotate with the rotation of the rotary ball spline 649. The driving fixture group 66 includes a driving gear shaft meshing with the driving gear, and the driven fixture group 64 includes a driven gear shaft 642 meshing with the driven gear 647. The driving gear shaft is connected to a precision moment motor 67. When the precision moment motor 67 drives the rotation of the driving gear shaft, the rotation of the driving gear can be driven through the driving gear shaft. The rotation of the driving gear can drive the rotation of the rotating ball spline 649. The rotation of the rotating ball spline 649 drives the rotation of the driven gear 647. The rotation of the driven gear 647 rotates the driven gear shaft 642. The driving jig group 66 drives the rotation of the driven jig group 64, and finally, the precision moment motor 67 is used to realize synchronous rotation of the driving jig group 66 and the driven jig group 64, which allows the specimen 652 to rotate in a plane without twisting, improving the accuracy of the test. Furthermore, the driving jig group 66 and the driven jig group 64 can synchronize the axial tensile motion of the specimen 652 with the rotation of the specimen 652, and do not interfere with or affect each other, so that the in-situ testing machine 6 can adjust the observation angle simultaneously during mechanical loading.

[0021] The rotation angle of the sample 652 can be adjusted using the observation mode switching software, and the software reads the horizontal reference and angle of the jig unit and in-situ testing machine 6 through an absolute radial grating attached to the jig unit, compares it with the set target angle, and controls the precision moment motor 67 to rotate to the set angle. When the sample 652 is rotated to 0°, imaging with the SE detector 3 and EDS detector 2 is possible, when rotated to 70°, imaging with the EBSD detector 1 is possible, when rotated to 180°, SEM-DIC imaging is possible, and when rotated to 360°, imaging with the Raman objective lens 5 is possible.

[0022] As shown in Figures 5 and 6, the tension / compression loading unit 61 includes a bidirectional ball screw 611 and a pair of offset loading nut seats 63 attached to the bidirectional ball screw 611. When the bidirectional ball screw 611 rotates, the offset loading nut seats 63 can move synchronously in the opposite or rearward axial direction. One offset loading nut seat 63 is connected to the driving fixture body 654 of the driving fixture group 66, and the other offset loading nut seat 63 is connected to the driven fixture body 641 of the driven fixture group 64. When the offset loading nut seats 63 move axially, they drive the driving fixture group 66 and the driven fixture group 64, thereby loading tension or compression force into the specimen 652 in the axial direction. A pair of the bidirectional ball screws 611 are provided, and their ends rotate synchronously through gear meshing, thereby achieving stable axial movement of the offset loading nut seats 63. The tension / compression loading unit 61 may include a DC brushless motor connected to a two-stage reduction mechanism, through which power is transmitted to a bidirectional ball screw 611, and the offset nut seat 63 drives the relative motion of the driving jig group 66 and the driven jig group 64. The two-stage reduction mechanism may include a miter gear and a worm wheel, through which the DC brushless motor transmits power reduction torque to the meshed worm wheels via a pair of miter gears, and the two synchronously rotating worm wheels synchronously rotate the bidirectional ball screw 611 attached to the offset load nut seat 63, causing the offset load nut seat 63 to slide along two parallel linear guides. The axial direction of the specimen 652 and the axis of the bidirectional ball screw 611 can be located in the same plane, and at the same time, the axial direction of the linear displacement precision measuring unit 62 can also be located in this plane, so that the tension / compression loading unit 61 can effectively avoid inaccurate displacement measurement caused by poor device rigidity and large overturning moment when applying a large load.

[0023] As shown in FIG. 6, a precision tension-compression force sensor 645 is also provided. A rotary connecting shaft 644 is connected to the driven gear shaft 642, and the two are synchronously rotatable. The rotary connecting shaft 644 is rotatably connected to the sleeve via a pair of inverted second thrust ball bearings 646. A needle bearing 643 is provided on the outer diameter of the sleeve, and the needle bearing 643 is mounted in a mounting hole of the driven jig body 641. The sleeve is connected to the precision tension-compression force sensor 645. A fastening screw determines the circumferential angle between the fasteners. When the driven gear shaft 642 rotates the driven jig group 64, the axial tension-compression force is transmitted to the precision tension-compression force sensor 645 via the rotary connecting shaft 644. The circumferential rotation of the rotary connecting shaft 644 is transmitted to the inner ring of the second thrust ball bearing 646. This allows the precision tension-compression force sensor 645 to measure the axial loading of the sample 652 without being affected by the axial rotation of the sample 652. That is, the driven jig group 64 is installed coaxially with the precision tension / compression force sensor 645, but is not connected to the same axis, and when the driven jig group 64 rotates the sample 652, the precision tension / compression force sensor 645 can be held so as not to rotate, and the measurement of the precision tension / compression force sensor 645 can be prevented from being affected.

[0024] As shown in Figures 5 and 7, the system includes a high-temperature loading unit 65 for heating sample 652 to high temperatures, and a high-temperature loading unit 65 for applying temperatures between room temperature and 1000°C to sample 652 and rotating and heating sample 652. The high-temperature loading unit 65 applies high temperatures in real time during mechanical loading and flux observation angle adjustment, synchronously applying tensile and compressive forces to sample 652, and subjecting sample 652 to mechanical-thermal coupling. This allows for multifaceted and in-depth research into the deformation and damage mechanisms of materials under mechanical-thermal coupling. In-situ tensile mechanics and temperature loading parameters can be set in the control software, and precise control of sample 652 loading displacement, loading speed, and loading force can be achieved through PID. Specifically, the high-temperature loading unit 65 may include a semicircular winding core 653 and a rotating heat-conducting core 659. The semicircular winding core 653 is wound with a nichrome wire for heating, and the rotating heat-conducting core 659 is wound around the outside of the sample 652 and rotates with the rotation of the sample 652. The outer diameter side of the rotating heat-conducting core 659 is attached to the inner diameter side of the semicircular winding core 653. At different angles of the sample 652, the rotating heat-conducting core 659 can transfer heat from the semicircular winding core 653 to the sample 652, and can maintain good heat conduction effect even when the sample 652 is rotated at different angles.

[0025] Furthermore, a multi-layer insulation layer 656, such as a three-layer insulation layer made of stainless steel, is provided on the exterior of the semicircular winding core 653 to effectively suppress the impact of thermal radiation on the detector's imaging performance. The insulation layer 656 is connected to a water-cooled plate 657 with an open flow path. The water-cooled plate 657 is connected to the first water-cooled pipe 651, which is a welded water-cooled pipe welded to the water-cooled plate 657. The cooling medium is then sent to the water-cooled plate 657, which cools the water-cooled plate 657 with water, minimizing the thermal impact on other components on the bottom plate of the in-situ testing machine 6. The water-cooled plate 657 is attached to the bottom plate of the in-situ testing machine 6 via an insulation plate 658, which can be made of carbon fiber. A spring 655 is provided between the water-cooled plate 657 and the heat-insulating plate 658. Adjusting the height of the spring 655 changes the height of the screw, thereby adjusting the relative height and heat-transfer area between the semicircular winding core 653 and the rotating heat-conducting core 659, and thus the heating effect on the sample 652. A second water-cooled pipe 631 is connected to the offset loading nut seat 63. The second water-cooled pipe 631 may be a bite-type water-cooled pipe connected to the offset loading nut seat 63, which can reduce the temperature of the offset loading nut seat 63. An annular flow path opens into the bearing hole that attaches the driving jig group 66 / driven jig group 64 to the offset loading nut seat 63. The annular flow path surrounds the needle bearing 643, thereby reducing the impact of temperature rise in the jig unit on the accuracy of the precision tension / compression force sensor 645 and the precision moment motor 67. The purpose of opening the annular passage in the offset loading nut seat 63 is to reduce the temperature of the jig unit and bearing through cooling of the cooling medium, and to prevent heat from being transferred to the precision tension / compression force sensor 645 during the high-temperature loading process, which would affect its measurement accuracy.

[0026] The stainless steel corrugated pipe connects the first water-cooled pipe 651 in the high-temperature loading unit 65 and the second water-cooled pipe 631 of the offset loading nut seat 63 to the electron microscope flange via a four-way joint, and the threaded joint is secondarily sealed by brazing to prevent leakage even at pressures of up to 0.5 MPa.

[0027] The driving fixture group 66 and the driven fixture group 64 move relative to each other, tensioning / compressing the sample 652. At the same time as tensioning / compressing the sample 652, the precision moment motor 67 rotates the driving fixture group 66 around its axis, which further drives the rotation of the driven fixture group 64 and the rotating ball spline 649 connected to the driving fixture group 66, ensuring synchronous rotation of the driving fixture group 66 and the driven fixture group 64. The rotating heat conduction core 659 comes into contact with the sample 652 and the semicircular winding core 653 and rotates simultaneously with the driving fixture group 66 and the driven fixture group 64 rotating around its axis, transferring heat from the semicircular winding core 653 to the sample 652 and applying high-temperature loading to the sample 652.

[0028] This disclosure provides a sample preparation method for preparing a sample 652 for an in-situ mechanical performance measurement device using the above-mentioned multiple techniques of a scanning electron microscope, as shown in Figures 1, 8, and 9. The prepared sample 652 has good surface smoothness and clear surface texture, and can simultaneously meet the imaging requirements for EBSD and SEM-DIC. This method includes the following: S1: Use a laser cutter to process the blank material to be measured into a dumbbell-shaped sample 652 of uniform thickness, and polish both sides of the sample 652 with waterproof abrasive paper until it has good adhesion with the inner groove surface of the rotating heat conduction core 659, thereby reducing the contact thermal resistance between the sample 652 and the rotating heat conduction core 659 in a vacuum. S2. Using a metallographic sample grinder, polish the upper and lower surfaces of the dumbbell-shaped specimen 652. Using increasingly larger grits of waterproof abrasive paper, alternately polish the upper and lower surfaces of specimen 652. The upper surface of specimen 652 was polished with 5000# abrasive paper until no obvious scratches remained. Then, a paraffin film was coated on the surface. The upper surface of specimen 652 was polished continuously. The sandpaper was replaced with abrasive cloth, and small-grain abrasive paste was applied continuously until a mirror finish was achieved. The specimen was then immersed in an electrolytic polishing solution to remove the oxide layer on the lower surface, allowing a clear pattern to be collected under EBSD. S3: The sample 652 is immersed in a turpentine oil solution heated in a water bath, ultrasonically cleaned, the paraffin film on the top surface of the sample 652 is removed, the sample is washed with absolute ethanol, and dried. S4: Using a femtosecond laser, 10 μm-wide scale lines are etched at 5 mm intervals on the edges of the reference distance segment on the top and bottom surfaces of sample 652 to determine the coordinates of each point on the reference distance segment of the sample. Five landmark points are then etched on each of the two surfaces, denoted as o, a, b, c, d and o', a', b', c', d', with their positions corresponding to each other in pairs, to serve as characteristic landmark points for spatial alignment. S5. Dissolve Al2O3 powder with a particle size of 500 μm in anhydrous ethanol by ultrasonic vibration for 5 minutes, let the cloudy solution stand for 3 minutes, put the upper layer of the clear liquid into the pot on the airbrush, adjust the airflow size and spray distance, and spray the Al2O3 solution evenly onto the underside of the sample 652. Place the sample 652 in an oven to dry, and use the uniformly distributed Al2O3 particles as a speckle pattern for SEM-DIC analysis.

[0029] The present disclosure provides a testing method using an in-situ mechanical performance measuring device that combines multiple techniques of a scanning electron microscope as described above, as shown in Figures 1 and 10, and includes the following content. S1, adjust the distance between the driving fixture group 66 and the driven fixture group 64, attach the sample 652 to the fixture unit, press the sample 652 against the inner groove surface of the rotating heat conduction core 659, evacuate the scanning electron microscope 8, adjust the tungsten filament current to obtain clear imaging, adjust the observation mode switching software, rotate the fixture unit to four positions of 0°, 70°, 180°, and 360°, initialize the angle adjustment, move the sample 652 from the pole piece 4 to under the Raman objective lens 5, return it to the original position, initialize the position adjustment, and record the corresponding spatial coordinate parameter A0 of the in-situ testing machine 6. Enter the experimental target temperature into the temperature loading interface of the in-situ high-temperature mechanical loading meter control software such as S2 or In-Situ Thermomechanical Pro. After the monitored temperature of the sample 652 reaches the set value, set the tension / compression rate and loading displacement parameters in the mechanical loading interface. Apply the load until the target value is reached, then stop loading and record the current time while maintaining the set mechanical loading until the end. S3: Operate the observation mode switching software, such as In-Situ PolyMode MicroImager, move the sample 652 under the pole piece 4 and rotate it to 0°, record the spatial state information of the in-situ testing machine 6 as A1, select the SE mode, and use the scanning electron microscope imaging software to control and operate various detectors sequentially to obtain in-situ high-temperature tensile / compression SEM and EDS images near point o on the top surface of the sample 652, and record the corresponding collection times. S4: Keep the position of the in-situ testing machine 6 unchanged, rotate the sample 652 by 70°, record the spatial state information of the in-situ testing machine 6 as A2, obtain in-situ high-temperature tensile / compression EBSD crystal structure information near point o on the top surface of the sample 652, then rotate the sample 652 by 180°, obtain a speckle distribution SEM image near point o′ on the bottom surface of the sample 652, record the spatial state information of the in-situ testing machine 6 as A3, and record the corresponding image collection time. S5, move the X-direction displacement platform 71 and the Y-direction displacement platform 72, move the sample 652 under the Raman objective lens 5 and rotate it to 0°, select the Raman mode, control the Raman system imaging, acquire a Raman image near point o on the top surface of the sample 652, record the spatial state information of the in-situ testing machine 6 as A4, and record the acquisition time. S6: Apply the spatial state information A1 to the observation mode switching software, such as the In-Situ PolyMode MicroImager, adjust the in-situ testing machine 6 to the initial observation state, set the loading parameters again, and after loading is completed, repeat the above steps S3, S4, and S5 to obtain the second group of five types of in-situ observation data under the force-thermal coupling effect. S7: Repeat steps S3, S4, S5, and S6 until the sample 652 breaks. The force and displacement curve of the sample 652 recorded in the in-situ loading control software is output. The acquired speckle distribution SEM image is input into the Vic-2D processing software. The software compares the relative change information of the microstructural feature morphology in two adjacent SEM images, and performs multiple spline interpolations on the data acquired from the images using the incremental correlation criterion to calculate and obtain the strain distribution on the underside of the sample 652.

[0030] As shown in Figures 1 and 11-13, the present disclosure provides a data processing method for processing data obtained by the above-mentioned test method, which performs fusion analysis of five types of asynchronous microscopic data collected at different times by five types of detectors at different positions on the sample 652, and provides a multifaceted and multi-source analysis of the material deformation and damage mechanism caused by force-thermal coupling. S1. Arrange the various types of micro-images acquired during the experimental process according to the timing of collection, determine the absolute time in space and time of sampling for each of the five types of acquired micro-data, process the imaging areas with different dimensions due to the different imaging principles of the five types of detectors, prepare the landmark points o, a, b, c, d and o', a', b', c', d' etched into the sample 652 production, determine the areas of the different observation areas and the corresponding spatial coordinates in the corresponding sample 652 target segments, and map each acquired image to the force-time curve and displacement-time curve collected in the in situ high-temperature mechanical loading control software. In step S2, the collection times of the five types of microscopic data, including SEM images, EDS images, EBSD images, SEM-DIC images, and Raman images, acquired asynchronously in step S1, are time-aligned with the collection times of the force-displacement curve. The data acquired by the five detectors with low collection frequencies are converted to the time nodes of the force-displacement curve with high sampling frequencies using the least common multiple method of time coordinates. The time alignment of the five corresponding detectors can be performed as follows:

[0031] An example will be explained in which the observation data obtained by the five types of detectors (SEM, EDS, EBSD, SEM-DIC, and Raman) processed in step S1 is extrapolated onto the observation array of the force-time curve, and the SEM observation data is converted into a force-time curve. a (n-1),t a (n)] is the SEM acquisition time t b (m-1), and the t of the force-displacement curve a The observation value at time (n-1) is (x a (n-1),y a (n-1),z a (n-1)), and t a The observed value at time (n) is (x a (n),y a (n), z a (n)), and by linear interpolation, t b (m) Time observation data (x b (m),y b (m), z b(m)) is obtained as follows.

[0032]

number

[0033] In step S3, initial images of the unstretched sample were extracted in four orientations: 0° in SEM / EDS mode, 70° in EBSD mode, 180° in SEM-DIC mode, and 360° in Raman mode. All four images were based on the etched landmark o on the sample. A common Cartesian coordinate system was constructed using the o point at 0° in SEM / EDS mode as the common reference coordinate origin, with the sample's short edge as the x-axis. For the other three orientations, each Cartesian coordinate system was constructed using its own o point as the coordinate origin and the sample's short edge as the x-axis. Using the angular and translational transformation formulas, the data measured in each of these three orientations in their own spatial coordinate systems were transformed and merged error-free into the common Cartesian coordinate system at 0°, achieving spatial alignment. Spatial alignment for the four corresponding spatial orientations was achieved as follows:

[0034] An example of aligning the 70° of the sample in the EBSD mode with the 0° of the sample in the SEM / EDS mode will be described. The coordinate system of the three mutually orthogonal unit vectors of the sample 70° in the EBSD mode and the sample 0° in the SEM / EDS mode is defined as {e xk ,e yk ,e zk} and {e x'k ,e y'k ,e z'k} and then oe x' ke y'k e z'k Coordinate systems and spatial coordinate systems oe xk e yk e zk between x'k , e y'k , e z'k The rotation angles of the three coordinate axes are φ k , η k and φ kThe coordinate vectors of the two orientations of the sample at 0° and 70° are P k =(x k ,y k ,z k ) and Pk'=(x k ,y k ,z k ) and the conversion relationship between them is defined as follows:

[0035]

number

[0036] Here, the rotation matrix R of the coordinate transformation k is as follows:

[0037]

number

[0038] In Raman mode, a translation transformation along the coordinate system is also required. The translation vector from the sample 180° coordinate system in Raman mode to the sample 0° common coordinate system in SEM / EDS mode is T ab =(t x ,t y ,t z ) T where the coordinate vector after rotation transformation at sample 180° relative to sample 0° is R b ', and the coordinates in the common coordinate system of the sample coordinates in the Raman mode are as follows:

[0039]

number

[0040] This completed the spatial alignment of the observation data between the two types of detectors.

[0041] In step S4, the data from six different sources, namely the spatiotemporal aligned SEM images, EDS images, EBSD images, SEM-DIC images, Raman images, and macroscopic force-displacement curves in steps S2 and S3, are merged into a single data source. A coordinate system with point o as the coordinate origin is constructed using the scale marks etched during the preparation of sample 652, and the initial time point t in the force-displacement curve is defined as the coordinate origin. a The spatial orientation P of the specimen at 0° in the SEM / EDS mode corresponds to (0) k =(x k ,y k ,z k ) is the initial time zero point and space zero point, and the time-aligned t b (m) Time observation data (x b (m),y b (m), z b (m)), and the spatial coordinates P at which the five types of detectors acquired data at the corresponding times when spatial alignment was completed in step S3. ab ', where the coordinates of the coordinate origin o corresponding to each point in the observation area of ​​the sample target segment are i ,y i ) and t n The spatial coordinates based on the common reference coordinate system in the five modes of SEM, EDS, EBSD, SEM-DIC, and Raman at time z1 = P ab1 ', z2=P ab2 ', z3=P ab3 ', z4=P ab4 ', z5=P ab5 ', and z1, z2, z3, z4, z5 are functions of time t, (x i ,y i ) i.e., φ(t) = (z1,z2,z3,z4,z5,t), and the multi-source data fusion for each point in sample 652 is W = (x i ,y i, φ(t)). By inputting the coordinate parameters (x, y) of any point on the sample 652 relative to the origin o and the corresponding time t during the loading process, the micromorphology, element distribution, crystal structure, strain distribution, corresponding molecular information, and average stress of the sample 652 at that point can be obtained, allowing independent and unified analysis of the deformation damage and failure mechanism due to mechanical-thermal coupling of the material from five aspects.

[0042] This disclosure provides a detailed description of four aspects, including the in-situ mechanical performance measurement device, sample preparation method, test method, and data processing method using a scanning electron microscope with multiple detection techniques. Overall, it describes a method for characterizing in-situ mechanical and thermal coupled testing of material mechanical behavior using five detection techniques within a scanning electron microscope. Through the above-mentioned series of processes, the final sample information can be obtained after the five types of data fusion, which has a multifaceted and profound effect on the important role that mechanical and thermal coupled effects play in the deformation and damage loss mechanisms of materials.

[0043] Although the present disclosure uses specific examples to describe the principles and embodiments of the present disclosure, the description of the above examples is only intended to facilitate understanding of the method and core idea of ​​the present disclosure, and at the same time, those skilled in the art will be able to make changes in the specific embodiments and application scope based on the idea of ​​the present disclosure. As such, the contents of this specification should not be construed as limitations on the present disclosure.

Claims

1. An in-situ mechanical performance measurement device using a scanning electron microscope with multiple techniques, a displacement platform and an in-situ testing machine attached to the displacement platform; The in-situ testing machine includes a jig unit, a rotation loading unit, and a tension / compression loading unit; The jig unit includes a driving jig group and a driven jig group, and the driving jig group and the driven jig group clamp both ends of the sample. The tension / compression loading unit is used to drive the driving jig group and the driven jig group to move in the opposite direction or backward. The displacement platform is used to move the sample to an SE mode position and a Raman mode position of a scanning electron microscope. The rotation loading unit drives the driving jig group and the driven jig group to rotate synchronously, and rotates the jig unit to 0° to obtain information on the microscopic shape of the sample while tension / compression loading the sample attached to the jig unit. an in-situ SEM measurement using an SE detector to obtain information on element content and distribution; an in-situ EDS measurement using an EDS detector to obtain information on element content and distribution; an in-situ EBSD measurement using an EBSD detector by rotating the sample by 70° to obtain information on crystal structure; an in-situ SEM-DIC measurement using an EBSD detector by rotating the sample by 180° to obtain information on strain distribution; and an in-situ Raman measurement using a Raman objective lens by rotating the sample by 360° to obtain information on molecular information.

2. The rotary loading unit includes a precision moment motor and a rotary ball spline; 2. The in-situ mechanical performance measuring device using a scanning electron microscope with multiple combined technologies according to claim 1, wherein the rotary ball spline is provided with a drive gear and a driven gear, the drive gear and the driven gear move along the axial direction of the rotary ball spline and rotate with the rotation of the rotary ball spline, the drive jig group includes a drive gear shaft meshing with the drive gear, the driven jig group includes a driven gear shaft meshing with the driven gear, and the drive gear shaft is connected to the precision moment motor.

3. 3. The in-situ mechanical performance measuring device for a scanning electron microscope using multiple technologies in combination as described in claim 2, wherein the tension / compression loading unit includes a bidirectional ball screw and a pair of offset loading nut seats attached to the bidirectional ball screw, one of the offset loading nut seats being connected to the driving jig group and the other of the offset loading nut seats being connected to the driven jig group, a pair of the bidirectional ball screws being provided, and the axial direction of the sample and the axis of the bidirectional ball screw being positioned on the same plane.

4. 4. The in-situ mechanical performance measurement device for a scanning electron microscope using multiple technologies as described in claim 3, characterized in that it includes a high-temperature loading unit, the high-temperature loading unit including a semicircular winding core and a rotating heat-conducting core, the rotating heat-conducting core is wound around the outside of the sample and rotates with the rotation of the sample, the outer diameter side of the rotating heat-conducting core is attached to the inner diameter side of the semicircular winding core, and heat from the semicircular winding core can be transferred to the sample at different angles of the sample by the rotating heat-conducting core.

5. 5. The in-situ mechanical performance measuring device using multiple technologies of a scanning electron microscope according to claim 4, wherein a multi-layer heat insulating layer is provided on the outside of the semicircular winding core, the heat insulating layer is connected to a water-cooled plate with an open flow path, the water-cooled plate is connected to a first water-cooled piping path, the water-cooled plate is attached to the bottom plate of the in-situ testing machine via the heat insulating plate, and the offset loading nut seat is connected to a second water-cooled piping.

6. A sample preparation method for preparing a sample for an in-situ mechanical performance measurement device using a multi-technique combination of a scanning electron microscope according to any one of claims 1 to 5, comprising: a first sample preparation step of processing a measurement target material blank into a dumbbell-shaped sample having a uniform thickness; a second sample preparation step, which includes polishing both the top and bottom surfaces of the sample, coating a paraffin film on the top surface of the sample after there is no obvious scratch on the top surface of the sample, and polishing the bottom surface of the sample to a mirror effect, and then immersing the sample in an electrolytic polishing solution to remove the bottom surface oxide layer, so that a clear pattern can be collected under EBSD; a third sample preparation step of ultrasonically cleaning the sample, removing the paraffin film on the upper surface of the sample, and thoroughly cleaning and drying the sample; a fourth sample preparation step in which 10 μm wide scale lines are etched at 5 mm intervals on the edges of the rectangular regions on the top and bottom surfaces of the sample, and five marking points are etched on each surface, denoted as o, a, b, c, d and o′, a′, b′, c′, d′, with two corresponding positions used as characteristic marking points for spatial alignment; and a fifth sample preparation step of creating a speckle pattern image for SEM-DIC analysis on the lower surface of the sample.

7. In the first sample preparation step, both side surfaces of the sample are polished to a good degree of adhesion with the inner groove surface of the rotary heat conduction core, thereby reducing the contact thermal resistance between the sample and the rotary heat conduction core in a vacuum; In the fifth sample preparation step, Al having a particle size of 500 μm ２ O ３ The powder was dissolved in absolute ethanol by ultrasonic vibration for 5 minutes, and the cloudy solution was allowed to stand for 3 minutes. The upper layer of the clear liquid was placed in the upper pot of the airbrush, and the size of the airflow and the spray distance were adjusted. ２ O ３ The solution was sprayed evenly on the underside of the sample, and the sample was placed in an oven to dry, resulting in a uniformly distributed Al ２ O ３ 7. The method for preparing a sample according to claim 6, wherein the particles are formed into a speckle pattern.

8. A measurement method using the in-situ mechanical performance measurement device using a multi-technique combined scanning electron microscope according to claim 1 and the sample preparation method according to claim 6, a first measurement step of mounting a sample on a fixture unit, evacuating the scanning electron microscope, adjusting the tungsten filament current to obtain clear imaging, adjusting the observation mode switching software, rotating the fixture unit to four sample angles of 0°, 70°, 180°, and 360°, initializing the angle adjustment, moving the sample from the pole piece to under the Raman objective lens, returning it to its original position, initializing the position adjustment, and recording the corresponding spatial coordinate parameter A0 of the in-situ tester; A second measurement step of setting and applying tension / compression speed and loading displacement parameters in the mechanical loading interface, stopping the loading after reaching the target value, and recording the current time while maintaining the set mechanical loading until the end; a third measurement step of operating observation mode switching software to move the sample under the pole piece and rotate it to 0°, recording the spatial state information of the in-situ testing machine as A1, selecting the SE mode, using scanning electron microscope imaging software to control and operate various detectors sequentially, obtaining in-situ tensile / compression SEM images and EDS images of the upper surface of the sample near point o by in-situ SEM measurement and in-situ EDS measurement, and recording the corresponding collection times; a fourth measurement step of maintaining the position of the in-situ testing machine unchanged, rotating the sample by 70°, recording spatial state information of the in-situ testing machine as A2, acquiring an in-situ tension / compression EBSD image of the upper surface of the sample near point o by in-situ EBSD measurement, then rotating the sample by 180°, acquiring an SEM-DIC image of the lower surface of the sample near point o' by in-situ SEM-DIC measurement, recording spatial state information of the in-situ testing machine as A3, and recording the corresponding image acquisition time; a fifth measurement step of moving a displacement platform, moving the sample under a Raman objective lens and rotating it to 0°, selecting a Raman mode, controlling Raman system imaging, acquiring a Raman image of the upper surface of the sample near point o by in-situ Raman measurement, recording the spatial state information of the in-situ tester as A4, and recording the acquisition time; a sixth measurement step of applying spatial state information A1 to observation mode switching software, adjusting the in-situ testing machine to an observation initial state, setting loading parameters again, and after loading is completed, repeating the third measurement step, the fourth measurement step, and the fifth measurement step to acquire an in-situ tension / compression SEM image and an EDS image of the upper surface of the sample of the second group near point o, an in-situ tension / compression EBSD image of the upper surface of the sample near point o, an SEM-DIC image of the lower surface o' of the sample, and a Raman image of the upper surface of the sample near point o; a seventh measurement step of repeating the third measurement step, the fourth measurement step, the fifth measurement step, and the sixth measurement step until the sample breaks, outputting the force and displacement curve of the sample recorded in in-situ loading control software, and inputting the acquired SEM-DIC image into a computer and performing calculations to obtain the strain distribution on the underside of the sample.

9. The testing method of claim 8, wherein in the second measurement step, the test target temperature is first input into the temperature loading interface of the in-situ loading control software, and after the monitored temperature of the sample reaches a set value, the subsequent contents of the tension / compression speed and loading displacement parameters are set to realize the force-thermal coupling effect on the sample.

10. A data processing method for processing data obtained by the test method according to claim 9, comprising: a first data processing step of arranging the SEM images, EDS images, EBSD images, SEM-DIC images, and Raman images acquired during the test according to the timing of collection, determining the time and space of sampling of each of the acquired SEM images, EDS images, EBSD images, SEM-DIC images, and Raman images, determining the areas of different observation regions and their corresponding spatial coordinates in the rectangular regions of the sample using landmark points o, a, b, c, d and o', a', b', c', d' etched during the sample preparation process, and mapping the acquired images one by one to the force-time curves and displacement-time curves collected in the in-situ loading control software to obtain force-displacement curves; a second data processing step of time-aligning the collection times of the SEM image, EDS image, EBSD image, SEM-DIC image, and Raman image asynchronously acquired in the first data processing step with the force-displacement curve, and converting the data acquired by the five types of detectors with low collection frequencies using a linear interpolation method into time nodes of the force-displacement curve with a high sampling frequency using a least common multiple method of time coordinates; a third data processing step in which initial images of the unstretched sample are extracted in four different orientations: sample 0° in SEM / EDS mode, sample 70° in EBSD mode, sample 180° in SEM-DIC mode, and sample 360° in Raman mode; a spatial common Cartesian coordinate system is constructed with the point o of the sample 0° image in SEM / EDS mode as the common reference coordinate origin and the sample short side direction as the x-axis; and independent Cartesian coordinate systems are constructed for the other three orientations, with the respective point o as the coordinate origin and the sample short side direction as the x-axis, and the data measured in each spatial coordinate system for each of these three orientations is transformed and merged without error into the common Cartesian coordinate system when the sample is 0° using formulas for angle transformation and translation transformation, thereby achieving spatial alignment; In the second and third data processing steps, data from six different sources, i.e., SEM images, EDS images, EBSD images, SEM-DIC images, Raman images, and force-displacement curves, which have been subjected to spatiotemporal alignment, are merged into one data source. A coordinate system is constructed using the scale lines etched during the sample preparation process, with point o as the coordinate origin, and each point in the rectangular area on the sample is assigned a clear coordinate (x ｉ , y ｉ ) and the data obtained by SEM, EDS, EBSD, SEM-DIC, and Raman are plotted as a function φ(t) = (z １ , z ２ , z ３ , z ４ , z ５ , t), and multi-source data is converted into W=(x ｉ , y ｉ , φ(t)), and by inputting the coordinate parameters (x, y) of any point in the sample relative to the origin o and the corresponding time t during the loading process, the micro-morphology, element distribution, crystal structure, strain distribution, corresponding molecular information and average stress of the sample at that point can be obtained, and the data processing method includes a fourth data processing step of independently and unifiedly analyzing the deformation damage and failure mechanism of the material under the force-thermal coupling action from five aspects.

Images