Scanning electron microscope multi-technology combined mechanical property in-situ testing device and analysis method

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 field of precision scientific instruments and material microscopic mechanical performance testing technologies, and particularly to a mechanical performance in-situ measurement device and analysis method by combining multiple technologies of a scanning electron microscope, a material in-situ measurement device by combining five types of detection technologies in a scanning electron microscope, and its sample preparation, testing and data processing methods, or a material in-situ measurement device and its sample preparation, testing and data processing methods, or a measurement device for a scanning surface electron microscope and the manufacturing, testing and data processing methods of a sample.

Background Art

[0002] Due to advantages such as good imaging three-dimensional effect, large imaging depth of field, wide field of view, and stepless adjustment of magnification, a scanning electron microscope (SEM) is widely applied to characterize the microstructure of materials. By integrating various types of detectors into a scanning electron microscope and utilizing the imaging characteristics of different detectors, microscopic morphology observation and analysis can be carried out across scales from macro to mesoscopic to microscopic for materials. Developing an in-situ test bench that can perform mechanics and high-temperature synchronous loading inside a scanning electron microscope is of great significance for studying the deformation damage and failure mechanism of materials due to the combined action of complex forces and thermal loading in actual use situations.

[0003] Based on the above characteristics, various mechanical performance in-situ test equipment under a scanning electron microscope has been developed at home and abroad. However, these equipment are only compatible with a single detector in the scanning electron microscope, and only one type of data among SEM / EBSD / SEM-DIC / Raman can be obtained in a single test, or more than four types of information of a batch of materials can be obtained through multiple tests, but four types of in-situ test information of important regions of the materials cannot be obtained simultaneously.

[0004] For example, five types of information, namely, the microscopic morphology (SEM), elemental content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) of a material under the combined action of force and heat, can be synchronously collected and subjected to fusion analysis. This is of great importance for profoundly revealing the deformation, damage, and failure mechanisms of the material at multiple levels under the combined action of force and heat. Therefore, it is of great significance to study a characterization method based on an in-situ test of the combined force and heat of the mechanical behavior of a material using five types of detection techniques in a scanning electron microscope.

Summary of the Invention

Problems to be Solved by the Invention

[0005] The objective of the present disclosure is to provide an in-situ measurement device and analysis method for mechanical properties using a multi-technology combination of a scanning electron microscope to solve the problems existing in the above-mentioned prior art. The mechanical loading of a sample is controlled by a tensile-compression loading unit, the angle of the sample is controlled by the rotation of the loading unit, the SE mode position and the Raman mode position are converted by a displacement platform, and various in-situ measurements of SEM, EDS, EBSD, SEM-DIC, and Raman on the sample in the scanning electron microscope can profoundly and comprehensively reveal the failure mechanism of the deformation and damage of the material, and provide a more novel technical means for scientifically establishing the relationship between the evolution of the material microstructure and the dynamic response of the macro performance under complex loads.

Means for Solving the Problems

[0006] To achieve the above objective, the present disclosure provides the following aspects.

[0007] The present disclosure includes a displacement platform and an in-situ testing machine attached to the displacement platform. The in-situ testing machine includes a fixture unit, a rotational loading unit, and a tensile-compressive loading unit. The fixture unit includes a driving fixture group and a driven fixture group. The driving fixture group and the driven fixture group are clamped at both ends of a sample. The tensile-compressive loading unit is used to drive the driving fixture group and the driven fixture group to move towards or away from each other. The displacement platform is used to move the sample to the SE mode position and the Raman mode position of a scanning electron microscope. The rotational loading unit drives the driving fixture group and the driven fixture group to rotate synchronously, and performs SEM, EDS, EBSD, SEM-DIC, and Raman in-situ measurements on samples at different angles while subjecting the samples to tensile-compressive loading, thereby providing a device for in-situ measurement of mechanical properties by combining multiple techniques of a scanning electron microscope. Preferably, the rotational loading unit includes a precision moment motor and a rotary ball spline. The rotary ball spline is provided with a driving gear and a driven gear. The driving gear and the driven gear can move along the axial direction of the rotary ball spline and rotate along with the rotation of the rotary ball spline. The driving fixture group includes a driving gear shaft meshing with the driving gear. The driven fixture group includes a driven gear shaft meshing with the driven gear. The driving gear shaft is connected to the precision moment motor. Preferably, the tensile-compressive 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 is connected to the driving fixture group, and the other offset loading nut seat is connected to the driven fixture group. A pair of the bidirectional ball screws is provided, and the ends realize synchronous rotation through gear meshing. The axial direction of the sample and the axis of the bidirectional ball screw are located in the same plane. Preferably, it includes a high-temperature loading unit, and the high-temperature loading unit includes a semi-circular winding core and a rotating heat conduction core. The rotating heat conduction core is wrapped outside the sample and rotates along with the rotation of the sample. The outer diameter side of the rotating heat conduction core is attached to the inner diameter side of the semi-circular winding core in a bonded manner, and the heat of the semi-circular winding core can be transmitted to the sample by the rotating heat conduction core at different angles of the sample. Preferably, a multi-layer heat insulation layer is provided outside the semi-circular winding core. The heat insulation layer is connected to a water-cooled plate with a flow path opened. The water-cooled plate is connected to a first water-cooling pipeline. The water-cooled plate is attached to the bottom plate of the in-situ tester through a heat insulation plate, and the offset loading nut seat is connected to a second water-cooling pipeline.

[0008] The present disclosure a first sample adjustment step of processing a measurement target material blank into a dumbbell-shaped sample with a uniform thickness, polishing the upper and lower surfaces of the sample, coating a paraffin film on the surface after there are no obvious scratches on the upper surface of the sample, polishing the lower surface of the sample until a mirror effect is achieved, and then immersing the sample in an electrolytic polishing solution to remove the lower surface oxide layer so that a clear pattern can be collected under EBSD, which is a second sample adjustment step, an ultrasonic cleaning of the sample, removing the paraffin film on the upper surface of the sample, and thoroughly cleaning and drying it, which is a third sample adjustment step, etching scale lines with a width of 10 μm at intervals of 5 mm on the upper and lower surfaces of the sample at the gauge segment edges, etching five mark points on each of the two surfaces, denoted as o, a, b, c, d and o′, a′, b′, c′, d′ respectively, and corresponding two positions to each other to serve as characteristic mark points for spatial alignment, which is a fourth sample adjustment step, and a fifth sample adjustment step of making a speckle pattern diagram for SEM-DIC analysis on the lower surface of the sample. A sample preparation method for preparing a sample of the mechanical property in-situ measurement device using a combination of scanning electron microscope multi-techniques as described above is provided. Preferably, in the first sample adjustment step, both side surfaces of the sample are polished until they have a good adhesion with the inner groove surface of the rotary heat conduction core, reducing the contact thermal resistance between the sample in vacuum and the rotary heat conduction core. In the fifth sample adjustment step, Al2O3 powder with a particle size of 500 μm is dissolved in absolute ethanol by ultrasonic vibration for 5 minutes, the turbid solution is allowed to stand for 3 minutes, the upper clear liquid is taken into the upper pot of the airbrush, the magnitude of the air flow and the spray distance are adjusted, the Al2O3 solution is uniformly sprayed on the lower surface of the sample, the sample is placed in an oven to dry, and the uniformly distributed Al2O3 particles are used as a speckle pattern diagram.

[0009] The present disclosure A first measurement step of attaching the sample to the jig unit, evacuating the scanning electron microscope, adjusting the tungsten filament current for clear imaging, adjusting the observation mode switching software, rotating the jig unit to four states of 0°, 70°, 180°, and 360° of the sample for angle adjustment initialization, moving the sample from the pole piece under the Raman objective lens and then back to the original position for position adjustment initialization, and recording the corresponding spatial coordinate parameter A0 of the in-situ tester. S2. A second measurement step of setting the tensile / compression speed and loading displacement parameters in the mechanical loading interface, stopping the loading after reaching the applied target value, and recording the current time while maintaining the set mechanical loading until the end. Operating the observation mode switching software, moving the sample under the pole piece and rotating it to 0°, recording the spatial state information of the in-situ tester as A1, selecting the SE mode, controlling and sequentially operating various detectors using the scanning electron microscope imaging software, acquiring the in-situ tensile / compression SEM and EDS images near the o point on the upper surface of the sample, and recording the corresponding acquisition time. Maintain the position of the original position tester unchanged, rotate the sample by 70°, record the spatial state information of the original position tester as A2, obtain the original position tensile / compression EBSD crystal structure information near point o on the upper surface of the sample, then rotate the sample by 180°, obtain the speckle distribution SEM image near o' on the lower surface of the sample, record the spatial state information of the original position tester as A3, and record the corresponding image acquisition time in the fourth measurement step; Move the displacement platform, move the sample under the Raman objective lens and rotate it to 0°, select the Raman mode, control the Raman system imaging, obtain the Raman image near point o on the upper surface of the sample, record the spatial state information of the original position tester as A4, and record the acquisition time in the fifth measurement step; Apply the spatial state information A1 to the observation mode switching software, adjust the original position tester to the initial observation state, set the loading parameters again, and after the loading is completed, repeat steps S3, S4, and S5 to obtain the second group of five types of original position observation data in the sixth measurement step; Repeat steps S3, S4, S5, and S6 until the sample breaks, output the force-displacement curve of the sample recorded by the original position loading control software, input the obtained speckle distribution SEM image into the Vic-2D processing software, and calculate the strain distribution on the lower surface of the sample. Provide a measurement method using the mechanical performance in-situ measurement device with combined multi-techniques of the scanning electron microscope as described above. Preferably, in the second measurement step, first input the test target temperature into the temperature loading interface of the original position loading control software. After the monitored temperature of the sample reaches the set value, set the subsequent contents of the tensile / compression speed and loading displacement parameters to realize the force-thermal coupling effect on the sample.

[0010] In the first data processing step, sort out various types of microscopic images and acquisition times obtained during the matching test, determine that the acquisition area of the sample is located in the gauge segment of the sample, and map the obtained images one by one to the force-time curve; Collect the acquisition times of the force-displacement curve, SEM image, EDS image, EBSD image, SEM-DIC image, and Raman image obtained asynchronously, perform time alignment, and use the linear interpolation method to convert the data obtained by five types of detectors with low acquisition frequencies to the time nodes of the force-displacement curve with a high sampling frequency. This is the second data processing step. Extract the initial images of the sample without tension in four postures: 0° of the sample in SEM / EDS mode, 70° of the sample in EBSD mode, 180° of the sample in SEM-DIC mode, and 360° of the sample in Raman mode. Use the o point of the 0° sample image in SEM / EDS mode as the common reference coordinate origin, set the short side direction of the sample as the x-axis, and construct a common spatial rectangular coordinate system. Under the other three postures, use each o point as the coordinate origin, set the short side direction of the sample as the x-axis, and construct independent rectangular coordinate systems respectively. Utilize the formulas for angle conversion and translation transformation to convert and fuse the data measured in their own spatial coordinate systems to the common rectangular coordinate system at 0° of the sample without error under these three postures, thereby realizing spatial alignment. This is the third data processing step. In the second and third data processing steps, fuse the six types of data from different sources that have undergone spatio-temporal alignment into one data source. Use the etched scale lines in sample preparation to construct a coordinate system with the o point as the coordinate origin, and assign clear coordinates (x i , y i ) to each point on the gauge segment of the sample. Convert the data obtained by SEM, EDS, EBSD, SEM-DIC, and Raman into a function φ(t) = (z1, z2, z3, z4, z5, t) related to time t, and fuse the multi-source data into W = (x i , y i , φ(t)). When 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 microscopic morphology, element distribution, crystal structure, strain distribution, corresponding molecular information, and average stress of the sample at that point can be obtained, and the deformation damage and failure mechanism of the material under the coupled action of force and heat are independently and uniformly analyzed from five aspects. This is the fourth data processing step. A data processing method is provided, characterized by including the above steps.

Advantages of the Invention

[0011] The present disclosure achieves the following technical effects over the prior art. For the conventional in-situ measurement of mechanical properties under a scanning electron microscope, only local area information can be obtained by a single detector, or material damage information at different times of different parts can be obtained by multiple detectors. It is difficult to synchronously, isotropically, and multi-dimensionally acquire the drawbacks of the microscopic behavior of the key areas of material deformation, damage, and failure. In contrast, an in-situ mechanical property measurement device using a combination of multiple scanning electron microscope techniques is provided. When applying tensile and compressive forces to a sample, the position of the in-situ testing machine with respect to the pole piece (SE mode position) and the Raman objective lens (Raman mode position) is adjusted to realize the switching between the SE mode and the Raman mode. The angle of the sample is controlled by a rotary loading unit, and the relative angle between the sample and the pole piece is adjusted to meet the imaging requirements of three different observation modes: SEM / EDS, SEM-DIC, and EBSD. The microscopic morphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) of a specific area under the mechanical action of the sample are obtained to comprehensively and profoundly reveal the deformation, damage, and failure mechanism of the material, and to scientifically establish the relationship between the evolution of the material microstructure and the dynamic response of the macro performance under complex loads, a more novel technical means is provided. The present disclosure can further install a high-temperature loading unit, apply high temperature simultaneously while applying tensile and compressive forces to the sample, and can conduct a comprehensive and profound study on the deformation, damage, and failure mechanism of the material under the coupled action of force and heat. By designing a specific data processing method, the present disclosure can fuse and analyze data such as microscopic morphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) through spatio-temporal alignment, and plays an important role in comprehensively and profoundly revealing the deformation, damage, and failure mechanism of the material under the coupled action of force and heat.

Brief Description of the Drawings

[0012]

Figure 1

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Figure 13

[0013] To more clearly explain the technical solutions in the embodiments or the prior art of the present disclosure, the drawings necessary for use in the embodiments are 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 creative labor. Here, 1. EBSD detector, 2. EDS detector, 3. SE detector, 4. pole piece, 5. Raman objective lens, 6. in-situ tester, 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, 646. second thrust ball bearing, 647. driven gear, 648. first thrust ball bearing, 649. rotating ball spline, 65. high-temperature loading unit, 651. first water-cooling pipe, 652. sample, 653. semi-circular winding core, 654. driving jig body, 655. spring, 656. heat insulation layer, 657. water-cooling plate, 658. heat insulation 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.

Embodiments for Carrying Out the Invention

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

[0015] The objective of the present disclosure is to provide a device and an analysis method for in-situ measurement of mechanical properties by using a multi-technology combination of a scanning electron microscope to solve conventional problems. The scanning electron microscope is a scanning electron microscope, and the multi-technology combination refers to the combination of five types of detection technologies. The five types of detection technologies include 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. The present disclosure controls the mechanical loading of the sample by a tensile compression loading unit, controls the angle of the sample by a rotational loading unit, converts the SE mode position and the Raman mode position by a displacement platform, and can perform various in-situ measurements of SEM, EDS, EBSD, SEM-DIC, and Raman on the sample in the scanning electron microscope, can comprehensively and profoundly reveal the deformation damage failure mechanism of the material, and provides a more novel technical means for scientifically establishing the relationship between the evolution of the material microstructure and the dynamic response of the macro performance under complex loads.

[0016] To make the above objectives, features, and advantages of the present disclosure clearer and more understandable, the present disclosure will be further described in detail below in combination with the accompanying drawings and specific embodiments.

[0017] As shown in FIGS. 1, 2 to 7, the present disclosure provides a device for in-situ measurement of mechanical properties by using a multi-technology combination of a scanning electron microscope, including 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, and the displacement platform can move the position of the in-situ testing machine 6 and convert it at different mode positions. The in-situ testing machine 6 includes a jig unit, a rotational loading unit, and a tensile-compressive loading unit 61. Here, the jig unit includes a driving jig group 66 and a driven jig group 64. The driving jig group 66 and the driven jig group 64 are clamped at both ends of the sample 652. The tensile-compressive loading unit 61 is used to drive the driving jig group 66 and the driven jig group 64 to move towards or away from each other, and is further used to realize the loading of compressive force and tensile force on the sample 652. The displacement platform can move the sample 652 to the SE mode position, which is the pole piece of the scanning electron microscope 8, 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 rotational loading unit drives the driving jig group 66 and the driven jig group 64 to rotate synchronously, adjusts the imaging angle between the sample 652 and five types of detectors, and can perform SEM, EDS, EBSD, SEM-DIC, and Raman in-situ tests on the sample at different angles while applying tensile-compressive loading to the sample.

[0018] The scanning electron microscope 8 uses a tungsten filament scanning electron microscope 8, and the scanning electron microscope 8 includes five types of detectors: an EBSD detector 1 (receiver), an EDS detector 2 (receiver), an SE detector 3 (receiver), a pole piece 4 (transmission source), and a Raman objective lens 5 (both a transmission source and a receiver). By moving the in-situ tester 6 on the X-direction displacement platform 71 and the Y-direction displacement platform 72 in the Y direction, the sample 652 can be positioned under the pole piece 4 or under the Raman objective lens 5, and the switching between the SE mode and the Raman mode can be completed. The imaging principle is that an electron beam is emitted from the pole piece 4, incident on the surface of the sample 652, exciting the surface of the sample 652 to generate secondary electrons. The secondary electrons are received by the SE detector 3, processed to obtain an SEM image. The secondary electrons are received by the EBSD detector 1, processed to obtain an EBSD image. The secondary electrons are received by the EDS detector 2, processed to obtain an EDS image. On the other hand, based on the obtained SEM image, the SEM-DIC image is obtained through post-processing, that is, by identifying the pixel changes in multiple images before and after, through VIC-2D software processing, a series of mechanics, mathematics, and finite element calculations are performed to obtain the strain distribution of the sample 652, that is, the so-called SEM-DIC image. However, for metal materials, grinding and buffing are often performed. In the case of SEM-DIC software processing, since there are no characteristic points, the corresponding changes cannot be accurately identified, so it is necessary to artificially spray speckle particles. In order to simultaneously observe the microscopic morphology and strain distribution (SEM-DIC image information) of one region on one sample 652, the microscopic morphology can be observed on one surface of the sample 652, speckle particles can be sprayed on the other surface, the SEM image of that surface can be obtained, processed, and then the SEM-DIC image can be obtained. Therefore, it is necessary to complete the rotation of the sample 652. That is, in the SEM mode, the sample 652 is at 0°, and in the SEM-DIC mode, the sample 652 is at 180°.

[0019] In contrast to the in-situ measurement of mechanical properties under a conventional scanning electron microscope 8, with a single detector, only local area information can be obtained, or with multiple detectors, material damage information at different times in different parts can be obtained. It is difficult to synchronously, isotropically, and multi-dimensionally acquire the drawbacks of the microscopic behavior of the key regions of material deformation, damage, and failure. Therefore, a device for in-situ measurement of mechanical properties by combining multiple technologies of a scanning electron microscope is provided. When applying tensile and compressive forces to the sample 652, in order to realize the switching between the SE mode and the Raman mode, the position between the pole piece 4 (SE mode position) of the in-situ testing machine 6 and the Raman objective lens 5 (Raman mode position) can be adjusted. The angle of the sample 652 is controlled by a rotational loading unit, and the relative angle between the sample 652 and the pole piece 4 is adjusted to meet the imaging requirements of three different observation modes: SEM / EDS, SEM-DIC, and EBSD. The microscopic morphology (SEM), element content and distribution (EDS), strain distribution (SEM-DIC), crystal structure (EBSD), and molecular information (Raman) of a specific region under the mechanical action of the sample 652 are acquired to comprehensively and profoundly reveal the deformation, damage, and failure mechanism of the material.

[0020] As shown in FIGS. 3 to 6, the rotary loading unit includes a precision moment motor 67 and a rotary ball spline 649, and the axial direction of the rotary ball spline 649 is arranged parallel to the axial direction of the sample 652. A drive gear (not shown, the structure is the same as that of the driven gear 647) and a driven gear 647 are provided on the rotary ball spline 649. Taking the driven gear 647 as an example, the driven gear 647 fits into the spline groove of the rotary ball spline 649 and cannot rotate relatively, but can move axially relatively. The rotary ball spline 649 is supported via a first thrust ball bearing 648, that is, 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 in the axial direction of the rotary ball spline 649 and rotate along with the rotation of the rotary ball spline 649. The drive jig group 66 includes a drive gear shaft that meshes with the drive gear, and the driven jig group 64 includes a driven gear shaft 642 that meshes with the driven gear 647. The drive gear shaft is connected to the precision moment motor 67. When the precision moment motor 67 drives the rotation of the drive gear shaft, the rotation of the drive gear can be driven through the drive gear shaft. The rotation of the drive gear can drive the rotation of the rotary ball spline 649. The rotation of the rotary ball spline 649 can drive the rotation of the driven gear 647. The rotation of the driven gear 647 can drive the rotation of the driven gear shaft 642, and further drive the rotation of the driven jig group 64. Finally, the synchronous rotation of the drive jig group 66 and the driven jig group 64 can be realized by using the precision moment motor 67. Thereby, the sample 652 can be rotated in a plane without screwing, and the test accuracy can be improved. In addition, the drive jig group 66 and the driven jig group 64 can perform the axial tension operation of the sample 652 and the rotation of the sample 652 synchronously, without interfering with each other and without affecting each other. Therefore, the in-situ tester 6 can adjust the observation angle simultaneously during mechanical loading.

[0021] The rotation angle of the sample 652 can be adjusted by the observation mode switching software. The software reads the angle between the jig unit and the horizontal reference of the in-situ tester 6 through the 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 rotates to 0°, imaging of the SE detector 3 and the EDS detector 2 is possible; when it rotates to 70°, imaging of the EBSD detector 1 is possible; when it rotates to 180°, SEM-DIC imaging is possible; and when it rotates to 360°, imaging of the Raman objective lens 5 is possible.

[0022] As shown in FIGS. 5 and 6, the tensile-compressive loading unit 61 includes a bidirectional ball screw 611 and an offset loading nut seat 63 as a pair attached to the bidirectional ball screw 611. When the bidirectional ball screw 611 rotates, the offset loading nut seat 63 can move synchronously in the axial direction either towards or away from each other. One offset loading nut seat 63 is connected to the driving jig body 654 of the driving jig group 66, and the other offset loading nut seat 63 is connected to the driven jig body 641 of the driven jig group 64. When the offset loading nut seat 63 moves axially, it drives the driving jig group 66 and the driven jig group 64, and can realize the loading of tensile force or compressive force on the sample 652 in the axial direction. A pair of the bidirectional ball screws 611 is provided, and the ends rotate synchronously by the meshing of gears, and the ends realize synchronous rotation by the meshing of gears, and further realize the stable driving of the offset load nut seat 63 in the axial direction. The tensile-compressive loading unit 61 may include a DC brushless motor. The DC brushless motor is connected to a two-stage reduction mechanism, and power is transmitted to the bidirectional ball screw 611 through the two-stage reduction mechanism, and the offset nut seat 63 can drive the relative movement between the driving jig group 66 and the driven jig group 64. The two-stage reduction mechanism may include a planetary gear and a worm wheel. The DC brushless motor transmits the power reduction torque to the meshing worm wheels through a pair of planetary gears, and the two synchronously rotating worm wheels synchronously rotate the bidirectional ball screw 611 attached to the offset load nut seat 63, and slide the offset load nut seat 63 along two parallelly attached linear guides. The axial direction of the sample 652 and the axis of the bidirectional ball screw 611 can be located in the same plane. At the same time, the axial direction of the linear displacement precision measurement unit 62 can also be located in this plane. The tensile-compressive loading unit 61 can effectively avoid the inaccurate displacement measurement caused by the poor device rigidity and large overturning moment when applying a large loading.

[0023] As shown in FIG. 6, a precision tensile-compressive force sensor 645 is also provided. A rotary connecting shaft 644 is connected to the driven gear shaft 642, and the two can rotate synchronously. The rotary connecting shaft 644 is rotatably connected into the sleeve via a pair of reversely mounted second thrust ball bearings 646. A needle bearing 643 is provided on the outer diameter side of the sleeve. The needle bearing 643 is mounted in the mounting hole of the driven jig body 641. The sleeve is connected to the precision tensile-compressive force sensor 645, and the circumferential angle between the fasteners is positioned by a fastening screw. When the driven gear shaft 642 rotates the driven jig group 64, the axial tensile-compressive force is transmitted to the precision tensile-compressive force sensor 645 via the rotary connecting shaft 644. However, the circumferential rotation of the rotary connecting shaft 644 is transmitted to the inner ring of the second thrust ball bearing 646, and the precision tensile-compressive force sensor 645 can measure the axial loading of the sample 652, ensuring that it is not accompanied by the rotation of the sample 652 about its axis. That is, the driven jig group 64 is installed coaxially with the precision tensile-compressive force sensor 645 but is not coaxially connected. When the driven jig group 64 rotates the sample 652, the precision tensile-compressive force sensor 645 can be held so as not to rotate, and the measurement of the precision tensile-compressive force sensor 645 can be prevented from being affected.

[0024] As shown in FIGS. 5 and 7, a high-temperature loading unit 65 for heating the sample 652 at a high temperature and a high-temperature loading unit 65 that can apply a temperature loading of room temperature to 1000° C. to the sample 652 and heat while following the rotation of the sample 652 are included. The high-temperature loading unit 65 can load a high-temperature loading in real time during the processes of mechanical loading and beam current observation angle adjustment, and can apply a high temperature synchronously when applying a tensile and compressive force to the sample 652, and can apply a thermo-mechanical coupling action to the sample 652. Furthermore, a comprehensive and in-depth study can be conducted on the deformation, damage, and failure mechanisms of the material under the thermo-mechanical coupling action. By setting the in-situ tensile mechanics and temperature loading parameters in the control software, accurate control of the loading displacement, loading speed, and loading force of the sample 652 can be achieved through PID. Specifically, the high-temperature loading unit 65 may include a semi-circular winding core 653 and a rotating heat conduction core 659. The semi-circular winding core 653 is wound with a Nichrome wire for heating. The rotating heat conduction core 659 is wound around the outside of the sample 652 and rotates as the sample 652 rotates. The outer diameter side of the rotating heat conduction core 659 is attached by being bonded to the inner diameter side of the semi-circular winding core 653. At different angles of the sample 652, the rotating heat conduction core 659 can transfer the heat of the semi-circular winding core 653 to the sample 652, and a good heat conduction effect can be maintained even when the sample 652 is at different rotation angles.

[0025] Furthermore, outside the semi-circular winding core 653, a multi-layer heat insulation layer 656, for example, a heat insulation layer 656 with three layers of stainless steel material, is provided, effectively suppressing the influence of thermal radiation on the imaging effect of the detector. The heat insulation layer 656 is connected to a water-cooled plate 657 with an open flow path. The water-cooled plate 657 is connected to a first water-cooling pipe 651. The first water-cooling pipe 651 adopts a welded water-cooling pipe, and the welded water-cooling pipe is welded to the water-cooled plate 657 to send a cooling medium to the water-cooled plate 657, water-cool the water-cooled plate 657, and reduce the thermal influence on other components on the bottom plate of the in-situ tester 6 from high temperature. The water-cooled plate 657 can be made of a copper material with good thermal conductivity. The water-cooled plate 657 is attached to the bottom plate of the in-situ tester 6 via a heat insulation plate 658, and the heat insulation plate 658 can use a carbon fiber material. A spring 655 is provided between the water-cooled plate 657 and the heat insulation plate 658. By adjusting the height at which the spring 655 is attached, the height of the screw can be changed, the relative height and the contact heat transfer area between the semi-circular winding core 653 and the rotary heat conduction core 659 can be adjusted, and furthermore, the heating effect on the sample 652 can be adjusted. A second water-cooling pipe 631 is connected to the offset loading nut seat 63. The second water-cooling pipe 631 may use an interference-fit water-cooling pipe. The interference-fit water-cooling pipe is connected to the offset loading nut seat 63, and the temperature of the offset loading nut seat 63 can be reduced. An annular flow path is opened in the bearing hole for attaching 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, reducing the influence of the temperature rise of the jig unit on the accuracy of the precision tensile compression force sensor 645 and the precision moment motor 67. The purpose of opening the annular flow path in the offset loading nut seat 63 is to lower the temperature of the jig unit and the bearing by cooling the cooling medium, and avoid heat being transferred to the precision tensile compression force sensor 645 during the high-temperature loading process and affecting its measurement accuracy.

[0026] The stainless steel corrugated tube 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 through a four-way joint, and the screw joint is secondarily sealed by brazing so that the pipeline does not leak even under a pressure within 0.5 MPa.

[0027] The driving jig group 66 and the driven jig group 64 move relatively to realize the tension / compression of the sample 652. While the sample 652 is being tensioned / compressed, the precision moment motor 67 rotates the driving jig group 66 around the axis, and further drives the rotation of the rotating ball spline 649 connected to the driven jig group 64 and the driving jig group 66 to ensure the synchronous rotation of the driving jig group 66 and the driven jig group 64. The rotating heat conduction core 659 contacts the sample 652 and the semi-circular winding core 653, and rotates simultaneously when the driving jig group 66 and the driven jig group 64 rotate around the axis, transferring heat from the semi-circular winding core 653 to the sample 652, so that high-temperature loading can be applied to the sample 652.

[0028] As shown in FIGS. 1, 8 and 9, the present disclosure provides a sample preparation method for preparing the sample 652 of the mechanical performance in-situ measurement device by using the multi-technology combination of the scanning electron microscope described above. The prepared sample 652 has good surface smoothness and clear surface texture, and can simultaneously meet the imaging conditions of EBSD and SEM-DIC. It includes the following contents. S1. Use a laser cutter to process the measurement target material blank into a dumbbell-shaped sample 652 with a uniform thickness, and polish both side surfaces of the sample 652 with waterproof abrasive paper until they have good adhesion to the inner groove surface of the rotating heat conduction core 659, so as to reduce the contact thermal resistance between the sample 652 in vacuum and the rotating heat conduction core 659. S2. Using a metal tissue sample grinder and polisher, polish the upper and lower surfaces of the dumbbell-shaped sample 652. Continuously increase the grit size of the waterproof abrasive paper and alternately polish the upper and lower surfaces of the sample 652. After polishing the upper surface of the sample 652 with 5000# abrasive paper until there are no obvious scratches, coat the paraffin film on its surface. Continue to polish the upper surface of the sample 652, replace the sandpaper with polishing cloth, and continuously apply a polishing paste with a small particle size until a mirror effect appears. Then, immerse it in an electrolytic polishing solution to remove the oxide layer on the lower surface of the sample 652 so that a clear pattern can be collected under EBSD. S3. Immerse the sample 652 in a solution of turpentine oil heated in a water bath, perform ultrasonic cleaning to remove the paraffin film on the upper surface of the sample 652, wash it with anhydrous ethanol, and dry it. S4. Using a femtosecond laser, etch scale lines with a width of 10 μm at intervals of 5 mm on the edges of the gauge segment on the upper and lower surfaces of the sample 652 to finish, and calibrate the coordinates of each point of the gauge segment of the sample. Then, etch five marking points on each of the two surfaces, denoted as o, a, b, c, d and o', a', b', c', d', and make their positions correspond in pairs to be characteristic marking 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 turbid solution stand for 3 minutes, take the upper-layer clear liquid into the pot on the airbrush, adjust the magnitude of the air flow and the spraying distance, spray the Al2O3 solution evenly on the lower surface of the sample 652, place the sample 652 in an oven to dry, and use the uniformly distributed Al2O3 particles as a speckle pattern diagram for SEM-DIC analysis.

[0029] As shown in FIGS. 1 and 10, the present disclosure provides a test method using the mechanical performance in-situ measurement device by combining multi-techniques of the scanning electron microscope as described above, including the following content. S1. Adjust the distance between the driving jig group 66 and the driven jig group 64, attach the sample 652 to the jig unit, make the sample 652 adhere to the inner groove surface of the rotary heat conduction core 659, evacuate the scanning electron microscope 8, adjust the tungsten filament current for clear imaging, adjust the observation mode switching software, rotate the jig unit to four states of 0°, 70°, 180°, and 360° of the sample, perform the initialization of the angle adjustment, move the sample 652 from the pole piece 4 under the Raman objective lens 5 and then back to the original position, perform the initialization of the position adjustment, and record the corresponding spatial coordinate parameter A0 of the original position tester 6. S2. Input the experimental target temperature into the temperature loading interface of the in-situ high-temperature mechanical loading meter control software such as In-Situ Thermomechanical Pro. After the monitored temperature of the sample 652 reaches the set value, set the tensile / compression speed and loading displacement parameters in the mechanical loading interface, apply them until the target value is reached, then stop the 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 original position tester 6 as A1, select the SE mode, control and operate various detectors in sequence using the scanning electron microscope imaging software, obtain the in-situ high-temperature tensile / compression SEM and EDS images near the o point on the upper surface of the sample 652, and record the corresponding acquisition time. S4. Keep the position of the original position tester 6 unchanged, rotate the sample 652 to 70°, record the spatial state information of the original position tester 6 as A2, obtain the in-situ high-temperature tensile / compression EBSD crystal structure information near the o point on the upper surface of the sample 652, then rotate the sample 652 to 180°, obtain the speckle distribution SEM image near the o' point on the lower surface of the sample 652, record the spatial state information of the original position tester 6 as A3, and record the corresponding image acquisition 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, rotate it to 0°, select the Raman mode, control the Raman system imaging, obtain the Raman image near point o on the upper surface of the sample 652, record the spatial state information of the in-situ testing machine 6 as A4, and record the sampling time. S6. Apply the spatial state information A1 to the observation mode switching software, such as In-Situ PolyMode MicroImager, adjust the in-situ testing machine 6 to the initial observation state, set the loading parameters again, and after the loading is completed, repeat the above steps S3, S4, S5 to obtain the second group of 5 types of in-situ observation data under the coupled thermo-mechanical action. S7. Repeat the above steps S3, S4, S5, S6 until the sample 652 breaks, output the force and displacement curve of the sample 652 recorded in the in-situ loading control software, input the obtained speckle distribution SEM image into the Vic-2D processing software, and the software compares the relative change information of the fine structure feature forms in two adjacent SEM images, performs multiple spline interpolations on the data obtained from the images using the incremental correlation criterion, and calculates the strain distribution on the lower surface of the sample 652.

[0030] As shown in FIGS. 1, 11 to 13, the present disclosure provides a data processing method for processing the data obtained by the aforementioned test method, fuses and analyzes five types of asynchronous microscopic data at different positions of the sample 652 obtained by five types of detectors at different collection times, and provides a deformation, damage and failure mechanism of the material due to the coupled thermo-mechanical action by multi-faceted and multi-source analysis. It includes the following content. S1. According to the timing of collecting various types of microscopic images obtained during the experiment process, arrange them, determine the absolute time in space-time at the sampling time of each of the five types of microscopic data obtained, process the imaging area of the inconsistent dimensions due to the differences in the imaging principles of the five types of detectors, prepare the marked points o, a, b, c, d and o′, a′, b′, c′, d′ etched on the sample 652, determine the area of different observation regions and the corresponding spatial coordinates in the sample 652 gauge segment, and then map each of the obtained images one by one to the force-time curve and displacement-time curve collected in the in-situ high-temperature thermodynamic loading control software. S2. Align the collection times of the five types of microscopic data such as SEM images, EDS images, EBSD images, SEM-DIC images, and Raman images obtained asynchronously before and after in step S1 with the force-displacement curve, and convert the data obtained by the five types of detectors with low collection frequencies to the time nodes of the force-displacement curve with a high sampling frequency by the least common multiple method of time coordinates. The time alignment of the corresponding five types of detectors can be performed as follows.

[0031] Estimate the observation data obtained by the five types of detectors of SEM, EDS, EBSD, SEM-DIC, and Raman processed in step S1 on the observation array of the force-time curve, and explain an example of converting the observation data of SEM to the force-time curve. The observation time [t a (n - 1), t a (n)] on the force-time curve includes the collection time t b (m - 1) of SEM, and the observed value at the time t a (n - 1) of the force-displacement curve is (x a (n - 1), y a (n - 1), z a (n - 1)), and the observed value at the time t a (n) is (x a (n), y a (n), z a (n)). By linear interpolation, the observed data (x b (m), y b (m), z b (m), z b(m)) is obtained. It is as follows.

[0032]

Number

[0033] S3. Extract the initial images of the sample without tension in four postures of 0° of the sample in SEM / EDS mode, 70° of the sample in EBSD mode, 180° of the sample in SEM-DIC mode, and 360° of the sample in Raman mode processed in step S1. All four types of photos use the etching mark point o of the sample as the coordinate origin. With the o point of the sample at 0° in SEM / EDS mode as the common reference coordinate origin and the short side direction of the sample as the x-axis, a common spatial rectangular coordinate system was constructed. For the other three postures, with each o point as the coordinate origin and the short side direction of the sample as the x-axis, their respective rectangular coordinate systems were constructed. Using the formulas for angle conversion and translation transformation, under these three postures, the data measured in their own spatial coordinate systems was transformed and fused into the common rectangular coordinate system of the sample at 0° without error to achieve spatial alignment. The spatial alignment for the corresponding four spatial postures can be performed as follows.

[0034] An example of aligning 70° of the sample in EBSD mode with 0° of the sample in SEM / EDS mode will be described. For the coordinate systems of the three mutually perpendicular unit vectors of the sample at 70° in EBSD mode and the sample at 0° in SEM / EDS mode, they are respectively {e xk , e yk , e zk} and {e x'k , e y'k , e z'k}, and the rotation angles of the three coordinate axes of e x' ke y'k e z'k coordinate system and the spatial coordinate system oe xk e yk e zk are respectively φ x'k , η y'k , and φ z'k between e k , η k and φ kand the coordinate vectors of the two postures 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 the two is defined as follows.

[0035]

Number

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

[0037]

Number

[0038] In the Raman mode, it is also necessary to perform a translational transformation along the coordinate system. The translational vector from the coordinate system of the sample at 180° to the common coordinate system of the sample at 0° in the SEM / EDS mode in the Raman mode is T ab =(t x , t y , t z ) T , where the coordinate vector after the rotational transformation of the sample at 180° with respect to the sample at 0° is R b ′, and the coordinates of the sample in the common coordinate system in the Raman mode are as follows.

[0039]

Number

[0040] Thus, the spatial alignment of the observation data between the two types of detectors is completed.

[0041] S4. Fuse the data from six different sources, namely the SEM images, EDS images, EBSD images, SEM-DIC images, Raman images, and macro force-displacement curves that are spatio-temporally aligned in steps S2 and S3, into one data source. Construct a coordinate system with point o as the origin using the scale lines etched during the preparation process of sample 652, and the initial time point t a (0) corresponding to the spatial orientation P of the sample at 0° in the SEM / EDS mode k =(x k ,y k ,z k ) as the initial time zero point and spatial zero point, and the temporally aligned t b (m) time observation data (x b (m),y b (m),z b (m)), and the spatial coordinates P ab ' obtained by five types of detectors at the corresponding time when the spatial alignment is completed in step S3 are fused. Here, in the observation region of the sample gauge segment, there are corresponding coordinates (x i ,y i ) of the origin o corresponding to each point, and the spatial coordinates based on the common reference coordinate system in the five modes of SEM, EDS, EBSD, SEM-DIC, and Raman at time t n are z1 = P ab1 ', z2 = P ab2 ', z3 = P ab3 ', z4 = P ab4 ', z5 = P ab5 ' respectively. Also, z1, z2, z3, z4, z5 are functions of time t, and (x i ,y i ) i.e., φ(t) = (z1, z2, z3, z4, z5, t), and the multi-source data fusion of each point in sample 652 is W = (x i ,y i, φ(t)). By inputting the coordinate parameters (x, y) of any point of the sample 652 with respect to the origin o and the corresponding time t during the loading process, the microscopic morphology, elemental distribution, crystal structure, strain distribution, corresponding molecular information, and average stress of the sample 652 at that point can be obtained, and the deformation damage and failure mechanism due to the force-thermal coupling of the material can be analyzed independently and uniformly from five aspects.

[0042] The present disclosure is described in detail from four aspects, such as a device for in-situ measurement of mechanical properties by combining multiple techniques of a scanning electron microscope, a sample preparation method, a test method, and a data processing method. Overall, a method for characterizing the force-thermal coupling in-situ test of the mechanical behavior of materials by combining five types of detection techniques in a scanning electron microscope is described. After the above series of processes, finally, sample information after fusing five types of data can be obtained, and it is profoundly and comprehensively revealed that it plays an important role in the deformation, damage, and failure mechanism of materials under the action of force-thermal coupling.

[0043] Specific examples are used in the present disclosure to describe the principles and embodiments of the present disclosure. However, the description of the above examples is only for helping to understand the method and its core idea of the present disclosure. At the same time, those skilled in the art will have changes in specific embodiments and application scopes based on the idea of the present disclosure. As described above, the content of this specification should not be understood as a limitation to the present disclosure.

Claims

1. A device for in-situ measurement of mechanical properties by using a combination of multiple technologies of a scanning electron microscope, comprising: a displacement platform and an in-situ testing machine attached to the displacement platform, the in-situ testing machine includes a jig unit, a rotational loading unit, and a tensile-compressive loading unit, the jig unit includes a driving jig group and a driven jig group, the driving jig group and the driven jig group are clamped at both ends of a sample, the tensile-compressive loading unit is used to drive the driving jig group and the driven jig group to move towards each other or in opposite directions, the displacement platform is used to move the sample to the SE mode position and the Raman mode position of the scanning electron microscope, the rotational loading unit drives the driving jig group and the driven jig group to rotate synchronously, and SEM, EDS, EBSD, SEM-DIC, and Raman in-situ measurements are respectively performed on samples at different angles while the sample is under tensile-compressive loading. A device for in-situ measurement of mechanical properties by using a combination of multiple technologies of a scanning electron microscope, characterized in that.

2. The rotational loading unit includes a precision moment motor and a rotary ball spline, a driving gear and a driven gear are provided on the rotary ball spline, the driving gear and the driven gear can move along the axial direction of the rotary ball spline and rotate along with the rotation of the rotary ball spline, the driving jig group includes a driving gear shaft meshing with the driving gear, the driven jig group includes a driven gear shaft meshing with the driven gear, and the driving gear shaft is connected to the precision moment motor. The device for in-situ measurement of mechanical properties by using a combination of multiple technologies of a scanning electron microscope according to Claim 1, characterized in that.

3. The tensile-compressive 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 is connected to the driving jig group, and the other offset loading nut seat is connected to the driven jig group. A pair of bidirectional ball screws is provided, and synchronous rotation is realized by the meshing of gears at the ends. The axial direction of the sample and the axis of the bidirectional ball screw are located in the same plane. The device for in-situ measurement of mechanical properties by using a combination of multiple technologies of a scanning electron microscope according to Claim 2, characterized in that.

4. A high-temperature loading unit is included, and the high-temperature loading unit includes a semi-circular bobbin and a rotating heat conduction core. The rotating heat conduction core is wrapped around the outside of the sample and rotates as the sample rotates. The outer diameter side of the rotating heat conduction core is attached by being bonded to the inner diameter side of the semi-circular bobbin. The heat of the semi-circular bobbin can be transmitted to the sample by the rotating heat conduction core at different angles of the sample. The mechanical property in-situ measurement device using a combination of multiple technologies of a scanning electron microscope according to claim 3, characterized in that.

5. A multi-layer heat insulation layer is provided on the outside of the semi-circular winding core. The heat insulation layer is connected to a water-cooled plate with an open flow path. The water-cooled plate is connected to a first water-cooling pipeline. The water-cooled plate is attached to the bottom plate of the in-situ testing machine through a heat insulation plate. The offset loading nut seat is connected to a second water-cooling pipeline. The mechanical property in-situ measurement device using a combination of multiple technologies of a scanning electron microscope according to claim 4, characterized in that.

6. A sample preparation method for preparing a sample of the mechanical property in-situ measurement device using a combination of multiple technologies of a scanning electron microscope according to any one of claims 1 to 5, A first sample adjustment step of processing a measurement target material blank into a dumbbell-shaped sample with a uniform thickness, A second sample adjustment step of polishing the upper and lower surfaces of the sample, coating a paraffin film on the surface after no obvious scratches remain on the upper surface of the sample, polishing the lower surface of the sample until a mirror effect is achieved, and then immersing the sample in an electrolytic polishing solution to remove the lower surface oxide layer so that a clear pattern can be collected under EBSD, A third sample adjustment step of ultrasonically cleaning the sample, removing the paraffin film on the upper surface of the sample, and thoroughly cleaning and drying it, A fourth sample adjustment step of finishing scale lines with a width of 10 μm at intervals of 5 mm by etching on the gage segment edges of the upper and lower surfaces of the sample, etching five marking points on each of the two surfaces, denoted as o, a, b, c, d and o', a', b', c', d', and corresponding their positions in pairs to serve as characteristic marking points for spatial alignment, A fifth sample adjustment step of producing a speckle pattern diagram for SEM-DIC analysis on the lower surface of the sample. The sample preparation method is characterized by including the above steps.

7. In the first sample adjustment step, both side surfaces of the sample are polished until a good degree of adhesion is achieved with the inner groove surface of the rotating heat conduction core, reducing the contact thermal resistance between the sample and the rotating heat conduction core in a vacuum. In the fifth sample adjustment step, Al with a particle size of 500 μm ２ O ３ powder is dissolved in absolute ethanol by ultrasonic vibration for 5 minutes, the turbid solution is allowed to stand for 3 minutes, the upper clear liquid is taken into the upper pot of the airbrush, the magnitude of the air flow and the spray distance are adjusted, and the Al ２ O ３ solution is uniformly sprayed on the lower surface of the sample, the sample is placed in an oven and dried, and the uniformly distributed Al ２ O ３ particles are used as a speckle pattern diagram. The sample preparation method according to claim 6, characterized in that.

8. A measurement method using the apparatus for in-situ measurement of mechanical properties by combined multi-techniques of a scanning electron microscope according to any one of Claims 1 to 5, comprising: a first measurement step of attaching a sample to a jig unit, evacuating the scanning electron microscope, adjusting the tungsten filament current for clear imaging, adjusting observation mode switching software, rotating the jig unit to four states of 0°, 70°, 180°, and 360° of the sample for angle adjustment initialization, moving the sample under a Raman objective lens from a pole piece and then back to the original position for position adjustment initialization, and recording the corresponding spatial coordinate parameter A0 of the in-situ tester; a second measurement step of setting tensile / compression speed and loading displacement parameters in a mechanical loading interface, applying them, 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 the observation mode switching software, moving the sample under the pole piece and rotating it to 0°, recording the spatial state information of the in-situ tester as A1, selecting the SE mode, controlling and sequentially operating various detectors using scanning electron microscope imaging software, acquiring in-situ tensile / compression SEM and EDS images near point o on the upper surface of the sample, and recording the corresponding acquisition time; a fourth measurement step of maintaining the position of the in-situ tester unchanged, rotating the sample to 70°, recording the spatial state information of the in-situ tester as A2, acquiring in-situ tensile / compression EBSD crystal structure information near point o on the upper surface of the sample, then rotating the sample to 180°, acquiring a speckle distribution SEM image near point o' on the lower surface of the sample, recording the spatial state information of the in-situ tester as A3, and recording the corresponding image acquisition time; a fifth measurement step of moving a displacement platform, moving the sample under the Raman objective lens and rotating it to 0°, selecting the Raman mode, controlling Raman system imaging, acquiring a Raman image near point o on the upper surface of the sample, recording the spatial state information of the in-situ tester as A4, and recording the acquisition time; Apply the spatial state information A1 to the observation mode switching software, adjust the original position tester to the initial observation state, set the loading parameters again, and after the loading is completed, repeat the third measurement step, the fourth measurement step, and the fifth measurement step to obtain a sixth measurement step of five types of original position observation data of the second group. Until the sample breaks, repeat the third measurement step, the fourth measurement step, the fifth measurement step, and the sixth measurement step, output the force-displacement curve of the sample recorded in the original position loading control software, input the obtained speckle distribution SEM image into the Vic-2D processing software, and calculate to obtain the strain distribution on the lower surface of the sample. A test method characterized by including a seventh measurement step.

9. In the second measurement step, first input the test target temperature into the temperature loading interface of the original position loading control software. After the monitored temperature of the sample reaches the set value, set the subsequent contents of the tensile / compression speed and the loading displacement parameters to realize the force-thermal coupling effect on the sample. The test method according to claim 8, characterized in that.

10. A data processing method for processing the data obtained by the test method according to claim 9, Sort out various types of microscopic images and collection times obtained during the matching test, determine that the collection area of the sample is located in the gauge segment of the sample, and map the obtained images one by one to the force-time curve. The first data processing step. Time-align the collection times of the force-displacement curve, SEM image, EDS image, EBSD image, SEM-DIC image, and Raman image obtained asynchronously, and use the linear interpolation method to convert the data obtained by five types of detectors with low collection frequencies to the time nodes of the force-displacement curve with a high sampling frequency. The second data processing step. Extract the initial images of the sample without tension in four postures: the sample at 0° in SEM / EDS mode, the sample at 70° in EBSD mode, the sample at 180° in SEM-DIC mode, and the sample at 360° in Raman mode. Set the o point of the 0° image of the sample in SEM / EDS mode as the common reference coordinate origin, and construct a common spatial rectangular coordinate system with the short side direction of the sample as the x-axis. Under the other three postures, set each o point as the coordinate origin, and with the short side direction of the sample as the x-axis, construct independent rectangular coordinate systems respectively. Utilize the formulas for angle conversion and translation transformation to convert and fuse the data measured in their own spatial coordinate systems without error into the common rectangular coordinate system of the sample at 0° under these three postures, thereby realizing the third data processing step of spatial alignment. In the second and third data processing steps, data from six different sources that have undergone spatio-temporal alignment are fused into one data source. Using the scale lines etched during the sample preparation process, a coordinate system with the o point as the coordinate origin is constructed, and clear coordinates (x ｉ , y ｉ ) are assigned to each point of the gauge segment on the sample. The data obtained by SEM, EDS, EBSD, SEM-DIC, and Raman are converted into a function φ(t) = (z １ , z ２ , z ３ , z ４ , z ５ , t) with respect to time t. The multi-source data is fused into W = (x ｉ , y ｉ , φ(t)). When the coordinate parameters (x, y) of any point in the sample with respect to the origin o and the time t during the corresponding loading process are input, the microscopic morphology, elemental distribution, crystal structure, strain distribution, corresponding molecular information, and average stress of the sample at that point can be obtained. It includes a fourth data processing step of independently and uniformly analyzing the deformation damage and failure mechanism of the material under the action of thermo-mechanical coupling from five aspects. A data processing method characterized by this.

Images