Microscopic analysis method and shared coordinate system for different microscopic devices

Abstract

The application discloses a microscopic analysis method and a shared coordinate system of different microscopes, and belongs to the technical field of material microstructure research. The shared coordinate system comprises: a piezoelectric ceramic platform connected with a controller; a sample holder fixing frame detachably connected with the piezoelectric ceramic platform; and a sample holder installed on the sample holder fixing frame and used for placing a sample. Based on the shared coordinate system, the same micro area of the sample can be coupled and characterized by different microscopes through coordinate positioning and coordinate conversion between the different microscopes and the sample holder. The method has high universality, and even the microscopes produced by different manufacturers can be used in combination. Moreover, the positioning precision is high, and the combination effect is good.

Description

Technical Field

[0001] This invention belongs to the field of material microstructure research technology, specifically relating to a microscopic analysis method and a shared coordinate system that uses different microscopic devices in combination. Background Technology

[0002] Optical microscopy (OM), scanning electron microscopy (SEM), and scanning probe microscopy (SPM) are the main analytical tools for studying the microstructure of materials. Each type of microscope has its own strengths. OM imaging is typically based on reflected light, transmitted light, or fluorescence, providing information such as grain size, distribution, anisotropy, and three-dimensional surface morphology of samples with a large field of view. SEM uses an electron beam as a light source and observes and analyzes samples based on the various signals generated after the electron beam interacts with the sample. With various accessories, it can provide information on the surface morphology, composition, structure, orientation, and luminescence properties of samples. SPM is a general term encompassing a series of microscopes that use probes to scan and image the sample, including a range of novel probe-based scanning imaging techniques such as scanning tunneling microscopy (STM), atomic force microscopy (AFM), magnetic force microscopy (MFM), scanning Kelvin probe force microscopy (SKPFM), and piezoelectric force microscopy (PFM). SPM can not only detect the physical properties of materials such as force, electricity, magnetism, and light, but also can be used to detect physical parameters such as sample surface morphology, micro-area conductivity, friction, and surface potential.

[0003] It is evident that different microscopic characterization methods are complementary. As the research on materials deepens, it is usually necessary to use different microscopic analysis equipment to perform coupled characterization of the same micro-region of the material.

[0004] Currently, there are commercially available products for multi-device co-operation, such as the German Zeiss Shuttle&Find optical-electronic co-operation system. This system is a co-operational microscopy technique that connects optical microscopes (ZEISS Axio Imager 2), electron and ion microscopes (Mineral Analysis Scanning Electron Microscope (AMICSCAN), Focused Ion Beam Scanning Electron Microscope (FIB-SEM), and Focused Ion Beam Helium Ion Microscope (FIB-HIM)) installed in the laboratory. This co-operation is only compatible with Zeiss products and cannot be used with instruments from other manufacturers. The newly launched Hitachi SU8200 series field emission scanning electron microscope and AFM5500M atomic force microscope in Japan achieve motor stage coordinate sharing. GETec Microscopy integrates AFM and SEM into AFSEM, enabling AFM and SEM co-operation. Commercial co-operation is limited to use between different instruments of the same brand and is not suitable for use with instruments from multiple brands.

[0005] In addition, commonly used combined methods, such as marking feature points with a hardness tester and FIB and then locating based on the feature points (Z. Wang, et al. Scientific Reports, 2016, 6:38335), are time-consuming and labor-intensive, and have poor positioning accuracy. Printing coordinate grids on silicon wafers to locate regions of interest (Jinchao Liu, et al. Scanning, 2021, 2021) is only applicable to powder materials and not to bulk materials, and silicon wafers cannot be reused.

[0006] In summary, there is currently a lack of a universally applicable and highly accurate coordinate system for SEM, SPM, and OM microscopic analysis, enabling rapid and high-precision multi-device integration. Summary of the Invention

[0007] This invention addresses the aforementioned problems in existing technologies by proposing a rapid, high-precision microscopic analysis method and a shared coordinate system for the combined use of multiple devices.

[0008] This invention can be achieved through the following technical solutions:

[0009] A microscopic analysis method using different microscopic instruments, when SEM is coupled to SPM / OM, includes the following steps:

[0010] S11. The coordinate system of the sample holder in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0).

[0011] S12. Preset the coordinate system of SEM and SPM / OM to Cs. Place the sample holder containing the sample into the SEM sample cavity. In the field of view of SEM, adjust the Ch coordinate system to be parallel to the Cs coordinate system in the same direction.

[0012] S13. Move the SEM sample stage in the Cs coordinate system to the sample holder origin and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as the origin Cs(X0, Y0) in the Cs coordinate system.

[0013] S14. Move the SEM sample stage to the target area of ​​the sample feature points, acquire the topographic image of the target area and its vicinity, read the coordinates of the target area as Cs(X1, Y1) in the Cs coordinate system, and calculate the coordinates of the sample feature points in the Ch coordinate system as Ch(X1, Y1). h Y h ) = (X1-X0, Y1-Y0);

[0014] S15. Remove the sample holder from the SEM sample cavity and put it back into the shared coordinate system. Place the entire shared coordinate system on the SPM / OM sample stage. Move the SPM / OM sample stage so that the optical path center of the SPM / OM coincides with Ch(X0, Y0), thereby achieving zeroing of the coordinates of the sample holder.

[0015] S16, with the SPM / OM sample stage stationary, move the piezoelectric ceramic stage of the shared coordinate system to Ch(X). h Y h ), to obtain the topographic image of the target area;

[0016] S17. Use software to compare and identify the target area topography image obtained by SPM / OM with the target area topography image obtained by SEM, improve positioning accuracy, and complete the joint positioning between SEM and SPM / OM.

[0017] A microscopic analysis method using different microscopic instruments, when SPM / OM is coupled to SEM, includes the following steps:

[0018] S21. The coordinate system of the sample holder in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0).

[0019] S22. Place the shared coordinate system on the SPM / OM sample stage, and move the SPM / OM sample stage so that the optical path center of the SPM / OM coincides with Ch(X0, Y0), thereby achieving zeroing of the coordinates of the sample holder.

[0020] S23. Keep the SPM / OM sample stage stationary, move the piezoelectric ceramic stage in the shared coordinate system to the target area Cs(X2, Y2), and obtain the feature points and the surrounding topography of the target area.

[0021] S24. Remove the sample holder from the shared coordinate system, place the sample holder inside the SEM sample chamber, and adjust the Ch coordinate system to be parallel to the Cs coordinate system in the same direction in the SEM field of view.

[0022] S25. Move the SEM sample stage in the Cs coordinate system to the origin of the sample holder coordinate system, and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as the origin Cs(X0, Y0) in the Cs coordinate system.

[0023] S26. Move the SEM sample stage to point Cs(Xs, Ys) = (X0+X2, Y0+Y2) in the Cs coordinate system to obtain the topographic image of the target area and its vicinity.

[0024] S27. Use software to compare and identify the target area topography image obtained by SEM with the target area topography image obtained by SPM / OM, improve positioning accuracy, and complete the joint positioning from SPM / OM to SEM.

[0025] A shared coordinate system for microscopic analysis methods using different microscopic instruments in combination includes:

[0026] A piezoelectric ceramic stage, which is connected to a controller;

[0027] A sample holder is detachably connected to the piezoelectric ceramic stage.

[0028] A sample holder, which is mounted on the sample holder holder and used to hold samples.

[0029] As a further improvement of the present invention, the sample holder is engraved with X and Y axes and multiple coordinate origin marks of different scales.

[0030] As a further improvement of the present invention, the sample holder determines the coordinate origin Ch(X0, Y0) by taking the average value of multiple points marked by the coordinate origin.

[0031] As a further improvement of the present invention, the piezoelectric ceramic stage measures the accuracy of different displacement strokes using a grating.

[0032] As a further improvement of the present invention, the sample holder fixing frame is provided with a sample holder placement groove, and the sample holder is placed in the sample holder placement groove.

[0033] As a further improvement of the present invention, the sample holder fixing frame can be configured as a flat plate structure, in which case the sample holder placement slot is formed on the top surface of the sample holder fixing frame.

[0034] As a further improvement of the present invention, the sample holder fixing frame can be configured as a Z-shaped structure, in which the two symmetrical sides of the sample holder fixing frame are respectively the connecting part and the mounting part. The connecting part is connected to the top surface of the sample holder fixing frame, the mounting part is located on the side of the sample holder fixing frame and extends outward, and the sample holder placement groove is opened in the mounting part.

[0035] As a further improvement of the present invention, when the sample is a block structure, the sample holder is configured as a grooved nail-shaped stage structure; when the sample is a sheet or powder, the sample holder is configured as a thin plate nail-shaped stage structure.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] 1. By setting up a shared coordinate system, the purpose of coupling characterization of the same micro-region of material by different microscopic analysis equipment can be achieved. This method has high universality and can be used even for microscopic analysis equipment produced by different manufacturers. In addition, the positioning accuracy is high, ensuring good joint effect.

[0038] 2. Compared with the commonly used positioning methods that use marked feature points and coordinate grids, this application improves the positioning accuracy through the design optimization of piezoelectric ceramic stage, image recognition comparison, and sample holder.

[0039] 3. Simultaneously, by reading and transforming the coordinates of the Cs coordinate system of the microscope and the Ch coordinate system of the sample holder, the time for finding feature points in the target area on the sample is shortened, and the efficiency of combining different microscopic analysis equipment is improved.

[0040] 4. The sample holder is engraved with X and Y axes as well as multiple coordinate origin marks of different scales, which makes it easy to clearly locate the coordinate origin at different magnifications. The coordinate origin Ch(X0, Y0) is determined by taking the average of multiple origin marks, which further improves the positioning accuracy of the coordinate origin Ch(X0, Y0) of the sample holder.

[0041] 5. The piezoelectric ceramic stage measures the accuracy of different displacement strokes using a grating. The grating plots an error change curve as the piezoelectric ceramic stage stroke increases, thus ensuring that the coordinate values ​​of the target area can be calibrated during final positioning. This eliminates the positioning error accumulated by the piezoelectric ceramic stage as the stroke increases, improving the positioning accuracy after combining SEM and SPM / OM.

[0042] 6. The sample holder can be configured into different shapes depending on the application scenario, such as a flat groove structure and a Z-shaped structure, to meet the needs of different application scenarios and improve its versatility and adaptability.

[0043] 7. Depending on the type of sample, such as block samples or powder samples, the sample holder can be configured with a corresponding grooved nail-shaped stage structure or a thin plate nail-shaped stage structure to improve the universality of the entire shared coordinate system. Attached Figure Description

[0044] Figure 1 This is a schematic diagram of the shared coordinate system of the present invention;

[0045] Figure 2 This is a schematic diagram of the Z-shaped sample holder and piezoelectric ceramic stage of the present invention;

[0046] Figure 3 This is a schematic diagram of the plate-shaped sample holder of the present invention;

[0047] Figure 4 This is a schematic diagram of the block sample leveling device of the present invention;

[0048] Figure 5 This is a schematic diagram of the multi-scale coordinate origin of the present invention;

[0049] Figure 6 This is a schematic diagram of the location of the coordinate origin of the present invention;

[0050] Figure 7 This is a grating topography diagram of the present invention.

[0051] In the figure, 100 is the piezoelectric ceramic stage; 110 is the controller; 120 is the sample holder fixing frame; 121 is the sample holder placement slot; 122 is the connecting part; 123 is the mounting part; 130 is the sample holder; and 140 is the block sample leveling device. Detailed Implementation

[0052] The following are specific embodiments of the present invention, which are described in conjunction with the accompanying drawings. However, the present invention is not limited to these embodiments.

[0053] like Figure 1-7 As shown, a microscopic analysis method using different microscopic instruments, when SEM is coupled to SPM / OM, includes the following steps:

[0054] S11. The coordinate system of sample holder 130 in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0).

[0055] S12. Preset the coordinate system of SEM and SPM / OM to Cs. Place the sample holder 130 containing the sample into the SEM sample cavity. In the field of view of SEM, adjust the Ch coordinate system to be parallel to the Cs coordinate system in the same direction, so as to facilitate the conversion of the target area coordinates between the Cs coordinate system and the Ch coordinate system.

[0056] S13. Move the SEM sample stage in the Cs coordinate system to the origin of the sample holder and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as the origin Cs(X0, Y0) in the Cs coordinate system. At this time, the origin of the sample holder 130 has been accurately located in the SEM.

[0057] S14. Move the SEM sample stage to the target area of ​​the sample feature points, acquire the topographic image of the target area and its vicinity, read the coordinates of the target area as Cs(X1, Y1) in the Cs coordinate system, and calculate the coordinates of the sample feature points in the Ch coordinate system as Ch(X1, Y1). h Y h )=(X1-X0,Y1-Y0), It is worth mentioning here that in step S14, the coordinate values ​​of the target area in the Cs coordinate system have been converted into the coordinate values ​​in the Ch coordinate system of the sample holder 130.

[0058] S15. Remove the sample holder 130 from the SEM sample cavity and put it back into the shared coordinate system. Place the entire shared coordinate system on the SPM / OM sample stage. By moving the SPM / OM sample stage, make the optical path center of the SPM / OM coincide with Ch(X0, Y0), so that the coordinates of the sample holder 130 are zeroed. This allows the shared coordinate system to accurately locate a certain coordinate point in the Ch coordinate system of the sample holder 130.

[0059] S16, SPM / OM sample stage remains stationary, move shared coordinate system until Ch(X) is reached. h Y h At this coordinate point, the topographic image of the target area is obtained. At this time, the target area obtained by SPM / OM and the target area obtained by SEM are the same area of ​​the sample.

[0060] S17. Using image recognition software, the target area shape image obtained by SPM / OM is compared and recognized with the target area shape image obtained by SEM to improve positioning accuracy. At the same time, the joint positioning between SEM and SPM / OM is completed.

[0061] Example 2

[0062] The difference between Example 2 and Example 1 is that the method in Example 1 is used for the combined application of SEM to SPM / OM, while the method in Example 2 is applicable to the combined application of SPM / OM to SEM. Specifically, Example 2 includes the following steps:

[0063] S21. The coordinate system of sample holder 130 in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0).

[0064] S22. Place the shared coordinate system on the SPM / OM sample stage. By moving the SPM / OM sample stage, make the optical path center of the SPM / OM coincide with Ch(X0, Y0), thereby realizing the zeroing of the coordinates of the sample holder 130. This ensures that the shared coordinate system can accurately locate any coordinate point in the Ch coordinate system of the sample holder 130.

[0065] S23. Keep the SPM / OM sample stage stationary. Move the piezoelectric ceramic stage 100 in the shared coordinate system to the target area Ch(X2, Y2) in the Ch coordinate system to obtain the feature points and the surrounding topography of the target area. The target area Ch(X2, Y2) is the area to be observed.

[0066] S24. Remove the sample holder 130 from the shared coordinate system, fix the sample holder 130 in the SEM sample cavity, and adjust the Ch coordinate system to be parallel to the Cs coordinate system in the field of view of the SEM to facilitate the conversion of the target area coordinates between the Cs coordinate system and the Ch coordinate system.

[0067] S25. Move the SEM sample stage in the Cs coordinate system to the origin of the sample holder and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as Cs(X0, Y0) in the Cs coordinate system. Accurately position the origin of the sample holder 130 in the SEM.

[0068] S26. Move the SEM sample stage to point Cs(Xs, Ys) = (X0+X2, Y0+Y2) in the Cs coordinate system to obtain the topographic image of the target area and its vicinity. At this time, the target area obtained by SEM and the target area obtained by SPM / OM are the same area of ​​the sample.

[0069] S27. Use software to compare and identify the target area topography image obtained by SEM with that obtained by SPM / OM to improve positioning accuracy and complete the joint positioning from SPM / OM to SEM.

[0070] It should be noted that the difference between the SEM-to-SPM / OM combination method in Example 1 and the SPM / OM-to-SEM combination method in Example 2 is because the SEM sample chamber is a vacuum environment. When searching for the target area of ​​the sample, the sample holder 130 remains stationary while the SEM sample stage moves. Therefore, the target area Cs(X1, Y1) is the coordinate value in the Cs coordinate system. Subsequently, Cs(X1, Y1) is transformed to the Ch coordinate system of the sample holder 130 to obtain the coordinate value of the target area as Ch(X1, Y1). h Y h ) = (X1-X0, Y1-Y0);

[0071] The SPM / OM sample stage is located in the atmospheric environment. When searching for the target area of ​​the sample, the SPM / OM remains stationary while the piezoelectric ceramic stage 100 in the shared coordinate system moves, driving the sample holder 130 to move as well. This movement occurs in the Ch coordinate system. Therefore, it is only necessary to move the SPM / OM sample stage so that its optical path center coincides with the origin of the sample holder coordinate system, thus zeroing the sample holder coordinate system. Then, the piezoelectric ceramic stage of the shared coordinate system is moved on the SPM / OM sample stage to Ch(X) h Y h Once this coordinate point is reached, SPM / OM and SEM can observe the same target area, thus enabling the combined use of SEM and SPM / OM.

[0072] Conversely, in Example 2, since the shared coordinate system moves on the SPM / OM sample stage, it moves in the Ch coordinate system. When the sample holder 130 is placed in the SEM sample cavity, the SEM sample stage only needs to be moved to Ch(X0, Y0) and then moved to the target area Cs(Xs, Ys) = (X0+X2, Y0+Y2) to enable the SEM and SPM / OM to observe the same area, thereby realizing the combined use of SPM / OM and SEM.

[0073] In summary, the methods provided in Examples 1 and 2 can achieve the purpose of coupled characterization of the same micro-region of a material by different microscopic analysis equipment. Furthermore, this method has high universality and can be used even with microscopic equipment from different manufacturers. It also has high positioning accuracy, ensuring good combined effect.

[0074] Example 3

[0075] This invention also provides a shared coordinate system for microscopic analysis that allows for the combined use of different microscopic instruments. In Embodiments 1 and 2, this shared coordinate system enables the combined use of SEM and SPM / OM. Specifically, the shared coordinate system includes:

[0076] A piezoelectric ceramic stage 100 is connected to a controller 110. The piezoelectric ceramic stage 100 has high precision to improve its positioning accuracy.

[0077] The sample holder 120 is detachably connected to the piezoelectric ceramic stage 100;

[0078] The sample holder 130 is mounted on the sample holder fixing frame 120 and is used to place the sample. The sample holder fixing frame 120 is connected to the piezoelectric ceramic stage 100 by fasteners to ensure that the sample holder 130 is parallel to the piezoelectric ceramic stage 100 and reduce the measurement error caused by sample tilting.

[0079] Preferably, the sample holder 130 is engraved with X and Y axes as well as multiple coordinate origin marks of different scales, which makes it easy to clearly locate the coordinate origin at different magnifications.

[0080] In a further preferred embodiment, the sample holder 130 determines the coordinate origin Ch(X0, Y0) by taking the average value of multiple points marked by the coordinate origin, thereby further improving the positioning accuracy of the coordinate origin Ch(X0, Y0) of the sample holder 130.

[0081] Preferably, the piezoelectric ceramic stage 100 measures the accuracy of different displacement strokes using a grating. It is worth mentioning that even though the piezoelectric ceramic stage 100 itself has high accuracy, it will still have a small error during movement. To eliminate this error, a curve of error change as the stroke of the piezoelectric ceramic stage 100 increases is plotted by grating measurement, thereby ensuring that the coordinate values ​​of the target area can be calibrated during final positioning and improving the positioning accuracy after SEM and SPM / OM are used together.

[0082] Preferably, the sample holder fixing frame 120 has a sample holder placement groove 121, the sample holder 130 is placed in the sample holder placement groove 121, and the sample holder 130 is fixed in the sample holder placement groove 121 by a positioning pin, so as to ensure that the sample holder 130 will not move, thereby ensuring that the sample is always in a fixed state and improving the observation accuracy.

[0083] Preferably, the sample holder fixing frame 120 can be configured as a flat plate structure, in which case the sample holder placement groove 121 is opened on the top surface of the sample holder fixing frame 120. Alternatively, the sample holder fixing frame 120 can be configured as a Z-shaped structure, in which case the two symmetrical sides of the sample holder fixing frame 120 are a connecting part 122 and a mounting part 123, respectively. The connecting part 122 is connected to the top surface of the sample holder fixing frame 120, and the mounting part 123 is located on the side of the sample holder fixing frame 120 and extends outward. The sample holder placement groove 121 is opened in the mounting part 123.

[0084] Specifically, the sample holder holder 120 is designed with a flat plate structure and a Z-shaped structure because the distance between the objective lens and the sample stage varies for different SPM / OM lenses. When the distance is large, the entire shared coordinate system can be placed on the sample stage, in which case the flat plate sample holder holder 120 can be used. When the distance is small, the Z-shaped sample holder holder 120 can be used, as long as the mounting part 123 with the sample holder 130 is placed on the sample stage. Therefore, the different shapes of the sample stage holder holder are to adapt to different usage environments. In addition to the flat plate structure and the Z-shaped structure, other shapes can also be used, which will not be described in detail here.

[0085] Preferably, when the sample is a block structure, the sample holder 130 is set as a grooved nail-shaped stage structure; when the sample is a sheet or powder, the sample holder 130 is set as a thin plate nail-shaped stage structure. Similarly, the shape and structure of the sample holder 130 can also be adapted to different samples to improve the universality and adaptability of the entire shared coordinate system.

[0086] Preferably, it also includes a block sample leveling device 140, specifically a leveling base that is adapted to the size of the sample holder 130 of the grooved nail stage. In use, the sample and sample holder 130 are inverted on the leveling base, and the sample is fixed to the sample holder 130 by fastening screws, thereby ensuring that the block sample and sample holder 130 are in the same plane, thereby reducing measurement error.

[0087] To better illustrate the technical solution of this application, the experimental structure and experimental procedure are described in detail below:

[0088] Experimental results:

[0089] Hot-deformed Nd-Fe-B magnets are formed by hot pressing of rapidly quenched strips. The rapidly quenched strips have uneven grain size, and during the forming process, coarse-grained regions form at the interfaces of these strips. Different from the coarse-grained regions are equiaxed grain regions. The grains in the coarse-grained regions exhibit several different growth patterns, and these different growth patterns have varying effects on the Nd-Fe-B magnetic structure. These different magnetic structures, in turn, lead to differences in the remanent magnetic properties of the magnets.

[0090] Electron backscatter diffraction (EBSD) is a SEM-based technique that provides microscopic crystallographic information about samples. Based on the coarse-grained regions of the aforementioned Nd-Fe-B material, EBSD can clearly and directly reflect the crystal growth patterns of these coarse-grained grains. Magneto-optical Kerr microscopy utilizes the magneto-optical Kerr effect of incident light and the magnetic field on the magnet surface to observe magnetic domain structures. Magnetic domains are small, oriented magnetized regions that differentiate during the spontaneous magnetization process of ferromagnetic materials to reduce static magnetic energy. Magnetic domains microscopically reflect the magnetization mechanism of ferromagnetic materials. Studying the changes in the magnetic domain structure of permanent magnet materials can not only explain the intrinsic magnetic properties of materials from the perspective of magnetic moments, but also infer the final magnetic performance of permanent magnet materials from the magnetic structure. Therefore, developing and designing a rapid, high-precision, multi-device sample stage for combined use, and employing a large-scale, multi-regional combination of EBSD and Kerr / MFM, is of great significance for researchers to take corresponding measures to improve the magnetic performance of permanent magnets.

[0091] Detailed experimental procedure:

[0092] (1) The prepared Nd-Fe-B magnet was hot-mounted with resin. After mounting, it was ground with 180 mesh, 600 mesh and 1200 mesh sandpaper respectively. After grinding, it was polished with 9μm, 3μm and 1μm diamond suspension respectively. Then, it was polished with 250nm Al2O3 solution. After polishing, the sample was cleaned and dried and the Nd-Fe-B block was taken out.

[0093] (2) Fix the polished Nd-Fe-B block onto the block sample holder, then fix the sample holder inside the scanning electron microscope (SEM) cavity and complete the vacuuming. Under SEM, rotate the sample holder along the X-axis to a horizontal position using the R-axis of the SEM. Tilt the sample stage to 60° using the T-axis of the SEM to locate the multi-scale origin. Figure 6 Record the coordinates of points A, B, C, and D in the sample tray. Take the average of the four coordinates as the origin point of the sample tray at point C. s The coordinates Cs(x0,y0) in the coordinate system are used for EBSD analysis of the coarse-grained Nd-Fe-B region. After the analysis, the coordinates Cs(x1,y1) of the target region are recorded. The coordinates of the target region in the sample holder coordinate system are Ch(x0,y0). h ,y h )=(x1-x o ,y1-y o ).

[0094] (3) Remove the sample holder and sample from the SEM, transfer them to the sample holder holder of the shared coordinate system, and secure them. Place the shared coordinate system on the Kerr optical microscope stage, and use the Kerr stage to move the shared coordinate system until the origin of the sample holder coincides with the center of the optical path. Move the piezoelectric ceramic stage of the shared coordinate system to point (x... h ,y h The system acquires topographic images of the target area and uses software to compare and identify the topographic images under a Kerr microscope and under SEM to calibrate the positioning accuracy. After positioning is completed, the magnetic domain structure of the target area is obtained.

[0095] (4) Repeat the above operation to perform large-scale multi-region characterization of the coarse-grained region.

[0096] (5) Analyze the EBSD data to obtain the orientation difference between the thermal deformation direction and the

[001] direction in the coarse grain region.

[0097] (6) Establish a model of the correspondence between grain orientation and magnetic domain structure, and quantitatively study the influence of grain orientation on magnetic structure.

[0098] (7) Investigate the influence of different magnetic structures on the magnetic properties of Nd-Fe-B magnets, and further analyze the influence of grain orientation in the coarse-grained region on the magnetic properties of the magnets. Provide data support for taking corresponding measures to improve the magnetism of Nd-Fe-B magnets.

[0099] The technical means disclosed in this invention are not limited to those described above, but also include technical solutions composed of any combination of the above technical features. The above are specific embodiments of this invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of this invention, and these improvements and modifications are also considered within the scope of protection of this invention.

[0100] It should be noted that all directional indications (such as up, down, left, right, front, back, etc.) in the embodiments of the present invention are only used to explain the relative positional relationship and movement of each component in a certain specific posture (as shown in the figure). If the specific posture changes, the directional indication will also change accordingly.

[0101] Furthermore, in this invention, descriptions involving terms such as "first," "second," and "a" are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0102] In this invention, unless otherwise explicitly specified and limited, the terms "connection," "fixed," etc., should be interpreted broadly. For example, "fixed" can mean a fixed connection, a detachable connection, or an integral part; it can mean a mechanical connection or an electrical connection; it can mean a direct connection or an indirect connection through an intermediate medium; it can mean the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0103] Furthermore, the technical solutions of the various embodiments of the present invention can be combined with each other, but only if they are feasible for those skilled in the art. If the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.

Claims

1. A microscopic analysis method using different microscopic instruments in combination, characterized in that, When using SEM to SPM / OM in combination, the following steps are included: S11. The coordinate system of the sample holder in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0). S12. Preset the coordinate system of SEM and SPM / OM to Cs. Place the sample holder containing the sample into the SEM sample cavity. In the field of view of SEM, adjust the Ch coordinate system to be parallel to the Cs coordinate system in the same direction. S13. Move the SEM sample stage in the Cs coordinate system to the sample holder origin and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as the origin Cs(X0, Y0) in the Cs coordinate system. S14. Move the SEM sample stage to the target area of ​​the sample feature points, obtain the topographic image of the target area and its vicinity, read the coordinate value of the target area in the Cs coordinate system as Cs(X1, Y1), and calculate the coordinates of the sample feature points in the Ch coordinate system as Ch(Xh, Yh) = (X1-X0, Y1-Y0). S15. Remove the sample holder from the SEM sample cavity and put it back into the shared coordinate system. Place the entire shared coordinate system on the SPM / OM sample stage. By moving the SPM / OM sample stage, make the optical path center of the SPM / OM coincide with Ch(X0, Y0) to achieve zero coordinates of the sample holder. S16. With the SPM / OM sample stage stationary, move the piezoelectric ceramic stage of the shared coordinate system to Ch(Xh, Yh) to obtain the topographic image of the target region. S17. Use software to compare and identify the target area topography image obtained by SPM / OM with the target area topography image obtained by SEM, improve positioning accuracy, and complete the joint positioning between SEM and SPM / OM. When SPM / OM is used in conjunction with SEM, the following steps are included: S21. The coordinate system of the sample holder in the preset shared coordinate system is Ch, and the origin of Ch is Ch(X0, Y0). S22. Place the shared coordinate system on the SPM / OM sample stage, and move the SPM / OM sample stage so that the optical path center of the SPM / OM coincides with Ch(X0, Y0), thereby achieving zeroing of the coordinates of the sample holder. S23. Keep the SPM / OM sample stage stationary, move the piezoelectric ceramic stage in the shared coordinate system to the target region Cs(X2, Y2), and obtain the feature points and the surrounding topography of the target region. S24. Remove the sample holder from the shared coordinate system, place the sample holder inside the SEM sample chamber, and adjust the Ch coordinate system to be parallel to the Cs coordinate system in the same direction in the SEM field of view. S25. Move the SEM sample stage in the Cs coordinate system to the origin of the sample holder coordinate system and accurately position it at Ch(X0, Y0). Record Ch(X0, Y0) as the origin Cs(X0, Y0) in the Cs coordinate system. S26. Move the SEM sample stage to point Cs(Xs, Ys) = (X0+X2, Y0+Y2) in the Cs coordinate system to obtain the topographic image of the target area and its vicinity. S27. Use software to compare and identify the target area topography image obtained by SEM with that obtained by SPM / OM to improve positioning accuracy and complete the joint positioning from SPM / OM to SEM.

2. A shared coordinate system applied to the microscopic analysis method of claim 1, characterized in that, include: A piezoelectric ceramic stage, which is connected to a controller; A sample holder is detachably connected to the piezoelectric ceramic stage; A sample holder, which is mounted on the sample holder holder and used to hold samples.

3. The coordinate system for combined SEM and SPM / OM microscopic analysis according to claim 2, characterized in that, The sample holder is engraved with X and Y axes as well as coordinate origin markers of multiple different scales.

4. The coordinate system for combined SEM and SPM / OM microscopic analysis according to claim 3, characterized in that, The sample holder determines the origin Ch(X0, Y0) by taking the average of multiple points marked by the origin.

5. The coordinate system for combined SEM and SPM / OM microscopic analysis according to claim 2, characterized in that, The piezoelectric ceramic stage measures the accuracy of different displacement strokes using a grating.

6. The microscopic analysis coordinate system for SEM and SPM / OM combined according to claim 2, characterized in that, The sample holder fixing frame has a sample holder placement slot, and the sample holder is placed in the sample holder placement slot.

7. The microscopic analysis coordinate system for SEM and SPM / OM combined according to claim 6, characterized in that, The sample holder fixing frame can be configured as a flat plate structure, in which case the sample holder placement slot is opened on the top surface of the sample holder fixing frame.

8. The microscopic analysis coordinate system for SEM and SPM / OM combined according to claim 6, characterized in that, The sample holder fixing frame can be configured as a Z-shaped structure, in which case the two symmetrical sides of the sample holder fixing frame are the connecting part and the mounting part, respectively. The connecting part is connected to the top surface of the sample holder fixing frame, the mounting part is located on the side of the sample holder fixing frame and extends outward, and the sample holder placement slot is opened in the mounting part.

9. The microscopic analysis coordinate system for SEM and SPM / OM combined according to claim 2, characterized in that, When the sample is in block form, the sample holder is configured as a grooved nail-shaped stage structure; when the sample is in sheet or powder form, the sample holder is configured as a thin plate nail-shaped stage structure.

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