System and method for realizing combination of FIB characterization and EBSD characterization, and sample mounting device

Abstract

The invention relates to the technical field of electron microscope sample preparation and characterization, and provides a system and a method for realizing combination of FIB characterization and EBSD characterization, and a sample mounting device. The sample mounting device can be used for an FIB characterization-EBSD characterization combined system and comprises a mounting table with a preset inclined plane, and a connecting structure used for being mounted to electron microscope equipment is arranged at the bottom of the mounting table; and the preset inclined surface of the mounting table is provided with a positioning structure for connecting the sample nailing table or / and a sample. When the sample is prepared through the FIB, the sample table with an inclination function is adopted, a grazing incidence method is used, any position of the surface can be machined, after FIB machining, the angle is adjusted through the sample table to meet the characterization condition of EBSD, and the application effect is good.

Description

Technical Field

[0001] The invention belongs to the technical field of electron microscope sample preparation and characterization, and in particular relates to a system, method and sample mounting device for realizing FIB characterization-EBSD characterization combination. Background Art

[0002] FIB (Focused ion beam) is a kind of ion beam that uses a highly focused ion beam (usually Ga + It is a micromachining technology that uses ions to cut, deposit, etch or modify the surface of materials. The principle is to achieve local removal or deposition by bombarding the material surface with ions. Combined with the SEM (Scanning electron microsopy) function, it can accurately locate specific areas for processing, so it is also called dual-beam electron microscope or FIB-SEM.

[0003] FIB is mainly used for the preparation of ultra-fine cross-section samples, cutting of ultra-thin slices and processing of complex geometric shapes. It is especially suitable for the exposure and analysis of microstructures. Its advantages lie in its nanometer-level processing accuracy and the ability to perform targeted selection and preparation of target areas. It is very suitable for the processing of microstructures and submicron-scale samples.

[0004] EBSD (Electron backscattering Diffraction) is a crystallographic analysis technique based on backscattered electron diffraction. It generates diffraction patterns through the interaction of high-energy electron beams with sample crystals, and obtains quantitative data such as crystal orientation, grain size, grain boundary type and texture information through computer analysis. The advantage of EBSD is that it has high resolution, can provide crystallographic information at the micron or even submicron scale, and can directly characterize the structural characteristics of the surface. It is often used for grain, grain boundary, phase change and texture analysis. In a dual-beam electron microscope, EBSD can work as a plug-in. The combination of FIB and EBSD gives full play to the advantages of both and provides a powerful tool for materials science research. First, FIB-prepared samples have high precision and high positioning, which can accurately expose specific areas (such as crystal defects, grain boundaries or characteristic grains) to ensure the accuracy of EBSD characterization. Secondly, FIB can significantly improve the quality of EBSD diffraction patterns by gradually removing the damaged layer on the surface of the material and optimizing the surface flatness during sample preparation. Finally, if the processing and characterization area is not very large, such as an area within a few hundred microns, the combination of the two is very efficient and time-saving. In general, the combination of FIB and EBSD can realize the complete research path from precise sample preparation to high-quality pattern calibration. It is suitable for high-precision characterization of complex crystal structures, micro-nano composite materials and special morphology samples. It is an indispensable technical means in the fields of materials science, electronic devices and metallurgy.

[0005] To ensure that the ion beam can be vertically incident into the sample area for precise removal or processing, the FIB usually requires the sample surface to be at an angle close to perpendicular to the ion beam (i.e., the tilt angle is 90° or close to 90°). This can ensure high precision in the etching depth and width of the ion beam, avoiding processing deviations or asymmetric morphologies caused by too small an incident angle.

[0006] In contrast, EBSD is a technique that generates backscattered diffraction patterns through the interaction between an electron beam and the inclined surface of a sample. To obtain clear diffraction patterns, EBSD requires a certain tilt angle between the sample surface and the electron beam. Generally, the tilt angle of the sample surface with respect to the horizontal plane is set to about 70° (tilting the sample surface towards the direction close to the EBSD detector). Such an angle can maximize the intensity of the diffraction signal while reducing the loss of backscattered electrons, thus ensuring clear diffraction patterns and a high signal-to-noise ratio. Moreover, to ensure that the diffraction patterns can be received by EBSD, the sample test surface should be free of strain damage, flat, and without obvious obstruction. The processing method with the ion beam at an angle close to perpendicular will damage the sample surface. On the contrary, if the ion beam is completely parallel to the sample surface, only the edge region can be processed and characterized. Therefore, FIB grazing incidence processing should be used, so that the processing area is not limited to the edge, but any position on the surface can be selected. This can accurately expose specific regions (such as small solder joints, crystal defects, grain boundaries, or characteristic grains), expanding the range of applicable samples. However, considering that the processed area may be only a relatively small region in the sample, it is necessary to accurately mark to ensure the alignment of the FIB processing area and the EBSD test area. For example, when processing an area of several hundred micrometers on a sample several millimeters or centimeters long, it is necessary to locate the processing area. After processing, if the position changes during EBSD characterization, it is necessary to quickly find the original processing area. Therefore, the FIB and EBSD have different angle requirements for the test surface - the FIB requires a sample surface almost perpendicular to the ion beam, while EBSD requires the sample surface to be tilted by about 70°. This angle difference needs to be particularly noted during the preparation and testing processes, otherwise it may lead to limited processing areas, processing precision deviations, or characterization result deviations.

[0007] However, there are few documents on the combined use of existing FIB processing and EBSD characterization. On the one hand, dual-beam electron microscopes equipped with EBSD are not particularly widespread, and the operating technical requirements are relatively high. FIB involves precise control of the ion beam to achieve high-quality sample processing, while EBSD has strict requirements for the surface quality and angle of the sample. Combining the two technologies significantly increases the complexity of the equipment and requires the experimenter to have operational experience in both FIB preparation and EBSD analysis at the same time, which makes the research threshold relatively high. On the second hand, there is less promotion and systematic summary of relevant technical methods. Since these studies often focus on high-end personalized material research, their experimental results may be limited to specific laboratories or materials and have not formed systematic technical solutions that are generally applicable to different fields, resulting in a limited number of current documents. Finally, FIB can cause damage to some samples, which may affect the pattern quality.

[0008] Regarding the prior art, invention patent CN201711150682.4 discloses a method for preparing an electron backscatter diffraction sample of a galvanized sheet surface coating using FIB. However, this method is applicable to cross-section preparation and characterization, and uses a processing method with the ion beam parallel to the cross-section. This method can only process a cross-section for EBSD characterization at the edge, and moreover, this method can only complete the FIB processing. After the processing is completed, the sample needs to be taken out, the angle needs to be adjusted, and then repositioned to perform EBSD characterization, which reduces the efficiency and increases the risk of sample contamination and oxidation. Invention patent CN202010175765.4 provides a method for characterizing the three-dimensional microstructure of ceramic coating materials based on FIB, which can suppress the image acquisition position drift caused by charging phenomena during the three-dimensional microscopic characterization process. First, the edge is trimmed by FIB to obtain a "nose-shaped" target area, and then subsequent processing and characterization are performed on the edge area. This method only limits the processing and characterization areas to the sample edge, and does not discuss how to achieve the angle transformation from FIB to EBSD characterization, nor does it discuss how to use a sample holder to achieve a large-angle transformation from -39° to 70°.

[0009] For a dual-beam electron microscope, the usual tilt angle range is from -4° to 70° or from -10° to 60°. If a usual sample stage (placed horizontally) is used, the FIB processing angle cannot be guaranteed (a very large negative tilt, such as -38° is required), and although the EBSD angle can be guaranteed, considering that characterizing at the maximum angle will limit the characterization area and endanger the safety of the EBSD detector, a special sample holder usually needs to be designed.

[0010] For the angle control of the sample, in the prior art, most experiments need to assume that the upper and lower surfaces of the sample are parallel to adjust the inclination angle, or use a fixed-angle adapter, and lack accurate angle measurement functions, which are prone to operation errors and angle imbalance. Moreover, in the prior art, the area matching between FIB processing and EBSD testing mainly relies on manual alignment by the operator, and position deviations often occur due to sample movement or rotation, resulting in misalignment between the detection area and the processing area.

[0011] It can be seen that in the current combined technology system of FIB processing and EBSD, there are problems such as insufficient process coherence, inaccurate angle adjustment, limited processing area on the sample surface, and deviation in the alignment of the experimental area, resulting in poor application effects. Summary of the Invention

[0012] The purpose of the present invention is to at least overcome one of the above deficiencies in the prior art, and provide a system, method, and sample mounting device for realizing the combination of FIB characterization - EBSD characterization, which has good application effects in the combined technology of FIB processing and EBSD.

[0013] The technical solution of the present invention is: a sample mounting device for a combined system of FIB characterization - EBSD characterization, including a mounting table with a preset inclined surface, and a connection structure for mounting to an electron microscope device is provided at the bottom of the mounting table; a positioning structure for connecting a sample nail table or / and a sample is provided on the preset inclined surface of the mounting table.

[0014] Optionally, the bottom surface of the mounting table is a bottom plane that fits the mounting surface of the electron microscope device, and the included angle between the preset inclined surface and the bottom plane is 20 degrees to 70 degrees; And / or, the mounting table is provided with a locking structure for locking the sample nail table or / and the sample.

[0015] Optionally, the connection structure at the bottom of the mounting table is a bottom plug column for a preset jack of a rotating table in the electron microscope device; And / or, the positioning structure is a plug hole, and the sample nail table has a nail table plug column that can be inserted into the plug hole.

[0016] The present invention also provides a system for realizing the combination of FIB characterization - EBSD characterization, including an electron microscope device, the electron microscope device includes a main sample stage, an SEM component, and an FIB component, and also includes the above-mentioned sample mounting device; the sample mounting device is detachably connected to the main sample stage, the SEM component and the FIB component are arranged above the main sample stage, the lens barrels of the SEM component and the FIB component both point in the direction of the main sample stage, and the lens barrels of the SEM component and the FIB component are arranged at an included angle.

[0017] Optionally, the barrel of the SEM component is perpendicular to the horizontal plane, and the included angle between the barrel of the FIB component and the barrel of the SEM component is between 50 degrees and 60 degrees.

[0018] The present invention also provides a method for realizing the combined use of FIB characterization - EBSD characterization. Using the above - mentioned system for realizing the combined use of FIB characterization - EBSD characterization, it includes the following steps: Measurement step: To measure the precise angle of the test surface of the sample relative to the horizontal plane, install the sample on the sample mounting device, and install the sample mounting device on the main sample stage. Observe the coincidence of the upper and lower edges of the sample through the electron microscope equipment and record the tilt angle θ1 of the main sample stage. It can be obtained that when the sample mounting device is placed horizontally, the included angle α between the processed surface of the sample and the horizontal plane is: 90° - θ1; FIB processing step: Rotate the main sample stage as a whole by 180°, and make the processed surface of the sample form an angle A with the barrel of the FIB component. The tilt angle θ2 of the main sample stage is θ2 = α - (90° - β)+ A°, where the range of the angle A is from 3° to 7°, and β is the included angle between the FIB barrel and the SEM barrel; EBSD characterization step: Rotate the main sample stage as a whole by 180° to face the EBSD detector, set the processed surface of the sample to form an angle B with the horizontal plane. The tilt angle θ3 of the main sample stage is θ3 = B - α, and the range of the angle B is from 65° to 75°.

[0019] Optionally, in the FIB processing step, the angle A is 5°; in the EBSD characterization step, the angle B is 70°.

[0020] Optionally, between the FIB processing step and the EBSD characterization step, there is also a step of aligning the FIB processing area with the EBSD test area: The area etched by the ion beam is used as a mark.

[0021] Optionally, in the FIB processing step, when the processing area is large, FIB processing is carried out with an acceleration voltage of 30 kV and a current of 65 nA.

[0022] Optionally, in the FIB processing step, when the processing area is small or the sample shows a curtain effect, the current is reduced.

[0023] The system, method, and sample mounting device for realizing the combined use of FIB characterization - EBSD characterization provided by the present invention adopt a sample stage with a tilting function when preparing samples by FIB, and use the grazing incidence method, so that any place on the surface can be processed. After FIB processing, the angle is adjusted by the sample stage to meet the characterization conditions of EBSD. Description of the Drawings

[0024] To more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the accompanying drawings required for the embodiments. Obviously, the accompanying drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other accompanying drawings can be obtained based on these drawings.

[0025] Figure 1 is a schematic cross-sectional view of a sample mounting device provided by an embodiment of the present invention; Figure 2 is a schematic side view of a sample mounting device and a main sample stage provided by an embodiment of the present invention; Figure 3 is a schematic view for observing whether the upper and lower edges of a sample coincide during the measurement step of a system for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 4 is a schematic view of FIB processing by a system for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 5 is a schematic view of EBSD characterization by a system for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 6 is an image after FIB processing by a method for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 7 is the EBSD result of EBSD characterization by a method for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 8 is a schematic view of a sample after ion beam processing in a method for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention; Figure 9 is another schematic view when the sample after ion beam processing is rotated to perform EBSD characterization in a method for realizing the combined use of FIB characterization and EBSD characterization provided by an embodiment of the present invention. Detailed implementation manners

[0026] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0027] It should be noted that the terms "arrangement" and "connection" should be understood in a broad sense. For example, it can be a direct arrangement or connection, or an indirect arrangement or connection through intermediate components or intermediate structures.

[0028] In addition, in the embodiments of the present invention, if there are terms indicating orientation or positional relationships such as "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., they are based on the orientation or positional relationship shown in the drawings or the conventional placement state or usage state. They are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the structures, features, devices or elements referred to must have a specific orientation or positional relationship, nor must they be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation to the present invention. In the description of the present invention, unless otherwise specified, the meaning of "a plurality of" is two or more.

[0029] In the specific embodiments, the various specific technical features and each embodiment described can be combined in any suitable manner without contradiction. For example, different embodiments can be formed by combining different specific technical features / embodiments. To avoid unnecessary repetition, various possible combination methods of the specific technical features / embodiments in the present invention will not be described separately.

[0030] As Figure 1 and Figure 2 shown, a sample mounting device provided by an embodiment of the present invention is used for a combined system of FIB characterization - EBSD characterization, and includes a mounting table 120 having a preset inclined surface 121. A connection structure for mounting to an electron microscope device (SEM) is provided at the bottom of the mounting table 120; a positioning structure for connecting the sample nail table 110 or / and the sample 910 is provided on the preset inclined surface 121 of the mounting table 120. The mounting table 120 can fix the sample 910 to be tested, so as to adjust the sample 910 to meet the angular requirements for both FIB and EBSD characterizations, and can facilitate measuring the angle of the sample 910 relative to the horizontal plane, thereby being beneficial to improving the accuracy of the test results and the reliability of the data.

[0031] Specifically, the bottom surface of the mounting table 120 is a bottom plane that fits the mounting surface of the electron microscope device. The mounting surface of the electron microscope device can be the mounting surface of the main sample stage 210 in the electron microscope device. The included angle between the preset inclined surface 121 and the bottom plane is 20 degrees to 70 degrees; in this embodiment, the included angle between the preset inclined surface 121 and the bottom plane is 45 degrees. The sample mounting device, as a sample holder, can stably and highly precisely fix the FIB processing and EBSD test areas.

[0032] Specifically, the mounting table 120 is provided with a locking structure for locking the sample nail table 110 or / and the sample 910, and the locking structure can be a screw or the like.

[0033] Specifically, the connection structure at the bottom of the mounting table 120 is a bottom plug-in post, which is used to plug into a preset jack of the rotating table (main sample stage 210) in the electron microscope device. The bottom plug-in post can be a cylinder and is plugged into the main sample stage 210 of the electron microscope device.

[0034] Specifically, the positioning structure is a plug-in hole, and the sample pin stage 110 has a pin stage plug-in post that can be plugged into the plug-in hole, which is convenient for installation.

[0035] In this embodiment, the sample mounting device has a 45° pre-tilt angle. There are reserved holes at the upper part of its mounting table 120 (pre-tilt table), into which the commonly used sample pin stage 110 in the electron microscope can be inserted, and the lower part has a structure that can be fixed to the main sample stage 210. During testing, the sample 910 can first be fixed on the sample pin stage 110, then the sample pin stage 110 is inserted into the reserved hole at the upper part of the pre-tilt table, and is fastened by a bolt on the side of the pre-tilt table, so that the sample pin stage 110 and the sample 910 are firmly combined, and then the entire pre-tilt table is inserted into the main sample stage 210 of the electron microscope to complete the installation.

[0036] In specific applications, the sample 910 needs to be basically flat. After being placed on the pin stage, the sample test surface (processing and characterization surface) is basically parallel to the horizontal plane. After being placed on the 45° pre-tilt table, the sample test surface forms an angle of approximately 45° with the horizontal plane. In specific applications, the surface (sample test surface) and the bottom surface of the sample are often not flat. After the sample is placed on the general pin stage 110, the processing and characterization surface forms a small angle relative to the general pin stage 110, and subsequent precise measurement is required to improve the accuracy of the test results and the reliability of the data.

[0037] In specific applications, the sample 910 usually needs to be mechanically polished to make the surface smooth and make the surface and bottom surface of the sample 910 as flat as possible. In specific applications, the entire sample 910 can be coated, which can prevent charging phenomena caused by some non-conductive oxidation regions, dirty regions or resins, which may interfere with SEM observation and FIB processing. It can also use ion beam etching area marking after processing to ensure the alignment of the FIB processing area and the EBSD test area.

[0038] Such as Figures 3 to 5As shown in the figure, the present invention also provides a system for realizing the combined use of FIB characterization and EBSD characterization, including an electron microscope device, the electron microscope device including a main sample stage 210, an SEM component 310 and an FIB component 320, and further including the above-mentioned sample mounting device (sample holder); the sample mounting device is detachably connected to the main sample stage 210, the SEM component 310 and the FIB component 320 are arranged above the main sample stage 210, the lens barrels of the SEM component 310 and the FIB component 320 both point in the direction of the main sample stage 210, and the lens barrels of the SEM component 310 (lens barrel main axis) and the FIB component 320 (lens barrel main axis) are arranged at an angle.

[0039] Specifically, the lens barrel of the SEM component 310 is perpendicular to the horizontal plane, and the angle between the lens barrel of the FIB component 320 and the lens barrel of the SEM component 310 is between 50 degrees and 60 degrees. In this embodiment, the angle between the lens barrel of the FIB component 320 and the lens barrel of the SEM component 310 is 52 degrees or 54 degrees.

[0040] The present invention also provides a method for realizing the combined use of FIB characterization and EBSD characterization. Using the above-mentioned system for realizing the combined use of FIB characterization and EBSD characterization, the method includes the following steps: Measurement step: To measure the precise angle of the sample test surface relative to the horizontal plane, as Figure 3 shown, install the sample on the sample mounting device and install the sample mounting device on the main sample stage 210. Observe the upper and lower edges of the sample 910 through the electron microscope device and record the inclination angle θ1 of the main sample stage 210. It can be obtained that when the sample mounting device is placed horizontally, the angle α between the sample processing surface and the horizontal plane is: 90° - θ1.

[0041] FIB processing step: Rotate the entire main sample stage 210 around its own rotation axis by 180°, and make the sample processing surface form an angle A with the lens barrel of the FIB component 320. As Figure 4 shown, the inclination angle θ2 of the main sample stage 210 = α - (90° - β) + A°, and the range of the angle A is 3° to 7°; EBSD characterization step: Rotate the entire main sample stage 210 around its own rotation axis by 180° to face the EBSD detector. As Figure 5 shown, set the sample processing surface to form an angle B with the horizontal plane. The inclination angle θ3 of the main sample stage 210 = B - α, and the range of the angle B is 65° to 75°.

[0042] Specifically, in the FIB processing step, the angle A is 5°.

[0043] Specifically, in the EBSD characterization step, the angle B is 70°.

[0044] Specifically, between the FIB processing step and the EBSD characterization step, there is also a step of aligning the FIB processing area with the EBSD test area: observing the ion beam etching area on the sample 910 in the scanning electron microscope. This area shows obvious image contrast with the surrounding area and can be used as a marker.

[0045] Specifically, in the FIB processing step, when the processed area is larger than the set area, FIB processing is carried out with an acceleration voltage of 30 kV and a current of 65 nA. Because in the application of the FIB processing step, especially when using gallium ions for processing, it mainly focuses on precision processing at the micro-nano scale and is usually applicable to a relatively small area. The processed cross-section is often less than dozens of micrometers. However, in this embodiment, it is applied to the processing for EBSD, which belongs to polishing processing. In the EBSD step, sometimes it is necessary to characterize an area of several hundred micrometers by several hundred micrometers to be representative. If a current of several nanoamperes or picoamperes is used for processing, it is very time-consuming and has low cost performance. Therefore, in this embodiment, large-current polishing is used to achieve high efficiency and cost performance.

[0046] Specifically, in the FIB processing step, when the processed area in the sample 910 is small or the curtain effect appears, the current is reduced. If the 30 kV voltage causes damage to the sample surface and results in poor EBSD patterns, a voltage of 5 kV can be additionally used to clean the surface of the sample 910. If the size of the processed area in the FIB processing step is very small, after reducing the current, the smaller current can not only complete the processing quickly but also improve the positioning accuracy.

[0047] In this embodiment, after installing and loading the sample 910 into the electron microscope, the combined steps are as follows: Step 1: Measurement step, measuring the precise angle of the sample test surface (processed surface) relative to the horizontal plane. Tilt the main sample stage 210, and determine whether the processed and characterized surface (processed surface) is parallel to the horizontal plane by observing whether the upper and lower edges of the sample 910 coincide through the scanning electron microscope. If the upper and lower edges of the sample 910 coincide, and the tilt angle of the main sample stage 210 at this time is θ1, then the angle α between the sample processed surface and the horizontal plane when the pre-tilt stage is horizontally placed is: 90° - θ1.

[0048] If after the sample 910 is placed on the nail stage, the processed and characterized surface is parallel to the horizontal plane, and after it is placed on the 45° pre-tilt stage, if the upper and lower edges coincide during measurement and the tilt angle of the main sample stage 210 at this time is 45°, then after calculation, this processed and characterized surface forms a 45° angle with the horizontal plane. By accurately measuring the angle, the angle requirements for subsequent FIB processing and EBSD characterization can be ensured.

[0049] Step 2: FIB processing step. The sample mounting device is rotated reversely and tilted to perform FIB processing. The main sample stage 210 rotates 180° as a whole, and then the sample processing surface makes an angle of 5° with the ion beam. To achieve this angle, the angle θ2 that the main sample stage 210 needs to be tilted is θ2 = α - (90° - β) + 5°, that is, θ2 = α + β - 85°. Where β is the angle between the SEM column and the FIB column, usually 52° or 54°. If α is 45 degrees and β is 54 degrees, the value of θ2 is 14°.

[0050] In this embodiment, the processing surface makes an angle of 5° with the ion beam. If the angle is less than this value, problems such as difficult positioning, low processing efficiency, and low processing accuracy will occur. If the angle is greater than this value, deviating from grazing incidence processing may cause problems such as rough processing surface and large damage to the sample 910. When the angle is greater than this value, the ion beam incident on the sample surface will aggravate negative effects such as ion implantation, amorphization, and phase transformation.

[0051] In the FIB processing step, if the processing area is relatively large, such as an area of 500 microns by 500 microns, a 30 kV acceleration voltage and a large current of 65 nA can be used. The sample is cut or milled by the ion beam to expose its internal structure. The overlap (pixel overlap) is selected as 95%, the dose is 2 - 3, and the cycle (number of cycles) is selected as 1. Pixel overlap refers to the overlapping part between adjacent processing areas during multiple processing processes. Selecting an appropriate pixel overlap can reduce processing traces and improve the smoothness of the processing area. The pixel overlap can be selected as 95%, which can ensure sufficient overlap between adjacent processing areas, thus reducing processing traces without significantly increasing the processing time. The dose refers to the energy deposition amount of the ion beam per unit area. An appropriate dose can balance the processing speed and surface quality to ensure a high-quality processing surface within a reasonable time. The number of cycles refers to the number of times of processing the same area. In the FIB processing step of this embodiment, the processing sequence from bottom to top is adopted, and the processing can usually be completed in ten to twenty minutes; if the processing area is small, a small beam current can be used, and the processing can be completed in a few minutes or dozens of seconds; if there is a curtain effect, the current is reduced to one-third of the previous value and the dose is reduced to 0.5 for reprocessing. Most samples can be subjected to EBSD characterization after the above processing. Some phases of the sample will be damaged by the ion beam, and then a voltage of 5 kV can be used for cleaning, and clear patterns can be obtained in the EBSD characterization.

[0052] Step 3: Rotate and tilt the main sample stage 210 in the reverse direction again for EBSD characterization. The entire main sample stage 210 is rotated 180° to face the EBSD detector 330. The normal line of the sample 910 is adjusted to form an angle of 20° with the horizontal plane (the sample surface forms an angle of 70° with the horizontal line, and the normal line of the sample surface forms an angle of 20° with the horizontal plane). To achieve this angle, the angle by which the main sample stage 210 needs to be tilted is: θ3 = 70° - α. Then, the EBSD detector 330 is inserted for characterization.

[0053] Between Step 2 and Step 3, for the convenience of aligning the FIB processing area and the EBSD test area, the ion beam etching area can be used as a marker. The sample as a whole can be coated, which can prevent charging phenomena caused by some non-conductive oxidation areas, dirty areas, or resins, interfering with SEM observation and FIB processing. It can also highlight the processing area after processing. In specific applications, the electron beam acceleration voltage is set to be less than 5 kV, and the in-lens detector is used. It is very easy to locate the processing area. In this way, after FIB processing and after the main sample stage 210 is tilted, it is easier to re-locate the processing area for EBSD characterization by reducing the magnification for observation. Figure 6 is an image after FIB processing by a method for realizing the combined use of FIB characterization - EBSD characterization provided by an embodiment of the present invention; Figure 7 is the EBSD result of EBSD characterization by a method for realizing the combined use of FIB characterization - EBSD characterization provided by an embodiment of the present invention.

[0054] Figure 8 shows the position of the sample after ion beam processing. It can be seen that the processed area is very clear (the dark area) and is easy to find. Before FIB processing, the surface of the sample is platinum-plated. While the ion beam etching area processes the surface for EBSD characterization, it also etches away the platinum on the surface. Therefore, the ion beam etching area can be used as a marker and is very easy to find during EBSD characterization. Otherwise, even if the sample has a processing area, it may not be easy to find the processing area of the sample after rotation and tilting. Figure 9 is the position of the processing area during EBSD characterization, and it can be seen that it is easy to find.

[0055] The sample mounting device in this embodiment can be mounted on the main sample stage 210 of an electron microscope (SEM), providing precise angle adjustment function to meet the requirements of FIB and EBSD for sample tilt angle. The sample mounting device has a compact structure, can stably and highly precisely fix the FIB processing and EBSD testing areas, avoid sample offset, improve the experimental reliability of the combination of the two technologies, support the measurement and recording of the sample tilt angle, ensure high repeatability and consistency of the experiment, reduce the human interference and damage during the sample switching between devices, and enhance the robustness of the entire process. Moreover, the two-way adjustment (positive and negative angles) of the sample angle meets various complex experimental requirements, can switch the angle at any time without affecting the stability of processing and testing. Strictly control the tilt angle adjustment error, especially achieve angle matching between 70° EBSD testing and grazing incidence FIB processing, and improve the accuracy and repeatability of experimental results.

[0056] In this embodiment, by controlling the angle, voltage, and current of the ion beam, the sample processing efficiency is significantly improved, the processing time is shortened to the greatest extent, and the ion source consumption during the processing is reduced. At the same time, the damage to the non-target area is reduced, higher processing area selectivity is achieved, and the fine processing of complex microstructures (such as grain boundaries, multiphase composites) becomes possible. The optimized processing method reduces the thickness of the surface strain layer of the sample, laying a high-quality surface condition for the subsequent optimization of EBSD data acquisition and improving the crystallographic analysis accuracy. In this embodiment, the FIB processing and EBSD testing area alignment technology is adopted. Based on sample marking and precise position calibration, the precise alignment between the processing area and the testing area is ensured, and the experimental error caused by position deviation is significantly reduced. Moreover, the marking method is flexible, adaptable to different sample geometries, improves the compatibility of the device between sample processing and testing, and can be popularized and applied in more complex experiments.

[0057] In this embodiment, the sample holder is combined with the optimized processing and combined use process to form an efficient and stable FIB-EBSD integrated operation system, deeply integrating the advantages of the two technologies. It saves the time cost of switching and adjusting between devices and improves the rapid response ability of the entire process from sample preparation to characterization. While ensuring the pollution-free migration of the sample, it greatly reduces the interference of the environment on the experimental results. The sample mounting device provides a high-quality sample fixing basis as a special sample holder. The FIB fine processing reduces the surface damage layer of the sample and optimizes the diffraction signal intensity and pattern quality of EBSD.

[0058] The FIB processing and EBSD testing areas are precisely calibrated through the alignment technology, narrowing the experimental error range and providing clearer and more reliable analysis results of microstructures and crystallographic characteristics.

[0059] The dedicated sample holder and optimized process are not only applicable to grain boundary, phase boundary and defect analysis, but also greatly improve the micro-area analysis capabilities of multiphase materials, nanomaterials and composite materials.

[0060] The present invention significantly improves the efficiency of FIB processing and EBSD testing, shortens the time for single sample preparation and testing, enables researchers to focus more on scientific research itself, and improves the efficiency and quality of scientific research output. The combination of FIB processing and EBSD characterization reduces the risk of failure and uncertainties in the experimental process, and lowers the experimental cost. The dedicated sample holder designed in the present invention and its optimized technical process have good versatility and can be widely applied to scanning electron microscopes and FIB instruments of different brands and models, providing standardized guidance for the combination of FIB and EBSD technologies to a certain extent, simplifying the operation, lowering the technical threshold, and facilitating the popularization and application of high-end scientific research equipment in the fields of materials science, electronic packaging, aerospace, etc.

[0061] In summary, in the current FIB processing and EBSD combined technology system, there are problems such as an incoherent process, difficult angle adjustment, limited processing area on the sample surface, and deviation in the alignment of the experimental area. The system, method, and sample mounting device provided by the present invention for realizing the combination of FIB characterization and EBSD characterization solve these technical bottlenecks through innovative design and optimized process flow, and adopt a dedicated sample holder to meet the requirements of different tilting angles of the sample for FIB processing and EBSD testing (FIB processing angle close to grazing incidence and EBSD testing angle of about 70°).

[0062] In the prior art, most experiments limit the processing area to the edge. Many experiments assume that the upper and lower surfaces of the sample are flat and parallel to the horizontal plane to adjust the angle, or use a fixed-angle adapter, and lack accurate angle measurement function, which is likely to bring operation errors and angle imbalance.

[0063] The system and method provided by the present invention for realizing the combination of FIB characterization and EBSD characterization can quickly adapt to the angle requirements from FIB to EBSD, without relying solely on fixed devices, avoiding experimental failures and repeated operations caused by angle deviation. Integrating the angle adjustment and processing fixation functions of the sample, avoiding frequent operation of the sample in different steps, optimizing the process flow, reducing human errors and improving efficiency. The sample holder structure is compatible with scanning electron microscopes, dual-beam systems and EBSD detection devices of multiple brands and models, expanding the scope of technical application and having strong adaptability.

[0064] In the prior art, FIB processing usually adopts general standard parameters, ignoring the customized requirements of specific target areas or sample characteristics, resulting in low local processing efficiency, obvious surface damage, and even excessive surface removal.

[0065] The present invention further refines the optimization scheme of FIB process parameters (ion beam voltage, current intensity, scanning mode, relative angle between the sample and the ion beam, etc.), achieving a better balance in terms of processing efficiency, surface quality, and regional selectivity. After optimizing the parameter settings, the material removal speed can be significantly increased while ensuring accuracy, and at the same time, the total experimental duration can be compressed, with higher efficiency. By optimizing the ion beam incident angle and gradually reducing the ion beam voltage, the strain and the thickness of the damaged layer on the processed surface layer of the sample are significantly reduced, providing conditions for high-quality EBSD data acquisition in the subsequent process. The processing accuracy is significantly improved, enabling fine processing in the target area and avoiding interference with non-target areas, making the analysis of micro grain boundaries, phase boundaries, defect positions, etc. more reliable.

[0066] In the prior art, the regional matching between FIB processing and EBSD testing mainly relies on manual alignment by operators, and position deviations often occur due to sample movement or rotation, resulting in misalignment between the detection area and the processing area.

[0067] The present invention introduces a sample alignment method based on physical markers (such as the ion beam etching area as a marker), ensuring direct alignment between the processing area and the testing area, improving the alignment accuracy. By etching the marker, the target area processed by FIB can be quickly found with the help of an electron microscope, avoiding the time-consuming process of repeatedly searching for the target position. The marking method ensures the precise matching of the processing window and the EBSD testing window, reducing the regional offset error caused by equipment switching. For complex topography or multi-layer samples, the alignment accuracy is particularly prominent, effectively improving the microanalysis ability of special samples (such as multi-phase materials) and being applicable to diverse samples.

[0068] In the prior art, although some high-end main sample stages 210 support multi-axis adjustment, inclination disorders or calibration errors often occur during the actual adjustment process; lower-end devices completely rely on manual settings and are difficult to meet the high-precision requirements.

[0069] The present invention can accurately measure and dynamically adjust the sample inclination well, meeting the requirements of nearly vertical FIB processing and a 70° inclination for EBSD testing, and can quickly switch between the two while maintaining accuracy, meeting multiple technical angle requirements: quickly and accurately achieving seamless switching between the angles of FIB processing and EBSD testing, especially avoiding process interruptions caused by angle mismatches in complex experiments. The continuous and refined angle adjustment ability significantly improves the accuracy and fineness of testing, especially suitable for the characterization of complex geometric samples or multi-layer samples. The dynamic adjustment process does not require external complex equipment expansion, realizing the effective utilization of existing instrument resources and reducing the experimental cost.

[0070] In the prior art, the combined use process of FIB processing and EBSD testing is relatively fragmented. Usually, multiple adjustment steps need to be manually completed, resulting in a long process, high errors, and low efficiency. The present invention integrates the above technical improvements to form an efficient combined use process from sample preparation to processing and testing. The experimental efficiency is significantly improved. Through process optimization, the entire operation cycle from sample processing to testing is significantly shortened, and at the same time, the time waste caused by multiple repeated alignment and losses is reduced. The integrated design of the sample holder, processing parameters, and marker alignment ensures the continuity of testing and the reliability of the process. The results of processing and characterization are highly consistent, enhancing the reliability of the combined use.

[0071] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, or improvements made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A sample mounting device, characterized in that: A combined system for FIB characterization-EBSD characterization includes a mounting table with a preset inclined surface, wherein a connection structure for mounting to an electron microscope device is provided at the bottom of the mounting table; and a positioning structure for connecting a sample nail table or / and a sample is provided on the preset inclined surface of the mounting table.

2. The sample mounting device according to claim 1, characterized in that: The bottom surface of the mounting platform is a bottom plane that fits the mounting surface of the electron microscope device, and the angle between the preset inclined surface and the bottom plane is 20 degrees to 70 degrees; And / or, the mounting platform is provided with a locking structure for locking the sample nail platform and / or the sample.

3. The sample mounting device according to claim 1 or 2, characterized in that: The connection structure at the bottom of the mounting platform is a bottom plug-in column, which is used for the preset socket of the rotating platform in the electron microscope device; And / or, the positioning structure is a plug-in hole, and the sample nail table has a nail table plug-in column that can be plugged into the plug-in hole.

4. A system for realizing FIB characterization-EBSD characterization combination, characterized in that: It comprises an electron microscope device, which comprises a main sample stage, a SEM component and a FIB component, and also comprises a sample mounting device as described in any one of claims 1 to 3; the sample mounting device is detachably connected to the main sample stage, the SEM component and the FIB component are arranged above the main sample stage, the lens barrel of the SEM component and the lens barrel of the FIB component both point in the direction of the main sample stage, and the lens barrel of the SEM component and the lens barrel of the FIB component are arranged at an angle.

5. The system for realizing FIB characterization-EBSD characterization combination according to claim 4, characterized in that: The lens barrel of the SEM component is perpendicular to a horizontal plane, and an angle between the lens barrel of the FIB component and the lens barrel of the SEM component is between 50 degrees and 60 degrees.

6. A method for realizing FIB characterization-EBSD characterization combination, characterized in that: The system for realizing FIB characterization-EBSD characterization combination as claimed in claim 4 or 5 comprises the following steps: Measuring steps: to measure the precise angle of the sample test surface relative to the horizontal plane, the sample is mounted on the sample mounting device, and the sample mounting device is mounted on the main sample stage, and the overlap of the upper and lower edges of the sample is observed by an electron microscope and the inclination angle θ1 of the main sample stage is recorded, and it is found that when the sample mounting device is placed horizontally, the angle α between the sample processing surface and the horizontal plane is: 90°- θ1; FIB processing step: rotating the main sample stage as a whole by 180°, and making the sample processing surface form an angle A with the lens barrel of the FIB component, the main sample stage is tilted at an angle θ2=α-(90°-β)+A°, and the angle A ranges from 3° to 7°; EBSD characterization steps: the main sample stage is rotated 180° as a whole to face the EBSD detector, and the sample processing surface is set to an angle B with the horizontal plane. The main sample stage is tilted at an angle θ3=B-α, and the angle B ranges from 65° to 75°.

7. The method for realizing FIB characterization-EBSD characterization combination according to claim 6, characterized in that: In the FIB processing step, the angle A is 5°; In the EBSD characterization step, the angle B is 70°.

8. The method for realizing FIB characterization-EBSD characterization combination according to claim 6, characterized in that: Between the FIB processing step and the EBSD characterization step, there is also a step of aligning the FIB processing area with the EBSD test area: marking the sample by using the ion beam etching area as a mark.

9. The method for realizing FIB characterization-EBSD characterization combination according to claim 6, characterized in that: In the FIB processing step, when the processing area is large, FIB processing is performed using an acceleration voltage of 30 kV and a current of 65 nA.

10. The method for realizing FIB characterization-EBSD characterization combination according to claim 6, characterized in that: In the FIB processing step, when the processing area is small or the sample has a curtain effect, the current is reduced.

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