Analysis method of copper foil section sample

Abstract

The invention discloses a copper foil section sample analysis method, which relates to the technical field of material detection and analysis, and is characterized in that the surface of a to-be-analyzed surface of a to-be-detected sample made of a metal sample or a non-metal sample is subjected to rough machining sample preparation operation through a plasma beam electron beam double-beam electron microscope PFIB, so that the surface smoothness of the to-be-analyzed surface reaches a preset value; the method comprises the following steps: obtaining a current sample meeting a preset condition, continuing to carry out finish machining sample preparation operation on the current sample through PFIB and a current parameter greater than a rough machining sample preparation operation so as to prepare a target sample meeting the EBSD characterization requirement, and carrying out EBSD characterization operation on the target sample through PFIB so as to obtain an analysis result of a to-be-detected sample. And a prepared sample can be ground and polished. The sample is not scratched, the sample is not deformed, blurring of the grain boundary during EBSD analysis caused by sample scratching and sample deformation is avoided, the integrity and authenticity of the surface of the sample are ensured, and the accuracy of analysis data is further ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of metal microscopic analysis, and particularly relates to a method for analyzing a copper foil cross-section sample. Background Art

[0002] In the field of materials science, in-depth understanding of the microstructure of materials is the key to optimizing material properties. With the development of technology, the Electron Back Scatter Diffraction (EBSD) technology has emerged, which can provide key information such as grain orientation, grain boundary characteristics, and phase distribution of materials. EBSD sample preparation includes steps such as wire cutting, degreasing, embedding, grinding, and polishing (mechanical polishing and electrolytic polishing). During the sample preparation process, grinding, mechanical polishing, and electrolytic polishing are three key steps, and such steps usually involve gradually grinding using sandpapers of multiple particle sizes, and then performing chemical or electrolytic polishing.

[0003] However, during mechanical grinding, the surface of the sample is easily scratched and deformed, resulting in blurred grain boundaries during EBSD analysis, leading to surface damage and sample distortion of the sample, and affecting the accuracy of data. In addition, although electrolytic polishing can improve surface smoothness, when dealing with complex microstructures, there may still be residual surface defects, which have an adverse impact on EBSD analysis. Summary of the Invention

[0004] The main objective of the present invention is to propose a method for analyzing a copper foil cross-section sample, aiming to solve the technical problem in the prior art that during mechanical grinding, the surface of the sample is easily scratched and deformed, resulting in blurred grain boundaries during EBSD analysis, leading to surface damage and sample distortion of the sample, and affecting the accuracy of data.

[0005] To achieve the above objective, in the first aspect, a method for analyzing a sample cross-section proposed by the present invention includes the following steps:

[0006] Performing rough machining sample preparation on the surface of the surface to be analyzed of the sample to be measured by a Plasma Focused Ion Beam (PFIB) to obtain a current sample meeting preset conditions; wherein, the preset conditions are that the surface smoothness of the sample to be measured reaches a preset value, and the sample to be measured is a metal sample or an alloy sample;

[0007] Performing finish machining sample preparation on the current sample by the PFIB to prepare a target sample meeting the EBSD characterization requirements; wherein, the current parameter of the finish machining sample preparation is less than the current parameter of the rough machining sample preparation;

[0008] Performing EBSD characterization on the target sample by the PFIB to obtain the analysis result of the sample to be measured.

[0009] In one embodiment, the step of performing rough machining sample preparation on the surface of the surface to be analyzed of the sample to be tested by a plasma beam electron beam dual-beam electron microscope PFIB to obtain a current sample meeting preset conditions includes:

[0010] Performing rough machining sample preparation on the surface of the surface to be analyzed of the sample to be tested by the PFIB with a first current to obtain a current sample meeting the preset conditions; wherein, the first current is I 1 , I 1 Satisfies: 0.2 μA ≤ A ≤ 2.5 μA.

[0011] In one embodiment, the step of performing finish machining sample preparation on the current sample by the PFIB to prepare a target sample meeting the EBSD characterization requirements includes:

[0012] Performing finish machining sample preparation on the current sample by the PFIB with a second current to prepare a target sample meeting the EBSD characterization requirements; wherein, the second current is I 2 , I 2 Satisfies: 15 nA ≤ B ≤ 60 nA.

[0013] In one embodiment, before the step of performing rough machining sample preparation on the surface of the surface to be analyzed of the sample to be tested by a plasma beam electron beam dual-beam electron microscope PFIB to obtain a current sample meeting preset conditions, the method further includes:

[0014] Depositing a platinum protective layer on a surface of the sample to be tested by the PFIB to obtain a surface to be analyzed.

[0015] In one embodiment, the thickness of the platinum protective layer is C, and C satisfies: 1 μm ≤ C ≤ 4 μm.

[0016] In one embodiment, before the step of depositing a platinum protective layer on a surface of the sample to be tested by the PFIB to obtain a surface to be analyzed, the method further includes:

[0017] Fixing the sample to be tested on a pre-tilting stage with a preset inclination angle; wherein, the preset inclination angle is 36°;

[0018] Controlling the pre-tilting stage to tilt by a first angle so that the surface of the sample to be tested is perpendicular to the direction of the ion beam emitted by the PFIB; wherein, the first angle is 16°;

[0019] Obtaining a target area on the sample to be tested.

[0020] In one embodiment, the step of performing EBSD characterization on the target sample by the PFIB to obtain the analysis result of the sample to be tested includes:

[0021] After the PFIB descends to a preset position and rotates a preset angle, perform EBSD characterization operation on the target sample with a third current to obtain the analysis result of the sample to be measured; wherein, the preset position is that the height of the sample stage is 16 mm, the preset angle is 180°, and the third current is I 3 , I 3 is 13 nA.

[0022] In one embodiment, the sample preparation width of the rough machining sample preparation operation is D, and 20 μm ≤ D ≤ 30 μm.

[0023] In one embodiment, the sample to be measured is a copper foil sample.

[0024] In one embodiment, the sample preparation area of the sample to be measured is E, 1 mm 2 ≤ E ≤ 2 mm 2 .

[0025] When the technical solution of the present invention is used, perform rough machining sample preparation operation on the surface of the surface to be analyzed of the sample to be measured made of a metal sample or a non-metal sample through a plasma beam electron beam dual-beam electron microscope PFIB, so that the surface smoothness of the surface to be analyzed reaches a preset value, and obtain the current sample that meets the preset conditions. Continue to perform fine machining sample preparation operation on the current sample through PFIB with current parameters greater than those during the rough machining sample preparation operation to prepare a target sample that meets the EBSD characterization requirements. Perform EBSD characterization operation on the target sample through PFIB to obtain the analysis result of the sample to be measured, which also enables the present invention to grind and polish the sample during sample preparation. At the same time, since the current magnitudes used during the rough machining sample preparation operation and the fine machining sample preparation operation are different, and the current magnitude of the fine machining sample preparation operation is greater than that during the rough machining, the present invention will not scratch the sample or cause the sample to deform during sample preparation, avoiding the grain boundary blur during EBSD analysis caused by scratching the sample and sample deformation, ensuring the integrity and authenticity of the sample surface, and thus ensuring the accuracy of the analysis data. In addition, the present invention adopts the cooperation of the rough machining sample preparation operation and the fine machining sample preparation operation to achieve the purpose of polishing the complex microstructure to change the surface smoothness of the sample, avoiding residual surface defects. Description of the Drawings

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on the structures shown in these drawings.

[0027] Figure 1 Flow chart of the sample cross-section analysis method provided by the present invention;

[0028] Figure 2 Flow chart of some specific embodiments of the examples of the present invention;

[0029] Figure 3 EBSD inverse pole figure of the copper foil cross-section sample provided by the present invention with respect to the horizontal direction;

[0030] Figure 4 EBSD inverse pole figure corresponding to the first embodiment provided by the present invention;

[0031] Figure 5 EBSD inverse pole figure corresponding to the second embodiment provided by the present invention;

[0032] Figure 6 EBSD inverse pole figure corresponding to the third embodiment provided by the present invention;

[0033] Figure 7 EBSD inverse pole figure of the initial state of the copper foil cross-section provided by the present invention.

[0034] The realization, functional features and advantages of the object of the present invention will be further described in conjunction with the embodiments with reference to the accompanying drawings. Detailed implementation manners

[0035] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.

[0036] It should be noted that if there are directional indications (such as up, down, left, right, front, back...) involved in the embodiments of the present invention, the directional indications are only used to explain the relative positional relationship and movement conditions between components in a certain specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0037] In addition, if the embodiments of the present invention involve descriptions such as "first" and "second", the descriptions of "first", "second", etc. are only for descriptive purposes and should not be construed as indicating or implying their relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one such feature. In addition, if "and / or" or "and / or" appears throughout the text, its meaning includes three parallel scenarios. Taking "A and / or B" as an example, it includes scenario A, scenario B, or the scenario where both A and B are satisfied simultaneously. In addition, the technical solutions between various embodiments can be combined with each other, but it must be based on the ability of those of ordinary skill in the art to implement. When the combination of technical solutions results in contradictions or is unable to be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0038] The present invention provides a method for analyzing a copper foil cross-section sample.

[0039] Please refer to Figures 1 to 7 , for ease of understanding, the method for analyzing a sample cross-section includes the following steps:

[0040] S100. Perform rough machining sample preparation on the surface of the surface to be analyzed of the sample to be tested through a plasma focused ion beam (PFIB) to obtain a current sample meeting preset conditions; wherein, the preset conditions are that the surface smoothness of the sample to be tested reaches a preset value, and the sample to be tested is a metal sample or an alloy sample.

[0041] More specifically, step S100 includes:

[0042] Perform rough machining sample preparation on the surface of the surface to be analyzed of the sample to be tested through the PFIB with a first current to obtain a current sample meeting the preset conditions; wherein, the first current is I 1 , I 1 satisfies: 0.2 μA ≤ A ≤ 2.5 μA.

[0043] It should be specifically and clearly noted that the sample preparation width of the exemplary rough machining sample preparation is D, 20 μm ≤ D ≤ 30 μm. The sample to be tested is a copper foil sample. The sample preparation area of the sample to be tested is E, 1 mm 2 ≤ E ≤ 2 mm 2 .

[0044] In this embodiment, the specific process of performing primary processing on the surface of the surface to be analyzed through a plasma focused ion beam (Plasma Focused Ion Beam) is as follows:

[0045] Sample preparation: Cut a small piece of sample from the copper foil specimen using scissors, and the size can be controlled within 1 mm 2-2 mm 2 or so for easy fixation on the PFIB sample stage. Fix the sample on the 36° side of the 54 / 36° pre-tilt stage using conductive adhesive.

[0046] Pretreatment: Place the sample into the electron microscope, start the PFIB system, raise the sample stage to a height of 4 mm. Locate the target area and tilt the sample stage by 16° to make the sample surface perpendicular to the ion beam direction, providing the optimal ion beam incident angle (52°) for subsequent processing.

[0047] Pt protective layer deposition: Deposit a platinum (Pt) protective layer on the target area using an ion beam to prevent damage to the sample during the ion beam processing. The deposition thickness of this protective layer can be controlled between 1 μm and 4 μm to ensure cross-section integrity and non-destructiveness. The protective layer is deposited to protect the integrity of the cross-section sample. In the first embodiment, the protective layer was not deposited, and part of the cross-section was damaged, and the EBSD characterization area was incomplete.

[0048] Rough machining sample preparation operation: Set the ion beam voltage and current to 30 kV and 0.2 μA - 2.5 μA, and perform preliminary rough machining on the copper foil sample to remove unnecessary rough and irregular copper foil cross-sections, exposing a relatively regular copper foil cross-section. The rough machining speed is relatively fast in this step, but it will be controlled within a certain width (20 μm to 30 μm) to avoid damaging the structural integrity of the sample.

[0049] S200. Perform a finish machining sample preparation operation on the current sample through the PFIB to prepare a target sample that meets the EBSD characterization requirements; wherein, the current parameter of the finish machining sample preparation operation is less than the current parameter of the rough machining sample preparation operation;

[0050] More specifically, step S200 includes:

[0051] Perform a finish machining sample preparation operation on the current sample through the PFIB with a second current to prepare a target sample that meets the EBSD characterization requirements; wherein, the second current is I 2 , I 2 satisfies: 15 nA ≤ B ≤ 60 nA.

[0052] In this embodiment, when performing the finish machining sample preparation operation: Adjust the ion beam current to 15 nA - 60 nA while maintaining a voltage of 30 kV to reduce the damage introduced by rough machining and further flatten the cross-section, ensuring that the sample thickness and surface flatness meet the EBSD analysis requirements.

[0053] S300. Perform an EBSD characterization operation on the target sample through the PFIB to obtain the analysis result of the sample to be tested.

[0054] More specifically, step S300 includes:

[0055] After the PFIB descends to a preset position and rotates a preset angle, perform EBSD characterization on the target sample with a third current to obtain the analysis result of the sample to be measured; wherein, the preset position is that the height of the sample stage is 16 mm, the preset angle is 180°, and the third current is I 3 , I 3 is 13 nA.

[0056] In this embodiment, when performing EBSD characterization, lower the height of the sample stage to 16 mm, rotate the sample stage 180°, set the electron beam voltage and current to 20 kV and 13 nA respectively, and perform EBSD characterization to ensure obtaining high-quality crystal orientation, grain boundary and phase distribution information.

[0057] In this embodiment, the surface of the surface to be analyzed of the sample to be measured made of a metal sample or a non-metal sample is rough processed by a plasma focused ion beam (PFIB) to make the surface smoothness of the surface to be analyzed reach a preset value, and a current sample meeting the preset conditions is obtained. Then, continue to perform fine processing on the current sample by PFIB with a current parameter greater than that during the rough processing to prepare a target sample that meets the requirements of EBSD characterization. Perform EBSD characterization on the target sample by PFIB to obtain the analysis result of the sample to be measured. That is, when making a sample in the present invention, grinding and polishing can be performed on the sample to be made. At the same time, since the current magnitudes used during the rough processing and the fine processing are different, and the current magnitude during the fine processing is greater than that during the rough processing, when making a sample in the present invention, the sample will not be scratched and will not be deformed, avoiding the blurring of grain boundaries during EBSD analysis caused by scratching the sample and sample deformation, ensuring the integrity and authenticity of the sample surface, and thus ensuring the accuracy of the analysis data. In addition, the present invention uses the cooperation of rough processing and fine processing to achieve the purpose of polishing complex microstructures to change the surface smoothness of the sample, avoiding residual surface defects.

[0058] Please refer to Figure 4 , in the first embodiment of the example of the present invention, the EBSD analysis method for a copper foil sample is:

[0059] Sample preparation: Cut a small piece of sample from a copper foil specimen with scissors, fix it on the 36° side of a 54 / 36° pre-tilting stage with conductive glue, and place it in the electron microscope.

[0060] Rough machining: Start the PFIB system and raise the sample stage height to 4 mm. Select the region of interest and tilt the sample by 16° to ensure that the sample cross-section is perpendicular to the ion beam direction. Set the ion beam voltage to 30 kV and the current to 0.5 μA, and perform rough machining on the sample.

[0061] EBSD characterization: Lower the sample stage to 16 mm and rotate it by 180°. Set the electron beam voltage to 20 kV and the current to 13 nA, and perform EBSD characterization on the sample cross-section. Under this step, the stable setting of the electron beam ensures the high-resolution orientation image quality of the sample.

[0062] Due to the uneven surface of the sample, the "curtain effect" of the cross-section is severe, so columnar crystal structures of copper can be seen inside the sample in the figure. In addition, due to the relatively large bombardment beam current, the lower part of the inverse pole figure is severely amorphous, so the indexing rate of the Kikuchi patterns of the samples prepared under this condition is poor.

[0063] Please refer to Figure 5 , in the second embodiment of the example of the present invention, the EBSD analysis method for the copper foil sample is as follows:

[0064] Sample preparation: Also use scissors to cut small pieces of the sample from the copper foil specimen, fix it on the 36° side of the 54 / 36° pre-tilting stage with conductive glue, and place it in the electron microscope.

[0065] Rough machining: Start the PFIB system, set the sample stage height to 4 mm, and locate the region of interest. Tilt the sample by 16° to ensure that the cross-section is perpendicular to the ion beam direction. Deposit a Pt protective layer (ion beam voltage is 12 kV, current is 8 nA) on the region of interest to avoid damage caused by machining. Set the ion beam voltage to 30 kV and the current to 0.2 μA, and perform rough machining on the sample.

[0066] EBSD characterization: Lower the sample stage to 16 mm and rotate the sample stage by 180°. Set the electron beam voltage and current to 20 kV and 13 nA respectively, and perform EBSD characterization on the cross-section. Under this setting, the obtained sample crystal orientation information has good resolution and clarity.

[0067] Compared with the first embodiment, the processing beam current of this sample is smaller, so the "curtain effect" of the sample cross-section is not severe. In the figure, it can be seen that in addition to the columnar crystal structure inside the sample, there are also some fine equiaxed crystals. Near the sample surface at the lower part of the inverse pole figure, due to the formation of amorphous during beam bombardment, the patterns in some regions still cannot be analyzed.

[0068] Please refer to Figure 6 , in the third embodiment of the example of the present invention, the EBSD analysis method for the copper foil sample is as follows:

[0069] Sample preparation: Similarly, cut small pieces of samples from the copper foil specimens using scissors, fix them on the 36° side of the 54 / 36° pre-tilting stage with conductive adhesive, and place them into the electron microscope.

[0070] Rough machining: Start the PFIB system, set the sample stage height to 4 mm, and locate the region of interest. Tilt the sample by 16° to ensure that the cross-section is perpendicular to the ion beam direction. Deposit a Pt protective layer on the region of interest (ion beam voltage is 12 kV, current is 8 nA) to avoid damage caused by machining. Set the ion beam voltage to 30 kV and the current to 0.5 μA to perform rough machining on the sample. This high-current parameter is used for faster material removal, suitable for the initial cutting of a larger cross-section, revealing the sample cross-section in a shorter time. However, this step is suitable for sample preparation cases with lower surface accuracy requirements.

[0071] Finish machining: Reduce the ion beam current to 60 nA while maintaining a voltage of 30 kV, and further perform fine machining on the sample cross-section to remove the microscopic roughness introduced by rough machining and ensure that the cross-section surface meets the EBSD requirements.

[0072] EBSD characterization: Lower the sample stage to 16 mm and rotate the sample stage by 180°.

[0073] Set the electron beam voltage and current to 20 kV and 13 nA respectively, and perform EBSD characterization on the cross-section. Under this setting, the obtained sample crystal orientation information has good resolution and clarity.

[0074] Due to the deposition of the protective layer, no "curtains" generated by ion beam bombardment are formed on the sample surface. Therefore, compared with the first embodiment and the second embodiment, the proportion of fine equiaxed crystal grains inside the cross-section sample is the largest. In addition, after the deposition of the protective layer, the pattern resolution near the sample surface below the inverse pole figure is higher. This shows that depositing a Pt protective layer can effectively prevent the generation of amorphous.

[0075] In the preparation of copper foil cross-section samples, by adjusting the ion beam current multiple times, the rough machining and finish machining steps are optimized. After adding the Pt protective layer, the cross-section damage is significantly reduced, and the prepared samples obtain higher resolution in EBSD testing, proving the effectiveness and feasibility of the present invention in microstructure research.

[0076] The present invention provides an efficient and low-damage method for preparing copper foil cross-section samples. Through multi-step ion beam processing and protective layer deposition, the samples maintain high crystal integrity and surface flatness in EBSD analysis, and more microscopic detail information can also be obtained.

[0077] Cross-sectional view of the original untreated copper foil (the original cross-section without PFIB treatment is uneven and curled, and the EBSD results show very few details, unable to reflect the true information of the grain orientation and grain boundaries of the copper foil cross-section).

[0078] In one embodiment, before step S100, the method further includes:

[0079] S400. Depositing a platinum protective layer on a surface of the sample to be measured through the PFIB to obtain a surface to be analyzed.

[0080] In this embodiment, the thickness of the platinum protective layer deposited on the surface of the sample to be measured is C, and C satisfies: 1μm ≤ C ≤ 4μm.

[0081] In one embodiment, before step S400, the method further includes:

[0082] S500. Fixing the sample to be measured on the pre-tilting stage with a preset inclination angle; wherein, the preset inclination angle is 36°.

[0083] In this embodiment, when fixing the sample to be measured on the pre-tilting stage, a conductive adhesive can be used to fix the sample to be measured on the pre-tilting stage.

[0084] S600. Controlling the pre-tilting stage to tilt by a first angle so that the surface of the sample to be measured is perpendicular to the direction of the ion beam emitted by the PFIB; wherein, the first angle is 16°.

[0085] In this embodiment, since the direction of the ion beam emitted by the PFIB is a fixed direction, in order to improve the deposition effect of the platinum protective layer, the inclination angle of the pre-tilting stage should be such that the surface of the tilting stage is perpendicular to the emission direction of the ion beam to be measured.

[0086] S700. Obtaining a target area on the sample to be measured.

[0087] In this embodiment, an exemplary target area is the area where the platinum protective layer is deposited.

[0088] The above is only an exemplary embodiment of the present invention, and does not limit the patent scope of the present invention. Any equivalent structural transformation made under the technical concept of the present invention by using the content of the specification and drawings of the present invention, or directly / indirectly applied in other related technical fields, is included in the patent protection scope of the present invention.

Claims

1. A sample cross-section analysis method, characterized in that: The steps include: The surface of the sample to be analyzed is rough-processed and sampled by a plasma beam electron beam dual-beam electron microscope PFIB to obtain a current sample that meets a preset condition; wherein the preset condition is that the surface smoothness of the sample to be tested reaches a preset value, and the sample to be tested is a metal sample or an alloy sample; Performing a fine processing sample preparation operation on the current sample by the PFIB to prepare a target sample that meets the EBSD characterization requirements; wherein the current parameter of the fine processing sample preparation operation is smaller than the current parameter of the rough processing sample preparation operation; The PFIB is used to perform EBSD characterization on the target sample to obtain the analysis result of the sample to be tested.

2. The sample cross-section analysis method according to claim 1, characterized in that: The step of performing rough processing and sample preparation on the surface of the sample to be analyzed by using a plasma beam electron beam dual beam electron microscope PFIB to obtain a current sample that meets the preset conditions includes: The PFIB performs rough processing on the surface of the to-be-analyzed surface of the to-be-tested sample with a first current to obtain a current sample that meets the preset conditions; wherein the first current is I1, and I1 satisfies: 0.2μA≤A≤2.5μA.

3. The sample cross-section analysis method according to claim 1, characterized in that: The step of performing fine processing and sample preparation on the current sample by the PFIB to prepare a target sample that meets the EBSD characterization requirements includes: The current sample is finely processed and prepared by the PFIB with a second current to obtain a target sample that meets the EBSD characterization requirements; wherein the second current is I2, and I2 satisfies: 15nA≤B≤60nA.

4. The sample cross-section analysis method according to claim 1, characterized in that: Before the step of performing rough processing on the surface of the to-be-analyzed surface of the sample to be tested by the plasma beam electron beam dual beam electron microscope PFIB to obtain the current sample meeting the preset conditions, the method further comprises: A platinum protective layer is deposited on a surface of the sample to be tested by the PFIB to obtain a surface to be analyzed.

5. The sample cross-section analysis method according to claim 4, characterized in that: The thickness of the platinum protective layer is C, and C satisfies: 1 μm≤C≤4 μm.

6. The sample cross-section analysis method according to claim 4, characterized in that: Before the step of depositing a platinum protective layer on a surface of the sample to be tested by the PFIB to obtain a surface to be analyzed, the method further includes: Fixing the sample to be tested on a pre-tilting table with a preset inclination angle; wherein the preset inclination angle is 36°; Controlling the pre-tilt stage to tilt at a first angle so that the surface of the sample to be tested is perpendicular to the direction of the ion beam emitted by the PFIB; wherein the first angle is 16°; A target area is obtained on the sample to be tested.

7. The sample cross-section analysis method according to any one of claims 1 to 6, characterized in that: The step of performing EBSD characterization on the target sample by using the PFIB to obtain the analysis result of the sample to be tested includes: The PFIB is lowered to a preset position and rotated by a preset angle, and then an EBSD characterization operation is performed on the target sample with a third current to obtain an analysis result of the sample to be tested; wherein, the preset position is that the height of the sample stage is 16 mm, the preset angle is 180°, and the third current is I3, and I3 is 13nA.

8. The sample cross-section analysis method according to any one of claims 1 to 6, characterized in that: The sample preparation width of the rough processing sample preparation operation is D, 20μm≤D≤30μm.

9. The sample cross-section analysis method according to any one of claims 1 to 6, characterized in that: The sample to be tested is a copper foil sample.

10. The sample cross-section analysis method according to any one of claims 1 to 6, characterized in that: The sample preparation area of ​​the sample to be tested is E, 1mm1≤E≤2mm1.

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