A focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method

Abstract

The present invention relates to the field of three-dimensional reconstruction technology, and in particular to a focused ion beam-scanning electron microscope three-dimensional structure reconstruction correction method, comprising: processing a material to obtain a material sample having a spherical particle attachment layer; filling pores with a component containing epoxy resin under vacuum conditions; after the epoxy resin is completely cured, processing the sample to be tested to expose the material and spherical particles along the normal direction of the spherical particle attachment layer; polishing the exposed material and the junction of the spherical particles to determine the area of ​​interest; cutting and scanning the area of ​​interest with a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence, and performing three-dimensional reconstruction to obtain a three-dimensional digitized image; and correcting the three-dimensional digitized image based on the size and shape of the spherical particles. The present invention can correct the three-dimensional reconstruction results of the micro-nano structure of the material by a focused ion beam-scanning electron microscope to obtain a high-precision three-dimensional reconstructed image.

Description

Technical Field

[0001] The invention relates to the technical field of three-dimensional reconstruction, and in particular to a focused ion beam-scanning electron microscope three-dimensional structure reconstruction correction method. Background Art

[0002] 3D reconstruction based on focused ion beam-scanning electron microscopy (FIB-SEM) is a relatively mature 3D reconstruction technology. This technology can achieve a maximum resolution of 3nm and is very suitable for reconstructing micro-nano structures in porous materials. However, when this technology is actually used, in order to make the focused ion beam perpendicular to the surface of the sample being measured, the inclination angle of the sample stage must be maintained at 54°. This results in the scanning electron microscope's viewing angle not being completely facing the sample surface during the formation of a series of slices, but having a certain amount of inclination. At the same time, the scanning electron microscope will have a certain amount of drift during the process of taking a series of two-dimensional images of slices. These two factors will interfere with the final 3D reconstruction results, resulting in the problem of distortion in the obtained microstructure 3D digital image, reducing the accuracy of 3D reconstruction, and thus affecting the subsequent further quantitative analysis of the material's micro-nano structure. Summary of the invention

[0003] 1. Technical issues to be resolved

[0004] The technical problem to be solved by the present invention is to solve the problem in the prior art that the three-dimensional reconstruction results are distorted due to interference introduced by lens tilt and drift, so as to achieve high-precision three-dimensional reconstruction of the micro-nano structure of functional porous materials.

[0005] (II) Technical solution

[0006] In order to solve the above technical problems, the present invention provides a focused ion beam-scanning electron microscope three-dimensional structure reconstruction correction method, comprising:

[0007] Processing the material to obtain at least one cross section, and using the cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer;

[0008] Under vacuum conditions, using a component containing epoxy resin to fill pores in the material sample to obtain a filled sample to be tested;

[0009] After the epoxy resin is completely cured, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer;

[0010] Polishing the exposed material and the interface between the spherical particles to determine the area of ​​interest;

[0011] Using a focused ion beam-scanning electron microscope to cut and scan the region of interest, obtain a two-dimensional image sequence, and perform three-dimensional reconstruction to obtain a three-dimensional digital image;

[0012] The three-dimensional digitized image is corrected based on the size and shape of the spherical particles.

[0013] Optionally, the focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method further includes:

[0014] The corrected three-dimensional digitized image is cropped to obtain a three-dimensional reconstructed image of the micro-nano structure of the material.

[0015] Optionally, the diameter of the spherical particles is of the same order of magnitude as the characteristic size of the micro-nano structure of the material.

[0016] Optionally, the focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method further includes:

[0017] Prior to pore filling of the material samples, the components including the epoxy resin were degassed under vacuum.

[0018] Optionally, under vacuum conditions, when the pores of the material sample are filled with a component containing epoxy resin, the vacuum degree ranges from 0.1 to 0.15 atm.

[0019] Optionally, the focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method further includes:

[0020] After the pores of the material sample are filled, the sample to be tested is allowed to stand for no less than 12 hours.

[0021] Optionally, polishing the exposed material and the interface between the spherical particles comprises:

[0022] An ion beam polisher is used to find clear material and the interface between the spherical particles, and the interface is ion beam polished.

[0023] Optionally, the epoxy resin is EpoFix Kit cold mounting epoxy resin.

[0024] Optionally, processing the material to obtain at least one cross section includes:

[0025] Cut and grind the material to obtain two perpendicular cross sections with smooth surfaces;

[0026] Processing the sample to be tested to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer includes:

[0027] The sample to be tested is polished until a cross section where the spherical particles are not adhered is exposed.

[0028] The present invention also provides a focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method, comprising:

[0029] Processing the material to obtain at least one cross section, and using the cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer;

[0030] Under vacuum conditions, using a component containing epoxy resin to fill pores in the material sample to obtain a filled sample to be tested;

[0031] After the epoxy resin is completely cured, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer;

[0032] Polishing the exposed material and the interface between the spherical particles to determine the area of ​​interest;

[0033] Using a focused ion beam-scanning electron microscope to cut and scan the region of interest to obtain a two-dimensional image sequence;

[0034] Correcting the three-dimensional digitized image based on the size and shape of the spherical particles;

[0035] Based on the shape of the spherical particles, the two-dimensional image sequence is corrected one by one, and three-dimensional reconstruction is performed based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image.

[0036] (III) Beneficial effects

[0037] The above-mentioned technical scheme of the present invention has the following advantages: The present invention provides a focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method. The present invention uses the size and shape of spherical particles to correct the three-dimensional digital image obtained by the focused ion beam-scanning electron microscope three-dimensional reconstruction technology, which can effectively correct the microstructure distortion phenomenon caused by a certain tilt angle and drift between the scanning electron microscope imaging lens and the ion beam, and realize accurate three-dimensional reconstruction of the micro-nanoscale structure inside the material. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 It is a schematic diagram of the steps of a focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method in an embodiment of the present invention;

[0039] Figure 2 is a schematic diagram of the structure of a sample to be tested in an embodiment of the present invention;

[0040] Figure 3 is a schematic diagram of a continuous two-dimensional image sequence obtained in an embodiment of the present invention;

[0041] Figure 4 is a schematic diagram of a three-dimensional digital image obtained by three-dimensional reconstruction in an embodiment of the present invention;

[0042] Figure 5 is a schematic diagram of correcting xy plane data in a three-dimensional digitized image in an embodiment of the present invention;

[0043] Figure 6(a) to Figure 6(c) is an image of the spherical particle attachment layer region in the xz plane direction in an embodiment of the present invention;

[0044] Figure 7(a) to Figure 7(c) is an image of the material region in the xz plane direction in an embodiment of the present invention;

[0045] Figure 8(a) to Figure 8(c) It is an image of the spherical particle attachment layer area and the material area in the yz plane direction in the embodiment of the present invention. DETAILED DESCRIPTION

[0046] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0047] As mentioned above, the prior art technology of three-dimensional reconstruction based on focused ion beam-scanning electron microscope is restricted by the actual structure and use environment of the focused ion beam-scanning electron microscope. There is a distortion phenomenon in the reconstruction result caused by a certain tilt angle and drift between the scanning electron microscope imaging lens and the ion beam, which affects the subsequent further quantitative analysis of the material micro-nano structure. At present, the existing methods cannot correct the three-dimensional reconstruction results of the focused ion beam-scanning electron microscope, and the accuracy of the obtained three-dimensional reconstructed image of the micro-nano structure is low. In view of this, the present invention proposes a three-dimensional structure reconstruction correction method that can correct the data collected by the focused ion beam-scanning electron microscope, so as to achieve accurate three-dimensional reconstruction of the material micro-nano structure.

[0048] like Figure 1 As shown, a focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method (hereinafter referred to as the method of the present invention) provided in an embodiment of the present invention comprises:

[0049] Step 100, processing the material to be analyzed to obtain at least one cross section, and using one cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer.

[0050] This step 100 is to perform preliminary processing on the material to be tested to obtain a flat cross section so as to expose the internal microstructure of the material. The cross-sectional area obtained by processing should be larger than the size of the desired reconstructed region. A plurality of spherical particles are adhered to a flat cross section, that is, a spherical particle attachment layer is formed on the surface of the material to be tested. The spherical particle attachment layer serves as a reference for correcting the measured data. The specific values ​​of the thickness of the spherical particle attachment layer and the number of spherical particles contained therein can be set according to actual conditions and are not further limited here.

[0051] Step 102: Under vacuum conditions, a component including epoxy resin is used to fill pores in a material sample having a spherical particle attachment layer to obtain a filled sample to be tested.

[0052] This step 102 fills the microstructure pores of the material itself and the gaps between the spherical particles in the spherical particle attachment layer, with the purpose of filtering out the interference caused by the pore background in the electron microscope image and improving the clarity of the three-dimensional reconstructed image.

[0053] Step 104, after the epoxy resin is completely cured, the sample to be tested is processed to form an exposed surface along the normal direction of the spherical particle attachment layer, that is, the direction perpendicular to the cross section of the spherical particles, to expose the material and the spherical particles.

[0054] This step 104 further processes the sample to be tested, for example, grinding or cutting the sample to be tested obtained in step 102 to remove part of the epoxy resin on the surface of the sample to be tested, so that the material and the spherical particle attachment layer are exposed for subsequent observation. The purpose of exposing the material and the spherical particles along the normal direction of the spherical particle attachment layer is to facilitate lateral observation and reconstruction of the specific microstructure at the interface between the material and the spherical particle attachment layer.

[0055] Step 106, polishing the exposed material and the interface between the spherical particles to determine the region of interest to be observed.

[0056] The region of interest to be observed should contain materials and multiple spherical particles. Preferably, at least 3 layers of spherical particles are visible, and more preferably, 4 to 5 layers of spherical particles are visible. If there are too few spherical particles in the selected region of interest, it is difficult to perform image correction, which may affect the accuracy of the correction result. If there are too many spherical particles in the selected region, they will occupy the observable material area.

[0057] Step 108, using a focused ion beam-scanning electron microscope to cut and scan the determined region of interest, obtain a continuous two-dimensional image sequence, and perform three-dimensional reconstruction based on the two-dimensional image sequence to obtain a three-dimensional digital image corresponding to the region of interest.

[0058] This step 108 alternately cuts and scans the region of interest containing the material and the plurality of spherical particles to obtain a continuous two-dimensional image sequence, and then aligns the obtained two-dimensional image sequence to achieve three-dimensional reconstruction. The thickness of the slice cut by the ion beam should be as uniform as possible and equal to the actual pixel size of the electron microscope two-dimensional image. The specific steps of three-dimensional reconstruction based on focused ion beam-scanning electron microscope can refer to the prior art, and will not be further described here.

[0059] Step 110, correcting the obtained three-dimensional digitized image based on the size and shape of the spherical particles.

[0060] This step 110 adopts image correction technology to correct the ellipsoidal particles of the spherical particle attachment layer in the obtained three-dimensional digital image to a spherical shape and original size. At the same time, the material area adjacent to the spherical particle attachment layer is also corrected, that is, the microstructure distortion caused by the tilt and drift of the lens is corrected, and a more realistic and accurate three-dimensional reconstruction result is obtained. The specific image correction step preferably includes operations such as scaling and shearing transformation of the three-dimensional image. The image correction can refer to the existing technology and will not be further described here.

[0061] Preferably, the method of the present invention further comprises:

[0062] Step 112, cropping the corrected three-dimensional digitized image to obtain a three-dimensional reconstructed image of the micro-nano structure of the material.

[0063] This step 112 removes the three-dimensionally reconstructed spherical particle attachment layer region in the corrected three-dimensional digitized image, and only retains the observed real material micro-nano structure, thus completing the accurate three-dimensional reconstruction of the micro-nano structure.

[0064] The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method provided by the present invention adds spherical particles for correction on the surface of the material, uses the original size and shape of the spherical particles as a reference, corrects the image data obtained by three-dimensional reconstruction, and then removes the spherical particle area used as a reference, and finally obtains a more accurate and realistic three-dimensional reconstructed image of the material's micro-nano structure. It can not only effectively suppress the microstructural distortion phenomenon caused by a certain tilt angle and drift between the scanning electron microscope imaging lens and the ion beam, but also has a simple, easy and low-cost implementation method, will not damage the structure of the material itself, and can provide strong technical support for studying the three-dimensional microstructure of the material.

[0065] In order to improve the reliability and accuracy of the correction, the diameter of the spherical particles in the method of the present invention is preferably of the same order of magnitude as the characteristic size (e.g., pore size) of the micro-nano structure of the material. The use of spherical particles of a size comparable to the characteristic size of the microstructure to be measured is not only conducive to observing the scanned image, but also when the three-dimensional reconstruction result of the spherical particles is restored to the original size and shape, the correction effect on the micro-nano structure of the material is closer to the actual situation.

[0066] Optionally, in step 100, the material is processed to obtain at least one cross section, and the cross section is polished with sandpaper until its surface is smooth, so that the spherical particles can be in close contact with the material, and the gap is narrowed so that the cross section can completely adhere to the powder of the spherical particles to form a spherical particle adhesion layer. The powder of spherical particles preferably uses existing spherical powders such as metal or ceramic. The relevant preparation technology is relatively mature and low in cost. The powder particles are very close to a sphere, and the powder particle size is similar. The size range difference is very small, which is helpful for image correction. Preferably, a scanning electron microscope observation of the spherical particle powder can be performed first, and after determining that the particles are spherical, the spherical particles can be adhered to the cross section.

[0067] Furthermore, in step 100, a plurality of spherical particles are adhered to a cross section to form a spherical particle adhesion layer. According to the adhesion characteristics of the spherical particle powder, a dry method or a wet method can be used for powder adhesion, so that the cross section can completely adhere to the spherical particle powder. For powders that can be directly adsorbed on the surface of the material in a dry state or with the help of external force, direct dry adhesion can be used; otherwise, a binder can be used to assist the spherical particle powder to adhere to the surface of the material. The specific method of forming the spherical particle adhesion layer can also refer to the prior art.

[0068] The ambient temperature for performing step 102 may be room temperature. The component containing epoxy resin in step 102 may be a mixture of epoxy resin and curing agent. The type of curing agent and the specific ratio of epoxy resin and curing agent may refer to the prior art. The epoxy resin may be a cold mounting epoxy resin for vacuum impregnation, such as EpoFix Kit cold mounting epoxy resin. The resin needs 12 hours to be completely cured at room temperature, has no shrinkage, is particularly suitable for vacuum impregnation, and has a transparent material.

[0069] Optionally, the method of the present invention further includes: degassing the component containing epoxy resin (such as a mixture of epoxy resin and curing agent) under vacuum conditions before pore filling of the material sample in step 102. Degassing the epoxy resin mixture under vacuum conditions first can further reduce bubbles introduced by stirring when preparing the component containing epoxy resin.

[0070] Optionally, in step 102, when the pores of the material sample are filled with a component containing epoxy resin under vacuum conditions, the vacuum degree range is preferably 0.1 to 0.15 atm. Too low a vacuum degree will result in incomplete impregnation of the epoxy resin, while too high a vacuum degree will cause the epoxy resin to boil and introduce bubbles. When filling, the sample can be immersed in the component containing epoxy resin for pore filling, or the pore filling can be performed by slowly flowing the component containing epoxy resin over the surface of the sample to be tested. When slowly flowing over the surface of the material sample, the flow rate of the component containing epoxy resin is preferably not more than 0.25 mm / s, so as to fully fill the pores.

[0071] Furthermore, the method of the present invention further comprises: after the pores of the material sample are filled in step 102, the sample to be tested is allowed to stand for no less than 12 hours so that the bubbles are completely removed and the epoxy resin is completely cured. The standing condition may be room temperature.

[0072] Optionally, in step 106, polishing is performed on the exposed material and the interface between the spherical particles, including:

[0073] Use an ion beam polisher to find clear material and spherical particle interfaces, and perform ion beam polishing on the interfaces.

[0074] After polishing, the polished area can be viewed using a scanning electron microscope to more easily locate the area of ​​interest containing the material and spherical particles. Figure 2 Schematic diagram of the structure of a sample to be tested in an embodiment of the present invention, including a material area 1, a spherical particle attachment layer area 2 and an epoxy resin area 3. Figure 2 The direction indicated by the middle arrow is the ion beam polishing position.

[0075] In some preferred embodiments, the method of the present invention, step 100, processes the material to obtain at least one cross section, including:

[0076] Cut and grind the material to obtain two perpendicular cross sections with smooth surfaces;

[0077] Accordingly, in step 104, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer, including:

[0078] The sample to be tested is ground until the cross section where the material does not adhere to the spherical particles is exposed.

[0079] In this embodiment, two vertical cross sections are obtained when the material is processed, wherein one cross section is used to adhere multiple spherical particles, and the other cross section perpendicular to the cross section is kept as it is for observation. In step 104, the sample to be tested is processed without cutting the material area, and the epoxy resin area is directly polished to expose the cross section where the spherical particles are not adhered. This can expose the material and the spherical particles, the junction between the spherical particles and the material, and the junction between the spherical particle adhesion layer and the cross section of the spherical particles not adhered.

[0080] See also Figure 3 to Figure 8(c) Furthermore, the present invention also performs three-dimensional reconstruction on nickel oxide-yttria stabilized zirconia material to verify the performance of the method of the present invention, specifically including:

[0081] In step 100, when the material is processed to obtain at least one cross section, two adjacent cross sections of the material to be tested are polished with 1000-grit sandpaper until the two cross sections are perpendicular to each other, and then one of the cross sections is selected, and spherical particle powder that has been confirmed to be spherical through scanning electron microscopy is glued on until the powder completely covers the cross section of the material sample, and the other cross section remains intact.

[0082] In step 102, the mixture of epoxy resin and curing agent is degassed under vacuum and room temperature conditions, and then the mixture of epoxy resin and curing agent is slowly flowed over the surface of the material sample to fill the pores of the material and the spherical particle attachment layer; wherein the vacuum degree floats between 0.1 and 0.15 atm to reduce bubbles.

[0083] In step 104, after the epoxy resin is completely cured, the sample to be tested is polished with 800-grit sandpaper until the cross section of the spherical particle powder not adhered is exposed, and the interface between the material and the epoxy resin is ion-beam polished. The epoxy resin is completely cured for at least 12 hours.

[0084] In step 106, a scanning electron microscope is used to observe the polished area, and a clear boundary between the spherical particles and the material can be seen. A focused ion beam-scanning electron microscope is used to alternately cut and scan the region of interest at the boundary to obtain a continuous two-dimensional image sequence, such as Figure 3 As shown, Figure 3 The direction indicated by the arrow in is the sequential direction of the two-dimensional image acquisition; then the two-dimensional image sequence is aligned to obtain a reconstructed three-dimensional digital image, such as Figure 4 As shown, Figure 4 The xyz coordinate system in is an artificially set reference coordinate system for display and explanation. Figure 4 The three-dimensional digital image includes a material area 1 and a spherical particle attachment layer area 2.

[0085] In step 108, the ellipsoidal particles in the three-dimensional digitized image are corrected to spherical particles through image correction technology, and finally a nanoscale three-dimensional reconstruction result of the porous material based on the spherical particle correction is obtained.

[0086] Figure 5 A schematic diagram of correcting xy plane data in a three-dimensional digitized image is shown. Figure 5 The left side shows the original xy plane data of the three-dimensional digitized image, and the right side shows the corrected xy plane data. Figure 6(a) to Figure 6(c) It is an image of the spherical particle attachment layer area in the xz plane direction in an embodiment of the present invention; wherein, FIG6(a) shows the uncorrected xz plane data of the three-dimensional digitized image, from which it can be seen that the spherical structure has been distorted, FIG6(b) shows the xz plane data after correction by the coordinate shearing operation, and FIG6(c) shows the xz plane data after correction by z-direction scaling. Figure 7(a) to Figure 7(c) It is an image of the material area in the xz plane direction in an embodiment of the present invention; wherein, FIG7(a) shows the uncorrected xz plane data of the three-dimensional digitized image, FIG7(b) shows the xz plane data after correction by the coordinate shearing operation, and FIG7(c) shows the xz plane data after z-direction scaling correction. Figure 8(a) to Figure 8(c) It is an image of the spherical particle attachment layer area and the material area in the yz plane direction in the embodiment of the present invention, wherein FIG8(a) shows the yz plane data of the uncorrected three-dimensional digital image, and it can be seen that the spherical structure has been distorted, FIG8(b) shows the yz plane data after the coordinate shearing operation correction, and FIG6(c) shows the yz plane data after the z-direction scaling correction. It can be seen that there is a certain error between the uncorrected three-dimensional structure calculation result and the three-dimensional structure calculation result after the spherical particle correction. The method of the present invention can obtain a more realistic material micro-nano structure.

[0087] In some embodiments, the present invention further provides a focused ion beam-scanning electron microscope three-dimensional structure reconstruction correction method, comprising the following steps:

[0088] Step 200, processing the material to obtain at least one cross section, and using the cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer;

[0089] Step 202, under vacuum conditions, using a component containing epoxy resin to fill pores in the material sample to obtain a filled sample to be tested;

[0090] Step 204, after the epoxy resin is completely cured, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer;

[0091] Step 206, polishing the exposed material and the interface of the spherical particles to determine the region of interest to be observed;

[0092] Step 208, using a focused ion beam-scanning electron microscope to cut and scan the region of interest to obtain a two-dimensional image sequence;

[0093] Step 210: based on the shape of the spherical particles, the two-dimensional image sequence is corrected one by one, and three-dimensional reconstruction is performed based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image.

[0094] Furthermore, the method further comprises:

[0095] Step 212, performing secondary correction on the three-dimensional digitized image based on the size and shape of the spherical particles.

[0096] In the above implementation, step 210 first corrects the acquired two-dimensional image sequence one by one, corrects the ellipse in the image to a circle, and then aligns the two-dimensional image sequence for three-dimensional reconstruction, which can also achieve the correction of the three-dimensional reconstruction result of the micro-nano structure. The other steps of this method are the same as the above-mentioned method of the present invention, and steps 200 to 206 correspond to steps 100 to 106 of the above-mentioned method of the present invention, and are based on the same concept as the above-mentioned implementation of the method of the present invention. The specific content can be found in the description of the above-mentioned implementation, and will not be repeated here.

[0097] In summary, the focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method provided by the present invention corrects the image deviation caused by the tilt and drift of the focused ion beam-scanning electron microscope (FIB-SEM) lens by gluing spherical particles, thereby realizing the true three-dimensional reconstruction of the micro-nanoscale structure of porous materials, and can provide a true digital model for quantitative research on the micro-nanoscale of materials.

[0098] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method, characterized in that: include: Processing the material to obtain at least one cross section, and using the cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer; Under vacuum conditions, using a component containing epoxy resin to fill pores in the material sample to obtain a filled sample to be tested; After the epoxy resin is completely cured, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer; Polishing the exposed material and the interface between the spherical particles to determine the area of ​​interest; Using a focused ion beam-scanning electron microscope to cut and scan the region of interest, obtain a two-dimensional image sequence, and perform three-dimensional reconstruction to obtain a three-dimensional digital image; The three-dimensional digitized image is corrected based on the size and shape of the spherical particles.

2. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: Also includes: The corrected three-dimensional digitized image is cropped to obtain a three-dimensional reconstructed image of the micro-nano structure of the material.

3. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: The diameter of the spherical particles is of the same order of magnitude as the characteristic size of the micro-nano structure of the material.

4. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: Also includes: Prior to pore filling of the material samples, the components including the epoxy resin were degassed under vacuum.

5. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 4, characterized in that: Under vacuum conditions, when the pores of the material sample are filled with a component containing epoxy resin, the vacuum degree ranges from 0.1 to 0.15 atm.

6. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 5, characterized in that: Also includes: After the pores of the material sample are filled, the sample to be tested is allowed to stand for no less than 12 hours.

7. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: The step of polishing the exposed material and the interface between the spherical particles comprises: An ion beam polisher is used to find clear material and the interface between the spherical particles, and the interface is ion beam polished.

8. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: The epoxy resin is EpoFix Kit cold mounting epoxy resin.

9. The focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method according to claim 1, characterized in that: The step of processing the material to obtain at least one cross section comprises: Cut and grind the material to obtain two perpendicular cross sections with smooth surfaces; Processing the sample to be tested to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer includes: The sample to be tested is polished until a cross section where the spherical particles are not adhered is exposed.

10. A focused ion beam-scanning electron microscope three-dimensional structure reconstruction and correction method, characterized in that: include: Processing the material to obtain at least one cross section, and using the cross section to adhere a plurality of spherical particles to obtain a material sample having a spherical particle attachment layer; Under vacuum conditions, using a component containing epoxy resin to fill pores in the material sample to obtain a filled sample to be tested; After the epoxy resin is completely cured, the sample to be tested is processed to expose the material and the spherical particles along the normal direction of the spherical particle attachment layer; Polishing the exposed material and the interface between the spherical particles to determine the area of ​​interest; Using a focused ion beam-scanning electron microscope to cut and scan the region of interest to obtain a two-dimensional image sequence; Based on the shape of the spherical particles, the two-dimensional image sequence is corrected one by one, and three-dimensional reconstruction is performed based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image; The three-dimensional digitized image is corrected based on the size and shape of the spherical particles.

Images