CN114723878A - Method for reconstructing and correcting three-dimensional structure of focused ion beam-scanning electron microscope - Google Patents
Method for reconstructing and correcting three-dimensional structure of focused ion beam-scanning electron microscope Download PDFInfo
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Abstract
The invention relates to the technical field of three-dimensional reconstruction, in particular to a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope, which comprises the following steps: processing the material to obtain a material sample with a spherical particle adhesion layer; under the vacuum condition, filling pores with a component containing epoxy resin; after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer; polishing the junction of the exposed material and the spherical particles to determine an interested area; cutting and scanning the region of interest by using a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence, and performing three-dimensional reconstruction to obtain a three-dimensional digital image; based on the size and shape of the spherical particles, a correction is made to the three-dimensional digitized image. The method can correct the three-dimensional reconstruction result of the focused ion beam-scanning electron microscope on the material micro-nano structure, and obtain a high-precision three-dimensional reconstruction image.
Description
Technical Field
The invention relates to the technical field of three-dimensional reconstruction, in particular to a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope.
Background
The three-dimensional reconstruction based on the focused ion beam-scanning electron microscope (FIB-SEM) is a mature three-dimensional reconstruction technology, can achieve the resolution of 3nm at most, and is very suitable for reconstructing micro-nano structures in porous materials. However, when the technology is actually used, in order to make the focused ion beam perpendicular to the surface of the sample to be measured, the inclination angle of the sample stage is kept at 54 °, which causes that the visual angle of the scanning electron microscope is not completely opposite to the surface of the sample but has a certain amount of inclination in the process of forming a series of slices, and meanwhile, the scanning electron microscope has a certain amount of drift in the process of shooting two-dimensional images of a series of slices, both factors can interfere with the final three-dimensional reconstruction result, so that the obtained three-dimensional digital image of the microstructure has the problem of aliasing, the precision of three-dimensional reconstruction is reduced, and further quantitative analysis of the subsequent micro-nano structure of the material is influenced.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problem that in the prior art, the three-dimensional reconstruction result is out of shape due to interference caused by lens inclination and drift, so that high-precision three-dimensional reconstruction of the micro-nano structure of the functional porous material is realized.
(II) technical scheme
In order to solve the technical problem, the invention provides a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope, which comprises the following steps:
processing the material to obtain at least one section, and sticking a plurality of spherical particles by using one section to obtain a material sample with a spherical particle adhesion layer;
under the vacuum condition, filling pores in the material sample by using a component containing epoxy resin to obtain a filled sample to be detected;
after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer;
polishing the junction of the exposed material and the spherical particles to determine an area of interest;
cutting and scanning the region of interest by adopting a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence, and performing three-dimensional reconstruction to obtain a three-dimensional digital image;
based on the size and shape of the spherical particles, a correction is made to the three-dimensional digitized image.
Optionally, the method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope further includes:
and cutting the corrected three-dimensional digital image to obtain a three-dimensional reconstructed image of the material micro-nano structure.
Optionally, the diameter of the spherical particles is of the same order of magnitude as the characteristic dimension of the material micro-nano-scale structure.
Optionally, the method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope further includes:
the epoxy-containing component was debubbled under vacuum prior to pore-filling the material sample.
Optionally, when the material sample is subjected to pore filling by using the component containing the epoxy resin under the vacuum condition, the vacuum degree ranges from 0.1 atm to 0.15 atm.
Optionally, the method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope further includes:
and after the material sample is subjected to pore filling, standing the sample to be detected for not less than 12 hours.
Optionally, the polishing the interface between the exposed material and the spherical particles includes:
and using an ion beam polishing machine to find a clear material and the junction of the spherical particles, and performing ion beam polishing on the junction.
Optionally, the epoxy resin is an EpoFix Kit cold-set epoxy resin.
Optionally, the processing the material to obtain at least one cross section includes:
cutting and polishing the material to obtain two sections which are vertical to each other and have smooth surfaces;
processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle attachment layer, wherein the processing comprises the following steps:
and polishing the sample to be detected until the section of the spherical particles which are not adhered is exposed.
The invention also provides a method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope, which comprises the following steps:
processing the material to obtain at least one section, and sticking a plurality of spherical particles by using one section to obtain a material sample with a spherical particle adhesion layer;
under the vacuum condition, filling pores in the material sample by using a component containing epoxy resin to obtain a filled sample to be detected;
after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer;
polishing the junction of the exposed material and the spherical particles to determine an area of interest;
cutting and scanning the region of interest by adopting a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence;
correcting the three-dimensional digitized image based on the size and shape of the spherical particles;
and correcting the two-dimensional image sequence one by one based on the shape of the spherical particles, and performing three-dimensional reconstruction based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image.
(III) advantageous effects
The technical scheme of the invention has the following advantages: the invention provides a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope, which corrects a three-dimensional digital image obtained by a focused ion beam-scanning electron microscope three-dimensional reconstruction technology by using the size and the shape of spherical particles, can effectively correct the micro-structure aliasing phenomenon generated by a certain inclination angle and drift between an imaging lens of the scanning electron microscope and an ion beam, and realizes the accurate three-dimensional reconstruction of a micro-nano structure in a material.
Drawings
FIG. 1 is a schematic illustration showing steps of a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a sample to be tested according to an embodiment of the present invention;
FIG. 3 is a schematic representation of a sequence of consecutive two-dimensional images obtained in an embodiment of the present invention;
FIG. 4 is a schematic diagram of a three-dimensional digitized image obtained by performing three-dimensional reconstruction in an embodiment of the present invention;
FIG. 5 is a schematic diagram of the correction of xy plane data in a three-dimensional digitized image according to an embodiment of the present invention;
FIGS. 6(a) to 6(c) are images of the region of the spherical particle adhesion layer in the xz-plane direction in the embodiment of the present invention;
FIGS. 7(a) to 7(c) are images of a material region in the xz-plane direction in the embodiment of the present invention;
fig. 8(a) to 8(c) are images of the spherical particle adhesion layer region and the material region in the yz plane direction in the example of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
As described above, in the prior art, the technology for performing three-dimensional reconstruction based on a focused ion beam-scanning electron microscope is restricted by the actual structure and the use environment of the focused ion beam-scanning electron microscope, and a reconstruction result aliasing phenomenon caused by a certain inclination angle and drift between an imaging lens of the scanning electron microscope and an ion beam exists, which affects subsequent further quantitative analysis of the material micro-nano structure. At present, the existing method cannot correct the three-dimensional reconstruction result of the focused ion beam-scanning electron microscope, and the precision of the obtained three-dimensional reconstruction image of the micro-nano structure is low. In view of the above, the present invention provides a three-dimensional structure reconstruction correction method capable of correcting data acquired by a focused ion beam-scanning electron microscope, so as to realize accurate three-dimensional reconstruction of a material micro-nano-scale structure.
As shown in fig. 1, a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope (the method of the present invention for short) provided in an embodiment of the present invention includes:
This step 100 performs a preliminary process 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 resulting from the machining should be larger than the size of the region desired to be reconstructed. A plurality of spherical particles are adhered on a flat section, namely a spherical particle adhesion layer is formed on the surface of a material to be measured, the function of the spherical particle adhesion layer is used as a reference for correcting measured data, and specific numerical values such as the thickness of the spherical particle adhesion layer and the number of the contained spherical particles can be set according to actual conditions, and are not further limited.
And 102, filling pores in the material sample with the spherical particle adhesion layer by using a component containing epoxy resin under a vacuum condition to obtain a filled sample to be detected.
In this step 102, the microstructure pores of the material itself and the gaps between the spherical particles in the spherical particle adhesion layer are filled, so as to filter out the interference caused by the pore background in the electron microscope image and improve the definition of the three-dimensional reconstructed image.
And 104, after the epoxy resin is completely cured, processing the sample to be tested, and forming an exposed surface along the normal direction of the spherical particle adhesion layer, namely the direction perpendicular to the section of the adhered spherical particles to expose the material and the spherical particles.
The sample to be tested is processed again in step 104, for example, the sample to be tested obtained in step 102 may be polished or cut to remove part of the epoxy resin on the surface of the sample to be tested, so as to expose the material and the spherical particle adhesion layer for subsequent observation. The material and the spherical particles are exposed along the normal direction of the spherical particle adhesion layer, so that the specific microstructure at the junction of the material and the spherical particle adhesion layer is convenient to observe and reconstruct from the side direction.
And step 106, polishing the junction of the exposed material and the spherical particles, and determining the region of interest to be observed.
The region of interest to be observed should contain a material and a plurality of spherical particles. Preferably, at least 3 layers of spherical particles can be seen, and more preferably, 4-5 layers of spherical particles can be seen. If too few spherical particles are in the selected region of interest, image correction is not easy to perform, which may affect the accuracy of the correction result, and if too many spherical particles are in the selected region, the observable material region may be invaded.
And 108, cutting and scanning the determined region of interest by using a focused ion beam-scanning electron microscope to obtain a continuous two-dimensional image sequence, and performing three-dimensional reconstruction based on the two-dimensional image sequence to obtain a three-dimensional digital image corresponding to the region of interest.
In this step 108, the region of interest including the material and the plurality of spherical particles is alternately cut and scanned to obtain a continuous two-dimensional image sequence, and then the obtained two-dimensional image sequence is aligned to realize three-dimensional reconstruction. The thickness of the ion beam cut slice is uniform as much as possible and is equal to the real size of the pixel of the two-dimensional image of the electron microscope. The specific steps of the three-dimensional reconstruction based on the focused ion beam-scanning electron microscope can refer to the prior art, and are not further described herein.
In this step 110, an image correction technique is adopted to correct the ellipsoidal particles of the spherical particle adhesion layer in the obtained three-dimensional digital image into a spherical shape and an original size, and at the same time, the material region adjacent to the spherical particle adhesion layer is also corrected, that is, the microstructure distortion caused by the lens tilt and drift is corrected, so as to obtain a more real and accurate three-dimensional reconstruction result. The specific image correction step preferably includes operations such as scaling and clipping transformation on the three-dimensional image, and the image correction may refer to the prior art and is not further described herein.
Preferably, the method of the present invention further comprises:
and 112, cutting the corrected three-dimensional digital image to obtain a three-dimensional reconstruction image of the material micro-nano structure.
In step 112, the three-dimensionally reconstructed spherical particle attachment layer region is removed from the corrected three-dimensional digitized image, and only the observed real material micro-nano structure is retained, i.e. the precise three-dimensional reconstruction of the micro-nano structure is completed.
According to the method for reconstructing and correcting the three-dimensional structure of the focusing ion beam-scanning electron microscope, spherical particles for correction are added on the surface of a material, the original size and the shape of the spherical particles are used as references, image data obtained by three-dimensional reconstruction are corrected, the spherical particle area used as the reference is removed, and a more accurate and real three-dimensional reconstruction image of the micro-nano structure of the material is finally obtained.
In order to improve the reliability and accuracy of the calibration, the diameter of the spherical particles in the method of the present invention is preferably the same order of magnitude as the characteristic dimension (e.g., pore size) of the micro-nano-scale structure of the material. The adoption of the spherical particles with the characteristic size equivalent to that of the microstructure to be detected is beneficial to observing and scanning the obtained image, and the correction effect on the micro-nano structure of the material is closer to the actual situation when the three-dimensional reconstruction result of the spherical particles is restored to the original size and shape.
Optionally, step 100, processing the material to obtain at least one section, further comprising sanding the section to a smooth surface so that the spherical particles can be in close contact with the material, and reducing the gap so that the section completely adheres to the powder of the spherical particles to form the spherical particle adhesion layer. The powder of spherical particles preferably adopts the existing powder of spherical particles of metal or ceramic and the like, the related preparation technology is mature, the cost is low, the powder particles are very close to spheres, the particle sizes of the powder particles are close, the size range difference is small, and the image correction is facilitated. Preferably, the scanning electron microscope observation of the spherical particle powder is firstly carried out, and after the particles are determined to be spherical, the spherical particles are adhered to the cross section.
Further, in step 100, a plurality of spherical particles are bonded to one cross section to form a spherical particle adhesion layer, and powder adhesion can be performed by a dry method or a wet method according to the adhesion characteristics of spherical particle powder, so that the spherical particle powder is completely bonded to the cross section. Powder which can be directly adsorbed on the surface of the material in a dry state or adsorbed on the surface of the material by virtue of external force can be directly attached by a dry method; otherwise, a binder may be used to assist the attachment of the powder of spherical particles to the surface of the material. The specific manner of forming the spherical particle adhesion layer can also be referred to in the art.
The ambient temperature at which step 102 is performed may be room temperature. The epoxy resin-containing component in step 102 can be a mixture of epoxy resin and a curing agent, the type of the curing agent and the specific ratio of the epoxy resin to the curing agent can refer to the prior art, the epoxy resin can be cold-inlaid epoxy resin for vacuum impregnation, such as EpoFix Kit cold-inlaid epoxy resin, the resin needs 12 hours for complete curing at room temperature, has no shrinkage, is particularly suitable for vacuum impregnation, and is transparent.
Optionally, the method of the present invention further comprises: prior to pore filling the material sample in step 102, the epoxy resin-containing component (e.g., a mixture of epoxy resin and curing agent) is debubbled under vacuum. The bubble removal process of the epoxy resin mixture under vacuum conditions is performed first, which can further reduce the bubbles introduced by stirring when preparing the epoxy resin-containing composition.
Optionally, in step 102, when the material sample is pore-filled with the component containing the epoxy resin under vacuum, the vacuum degree is preferably in the range of 0.1 to 0.15 atm. An excessively low vacuum may result in incomplete impregnation of the epoxy resin, and an excessively high vacuum may result in boiling of the epoxy resin and, instead, introduction of bubbles. When filling, the sample may be dipped into the epoxy resin-containing component to perform pore filling, or pore filling may be performed in such a manner that the epoxy resin-containing component slowly flows over the surface of the sample to be measured, and when slowly flowing over the surface of the material sample, the flow rate of the epoxy resin-containing component is preferably not more than 0.25mm/s, so as to sufficiently fill the pores.
Further, the method of the invention also comprises the following steps: after the material sample is subjected to pore filling in step 102, the sample to be measured is allowed to stand for not less than 12 hours, so that bubbles are completely removed and the epoxy resin is completely cured. Standing at room temperature.
Optionally, in step 106, polishing the exposed interface between the material and the spherical particles, including:
and (4) finding the clear junction of the material and the spherical particles by using an ion beam polishing machine, and performing ion beam polishing on the junction.
After polishing, the region of interest containing the material and spherical particles can be more easily located by using a scanning electron microscope to view the polished area. Fig. 2 is a schematic structural diagram of a sample to be tested according to an embodiment of the present invention, which includes a material region 1, a spherical particle attachment layer region 2, and an epoxy resin region 3, and a direction indicated by an arrow in fig. 2 is an ion beam polishing position.
In some preferred embodiments, the inventive method step 100 processes a material to obtain at least one cross-section, comprising:
cutting and polishing the material to obtain two sections which are vertical to each other and have smooth surfaces;
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 adhesion layer, including:
and polishing the sample to be detected until the cross section of the spherical particles which are not adhered to the material is exposed.
In this embodiment, two perpendicular cross sections are obtained when the material is processed, one of the cross sections is used for adhering a plurality of spherical particles, and the other cross section perpendicular to the cross section is kept as it is for observation, and the sample to be measured is processed in step 104 without cutting the material region, and the epoxy resin region is directly polished, so that the cross section where the spherical particles are not adhered is exposed, and the material and the spherical particles can be exposed along the normal direction of the spherical particle adhesion layer, and the cross section of the spherical particle adhesion layer and the cross section of the non-adhered spherical particles are also at the cross section of the spherical particle adhesion layer.
Referring to fig. 3 to 8(c), in addition, the present invention also aims at performing three-dimensional reconstruction on the nickel oxide-yttria-stabilized zirconia material to verify the performance of the method of the present invention, which specifically includes:
in step 100, processing the material to obtain at least one section, polishing two adjacent sections of the material to be detected by using 1000-mesh sand paper until the two sections are mutually vertical, then selecting one section, adhering spherical particle powder which is observed by a scanning electron microscope and determined to be spherical until the powder completely covers the section of the material sample, and keeping the other section intact.
In step 102, defoaming a mixture of epoxy resin and a curing agent under vacuum and room temperature conditions, and then enabling the mixture of epoxy resin and the curing agent to slowly flow over the surface of a material sample to fill the material and pores of a spherical particle adhesion layer; wherein the vacuum degree is floated at 0.1-0.15 atm to reduce bubbles.
And 104, after the epoxy resin is completely cured, polishing the sample to be detected by using 800-mesh sand paper until the section of the spherical particle powder which is not adhered is exposed, and performing ion beam polishing on the junction of the material and the epoxy resin. Wherein the epoxy resin complete cure time is at least 12 hours.
In step 106, a scanning electron microscope is used to view the polished part, so that a clear boundary between the spherical particles and the material can be seen, and 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, as shown in fig. 3, wherein the direction indicated by an arrow in fig. 3 is the sequential direction of two-dimensional image acquisition; then, the two-dimensional image sequence is aligned to obtain a reconstructed three-dimensional digitized image, as shown in fig. 4, an xyz coordinate system in fig. 4 is a reference coordinate system artificially set so as to show and explain, and the three-dimensional digitized image in fig. 4 includes a material region 1 and a spherical particle attachment layer region 2.
In step 108, the ellipsoidal particles in the three-dimensional digital image are corrected into spherical particles by an image correction technology, and finally, a nano-scale three-dimensional reconstruction result of the porous material based on the spherical particle correction is obtained.
Fig. 5 is a schematic diagram showing correction of xy plane data in a three-dimensional digitized image, the xy plane data of an original three-dimensional digitized image being shown on the left side of fig. 5, and xy plane data after correction being shown on the right side. FIGS. 6(a) to 6(c) are images of the region of the spherical particle adhesion layer in the xz-plane direction in the embodiment of the present invention; in fig. 6(a) shows the three-dimensional digitized image xz plane data without correction, it can be seen that the spherical structure is out of shape, fig. 6(b) shows the xz plane data after correction by the coordinate cropping operation, and fig. 6(c) shows the xz plane data after correction by the z-direction scaling. FIGS. 7(a) to 7(c) are images of a material region in the xz-plane direction in the embodiment of the present invention; in this case, fig. 7(a) shows three-dimensional digitized image xz plane data without correction, fig. 7(b) shows xz plane data corrected by a coordinate cropping operation, and fig. 7(c) shows xz plane data corrected by z-direction scaling. Fig. 8(a) to 8(c) are images of a spherical particle adhesion layer region and a material region in the yz plane direction in the embodiment of the present invention, in which fig. 8(a) shows yz plane data of a three-dimensional digitized image without correction, it can be seen that spherical structures are out of shape, fig. 8(b) shows yz plane data after correction by a coordinate cropping operation, and fig. 6(c) shows yz plane data after correction by z-direction scaling. It can be seen that there is a certain error between the calculation result of the uncorrected three-dimensional structure and the calculation result of the three-dimensional structure corrected by the spherical particles.
In some embodiments, the present invention further provides a method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope, comprising the following steps:
step 200, processing the material to obtain at least one section, and sticking a plurality of spherical particles by using one section to obtain a material sample with a spherical particle adhesion layer;
202, under a vacuum condition, filling pores in a material sample by using a component containing epoxy resin to obtain a filled sample to be detected;
step 204, after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer;
step 206, polishing the junction of the exposed material and the spherical particles to determine an area of interest to be observed;
208, cutting and scanning the region of interest by adopting a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence;
and 210, correcting the two-dimensional image sequence one by one based on the shape of the spherical particles, and performing three-dimensional reconstruction based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image.
Further, the method further comprises:
step 212, secondary correction is performed on the three-dimensional digitized image based on the size and shape of the spherical particles.
In the above embodiment, step 210 firstly corrects the acquired two-dimensional image sequence one by one, modifies the ellipse in the picture into a circle, and aligns the two-dimensional image sequence to perform three-dimensional reconstruction, so that the correction of the three-dimensional reconstruction result of the micro-nano structure can be realized. The other steps of the method are the same as the aforementioned method of the present invention, and steps 200 to 206 correspond to steps 100 to 106 of the aforementioned method of the present invention, and are based on the same concept as the aforementioned embodiment of the method of the present invention, and the detailed contents can be referred to the description in the aforementioned embodiment, and are not repeated here.
In summary, the method for correcting the three-dimensional structure reconstruction of the focused ion beam-scanning electron microscope provided by the invention corrects the image offset caused by the inclination and the drift of the lens of the focused ion beam-scanning electron microscope (FIB-SEM) in a mode of sticking spherical particles, realizes the real three-dimensional reconstruction of the micro-nano structure of the porous material, and can provide a real digital model for the quantitative research of the micro-nano scale of the material.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A focused ion beam-scanning electron microscope three-dimensional structure reconstruction correction method is characterized by comprising the following steps:
processing the material to obtain at least one section, and sticking a plurality of spherical particles by using one section to obtain a material sample with a spherical particle adhesion layer;
under the vacuum condition, filling pores in the material sample by using a component containing epoxy resin to obtain a filled sample to be detected;
after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer;
polishing the junction of the exposed material and the spherical particles to determine an area of interest;
cutting and scanning the region of interest by adopting a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence, and performing three-dimensional reconstruction to obtain a three-dimensional digital image;
based on the size and shape of the spherical particles, a correction is made to the three-dimensional digitized image.
2. The method for reconstructing and correcting the focused ion beam-scanning electron microscope three-dimensional structure according to claim 1, further comprising:
and cutting the corrected three-dimensional digital image to obtain a three-dimensional reconstruction image of the material micro-nano structure.
3. The method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope according to claim 1, wherein the method comprises the following steps:
the diameter of the spherical particles is the same as the order of magnitude of the characteristic size of the micro-nano structure of the material.
4. The method for reconstructing and correcting the focused ion beam-scanning electron microscope three-dimensional structure according to claim 1, further comprising:
the epoxy-containing component was debubbled under vacuum prior to pore-filling the material sample.
5. The method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope according to claim 4, wherein the method comprises the following steps:
and under the vacuum condition, when the component containing the epoxy resin is adopted to fill the pores of the material sample, the vacuum degree range is 0.1-0.15 atm.
6. The method according to claim 5, further comprising:
and after the material sample is subjected to pore filling, standing the sample to be detected for not less than 12 hours.
7. The method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope according to claim 1, wherein the method comprises the following steps:
the polishing of the exposed material and the spherical particle interface comprises:
and using an ion beam polishing machine to find a clear material and the junction of the spherical particles, and performing ion beam polishing on the junction.
8. The method for reconstructing and correcting the three-dimensional structure of the focused ion beam-scanning electron microscope according to claim 1, wherein the method comprises the following steps:
the epoxy resin is EpoFix Kit cold-set epoxy resin.
9. The method for reconstructing and correcting the three-dimensional structure of a focused ion beam-scanning electron microscope according to claim 1,
said machining of the material to obtain at least one section comprises:
cutting and polishing the material to obtain two sections which are vertical to each other and have smooth surfaces;
processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle attachment layer, wherein the processing comprises the following steps:
and polishing the sample to be detected until the section of the spherical particles which are not adhered is exposed.
10. A method for reconstructing and correcting a three-dimensional structure of a focused ion beam-scanning electron microscope is characterized by comprising the following steps:
processing the material to obtain at least one section, and sticking a plurality of spherical particles by using one section to obtain a material sample with a spherical particle adhesion layer;
under the vacuum condition, filling pores in the material sample by using a component containing epoxy resin to obtain a filled sample to be detected;
after the epoxy resin is completely cured, processing the sample to be tested, and exposing the material and the spherical particles along the normal direction of the spherical particle adhesion layer;
polishing the junction of the exposed material and the spherical particles to determine an area of interest;
cutting and scanning the region of interest by adopting a focused ion beam-scanning electron microscope to obtain a two-dimensional image sequence;
correcting the three-dimensional digitized image based on the size and shape of the spherical particles;
and correcting the two-dimensional image sequence one by one based on the shape of the spherical particles, and performing three-dimensional reconstruction based on the corrected two-dimensional image sequence to obtain a three-dimensional digital image.
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| CN115541643A (en) * | 2022-11-28 | 2022-12-30 | 江苏沙钢集团有限公司 | Method for reconstructing inclusions |
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