CN115541643A - Method for reconstructing inclusions - Google Patents
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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Abstract
The invention provides an inclusion reconstruction method, which is characterized in that in the process of reconstructing the appearance of inclusions by using a focused ion beam electron beam double-beam scanning electron microscope, the total thickness accumulated by a series of inclusion slices is calculated, the offset angle of the inclusion slices in the Z direction on a YZ plane is measured, and the offset of the inclusion slices is approximately obtained by using a trigonometric function relation, so that the offset correction is carried out on a reconstructed image, the finally obtained inclusion image is closer to the original appearance of the inclusions, the real space form and size of the inclusions are obtained, and data support is provided for researching the formation mechanism of the inclusions.
Description
Technical Field
The invention relates to the technical field of material detection, in particular to an inclusion reconstruction method.
Background
The focused ion beam is a micro-nano processing technology, the basic principle of which is similar to that of a scanning electron microscope, the ion beam emitted by an ion source is used as an incident beam after accelerated focusing, and solid atoms can be sputtered and stripped in the process of collision between high-energy ions and solid surface atoms.
The existence of non-metallic inclusions in the steel can destroy the continuity of the metal matrix, and has considerable harm to the mechanical property, the physical property and the chemical property of the steel. In order to research the morphology of inclusions, the inclusions are cut layer by using a focused ion beam electron beam dual-beam scanning electron microscope to reconstruct the three-dimensional morphology of the inclusions.
However, when reconstructing the morphology of the inclusions, the acquired image may shift upward in a direction opposite to the cutting direction due to the change of the cutting position, and if the acquired image is directly reconstructed, the morphology of the inclusions may be distorted, and the size may be inaccurate.
Disclosure of Invention
The invention aims to provide an inclusion reconstruction method.
The invention provides an inclusion reconstruction method, which comprises the following steps:
preparing a sample to be observed, searching for an interested inclusion on the surface of the sample to be observed, forming an XY axis plane by the plane where the inclusion is located, and forming pits on the left side, the right side and the lower side of the inclusion by utilizing a focused ion beam electron beam double-beam scanning electron microscope, wherein the inner wall surface of the pit on the lower side of the sample to be observed forms an XZ axis plane which is an observation surface;
cutting the observation surface layer by layer through a focused ion beam electron beam double-beam scanning electron microscope along the Y-axis direction to obtain a series of inclusion slices;
acquiring the inclusion slice image, calculating the accumulated total thickness corresponding to the inclusion slice, and acquiring the Z-direction offset angle of the inclusion slice on a YZ plane;
calculating the offset of each inclusion slice image, and performing offset correction on the inclusion slice image according to the offset, wherein the offset calculation formula is as follows:
ΔZ N =L N ×sinθ
wherein the content of the first and second substances,ΔZ N an offset is indicated and is indicated by,L N representing the total thickness accumulated by the nth slice of the inclusion,θrepresents an offset angle of the inclusion slice in the Z direction on the YZ plane;
and performing three-dimensional reconstruction on the inclusions based on the corrected inclusion slice images.
As a further improvement of the present invention, the step of cutting the inclusions layer by layer through a focused ion beam electron beam dual-beam scanning electron microscope to obtain a series of inclusion slices specifically comprises:
and cutting the inclusions layer by layer through a focused ion beam electron beam double-beam scanning electron microscope, and adjusting the slice thickness according to the sizes of the inclusions to obtain a plurality of serial inclusion slices with consistent thickness.
As a further improvement of the invention, the slice thickness range of the inclusions is 12 to 48nm.
As a further improvement of the present invention, the acquiring the inclusion slice image specifically includes:
each timenSlicing the inclusions to obtain an image of the slice of inclusions, whereinnAre preset parameters according to the size of the inclusions and the thickness of the slices.
As a further development of the invention, the parametersnHas a value in the range of 1~4.
As a further improvement of the present invention, the calculating the accumulated total thickness of the inclusion slices specifically includes:
slicing thickness and parameters based on said inclusionsnCalculating the cumulative total thickness corresponding to the inclusion slice by the following formula:
L
N
=(N-1)×n×d
wherein L is N Represents the Nth pageThe total thickness of the inclusion pieces accumulated, d represents the inclusion piece thickness.
As a further improvement of the invention, the slice current is controlled to be 1 to 2nA.
As a further improvement of the invention, the slicing current is controlled to be 1.5A, and an image of one inclusion slice is obtained every 2 inclusion slices.
As a further improvement of the invention, the sample to be observed is a steel casting blank sample.
As a further improvement of the present invention, the preparing of the sample to be observed specifically includes:
and (3) grinding the steel casting blank sample until the surface and the opposite surface of the steel casting blank sample are parallel and level, grinding and polishing the surface to be analyzed to a polished state, and spraying a Pt protective layer in an inclusion area.
The invention has the beneficial effects that: in the process of reconstructing the appearance of the inclusion by using a focused ion beam electron beam dual-beam scanning electron microscope, the invention calculates the total thickness accumulated by a series of inclusion slices, measures the offset angle of the inclusion slices in the Z direction on a YZ plane, and approximately obtains the offset of the inclusion slices by using a trigonometric function relationship, thereby carrying out offset correction on a reconstructed image, enabling the finally obtained inclusion image to be closer to the original appearance of the inclusion, further obtaining the real spatial form and size of the inclusion and providing data support for researching the formation mechanism of the inclusion.
Drawings
Fig. 1 is a schematic flow chart of an inclusion reconstruction method according to an embodiment of the present invention.
Fig. 2 is a schematic view of a sample to be observed in one embodiment of the present invention.
FIG. 3 is a scanning electron microscope image of the morphology of inclusions in an embodiment of the present invention.
Fig. 4 is an inclusion image reconstructed without offset correction of the inclusions in an embodiment of the present invention.
Fig. 5 is an inclusion image reconstructed after the inclusions are offset corrected according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and completely with reference to the following detailed description of the invention and the accompanying drawings. It is to be understood that the described embodiments are merely some embodiments of the invention, and not all embodiments. 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.
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention and are not to be construed as limiting the present invention.
As shown in fig. 1, the present invention provides an inclusion reconstruction method, which is used to solve the problem of image shift caused by cutting position change when a focused ion beam electron beam dual-beam scanning electron microscope is used to reconstruct the slice of an inclusion in an observation sample. The reconstructed image of the inclusion based on the method has smaller distortion than the actual structure of the inclusion, can better reflect the actual form of the inclusion, and comprises the following steps:
s1: preparing a sample to be observed, searching an interested inclusion on the surface of the sample to be observed, forming an XY axis plane by the plane where the inclusion is located, forming pits on the left side, the right side and the lower side of the inclusion by using a focused ion beam electron beam double-beam scanning electron microscope, wherein the inner wall surface of the pit on the lower side of the sample to be observed forms an XZ axis plane which is an observation surface.
S2: and cutting the inclusions layer by a focused ion beam electron beam double-beam scanning electron microscope along the Y-axis direction to obtain a series of inclusion slices.
S3: acquiring an image of the inclusion slice, calculating the total thickness accumulated by the corresponding inclusion slice, and acquiring the offset angle of the inclusion slice in the Z direction on the YZ plane.
S4: calculating the offset of each sundry inclusion slice image, and carrying out offset correction on the sundry inclusion slice image according to the offset, wherein the offset calculation formula is as follows:
ΔZ N =L N ×sinθ
wherein the content of the first and second substances,ΔZ N an offset is indicated and is indicated by,L N the total thickness accumulated by the nth inclusion slice is shown,θthe Z-direction deviation angle of the inclusion piece on the YZ plane is shown.
S5: and performing three-dimensional reconstruction on the inclusions based on the corrected inclusion slice images.
In the present embodiment, the method is described by taking the example of observing inclusions in a steel ingot sample, the inclusions in the steel are mainly non-metallic inclusions such as oxides, sulfides, nitrides, and the like, different inclusions have different sizes and forms, the three-dimensional spatial form of the inclusions is accurately reconstructed, and the form and the spatial size of the inclusions can be visually obtained. The shape of the inclusions can be spherical, irregular geometric shape, net shape and the like, and the shape and the size of the inclusions have influence on the performance of different steel products, so that the research on the spatial shape and the size of the inclusions has great significance on the research on the nucleation mechanism and the like of the inclusions.
In other embodiments of the invention, the method can also be used for observing inclusions in other material samples with higher requirements on the appearance of the inclusions.
Specifically, in step S1, it includes:
and (3) grinding the steel casting blank sample until the surface and the opposite surface of the steel casting blank sample are flush, grinding and polishing the surface to be analyzed to a polished state, and spraying a Pt protective layer in an inclusion area.
For example, for a steel casting blank sample, the steel casting blank sample can be processed into a sheet sample with the size of 10mm × 10mm × 2mm, then sand paper of 180#, 800#, 1200# and 1500# is sequentially selected according to the metallographic polishing step to grind a surface to be analyzed, and after the sand paper is ground to have no obvious scratch, the surface to be analyzed is polished by diamond suspension with the specification of 5 μm until the requirement of electron microscope analysis is met. And for the opposite surface of the surface to be analyzed, the surface to be analyzed is ground flat through 180# abrasive paper so as to ensure that the surface to be analyzed and the opposite surface are mutually parallel, and further ensure that the subsequent inclusion morphology reconstruction is accurate.
As shown in FIG. 2, a schematic diagram of a sample to be observed is shown, wherein a plane of an interested inclusion 1 on the surface of the sample to be observed is an XY-axis plane, a Pt protective layer with the size of 12 μm × 12 μm × 1.5 μm is sprayed on the area of the inclusion 1, pits are formed on the left side, the right side and the lower side of the inclusion 1 by using a focused ion beam electron beam double-beam scanning electron microscope, and the inner wall surface of the pit on the lower side of the sample to be observed forms an XZ-axis plane which is an observation surface 2.
Specifically, in step S2, it includes:
and cutting the observation surface 2 layer by layer through a focused ion beam electron beam double-beam scanning electron microscope, and adjusting the slice thickness according to the size of the inclusion 1 to obtain a plurality of serial inclusion slices with consistent thickness.
The focused ion beam is a micro-nano processing technology, the ion beam emitted by an ion source is used as an incident beam after accelerated focusing, and solid atoms can be sputtered and stripped in the process of collision between high-energy ions and atoms on the surface of the solid. The inclusion 1 is cut layer by layer through a focused ion beam to form a series of inclusion slices to obtain images of the inclusion slices, and the three-dimensional shape of the inclusion 1 in the space can be obtained after the images of the inclusion slices of different layers are spliced and reconstructed.
Further, in the present embodiment, the range of the slice thickness of each inclusion is controlled to 12 to 48nm according to the size of the general inclusion 1 in the steel casting blank, so that the time required for reconstruction is reduced and the efficiency is improved while the reconstruction accuracy of the inclusion 1 is ensured.
Further, in step S2, it further includes:
each timenSlicing the inclusion to obtain a back-scattered image of the inclusion slice, whereinnAre preset parameters according to the size of the inclusions 1 and the slice thickness. In the image, the boundary of the inclusion 1 is drawn by the contrast difference of the backscatter image of the inclusion 1, and the image is colored.
When the size of the inclusion 1 is large, images of inclusion slices may be acquired at intervals rather than continuously to further reduce the time required for reconstruction and improve efficiency. In the present embodiment, the parameter n has a value in the range of 1~4, depending on the size of the general inclusion 1 in the cast steel slab.
Further, in step S2, the slice current is controlled to be 1 to 2na. The current is controlled to ensure the flatness of the surface of the slice, and a curtain structure, namely a vertical stripe structure on a cutting surface when a sample is cut by a focused ion beam, is avoided. And the time required by slicing is controlled by controlling the current, so that the cutting efficiency is improved.
Preferably, in the present embodiment, the slice current is controlled to be 1.5A for a steel cast billet sample, and an image of one inclusion slice is obtained for every 2 inclusion slices, so that the reconstruction accuracy of the inclusions 1 is ensured and the reconstruction efficiency of the inclusions 1 is improved.
In another embodiment of the present invention, the slice current and parameters may be set for different material objectsnAnd the thickness of the inclusion slice and other parameters are adjusted adaptively.
According to the method, when the inclusion slice image is obtained, the Y-direction characteristic region is gradually reduced along with the change of the cutting position, the collected characteristic region picture is gradually moved upwards, so that the image generates an offset angle in the Z direction on the YZ plane, and at the moment, the three-dimensional appearance of the inclusion 1 reconstructed by directly splicing the picture generates a certain distortion, so that the offset correction is further performed through the step S3 and the step S4.
In step S3, it specifically includes:
slicing thickness and parameters based on inclusionsnThe cumulative total thickness of the corresponding inclusion slice is calculated by the following formula:
L
N
=(N-1)×n×d
wherein the content of the first and second substances,L N denotes the firstNThe total thickness accumulated by the pieces of the sundries clamped,dthe inclusion slice thickness is shown. The total thickness of the accumulated inclusion slices is the sum of the thicknesses of all the inclusion slices.
After the total thickness accumulated by the inclusion slices and the offset angle of the inclusion slices in the Z direction on the YZ plane are obtained, the offset of the inclusion slices is approximately calculated through a trigonometric function relation, and the calculation logic is simple and the accuracy is high. After the offset is obtained through calculation, the corresponding offset is subtracted from the inclusion slice image, and then splicing reconstruction is carried out. As shown in fig. 3, it is a two-dimensional scanning electron microscope picture of an inclusion 1, whose planar shape is similar to a circle with a diameter of 8 μm. As shown in fig. 4, for an inclusion 1 image reconstructed after the inclusion 1 is not subjected to offset correction, it can be seen that the inclusion 1 image is substantially in an elliptical shape, and has a size of about 7 μm × 11 μm, and has a relatively obvious distortion. As shown in fig. 5, for the inclusion 1 image reconstructed after the offset correction of the inclusion 1, it can be seen that compared with fig. 4, the appearance of the inclusion 1 image is closer to the planar appearance in fig. 3, i.e. more conforms to the original appearance of the inclusion 1, and the result is true and reliable.
In summary, in the process of reconstructing the morphology of the inclusion 1 by using a focused ion beam electron beam dual-beam scanning electron microscope, the embodiment calculates the total thickness accumulated by the series of inclusion slices, measures the offset angle of the inclusion slices in the Z direction on the YZ plane, and approximately obtains the offset of the inclusion slices by using the trigonometric function relationship, so as to perform offset correction on the reconstructed image, so that the finally obtained image of the inclusion 1 is closer to the original morphology of the inclusion 1, thereby obtaining the real spatial morphology and size of the inclusion 1, and providing data support for researching the formation mechanism of the inclusion 1.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention and is not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. An inclusion reconstruction method, characterized by comprising the steps of:
preparing a sample to be observed, searching for an interested inclusion on the surface of the sample to be observed, forming an XY axis plane by the plane where the inclusion is located, and forming pits on the left side, the right side and the lower side of the inclusion by utilizing a focused ion beam electron beam double-beam scanning electron microscope, wherein the inner wall surface of the pit on the lower side of the sample to be observed forms an XZ axis plane which is an observation surface;
cutting the observation surface layer by layer through a focused ion beam electron beam double-beam scanning electron microscope along the Y-axis direction to obtain a series of inclusion slices;
acquiring the image of the inclusion slice, calculating the accumulated total thickness corresponding to the inclusion slice, and acquiring the offset angle of the inclusion slice in the Z direction on the YZ plane;
calculating the offset of each inclusion slice image, and performing offset correction on the inclusion slice image according to the offset, wherein the offset calculation formula is as follows:
ΔZ N =L N ×sinθ
wherein the content of the first and second substances,ΔZ N an offset is indicated and the amount of the offset,L N representing the total thickness accumulated by the inclusion slice of the Nth sheet,θrepresents an offset angle of the inclusion slice in the Z direction on the YZ plane;
and performing three-dimensional reconstruction on the inclusions based on the corrected inclusion slice images.
2. The inclusion reconstruction method according to claim 1, wherein the step of cutting the inclusions layer by layer through a focused ion beam electron beam dual-beam scanning electron microscope to obtain a series of inclusion slices specifically comprises:
and cutting the inclusions layer by layer through a focused ion beam electron beam double-beam scanning electron microscope, and adjusting the slice thickness according to the sizes of the inclusions to obtain a plurality of serial inclusion slices with consistent thickness.
3. The inclusion reconstruction method according to claim 2, wherein the slice thickness of the inclusions is in a range of 12 to 48nm.
4. The inclusion reconstruction method according to claim 2, wherein the acquiring the inclusion slice image specifically includes:
each timenSlicing the inclusions to obtain an image of the slice of inclusions, whereinnAre preset parameters according to the size of the inclusions and the thickness of the slices.
5. The inclusion reconstruction method according to claim 4, wherein the parameter isnHas a value in the range of 1~4.
6. The inclusion reconstruction method according to claim 4, wherein the calculating the cumulative total thickness corresponding to the inclusion slice specifically comprises:
slicing thickness and parameters according to the inclusionsnCalculating the cumulative total thickness corresponding to the inclusion slice by the following formula:
L
N
=(N-1)×n×d
wherein L is N Represents the total thickness accumulated by the inclusion slice of the Nth picture, and d represents the thickness of the inclusion slice.
7. The inclusion reconstruction method according to claim 1, wherein the slice current is controlled to be 1 to 2nA.
8. The method for reconstructing inclusions according to claim 1, wherein a slicing current is controlled to be 1.5A, and an image of one piece of the inclusion slice is obtained for every 2 pieces of the inclusion slices.
9. The inclusion reconstruction method according to claim 1, wherein the specimen to be observed is a steel ingot specimen.
10. The inclusion reconstruction method according to claim 9, wherein the preparing of the specimen to be observed specifically includes:
and (3) polishing the steel casting blank sample until the surface and the opposite surface of the steel casting blank sample are flush, polishing the surface to be analyzed to a polished state, and spraying a Pt protective layer in an inclusion area.
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| 吴园园等: "聚焦离子束扫描电镜三维重构夹杂物的形态和分布", 《冶金分析》 * |
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