CN108088864B - Method and system for reconstructing three-dimensional microstructure of material - Google Patents
Method and system for reconstructing three-dimensional microstructure of material Download PDFInfo
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- CN108088864B CN108088864B CN201711343453.4A CN201711343453A CN108088864B CN 108088864 B CN108088864 B CN 108088864B CN 201711343453 A CN201711343453 A CN 201711343453A CN 108088864 B CN108088864 B CN 108088864B
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Abstract
The invention discloses a method and a system for reconstructing a three-dimensional microstructure of a material, wherein the method comprises the following steps: s1, etching a material to be detected to obtain a material section; s2, microstructure detection and element distribution detection are carried out on the material section to obtain a microstructure two-dimensional picture sequence and a component distribution two-dimensional picture sequence; and S3, acquiring a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence. The invention can obtain the three-dimensional distribution of the material components; the three-dimensional microstructure and the component distribution can be obtained simultaneously in the primary section etching, so that the secondary etching of the material section is avoided; the method utilizes the element component distribution as the standard of the solid-phase component division of the material, is more accurate than the method utilizing the gray threshold value at present, and the classification of the material component is more extensive.
Description
Technical Field
The invention relates to the field of material microstructure and component characterization, in particular to a method and a system for reconstructing a three-dimensional microstructure of a material.
Background
The microstructure and the composition distribution information of the material are decisive factors for determining the physical and chemical behaviors of the material. However, microstructure characterization and compositional distribution analysis have long been separate. The scanning electron microscope is one of the main tools for testing the microstructure of the material, and the scanning electron microscope can perform cross-scale measurement on the microstructure of the material from macro-to micro-and even nano-size, and is an important means for revealing the microscopic multilevel microstructure (such as grain size, phase distribution, interface characteristics, impurity distribution and the like) of the material. An EDS (X-ray Energy Dispersive Spectroscopy, EDS for short) is also called a microscopic electron probe, which is an instrument for analyzing substance elements, and is usually used in combination with a scanning electron microscope or a transmission electron microscope. The scanning electron microscope is configured with an X-ray energy spectrometer, and the microstructure and micro-area composition information of the material, the crystallographic orientation and other data can be connected. However, the detection of materials by these techniques is limited to the surface of the material and cannot be obtained for structural and material distributions within the material.
A Focused Ion Beam (FIB) technique can etch a material, so that the interior of the material is exposed, and the technique is a novel micromachining technique. Currently, focused ion beams are combined with scanning electron microscopy (FIB/SEM), which enables the acquisition of a series of two-dimensional image sequences of the internal microstructure of a material. However, at present, the three-dimensional reconstruction method of the material microstructure divides different material components by adjusting the gray level threshold of a two-dimensional image. The method has the defects that the threshold range is difficult to accurately determine, the image sequence is difficult to continuously adjust, and the group elements of the reconstructed three-dimensional microstructure are not accurately divided.
Disclosure of Invention
The embodiment of the invention provides a method and a system for reconstructing a three-dimensional microstructure of a material, which are used for obtaining three-dimensional distribution of material components and solving the problem that the three-dimensional microstructure is inaccurate in component division in the prior art.
In one aspect, an embodiment of the present invention provides a method for reconstructing a three-dimensional microstructure of a material, where the method includes:
s1, etching a material to be detected to obtain a material section;
s2, microstructure detection is carried out on the material section to obtain a microstructure two-dimensional picture of the section part, and the obtained microstructure two-dimensional picture is added to a microstructure two-dimensional picture sequence;
element distribution detection is carried out on the material section to obtain a component distribution two-dimensional picture of the section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence;
and S3, acquiring a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence.
Further, step S2 includes: judging whether the microstructure two-dimensional picture sequences and the component distribution two-dimensional picture sequences reach a preset number or not;
if yes, go to step S3;
and if not, continuously sampling the material to be detected until the sampling distance of the material to be detected reaches the preset sampling distance, and returning to the step S1.
Furthermore, when the material to be detected is continuously fed, the feeding direction is perpendicular to the material section direction.
Further, step S3 is specifically:
dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
according to the component distribution two-dimensional picture sequence, carrying out phase component division on a solid framework in the microstructure two-dimensional picture sequence;
and reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
In another aspect, an embodiment of the present invention provides a system for reconstructing a three-dimensional microstructure of a material, where the system includes:
the focused ion beam device is used for etching the material to be detected so as to obtain a material section;
the scanning electron microscope device is used for detecting the microstructure of the material section to obtain a microstructure two-dimensional picture of the section part, and adding the obtained microstructure two-dimensional picture to a microstructure two-dimensional picture sequence;
the X-ray energy spectrum device is used for carrying out element distribution detection on the material section so as to obtain a component distribution two-dimensional picture of the section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence;
and the image processing module is used for acquiring the corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence.
Further, the image processing module is further configured to:
and judging whether the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number.
Further, still include:
and the section progressive device is used for continuously sampling the material to be detected until the sampling distance of the material to be detected reaches a preset sampling distance.
Further, when the section progressive device carries out continuous sample introduction on the material to be detected, the sample introduction direction is perpendicular to the material section direction.
Further, if the image processing module judges that the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number, the image processing module acquires a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence;
and if the image processing module judges that the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence do not reach the preset number, the section progressive device continuously samples the material to be detected until the sample injection distance of the material to be detected reaches the preset sample injection distance, and then the step of obtaining the material section is returned.
Further, the image processing module obtains the corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence, specifically:
dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
according to the component distribution two-dimensional picture sequence, performing phase component division on a solid framework in the microstructure two-dimensional picture sequence;
and reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
The method and the system for reconstructing the three-dimensional microstructure of the material provided by the embodiment of the invention have the following beneficial effects:
1) a three-dimensional distribution of material composition can be obtained;
2) the three-dimensional microstructure and the component distribution can be obtained simultaneously in the primary section etching, so that the secondary etching of the material section is avoided;
3) the method utilizes the element component distribution as the standard of the solid-phase component division of the material, is more accurate than the method utilizing the gray threshold value at present, and the classification of the material component is more extensive.
Drawings
FIG. 1 is a flow chart of a method for reconstructing a three-dimensional microstructure of a material according to an embodiment;
FIG. 2 is a structural diagram of a three-dimensional microstructure reconstructing system of a material according to a third embodiment.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
The technical scheme provided by the invention is as follows: and performing section etching on the material by taking the focused ion beam as a material etching tool, performing joint detection of a scanning electron microscope and an energy spectrometer on the formed section to obtain a two-dimensional image of the microstructure and the component distribution, and reconstructing a three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence.
The following are specific examples of the present invention.
Example one
Fig. 1 is a flowchart of a method for reconstructing a three-dimensional microstructure of a material in this embodiment, as shown in fig. 1, the method for reconstructing a three-dimensional microstructure of a material in this embodiment includes:
s1, etching a material to be detected to obtain a material section;
in the step, a focused ion beam device is used for etching a material to be detected to obtain a material section; the focused ion beam is an ion beam generated by a Ga ion source, and is accelerated by an ion gun to etch the material; the acceleration voltage of the focused ion beam is adjusted according to different material properties.
In this embodiment, the acceleration voltage intensity of the focused ion beam emission gun may be set to 20kV, and the generated accelerated ion beam is used to perform cross-sectional etching on the material to be detected, where the cross-sectional area may be 5 μm × 5 μm.
S2, microstructure detection is carried out on the material section to obtain a microstructure two-dimensional picture of the section part, and the obtained microstructure two-dimensional picture is added to a microstructure two-dimensional picture sequence;
element distribution detection is carried out on the material section to obtain a component distribution two-dimensional picture of the section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence;
in the step, microstructure detection is carried out on the material section through a scanning electron microscope device so as to obtain a microstructure two-dimensional picture of the section part, and the obtained microstructure two-dimensional picture is added to a microstructure two-dimensional picture sequence;
scanning Electron Microscopy (SEM), a more modern tool for cell biology research invented in 1965, mainly uses secondary electron signal imaging to observe the surface morphology of a sample, i.e. scanning the sample with a very narrow electron beam, produces various effects by the interaction of the electron beam with the sample, among which is mainly the secondary electron emission of the sample. The secondary electrons can produce an enlarged topographical image of the sample surface, which is built up in time series as the sample is scanned, i.e., a point-by-point imaging method is used to obtain the enlarged image.
In this step, element distribution detection is performed on the material section by an X-ray energy spectrum device (energy spectrometer) to obtain a component distribution two-dimensional picture of a section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence.
An Energy Dispersive Spectrometer (EDS) is used for analyzing the types and contents of the elements in the micro-area of the material, and is matched with a scanning electron microscope and a transmission electron microscope.
In the step, the microstructure two-dimensional picture and the component distribution two-dimensional picture of the material to be detected can be obtained simultaneously, so that the simultaneous online detection of the microstructure detection and the component detection is realized.
And S3, acquiring a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence.
In this step, the image processing module obtains a corresponding three-dimensional microstructure through image processing according to a microstructure two-dimensional picture and a component distribution two-dimensional picture of a cross section part obtained by a scanning electron microscope device and an X-ray energy spectrum device, and the specific process includes:
s31, dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
s32, performing phase component division on a solid framework in the microstructure two-dimensional picture sequence according to the component distribution two-dimensional picture sequence;
in this step, the interphase partition of the solid skeleton is clarified by using the component distribution two-dimensional map, so that the composition of the solid skeleton is more detailed.
And S33, reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
In this embodiment, step S2 further includes: judging whether the microstructure two-dimensional picture sequences and the component distribution two-dimensional picture sequences reach a preset number or not;
if the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number, executing step S3;
and if the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence do not reach the preset number, continuously injecting the sample to the material to be detected until the sample injection distance of the material to be detected reaches the preset sample injection distance, and returning to the step S1.
When the continuous sample introduction is carried out on the material to be detected, the sample introduction direction is perpendicular to the material section direction.
In the step, a section progressive device is used for carrying out continuous sample introduction on the material, and the sample introduction direction is perpendicular to the section direction of the material;
in addition, the aim of cutting the particles in the material at multiple levels can be achieved by setting a preset sample introduction distance (such as 200 nanometers).
The method for reconstructing the three-dimensional microstructure of the material provided by the embodiment has the following beneficial effects:
1) a three-dimensional distribution of material composition can be obtained;
2) the three-dimensional microstructure and the component distribution can be obtained simultaneously in the primary section etching, so that the secondary etching of the material section is avoided;
3) the method utilizes the element component distribution as the standard of the solid-phase component division of the material, is more accurate than the method utilizing the gray threshold value at present, and the classification of the material component is more extensive.
Example two
In this embodiment, before reconstructing the three-dimensional microstructure of the material, the method further includes: the preparation process of the material comprises the following specific steps:
fully dry-grinding a certain amount of lithium ion battery positive electrode active material (lithium cobaltate), a conductive agent (carbon black) and a bonding agent (PVDF) according to a certain proportion, and adding a certain amount of NMP (N-methyl pyrrolidone) for wet grinding;
coating the ground slurry on an aluminum foil by scraping to form a porous material coating with a thickness of about 100 microns;
cutting the material into pieces with the size of 3mm × 3mm, and performing vapor deposition to guide gold;
the gold-plated sample was placed on a sample stage and the detection zone was determined by a scanning electron microscope apparatus.
In the embodiment, by a three-dimensional microstructure reconstruction method, element component distribution is used as a standard for dividing solid-phase components of the material, so that the components (conductive agent, adhesive, active substance and the like) of the porous electrode of the lithium ion battery can be obviously divided, and compared with the conventional method for utilizing a gray threshold, the method is more accurate and the classification of the material components is wider; and the three-dimensional distribution of the material composition can be obtained, which is not available in the current three-dimensional reconstruction methods.
EXAMPLE III
Fig. 2 is a structural diagram of a material three-dimensional microstructure reconstruction system in this embodiment, and as shown in fig. 2, the material three-dimensional microstructure reconstruction system in this embodiment includes:
the focused ion beam device 10 is used for etching the material to be detected so as to obtain a material section;
the scanning electron microscope device 20 is used for detecting the microstructure of the material section to obtain a microstructure two-dimensional picture of the section part, and adding the obtained microstructure two-dimensional picture to a microstructure two-dimensional picture sequence;
the X-ray energy spectrum device 30 is used for carrying out element distribution detection on the material section so as to obtain a component distribution two-dimensional picture of the section part, and adding the obtained component distribution two-dimensional picture to a component distribution two-dimensional picture sequence;
and the image processing module 40 is configured to obtain a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence.
The image processing module 40 is further configured to:
and judging whether the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number.
In this embodiment, the system further includes:
and the section progressive device 50 is used for continuously sampling the material to be detected until the sampling distance of the material to be detected reaches a preset sampling distance.
When the section progressive device 50 continuously samples the material to be detected, the sampling direction is perpendicular to the material section direction.
If the image processing module 40 judges that the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number, the image processing module 40 acquires a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence;
if the image processing module 40 judges that the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence do not reach the preset number, the section progressive device 50 continuously samples the material to be detected until the sample injection distance of the material to be detected reaches the preset sample injection distance, and then the step of obtaining the material section is returned, and the focused ion beam device 10 etches the material to be detected again to obtain a new material section.
The image processing module 40 obtains the corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence, specifically:
dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
according to the component distribution two-dimensional picture sequence, performing phase component division on a solid framework in the microstructure two-dimensional picture sequence;
and reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
In this embodiment, the system further includes a sample stage 60 for fixing the material to be measured, and the section progressive apparatus 50 is connected to the sample stage 60.
In this embodiment, the system further includes a housing 70 for protecting the various devices and modules within the system.
The material three-dimensional microstructure reconstruction system provided by the embodiment has the following beneficial effects:
1) a three-dimensional distribution of material composition can be obtained;
2) the three-dimensional microstructure and the component distribution can be obtained simultaneously in the primary section etching, so that the secondary etching of the material section is avoided;
3) the method utilizes the element component distribution as the standard of the solid-phase component division of the material, is more accurate than the method utilizing the gray threshold value at present, and the classification of the material component is more extensive.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (8)
1. A method for reconstructing a three-dimensional microstructure of a material, comprising:
s1, etching a material to be detected to obtain a material section;
s2, microstructure detection is carried out on the material section to obtain a microstructure two-dimensional picture of the section part, and the obtained microstructure two-dimensional picture is added to a microstructure two-dimensional picture sequence;
element distribution detection is carried out on the material section to obtain a component distribution two-dimensional picture of the section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence;
s3, acquiring a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence;
the step S3 specifically includes:
dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
according to the component distribution two-dimensional picture sequence, carrying out phase component division on a solid framework in the microstructure two-dimensional picture sequence;
and reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
2. The method for reconstructing a three-dimensional microstructure of a material according to claim 1, wherein the step S2 further includes: judging whether the microstructure two-dimensional picture sequences and the component distribution two-dimensional picture sequences reach a preset number or not;
if yes, go to step S3;
and if not, continuously sampling the material to be detected until the sampling distance of the material to be detected reaches the preset sampling distance, and returning to the step S1.
3. The method according to claim 2, wherein the sample introduction direction is perpendicular to the cross-sectional direction of the material when the material to be measured is continuously introduced.
4. A system for reconstructing a three-dimensional microstructure of a material, comprising:
the focused ion beam device is used for etching the material to be detected so as to obtain a material section;
the scanning electron microscope device is used for detecting the microstructure of the material section to obtain a microstructure two-dimensional picture of the section part, and adding the obtained microstructure two-dimensional picture to a microstructure two-dimensional picture sequence;
the X-ray energy spectrum device is used for carrying out element distribution detection on the material section so as to obtain a component distribution two-dimensional picture of the section part, and the obtained component distribution two-dimensional picture is added to a component distribution two-dimensional picture sequence;
the image processing module is used for acquiring a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence;
the image processing module obtains a corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence, and specifically comprises the following steps:
dividing the microstructure two-dimensional picture sequence into a solid skeleton and gaps by utilizing a gray threshold;
according to the component distribution two-dimensional picture sequence, performing phase component division on a solid framework in the microstructure two-dimensional picture sequence;
and reconstructing the microstructure two-dimensional picture sequence into a corresponding three-dimensional microstructure.
5. The system of claim 4, wherein the image processing module is further configured to:
and judging whether the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence reach the preset number.
6. The system of claim 4, further comprising:
and the section progressive device is used for continuously sampling the material to be detected until the sampling distance of the material to be detected reaches a preset sampling distance.
7. The system for reconstructing three-dimensional microstructure of material according to claim 6, wherein the cross-section progressive apparatus continuously feeds the material to be measured, and the feeding direction is perpendicular to the cross-section direction of the material.
8. The system for reconstructing a three-dimensional microstructure of a material according to claim 5, 6 or 7, wherein if the image processing module determines that the microstructure two-dimensional picture sequences and the component distribution two-dimensional picture sequences reach a preset number, the image processing module obtains the corresponding three-dimensional microstructure according to the microstructure two-dimensional picture sequences and the component distribution two-dimensional picture sequences;
and if the image processing module judges that the microstructure two-dimensional picture sequence and the component distribution two-dimensional picture sequence do not reach the preset number, the section progressive device continuously samples the material to be detected until the sample injection distance of the material to be detected reaches the preset sample injection distance, and then the step of obtaining the material section is returned.
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| CN109801375B (en) * | 2019-01-24 | 2021-02-09 | 电子科技大学 | Three-dimensional reconstruction method of porous material based on deep convolution anti-neural network |
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