CN117664963A - Three-dimensional reconstruction method for microstructure of material - Google Patents
Three-dimensional reconstruction method for microstructure of material Download PDFInfo
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Abstract
The invention provides a three-dimensional reconstruction method of a microstructure of a material, which comprises the following steps: pretreating the surface of a material to be tested; pressing microscopic indentation of the material to be measured into the material to be measured for positioning; acquiring three-dimensional height information of the surface of the microscopic indentation with high precision, and determining the height information of the first slice; collecting metallographic information of a first slice of a material to be detected; and carrying out three-dimensional reconstruction on the microstructure of the material by utilizing three-dimensional reconstruction software according to the indentation height information and the metallographic information of each slice. The invention combines the microscopic indentation positioning with the surface three-dimensional height information acquisition measurement and quantitative analysis, and obtains a method for directly obtaining the three-dimensional reconstruction of the microstructure by utilizing the three-dimensional height information.
Description
Technical Field
The invention relates to the technical field of material microstructure analysis and characterization, in particular to a method for three-dimensional reconstruction of a material microstructure.
Background
The three-dimensional reconstruction technology of the microstructure of the material is an important method for analyzing the spatial structure of the microstructure, and the spatial microstructure of the interior of the material is obtained through different imaging principles so as to provide a basic direction for material research and material modification. The existing three-dimensional reconstruction technology of the microstructure of the material mainly comprises a destructive detection method and a nondestructive detection method, wherein the nondestructive detection method comprises a microscopic CT (computed tomography), an industrial CT (computed tomography), synchronous radiation and the like. However, for the cross-scale detection characterization with higher requirement precision, small grain size and large acquisition area, the time consumption is high, the cost is high, and the efficiency is difficult to consider in time-space scale; the three-dimensional reconstruction technology for the lossy method is mainly based on three-dimensional reconstruction of continuous slices, and comprises a Focused Ion Beam (FIB) continuous slice, a mechanical polishing continuous slice and a high-precision metallographic polishing continuous slice method; the continuous slicing method for high-precision metallographic polishing has the characteristics of low sample preparation cost, accurate structure and compatible observation area and precision, and is one of important technologies for three-dimensional reconstruction.
According to the principle of continuous slicing, the method for obtaining the spatial structure of the microstructure of the material, particularly the microstructure of hard materials such as ceramics, metals and the like is an important method by carrying out microscopic indentation positioning and metallographic acquisition on the surface of the material at different depths and carrying out three-dimensional reconstruction of the microstructure, inclusions, defects, damages and the like by utilizing software. With the rapid development of material genome projects in recent years, the realization of a three-dimensional reconstruction high-throughput technology for microscopic tissues is one of the important points of future development. Three-dimensional reconstruction of centimeter-level samples (XY direction) can be achieved using a fully automatic high-throughput metallographic microscope or a high-throughput field emission scanning electron microscope.
At present, three-dimensional reconstruction of continuous slices mainly utilizes a micro Vickers indentation method to prefabricate micro indentations for space positioning point marking. The thickness of the layer of the serial slice can be calculated indirectly by measuring the projected area of the micro-indentation by using the linear relation between the projected area of the micro-indentation and the depth of the micro-indentation (136 DEG of micro-Vickers head) in the ideal shape. The method is simple, convenient and efficient, but has 2 problems of microscopic indentation profile deformation and plastic accumulation near the microscopic indentation, which can lead to certain errors in layer thickness measurement and easily lead to dislocation and errors in different slice tissue profiles.
Wherein, the micro-indentation profile deformation is due to the differential strain response generated after the plastic deformation of different materials; in particular, after the material containing residual stress is loaded by the pressure head, the micro-Vickers indentation contour is deformed, and the micro-Vickers indentation three-dimensional contour deviates from an ideal shape, so that the micro-indentation projection area and the micro-indentation depth do not strictly follow a linear relationship, and the error of layer thickness measurement is amplified. In the loading process of the pressure head, plastic deformation accumulation or warping is generated on the surface of the micro Vickers indentation, so that a certain error is easy to occur when the projection area of the micro Vickers indentation is measured.
Disclosure of Invention
The invention provides a three-dimensional reconstruction method of a material microstructure, which aims to solve the problems of height information errors caused by shape errors of indentation contours and height information errors caused by plastic accumulation or warping near micro-Vickers indentations.
In view of this, the present application provides a method for three-dimensional reconstruction of a microstructure of a material, comprising the steps of:
a) Pretreating the surface of a material to be tested;
b) Carrying out positioning marking of microscopic indentation on the material to be tested obtained in the step A) by using a full-automatic microscopic Vickers hardness tester;
c) Acquiring three-dimensional height profile information of the microscopic indentation of the material to be detected obtained in the step B) by using a high-precision three-dimensional optical profiler, and positioning the height information;
d) Removing plastic accumulation and/or warping around the microscopic indentation of the material to be tested obtained in the step C);
e) Taking the surface of the material to be measured obtained in the step D) as a first slice, and carrying out three-dimensional morphology acquisition on microscopic indentations of the first slice by utilizing a high-precision optical three-dimensional profiler to position height information;
f) Collecting metallographic information of the first slice;
acquiring a second slice of the material to be measured by combining metallographic polishing with a full-automatic optical microscope or a high-precision three-dimensional optical profiler, and acquiring the height information and metallographic information of the second slice;
g) Processing and information acquisition are carried out on the next slice according to the step F) until n slices and corresponding height information and metallographic information are obtained;
h) And three-dimensional reconstruction is carried out on the microstructure information of the n-layer slices by using three-dimensional reconstruction software.
Preferably, in step a), the pretreatment comprises metallographic grinding and metallographic polishing.
Preferably, step B) is specifically:
setting load, holding time, lattice quantity and pressure head spacing according to the hardness, elastic modulus and tissue structure characterization requirements of the material to be tested; the material to be measured is a small-size and/or small-area sample, the material to be measured is subjected to micro-Vickers indentation single-point positioning mark, the material to be measured is a large-size and/or large-area sample, and the material to be measured is subjected to micro-Vickers indentation high-throughput lattice point positioning mark.
Preferably, step C) is specifically:
and acquiring profile parameters of the microscopic indentation by using a high-precision three-dimensional optical profiler, and acquiring the three-dimensional height of the indentation of the material to be detected through height information distribution to acquire the height information of the microscopic indentation.
Preferably, in the step D), the plastic stacking and/or warping is removed and polished by a high-precision metallographic polisher, and the polishing is performed with the aid of the full-automatic metallographic microscope or the high-precision three-dimensional optical profiler.
Preferably, in step E), the high-precision optical three-dimensional profiler is a white light interference optical profiler, a super-depth-of-field microscope or a laser confocal microscope.
Preferably, in step F), the metallographic information is collected by a full-automatic metallographic microscope.
Preferably, the method for collecting the height information and the metallographic information of the second slice in the step F) specifically comprises the following steps:
and polishing the material to be detected by using a high-precision metallographic polishing instrument, simultaneously, judging the thickness of the second slice by using an optical profilometer or a full-automatic metallographic microscope for auxiliary observation, obtaining the second slice, and acquiring the height information of microscopic indentations of the second slice and the metallographic information of the region to be observed by using the full-automatic optical microscope.
Preferably, the tissue reconstruction specifically comprises:
and carrying out three-dimensional reconstruction on the slice sequence metallographic map by utilizing three-dimensional reconstruction software according to the height information and the metallographic information of each slice in the n layers of slices.
Preferably, the material to be measured is a metal material or a brittle nonmetallic material.
The application provides a three-dimensional reconstruction method for a microstructure of a material, which utilizes a high-precision three-dimensional optical profiler to directly measure the depth of microscopic indentation, avoids calculation errors caused by the depth converted by the geometric shape of a pressure head, and utilizes the high-precision three-dimensional optical profiler to directly measure the thickness of a continuous slice, thereby effectively improving the height information errors; meanwhile, plastic accumulation or warping around the indentation of the material to be measured is removed, the profile error of the microscopic indentation is reduced, and the depth of the microscopic indentation is directly measured by combining a three-dimensional profilometer, so that the height error is effectively avoided.
Drawings
FIG. 1 is a flow chart of the steps of the invention;
FIG. 2 is a schematic drawing (side view) of a microscopic Vickers indentation geometry;
FIG. 3 is a schematic (side view) of the loading of micro Vickers indentations to create plastic stacks and micro indentation profile deformations;
FIG. 4 is a high-precision three-dimensional optical profiler acquisition result of the three-dimensional height information of the polished surface micro-indentation and the nearby area of the ceramic matrix composite provided in example 1 of the present invention;
FIG. 5 is a variation of height information along the section line of FIG. 4;
FIG. 6 is a schematic representation of a micro Vickers indentation with a stepped profile according to example 1 of the present invention;
FIG. 7 is a variation of the height information along the black diagonal line in FIG. 6 (the difference in height of the dashed horizontal line represents the plastic stack height);
fig. 8 shows the actual measured change in height information from the diamond vertices of the micro vickers indentation to the center of the indentation (side view).
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
In view of the two error problems caused by information acquisition of a micro Vickers indentation positioning light mirror in the prior art, the application provides a three-dimensional reconstruction method of a material microstructure based on surface information detection, which selects a high-precision three-dimensional optical profiler as a surface height information measuring tool to directly obtain high-precision measurement of slice interlayer thickness information in a continuous slice three-dimensional reconstruction technology, improves interlayer thickness measurement precision, and provides a basis for accurate construction of three-dimensional reconstruction. Specifically, the embodiment of the invention discloses a three-dimensional reconstruction method of a microstructure of a material, which comprises the following steps:
a) Pretreating the surface of a material to be tested;
b) Carrying out positioning marking of microscopic indentation on the material to be tested obtained in the step A) by using a full-automatic microscopic Vickers hardness tester;
c) Acquiring three-dimensional height profile information of the microscopic indentation of the material to be detected obtained in the step B) by using a high-precision three-dimensional optical profiler, and positioning the height information;
d) Removing plastic accumulation and/or warping around the microscopic indentation of the material to be tested obtained in the step C);
e) Taking the surface of the material to be measured obtained in the step D) as a first slice, and carrying out three-dimensional morphology acquisition on microscopic indentations of the first slice by utilizing a high-precision optical three-dimensional profiler to position height information;
f) Collecting metallographic information of the first slice;
acquiring a second slice of the material to be measured by combining metallographic polishing with a full-automatic optical microscope or a high-precision three-dimensional optical profiler, and acquiring the height information and metallographic information of the second slice;
g) Processing and information acquisition are carried out on the next slice according to the step F) until n slices and corresponding height information and metallographic information are obtained;
h) And three-dimensional reconstruction is carried out on the microstructure information of the n-layer slices by using three-dimensional reconstruction software.
In the method for three-dimensional reconstruction of the microstructure of the material, firstly, the surface of the material to be measured is pretreated, specifically metallographic grinding and metallographic polishing are carried out on the surface of the material to be measured, and proper grinding and polishing abrasive materials (such as SiC and SiO) are selected according to the properties (hardness and wear resistance) and grain size of the material to be measured 2 Diamond, etc.), including sandpaper types (SiC, siO) 2 Sandpaper, diamond, etc.), abrasive particles (100 #, 200#, 400#, 600#, 800#, 1000#, 1200#, 1500#, 2000 #); the type of grinding fluid and the size of abrasive particles are set to a proper polishing process.
After surface pretreatment, the method adopts a full-automatic micro Vickers hardness tester to carry out positioning marks of microscopic indentation on the material to be tested; in the process, according to the information such as the hardness and the wear resistance of the material, proper parameters such as the microscopic indentation load are set, and the relative relation between the microscopic indentation size and the microstructure is observed through setting different loads (such as 1N, 2N, 5N, 10N and the like), so that the required load, the load retention time, the lattice quantity and the pressure head spacing are judged; if the material to be measured is a small-size and/or small-area sample, carrying out micro-Vickers indentation single-point positioning mark on the material to be measured, and if the material to be measured is a large-size and/or large-area sample, carrying out micro-Vickers indentation high-throughput lattice point positioning mark on the material to be measured.
According to the invention, the three-dimensional height profile information of the microscopic indentation on the surface of the material to be detected is acquired by utilizing a high-precision three-dimensional optical profiler, and the height information is positioned; the high-precision three-dimensional profiler can be specifically selected from a white light interference optical profiler, a laser confocal microscope or a super-depth-of-field microscope, acquisition parameters are set, and the height information of the microscopic indentation is acquired to obtain the height information distribution of the microscopic indentation and the nearby area.
Because the diamond-shaped pressure head presses the surface of the sample in the loading process of the micro-Vickers indentation, the plastic deformation form of the material is changed to the surface of the micro-Vickers indentation, so that plastic accumulation (pipe-up) or warping is generated near the micro-Vickers indentation; the creation of plastic build-up or warpage will affect the observation and accurate measurement of the microscopic indentation profile and height information, and therefore it is necessary to perform metallographic grinding and metallographic polishing on this information to remove the build-up or warpage height near the microscopic vickers indentation, so that the height difference for each slice can be obtained directly from the microscopic indentation edge height and the center minimum height. Therefore, plastic accumulation or warping around microscopic indentation of the material to be detected is removed, specifically metallographic grinding and metallographic polishing are utilized, and meanwhile, observation is carried out under a full-automatic optical microscope or a high-precision three-dimensional optical profilometer, so that plastic accumulation or warping on the surface of the microscopic Vickers indentation is accurately removed.
The method comprises the steps of firstly, carrying out a first layer of slicing on the surface of a material to be detected by using a high-precision optical three-dimensional profiler, collecting three-dimensional height profile information of microscopic Vickers indentation and the surface of a related area of the first layer of slicing, and positioning the height information; on the basis of removing plastic accumulation or warping height of microscopic indentations by combining metallographic polishing with optical microscope observation, the method and the device perform surface three-dimensional morphology information high-flux acquisition on the processed surface information of the material to be measured by using a white light interference three-dimensional optical profilometer, a laser confocal or super-depth-of-field microscope and the like, and obtain surface height information of a first slice microscopic vickers indentation micro-area and a sample region to be measured.
After the height information of the first slice is acquired, acquiring a metallographic structure of a corresponding area of the first slice by using a full-automatic metallographic microscope; and setting acquisition parameters such as microscope lens multiple, acquisition array number and the like according to analysis and observation requirements, and obtaining metallographic acquisition of the region to be detected of the first slice.
According to the invention, the second slice is subjected to height information and metallographic information acquisition, namely, metallographic grinding and metallographic polishing are utilized, and observation is carried out under a full-automatic optical microscope, so that the positioning height information and the metallographic information of the second slice are obtained; and repeating the steps of acquiring the second slice, the height information of the second slice and the metallographic information until all the information of the required n slices is obtained. The method comprises the steps of carrying out the next slice under the auxiliary observation of an optical microscope, namely, observing the microscopic indentation contour of a sample in a timing way in the high-precision metallographic polishing process, judging the depth of the next slice, and meeting the requirements after the depth of the slice is close to the target depth.
After n layers of slices are obtained, three-dimensional microstructure reconstruction is carried out on the acquired information by utilizing software according to the height information and the metallographic information of the slices at different levels, and then the obtained depth (depth positioning information) of each layer of slice and the metallographic image of the corresponding slice at each layer are utilized to carry out three-dimensional reconstruction on the microstructure of the material by combining three-dimensional reconstruction software (such as Avizo, dragonfly, mimics and the like).
The invention provides a method for three-dimensional reconstruction of a material microstructure based on surface information detection, which combines the prefabrication of microscopic indentation and the removal of plastic accumulation, and the direct observation and measurement of the height information of a high-precision three-dimensional optical profiler for microscopic indentation, and the high-throughput acquisition of full-automatic metallographic images, so as to realize the quantification of the thickness of a reconstructed lamellar of the three-dimensional microstructure of a continuous slice, and avoid the contour error of the microscopic indentation caused by the prefabrication of the microscopic indentation.
Compared with the conventional three-dimensional reconstruction method in the prior art, the three-dimensional reconstruction method for the microstructure of the material provided by the invention has the obvious advantages, and the following detailed description is provided:
1) The conventional continuous slice three-dimensional reconstruction technology converts indentation depth and inter-lamellar thickness by combining microscopic indentation projection area and microscopic indenter geometric relationship, and has the following defects: the projected area and depth of the microscopic indentations are not strictly proportional, so that certain errors are generated, and particularly when the microscopic indentations contain stress, the errors are increased; the method and the device utilize the high-precision three-dimensional profiler to directly measure the depth of the microscopic indentation, so that calculation errors caused by the depth converted by the geometric shape of the pressing head are avoided;
2) In the prior art, the three-dimensional reconstruction technology of continuous slices directly converts the micro-indentation depth and the lamellar thickness by utilizing the micro-indentation area, and has the defects that: in the process of generating the micro-indentation, the internal plastic deformation rheologically extrudes the material out of the micro-indentation, so that the surface plastic accumulation or warping is caused, the height of the surface plastic accumulation or warping is higher than that of a horizontal line, and a certain height error is caused by the phenomenon, particularly when the residual stress of a sample is compressive stress, the error is larger; the metallographic polishing removes surface plastic accumulation and/or warping, and meanwhile, the error can be avoided by directly measuring the depth of the microscopic indentation by using a three-dimensional profiler;
3) Because the profile of the micro-indentation may deviate from the geometric shape of the pressure head (more serious than that of the metal material) and cracks may be generated nearby to influence the shape of the indentation in the micro-vickers indentation loading process of the brittle non-metal material, the conventional method for converting the geometric shape of the pressure head applicable to the metal material may not be applicable, and the method is directly used for measuring the depth of the micro-indentation and removing plastic accumulation, so that the method is applicable to the metal material, the brittle non-metal material and the material, and the application range of the material is greatly widened.
For further understanding of the present invention, the method for three-dimensional reconstruction of a microstructure of a material according to the present invention will be described in detail with reference to examples, and the scope of the present invention is not limited by the following examples.
Example 1
As shown in FIGS. 1-5, the present embodiment selects high gradient directional solidification B 4 The C-based ceramic matrix composite is taken as a research object, and the implementation flow chart is shown in fig. 1, and the specific implementation steps are as follows:
s1) pair B 4 The surface of the C-based ceramic composite material is subjected to metallographic grinding and metallographic polishing treatment, and the method specifically comprises the following steps:
for high gradient directional solidification B prepared by optical floating zone method 4 C-based ceramic composite material, cutting the material to be detected by using a wire cutting device according to the observation requirement; according to the hardness and wear resistance of ceramic materials, a proper abrasive is selected, in the embodiment, siC sand paper (100 # to 2000 #), silicon dioxide or diamond grinding fluid (0.5 μm to 2.0 μm) is selected as the abrasive, a full-automatic metallographic grinding and polishing machine is selected, the rotating speed is set to be 50 rpm to 300rpm, and a sample needs to reach mirror smoothness and no obvious scratch is observed by an optical microscope;
s2) carrying out positioning marking on a sample by utilizing a micro Vickers hardness tester, wherein the positioning marking comprises the following steps:
according to B 4 C-based ceramic composite material hardness and size of region to be observed, setting load to 10-100N by using a full-automatic micro Vickers hardness tester (Qness Q10A+) and holding time to 5-20 s, and performing test on B 4 Positioning and marking the C-based eutectic ceramic composite material, wherein a schematic diagram of a side view observation of the surface of a micro Vickers indentation loaded sample is shown in FIG. 2;
s3, utilizing a high-precision three-dimensional optical profiler (Bruker Contour GT-X) to test B 4 The surface indentation micro-area of the C-based ceramic composite material sample and the three-dimensional height profile information of the surface of the area to be observed are collected, and the height information is positioned, specifically:
setting proper acquisition parameters according to the size of the region to be detected, and acquiring the surface three-dimensional morphology of microscopic vickers indentation and the height information of the nearby region to be observed by using a white light interference three-dimensional optical profiler (for example, bruker Contour GT-X optical profiler can be adopted) to obtain the height information;
s4, utilizing metallographic grinding and metallographic polishing, and simultaneously observing under an optical microscope (Leica DM 6000M) or a three-dimensional profilometer to remove plastic accumulation or warpage on the surface of the microscopic indentation, wherein the method specifically comprises the following steps:
selecting proper polishing solution, and using a full-automatic polishing machine to make the polishing solution B 4 C-based ceramic composite material sample is polished, and meanwhile, the surface of the sample is observed at regular time by using a full-automatic metallographic microscope or a three-dimensional optical profilometer until plastic accumulation or warping of the surface of the microscopic indentation is removed, as shown in fig. 3, the schematic diagram of the plastic accumulation or warping shape of the microscopic indentation is shown, and due to the diamond pressing of the microscopic Vickers indentationExtrusion of the head during loading, extrusion of the material to the outside of the microscopic indentations by plastic flow deformation produces plastic accumulation or warpage, which is exacerbated especially when the sample is subjected to residual compressive stress; FIG. 4 is B 4 The surface height information of the C-based authigenic composite material is loaded by a microscopic pressure head, so that the plastic accumulation or warping of the ceramic material is generated similarly to the plastic accumulation or warping of the metal material;
fig. 5 to 8 show three-dimensional information of the surface of the micro-indentation, and it can be seen that after the micro-vickers hardness tester is loaded, the height information near the diamond indenter is obviously higher (at the microscope observation level) than other areas of the sample (shown in fig. 4 and 5), so that certain errors can be generated for three-dimensional reconstruction; FIG. 6 is a stepped profile generated during the loading process of a micro-indentation, and when the longitudinal section is used for observing the height information, the profile information deviates from a straight line, so that the conventional observation by a metallographic microscope has certain error in combination with the conversion of the geometric shape of the micro-Vickers indentation, and particularly, the error is larger in the case of poor plasticity and internal stress, and the dislocation is caused during three-dimensional reconstruction;
s5, acquiring three-dimensional height profile information of the surface of the first layer of micro-indentation micro-area of the material to be detected by utilizing a high-precision three-dimensional optical profiler, and positioning the height information, wherein the method specifically comprises the following steps:
after observing and removing plastic accumulation or warping of microscopic indentations by using a white light interference three-dimensional optical profilometer (such as a Bruker Contour GT-X three-dimensional optical profilometer) or a full-automatic metallographic microscope (such as a Leica DM6000M optical microscope), acquiring the height information of a region to be observed of the first slice to obtain the surface height information of the microscopic indentation region and the region to be observed of the first slice;
s6, acquiring a metallographic structure of a region corresponding to the first layer by using a full-automatic metallographic microscope, wherein the metallographic structure comprises the following specific steps:
according to the size of the area to be acquired and the typical size of the microstructure, lens multiple is selected, and a full-automatic optical microscope (Leica DM 6000M) is used for acquiring the metallographic structure of the area to be acquired;
s7, obtaining positioning height information of a next slice by utilizing metallographic polishing and observing under a full-automatic optical microscope or a high-precision three-dimensional optical profiler, and repeating the steps S5 and S6 until the required n slices are obtained, wherein the method specifically comprises the following steps:
under the auxiliary observation of a full-automatic optical microscope or a high-precision three-dimensional optical profiler, the high-precision metallographic polished sample is observed at regular time, and when the optical microscope is used for observation, the next slice is judged by observing the microscopic indentation profile and combining the microscopic indentation pressure head trigonometric function relation; when the white light interference three-dimensional profilometer is used for observation, microscopic indentation height information is directly observed, the next layer of slice is judged, and when the slice depth is close to the target depth, namely the height information meets the requirement of continuous slice, namely the requirement of the step is met;
s8, after n layers of slices are obtained, three-dimensional microstructure reconstruction is carried out on the acquired information by utilizing software according to the height information and the metallographic structure of the continuous slices of different levels, and the method comprises the following steps:
and (3) performing three-dimensional reconstruction on the obtained serial slice metallographic results according to the serial slice height information by using software such as Avizo, dragonfly or chemicals.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for three-dimensional reconstruction of a microstructure of a material, comprising the steps of:
a) Pretreating the surface of a material to be tested;
b) Carrying out positioning marking of microscopic indentation on the material to be tested obtained in the step A) by using a full-automatic microscopic Vickers hardness tester;
c) Acquiring three-dimensional height profile information of the microscopic indentation of the material to be detected obtained in the step B) by using a high-precision three-dimensional optical profiler, and positioning the height information;
d) Removing plastic accumulation and/or warping around the microscopic indentation of the material to be tested obtained in the step C);
e) Taking the surface of the material to be measured obtained in the step D) as a first slice, and carrying out three-dimensional morphology acquisition on microscopic indentations of the first slice by utilizing a high-precision optical three-dimensional profiler to position height information;
f) Collecting metallographic information of the first slice;
acquiring a second slice of the material to be measured by combining metallographic polishing with a full-automatic optical microscope or a high-precision three-dimensional optical profiler, and acquiring the height information and metallographic information of the second slice;
g) Processing and information acquisition are carried out on the next slice according to the step F) until n slices and corresponding height information and metallographic information are obtained;
h) And three-dimensional reconstruction is carried out on the microstructure information of the n-layer slices by using three-dimensional reconstruction software.
2. The method according to claim 1, wherein in step a), the pretreatment comprises metallographic grinding and metallographic polishing.
3. The method according to claim 1, wherein step B) is specifically:
setting load, holding time, lattice quantity and pressure head spacing according to the hardness, elastic modulus and tissue structure characterization requirements of the material to be tested; the material to be measured is a small-size and/or small-area sample, the material to be measured is subjected to micro-Vickers indentation single-point positioning mark, the material to be measured is a large-size and/or large-area sample, and the material to be measured is subjected to micro-Vickers indentation high-throughput lattice point positioning mark.
4. A method according to claim 1 or 3, characterized in that step C) is specifically:
and acquiring profile parameters of the microscopic indentation by using a high-precision three-dimensional optical profiler, and acquiring the three-dimensional height of the indentation of the material to be detected through height information distribution to acquire the height information of the microscopic indentation.
5. The method according to claim 1, wherein in step D) the removal of plastic bulk and/or warpage is performed with the aid of a high precision metallographic polisher, said polishing being performed with the aid of the full automatic metallographic microscope or a high precision three-dimensional optical profiler.
6. The method of claim 1, wherein in step E) the high precision optical three-dimensional profiler is a white light interferometry optical profiler, a super depth of field microscope, or a confocal laser microscope.
7. The method according to claim 1, wherein in step F), the metallographic information is collected using a fully automated metallographic microscope.
8. The method according to claim 1, wherein the second slice height information and metallographic information acquisition in step F) is specifically:
and polishing the material to be detected by using a high-precision metallographic polishing instrument, simultaneously, judging the thickness of the second slice by using an optical profilometer or a full-automatic metallographic microscope for auxiliary observation, obtaining the second slice, and acquiring the height information of microscopic indentations of the second slice and the metallographic information of the region to be observed by using the full-automatic optical microscope.
9. The method according to claim 1, wherein the tissue reconstruction is in particular:
and carrying out three-dimensional reconstruction on the slice sequence metallographic map by utilizing three-dimensional reconstruction software according to the height information and the metallographic information of each slice in the n layers of slices.
10. The method of claim 1, wherein the material to be tested is a metallic material or a brittle nonmetallic material.
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